TW201738528A - Crucible measurement device, crucible measurement method, and crucible production method - Google Patents

Abstract

A crucible measurement device for measuring a silica glass crucible has: a light-emitting unit for emitting a laser beam at a silica glass crucible to be measured which has a straight cylindrical body section having an opening at the upper end thereof, and also has a floor section formed at the lower end of the straight cylindrical body section; and a scattering-state measurement unit for measuring the scattering state, which expresses the state of scattering of the laser beam that the light-emitting unit emitted into the silica glass crucible. Various states of scattering are expressed at the measured locations in the thickness direction of the silica glass crucible for the laser beam emitted by the light-emitting unit. When measuring, the scattering-state measurement unit measures the state of scattering at each of the locations in the thickness direction of the silica glass crucible.

Description

坩埚Measurement device, 坩埚 measurement method, and manufacturer of 坩埚 law

The present invention relates to a ruthenium measurement device, a ruthenium measurement method, and a ruthenium production method for measuring a layer structure in a thickness direction of a yttrium oxide glass crucible.

In the yttrium oxide glass crucible used for pulling the single crystal crucible, for example, by providing a transparent layer and a bubble-containing layer, etc., the generation of a brown ring during the pulling of the single crystal crucible is reduced, and heat is more easily performed. Control and improve the crystallinity of the single crystal germanium.

When the single crystal crucible is pulled, the cerium oxide glass crucible is exposed to the melting temperature of the crucible, that is, at a high temperature of about 1410 ° C or higher. In the case where the density of the bubbles in the bubble-containing layer is not uniform, for example, in the case where the bubble-containing layer is formed of a layer having a plurality of different bubble densities, since the coefficients of thermal expansion of the layers having different bubble densities are different, they are melted in the crucible. At high temperatures in the temperature, the layers with different bubble densities are subjected to different forces. Therefore, depending on the shape of the cerium oxide glass crucible, the quality of the cerium solution, the time of exposure to high temperature, and the like, there is a possibility that the cerium oxide cerium is deformed or broken.

On the other hand, for example, in the case where the yttrium oxide glass crucible is composed of a single layer in the thickness direction, the structural atoms of the yttria glass are also connected in a network shape in the thickness direction of the yttrium oxide glass crucible, and become the same yttrium oxide in the layer. The construction of the network. Therefore, when the bismuth oxide glass crucible is cracked, the network-like bond is broken, and the crack is expanded to a large area of the crucible, and as a result, cracks occur in the cerium oxide glass crucible. On the other hand, in the case where the yttria glass crucible is composed of a plurality of layers of a transparent layer and a bubble-containing layer in the thickness direction, or in the case where the yttrium oxide glass crucible is formed of a plurality of layers in the thickness direction transparent layer or the bubble-containing layer. Next, there are a plurality of interfaces in the thickness direction, and the interface of the yttrium oxide network is different with the interface portion as a boundary, so that the expansion of the crack stops at the interface portion.

As described above, since the layer structure in the thickness direction of the cerium oxide glass crucible has a large influence on heat resistance characteristics, impact resistance characteristics, and the like, it is important to measure the layer structure. However, since cerium oxide glass is transparent, when the size of a bubble is very small, these layer structures may not be fully observed by visual observation. Further, in the transparent layer, even if an abnormality is not observed by visual inspection or the like, there are cases where defects such as very small cracks are present.

If the defects such as the layer structure or very small crack of the yttrium oxide glass crucible are exposed to the ruthenium solution during the pulling of the single crystal ruthenium, it is possible to induce defects in the silicon ingot, and the design of the bismuth oxide bismuth glass ruthenium. In the quality control, etc., it is important to measure the layer structure of the bismuth oxide glass crucible or a defect such as a very small crack.

The yttrium oxide glass crucible used for the pulling of the single crystal crucible is generally produced by a rotary die method, so that it is difficult to control characteristics such as shape, interior, and the like. The produced cerium oxide glass crucible was measured in the following manner, but it was carried out in a non-contact manner because it was necessary to keep the inner surface of the cerium oxide glass crucible clean.

The produced yttrium oxide glass crucible was selected, and the layer structure and defects in the thickness direction of the produced yttrium oxide glass crucible were confirmed by the manner of destruction inspection. In general, the visual inspection is the same as the case of observing an object by an optical microscope or the like, and transmitted light or the like is used. For example, a thinned yttria glass crucible is provided on a line connecting the light source and the observation point, and the light is irradiated, and the transmitted light of the yttrium oxide glass crucible is visually observed or imaged to detect defects or the like in the glass.

In addition, as a method of inspecting the bismuth oxide glass crucible, the method described in Patent Document 1 is known, and an image is acquired in the depth direction of the bismuth oxide glass crucible while changing the depth of focus of the optical imaging device, and is inspected in a non-destructive manner. The bubbles in the cerium oxide glass crucible were measured to measure the bubble content.

Further, the method described in Patent Document 2 is also known, and the three-dimensional coordinates of the inner surface of the yttrium oxide glass crucible are obtained, and the Raman spectrum of the inner surface of the yttrium oxide glass crucible is measured at a plurality of measurement points, thereby determining the inner surface. The three-dimensional distribution of the Raman spectrum.

Further, the detection method described in Patent Document 3 and the patent document 4 are also known. Methods. In the detection method described in Patent Document 3, for example, ultraviolet light having a wavelength shorter than 365 nm is irradiated onto the wall surface of the yttrium oxide glass crucible, and the number of generated fluorescent spots of light having a wavelength of 400 nm to 600 nm is measured, thereby The impurities locally present in the cerium oxide glass crucible are detected, and the impurities are causes of crystal defects or the like when the single crystal crucible is pulled. In the method described in Patent Document 4, a laser is incident, an impurity component is determined based on the wavelength and intensity of the fluorescence generated by the incident, and the content of the impurity component is calculated, thereby detecting the bismuth oxide bismuth glass. An impurity component contained in the top surface of the inner surface.

However, in the visual inspection, when a layered structure is formed along the transmission direction of light as a whole on the transmission surface of light, the layer structure cannot be detected. In addition, when the defect or the like is small, for example, the intensity of the diffracted light or the like generated by the defect may be insufficient, and the defect or the like hidden in the transmitted light from the light source may not be detected. The inspection methods described in Patent Document 1 to Patent Document 3 are methods for measuring the shape of the yttrium oxide glass crucible or the state near the inner surface. Therefore, it is impossible to detect the thickness direction of the yttrium oxide glass crucible which cannot be detected by visual inspection or the like. Further layer constructions inside the transparent layer or inside the bubble-containing layer or defects such as very small cracks in the transparent layer.

Prior art literature

Patent literature

Patent Document 1: Japanese Laid-Open Patent Publication No. 2012-116713

Patent Document 2: Japanese Laid-Open Patent Publication No. 2013-133227

Patent Document 3: Japanese Patent Laid-Open No. Hei 3-146496

Patent Document 4: Japanese Laid-Open Patent Publication No. 2012-17243

An object of the present invention is to provide a technique capable of detecting a further layer structure or defect existing in a transparent layer or a bubble-containing layer which has not been detected in the past, without being destructively and simply.

The inventors have invented a method for the upper end face of yttrium oxide yttrium glass or yttrium oxide glass The inner surface of the vicinity of the upper end portion of the glass crucible is incident on the laser beam, and the scattered light at each position in the thickness direction inside the side wall portion of the cerium oxide glass crucible is observed, whereby the transparent layer or the undetectable layer in the conventional method can be found. The presence of further layer structures or defects or the like existing inside the bubble-containing layer is observed non-destructively and simply.

According to the method of the present invention, the layer structure, the defects, and the like inside the transparent layer or the bubble-containing layer can be observed in a non-destructive and simple manner. Further, in the manufacturing procedure of the yttrium oxide glass crucible, it is possible to discriminate the cerium oxide glass crucible having a certain defect or the like by performing the inspection of the present invention. Further, by using the yttria glass crucible that has passed through the manufacturing process, it is possible to reduce the occurrence of crystal defects of the single crystal bismuth ingot due to defects in ruthenium.

1‧‧‧Oxide glass

2‧‧‧Laser light source

3‧‧‧Photographing Department

4‧‧‧Lighting Department

21‧‧‧Ray Department

31‧‧‧Raman Spectrometry Department

311‧‧‧Rayleigh light removal filter

312‧‧ ‧ splitter

313‧‧‧Detector

FIG. 1 is a view showing an example of a configuration of a flaw measuring device according to a first embodiment of the present invention.

2 is a view showing an example of a state in which a state in which a cerium oxide glass crucible is incident on a laser is measured from the end surface direction.

3 is a view showing an example of a state in which a laser beam is incident on a laser beam from the end surface direction.

4 is a view showing an example of a state in which a laser beam is incident on a laser beam from the end surface direction.

FIG. 5 is a flowchart showing an example of a flow of a flaw measurement method according to the first embodiment.

Fig. 6 is a view showing an example of an actual measurement image.

Fig. 7 is a view showing an example of an actual measurement image.

FIG. 8 is a diagram showing an example of an actual measurement image.

FIG. 9 is a diagram showing an example of an actual measurement image.

Fig. 10 is a view showing internal residual stress of the yttria glass crucible shown in Fig. 6;

Fig. 11 is a view showing internal residual stress of the yttria glass crucible shown in Fig. 7;

Fig. 12 is a view showing an example of a scattering condition when a cross linear laser is used.

FIG. 13 is a view showing an example of a scattering state when a cross-linear laser is used.

FIG. 14 is a view showing an example of a configuration of a flaw measuring device according to a second embodiment.

FIG. 15 is a flowchart showing an example of a flow of a flaw measurement method according to the second embodiment.

Fig. 16 is a view showing the influence of the distance between the inner surface of the crucible and the illumination portion on the measurement of the scattering condition.

Fig. 17 is a view showing an example of a configuration of a flaw measuring device according to a third embodiment.

18 is a view showing an example of a position at which the sputum measuring device of the third embodiment performs Raman spectroscopy.

19 is a flow chart showing an example of a flow of a flaw measurement method according to the third embodiment.

Figure 20 is an example of an actually measured Raman spectrum.

Figure 21 is an example of an actually measured Raman spectrum.

The scattering state of the laser in this specification refers to a state in which the laser light is spread or intensified. Further, the light transmitting layer refers to a transparent layer and does not have a region such as a crack or the like. A layer in a bubble-containing layer or a transparent layer memory in which a defect such as a crack is referred to as a "light-scattering layer".

The yttrium oxide glass crucible according to the present embodiment has a shape including a cylindrical side wall portion (straight cylindrical portion) having an opening at the upper end; a curved bottom portion; and a side wall portion and a bottom portion which are curved compared with the bottom portion Big corner. Further, the upper end surface of the side wall portion of the yttria glass crucible is formed into an annular flat surface. Further, the cerium oxide glass crucible is composed of, for example, a plurality of layers from an inner surface toward an outer surface of the yttrium oxide glass crucible, wherein the plurality of layers include a transparent layer which cannot observe bubbles based on visual observation or image data, and can be observed. To the bubble-containing layer of bubbles, etc.

The cerium oxide glass crucible of the present embodiment is produced, for example, by a rotary die method. The rotary die method is a method in which cerium oxide powder is deposited by rotating a cerium oxide powder in a rotating (carbon) mold and arc-melting the deposited cerium oxide powder layer. Since the shape of the vicinity of the opening end portion of the yttrium oxide glass crucible is likely to be irregular, the opening end portion of the yttrium oxide glass crucible produced by the rotary die method is cut into a predetermined width to make the shape of the opening end portion uniform. .

For example, by rotating the polycrystalline germanium on the inside while rotating the above-described yttria glass crucible, the solution of the crucible is brought into contact with the seed crystal, and the seed crystal is pulled after the necking treatment, thereby producing a single crystal crucible. Further, in general, yttrium oxide glass crucible is used for each pulling of a single crystal crucible. That is, it is necessary to separately prepare the yttrium oxide glass crucible for each pulling of the single crystal crucible.

As an example of the above-described yttria glass crucible, the ratio of the thickness of the bubble-containing layer to the thickness of the transparent layer is 0.7 to 1.4 in the intermediate portion between the upper end and the lower end of the portion formed in the vertical direction of the yttrium oxide glass crucible, according to the structure The volume expansion due to heating can be minimized, and deformation or melt loss of the yttrium oxide glass crucible can be reduced (JP-A-2012-116713).

In addition, by forming a synthetic yttria glass layer, a natural yttria glass layer, an yttria-containing yttria glass layer, and a natural yttria glass layer from the inner surface toward the outer surface of the yttrium glass yttrium, the yttria glass can be reduced. Deformation or melting loss of 坩埚 (Japanese Patent Laid-Open No. 2012-6804).

Further, the roundness of the inner surface of the crucible and the roundness of the outer surface of the crucible are 0.4 or less with respect to the maximum wall thickness M of the same measurement height as the roundness, thereby enabling comparison at the time of pulling the single crystal crucible. High crystallization ratio (JP-A-2009-286651).

As described above, cerium oxide glass crucible having various structures is known. However, in the bismuth oxide glass crucible, the purpose of providing the transparent layer and the bubble-containing layer is to reduce the cause of the brown ring, etc., to improve the quality of the single crystal crucible to be pulled, and to control the heat of the single crystal crucible. It becomes easy to wait. However, in the transparent layer, even if no bubbles are observed based on visual observation or image data, there are cases where defects such as very small cracks are present. Further, it was observed in the visual observation that the bubble-containing layer composed of a single layer was actually composed of a multilayer structure. As described above, in the layer structure in the thickness direction of the yttrium oxide glass crucible, there are cases in which it is difficult to discriminate in the visual inspection. Such defects may cause damage to the bismuth oxide glass crucible during re-drawing or pulling of the single crystal crucible. Therefore, it is preferable to discriminate the cerium oxide glass crucible having such a defect beforehand. However, as described above, the yttria glass crucible having no defects or the yttrium oxide glass crucible having no defects is similarly regarded as a yttria glass crucible having a transparent layer and a bubble-containing layer in visual observation or the like. Therefore, there has been a problem that it is impossible to discriminate the cerium oxide glass crucible which has a problem in the layer structure in the thickness direction of the cerium oxide glass crucible by visual observation or the like.

As described above, the layer structure in the thickness direction of the cerium oxide glass crucible cannot be discriminated in advance by visual observation. Therefore, the layer structure in the thickness direction of the produced yttrium oxide glass crucible is measured by the technique of measuring the yttrium oxide glass crucible described in Patent Document 1 or Patent Documents 2 to 4. However, when the image analysis is performed in the thickness direction by the method described in Patent Document 1, for example, when the layer structure in the thickness direction of the entire circumference of the yttrium oxide glass crucible is determined, it is necessary to extend over the entire circumference of the bismuth oxide glass crucible in the thickness direction. Each point is measured, so it takes a lot of effort and time. Further, in the method described in Patent Document 1, since measurement is performed at each point in the thickness direction, only discontinuous analysis can be performed in the thickness direction. Further, the method described in Patent Document 1 is a method of measuring bubbles, and the structure of the transparent layer cannot be discriminated. As described above, when the layer structure in the thickness direction is to be measured by the method described in the cited document 1, there is a problem that it takes a lot of effort and time, continuous analysis cannot be performed in the thickness direction, and the measurement object is limited.

Further, the techniques described in Patent Document 2 to Patent Document 4 are techniques for measuring the state of the inner surface of the cerium oxide glass crucible. Therefore, in the techniques of Patent Document 2 to Patent Document 4, the layer structure in the thickness direction of the bismuth oxide glass crucible cannot be confirmed. As described above, in the techniques of Patent Document 1 or Patent Document 2 to Patent Document 4, there is a problem in that it is impossible to measure the layer structure in the thickness direction of the manufactured yttrium oxide glass crucible, or it takes a lot of effort and time in measurement. . Therefore, in general, a part of the produced cerium oxide glass crucible is selected and subjected to a failure inspection, thereby confirming the layer structure in the thickness direction of the produced cerium oxide glass crucible.

An evaluation device for a cerium oxide glass crucible according to one embodiment of the present invention is an evaluation device for a cerium oxide glass crucible manufactured by a rotary die method, and is applied to an upper end surface of a cerium oxide glass crucible or an upper end portion of a cerium oxide glass crucible. The laser beam on the inner side surface is measured at a scattering position at each position in the thickness direction inside the side wall portion of the cerium oxide glass crucible, and the cerium oxide glass crucible has a cylindrical straight portion having an opening at the upper end; a bottom portion; and a corner portion that connects the side wall portion and the bottom portion and has a larger curvature than the bottom portion, and an upper end of the straight cylindrical portion is formed flat.

Further, the ruthenium measurement method according to another aspect of the present invention employs the steps of: emitting a laser to the upper end surface of the yttrium oxide glass crucible as a measurement target or the inner surface near the upper end portion of the yttrium-doped yttrium glass, and measuring the injection into the oxidation. The scattering state of the laser in the glass crucible at various positions in the thickness direction inside the side wall portion of the cerium oxide glass crucible The crucible has a cylindrical straight portion having an opening at an upper end, a curved bottom portion, and a corner portion connecting the side wall portion and the bottom portion and having a larger curvature than the bottom portion, and the upper end of the straight cylindrical portion is flattened Ground formation.

According to the above invention, first, a laser such as a semiconductor laser or a solid laser which is located in the vicinity of the upper end portion of the yttrium oxide glass crucible is emitted from the inside or the outside of the yttrium-glass yttrium. Therefore, the laser beam incident on the yttrium oxide glass crucible is transmitted or partially scattered according to the layer structure in the thickness direction inside the side wall portion of the yttrium oxide glass crucible.

Specifically, the laser that enters the inside of the side wall portion of the yttria glass crucible is transmitted through the light transmitting layer without scattering or reflection. However, the laser scatters in the light scattering layer.

The scattering state of the laser beam incident on the yttrium oxide glass crucible is photographed by, for example, an imaging device, and the scattering state at each position in the thickness direction of the yttrium oxide glass crucible is measured.

The laser beam incident on the yttrium oxide glass crucible causes various scattering conditions such as transmission or partial scattering depending on the structure (transparent layer, bubble-containing layer, or presence or absence of defects) of the yttrium oxide glass crucible. Therefore, by photographing the end faces of the yttrium oxide glass crucible, it is possible to acquire image data corresponding to the layer structure in the thickness direction of the yttrium oxide glass crucible. By analyzing the image data, the layer structure in the thickness direction of the cerium oxide glass crucible can be continuously measured, and the layer structure in the thickness direction of the cerium oxide glass crucible can be measured non-destructively and simply.

According to the above invention, even if the transparent layer is scattered by a defect such as a crack, the laser beam incident on the iridium oxide glass crucible can be detected by measuring the scattering of the laser light, and the transparent layer which cannot be detected by visual inspection can be detected. Defects, etc. In addition, it is possible to measure whether or not a light transmitting layer or the like which is only required and has a sufficient thickness for performing single crystal pulling is formed on the innermost surface side of the yttrium oxide glass crucible. According to the above invention, it is possible to non-destructively and easily measure the layer structure in the thickness direction of the bismuth oxide glass crucible such as the thickness of the light transmitting layer or the light transmitting layer.

In the case where a thin light transmissive layer or a light scattering layer is formed on the inner surface side of the yttrium oxide glass crucible, when a single crystal germanium is produced, melting or the like of the light transmissive layer may cause a bubble containing layer or a defect such as a crack. The light scattering layer is exposed to the ruthenium solution. The uneven portion caused by defects such as bubbles or cracks in the light-scattering layer of the yttrium oxide glass yttrium appears in the cerium solution and the cerium oxide glass crucible The contact surface on which the so-called brown ring is concentrated. Therefore, there is a problem that crystal defects or the like may occur in the single crystal germanium after pulling. Therefore, it is preferable to form a light transmitting layer having a certain thickness on the inner surface side of the yttrium oxide glass crucible, and it is important to measure the layer structure in the thickness direction of the yttrium oxide glass crucible.

Further, according to the above invention, if the layer structure exists in the light scattering layer, the incident laser beam is scattered and the scattered light reflecting the layered structure is generated. Therefore, the layer structure can be known by measuring the scattered light. For example, if the scattered light intensity of the laser is uniform within a certain range, it is understood that the light scattering layer is composed of a single layer in the thickness direction of the crucible.

In the case where the bubble-containing layer includes a plurality of layers, the strength of the cerium oxide glass crucible or the like may be problematic due to the difference in the thermal expansion rates of the respective layers. Therefore, by making the bubble-containing layer a single layer, it is possible to reduce the possibility of breakage of the cerium oxide glass crucible due to the difference in the coefficient of thermal expansion. In order to reduce breakage of the cerium oxide glass crucible due to the difference in thermal expansion coefficient, it is preferable that the bubble-containing layer does not have a multilayer structure. In other words, by measuring the layer structure of the light-scattering layer or the bubble-containing layer as described above, it is possible to determine the cerium oxide glass crucible having a low possibility of breakage due to the difference in the coefficient of thermal expansion or the like.

Further, according to the above invention, for example, the thickness of the light-scattering layer and the shape of the boundary between the light-transmitting layer and the light-scattering layer can be measured, and it is possible to discriminate between the yttrium-doped yttrium glass yttrium and the light-transmitting layer having the thickness of the preferred light-scattering layer and light scattering. The interface of the boundaries between the layers is a preferred shape of yttrium oxide glass crucible.

In the process of crystal pulling, the 矽 solution interface is adjusted to be in the same position relative to the heater of the 矽 pulling device, and as the crystallization pull progresses, the 坩埚 is controlled to move upward. Therefore, in the single crystal crucible pulling, the temperature at the boundary portion between the growth portion of the single crystal germanium, that is, the solution in which the germanium solution becomes a single crystal germanium, and the crystal is at the melting point of the crucible, and in order to stabilize the boundary portion, it is necessary to Fine temperature control.

In the case where the yttrium oxide glass crucible is composed only of a transparent layer, when a heater is used to heat the ruthenium solution in the yttrium oxide glass crucible, the radiant heat from the heater is directly transmitted to the ruthenium solution interface through the ruthenium oxide ruthenium. Therefore, there is a case where temperature control is difficult. In order to perform appropriate temperature control during the pulling of the single crystal crucible, it is preferred to provide bubbles on the outer side of the transparent layer. a layer, and the bubble-containing layer has a suitable thickness. Therefore, by measuring the thickness of the light-scattering layer, it is possible to discriminate the cerium oxide glass crucible which can easily perform appropriate temperature control.

Further, according to the above invention, since the laser incident into the yttrium oxide glass crucible is scattered at the interface formed in the thickness direction of the yttrium oxide glass crucible, the interface can be measured by measuring the scattering of the laser. For example, when a laser beam is incident on a cerium oxide glass crucible, when the scattered light of the laser is observed at a plurality of points, it is understood that a plurality of interfaces are formed in the yttrium oxide glass crucible.

Generally, the yttria glass crucible is in the same state in the same layer. Therefore, once a crack is generated, the crack does not stop on the way but expands in the layer, sometimes causing cracks in the cerium oxide glass crucible. On the other hand, if there is an interface in the thickness direction, the yttrium oxide network structure in each layer is different, so that the crack stops expanding at the interface portion, and it is possible to prevent cracking of the cerium oxide glass crucible due to the expansion of the crack.

For example, a preferred layer structure can be formed by annealing the yttrium oxide glass crucible at a temperature equal to or higher than the fictive temperature. Therefore, by arranging the bismuth oxide glass crucible by the above-described invention and performing an annealing treatment, it is possible to produce a crucible which is difficult to crack.

Laser is emitted from each end position in the thickness direction of the bismuth oxide glass crucible from the end surface direction of the bismuth oxide glass crucible, and Raman scattering generated in accordance with the emitted laser beam is measured, whereby the thickness direction of the bismuth oxide glass crucible can be grasped. Layer structure. That is, instead of the above-described program, Raman scattering generated in accordance with the incident laser beam may be measured.

Further, in the above-described enthalpy measuring device, the light emitting portion may be configured to emit the laser beam from the inner side of the yttrium-glass lanthanum toward the thickness direction of the yttrium-glass ytterbium, and the scattering state measuring unit is configured to be measured from In the iridium oxide glass crucible of the target, the light emitting portion is incident on the annular end surface in the vicinity of the upper end opening portion of the portion of the laser beam, and the scattering state of the laser beam in the thickness direction inside the side wall portion of the yttrium oxide glass crucible is measured.

Further, the invention of the above-described ruthenium measurement method may be configured such that a laser beam is emitted from the inside to the outside of the yttrium oxide glass crucible in the thickness direction of the yttrium oxide glass crucible, and an upper end opening is incident from the laser beam of the bismuth oxide glass crucible. In the direction of the annular end surface around the portion, the state of the scattered light at various positions in the thickness direction of the inside of the side wall portion of the yttrium glass yttrium was measured.

In the present configuration, as a procedure for measuring the cerium oxide glass crucible, a laser light source is disposed inside the naturally cooled cerium oxide glass crucible from the inner side of the crucible to the thickness direction of the cerium oxide glass crucible to emit the laser.

In the present invention, for example, the scattering state of the laser beam incident on the yttrium oxide glass crucible may be imaged by an imaging device or the like from the direction of the annular end surface around the upper end opening of the yttrium oxide glass crucible. The laser is incident from the inside to the outside of the yttrium oxide glass crucible, thereby oxidizing the bismuth glass crucible to produce various scattering conditions. Therefore, when the scattering state of the laser beam incident into the yttrium oxide glass crucible is taken from the end face direction of the yttrium oxide glass crucible, image data corresponding to the layer structure in the thickness direction of the yttrium oxide glass crucible can be obtained. By analyzing the image data, the layer structure in the thickness direction of the cerium oxide glass crucible can be measured non-destructively and easily, and the cerium oxide glass crucible having a desired quality can be discriminated.

The laser beam is emitted from the inner side of the yttrium glass yttrium toward the thickness direction of the yttrium glass yttrium, and the scattering state of the laser inside the side wall portion of the yttrium glass yttrium is measured from the end surface direction, thereby removing the layer in the thickness direction of the yttrium glass yttrium. In addition to the structure, it is also possible to non-destructively and easily discriminate defects existing in the layer structure that cannot be confirmed by visual inspection. In addition, it is also possible to measure the thickness and the like of the light transmitting layer non-destructively and easily.

Further, the flaw measuring device may be configured to include an illumination unit that irradiates light of a predetermined wavelength corresponding to a wavelength of a laser beam emitted from the light emitting portion to a yttrium oxide glass crucible, and the scattering state measuring unit is configured to The scattering condition of the laser is measured by light illumination of the illumination unit.

Further, in the present invention, in the program for measuring the scattering state of the laser, illumination light of a predetermined wavelength corresponding to the wavelength of the emitted laser light may be irradiated to the yttrium oxide glass crucible, and the illumination light is irradiated. Measure the scattering of the laser.

According to the present structure, for example, when a red laser is emitted to the yttria glass, the blue illumination light is irradiated. In this case, an orange illumination or the like in which the hue is close to the color of the laser causes the scattering of the laser to be unobtrusive and is preferably avoided.

In this way, by measuring the scattering of the laser under the illumination light adjusted according to the wavelength of the laser Moreover, the scattering condition of the laser can be measured more clearly. Therefore, the layer structure in the thickness direction of the cerium oxide glass crucible can be measured with high precision, and the cerium oxide glass crucible having a layer structure having a desired thickness direction can be discriminated non-destructively and easily.

Further, the flaw measuring device may be configured such that the light emitting portion emits a horizontal laser as the laser.

The present invention may be configured to have a program for emitting a horizontal laser to the yttrium oxide glass crucible and measuring the scattering state of the incident horizontal laser at each position in the thickness direction of the yttrium oxide glass crucible.

Generally, a horizontal laser refers to a linear laser that is horizontal to the ground. According to this configuration, in the case of the yttrium oxide glass crucible, a horizontal laser beam is incident on the yttrium oxide glass crucible, and a scattering condition of various lasers corresponding to a structure including a cerium oxide glass crucible spread over a wide range can be obtained by an optical imaging device or the like. Its image data.

With such a configuration, the layer structure in the thickness direction of the bismuth oxide glass crucible can be measured at one time and efficiently for the layer structure in the thickness direction of the large-sized yttrium-glass yttrium into which the above-described horizontal laser is incident.

The cerium oxide glass layer is produced by depositing cerium oxide powder in a rotating carbon mold to arc-melt the deposited cerium oxide powder layer. Therefore, the layer structure of the transparent layer or the bubble-containing layer is symmetrical with respect to the central axis of the crucible. On the other hand, since the cerium oxide powder was deposited, the symmetry of the layer structure was not observed in the height direction of the cerium oxide glass crucible. Therefore, in order to grasp the characteristics of the yttrium oxide yttrium glass, it is more important to know the distribution of the layer structure in the height direction.

Here, if a vertical laser is used as the incident laser, the layer structure in the height direction of the crucible and the layer structure in the bubble containing layer and the like can be known in detail. Vertical laser refers to a linear laser in the vertical direction (for example, a laser that tilts a horizontal laser by 90 degrees). Also, by using a cross-linear laser, it is also possible to have both the advantages of horizontal laser and vertical laser.

Further, by causing the laser to be emitted in an oblique direction (a direction oblique to the depth direction of the bismuth glass crucible, the angle can be arbitrarily), for example, it is possible to determine how deep the defect exists.

Thus, the present invention is capable of utilizing various lasers.

Further, the above-described enthalpy measuring device is configured such that the light emitting portion is configured to emit a laser from each end position in the thickness direction of the yttrium oxide glass crucible from the end surface direction of the yttrium oxide glass crucible, and the scattering state measuring portion is The respective positions measure Raman scattering generated in accordance with the laser beam emitted from the light emitting portion as a scattering state of the laser.

Further, in the present invention, the laser beam may be emitted from each of the positions in the thickness direction of the yttrium oxide glass crucible from the end surface direction of the yttrium oxide glass crucible, and the pull generated by the emitted laser beam may be measured at each of the positions. Man scattering, as the scattering state of the laser.

According to this configuration, for example, the Rayleigh light removing filter is used to remove the Rayleigh light by the Rayleigh light removing filter, and the light is split by a spectroscope such as a diffraction grating, and detected by a detector or the like. Thereafter, it is converted into a Raman shift by an information processing device or the like and displayed.

It is generally known that in the case of Raman measurement of yttria glass, it is possible to measure a plurality of peaks such as a peak attributed to a planar four-membered ring and a peak attributed to a planar three-membered ring. However, in the case where the thickness direction of the yttrium-glass lanthanum includes a plurality of layer structures, since the yttrium oxide network structure is different in each layer, the wave value of each peak of the Raman shift at each position in the thickness direction is generated. deviation. Therefore, the layer structure of each layer can be measured by measuring the Raman shift at each position in the thickness direction of the yttrium oxide glass crucible.

According to the above configuration, even if it appears to be a portion of the transparent layer, if the layer structure is different, the above-described detection can be performed. Further, even if the bubble-containing layer has a plurality of layer structures, the above-described detection can be performed. As a result, it is possible to determine a cerium oxide glass crucible or the like which is likely to be deformed when the single crystal crucible is pulled up.

Further, in the above-described krypton measuring device, the light emitting portion is configured to emit laser light over a predetermined circumference of the entire bismuth oxide glass crucible, and the scattering state measuring portion is configured to measure and emit the light, respectively. The scattering condition of the laser corresponding to the laser emitted by the portion.

Further, in the present invention, the laser may be emitted at a predetermined predetermined interval over the entire circumference of the bismuth oxide glass crucible, and the scattering state of the laser corresponding to the emitted laser beam may be measured.

For example, when a laser beam is emitted from the inside of the yttrium oxide glass crucible in the thickness direction of the yttrium oxide glass crucible, the laser light source is rotated in a state where the laser beam is emitted, thereby spreading the entire circumference of the bismuth oxide glass crucible. Long shot into the laser.

Therefore, by causing the imaging device that captures the scattering state to move in cooperation with the rotation of the laser light source, it is possible to capture the scattering state of the laser generated over the entire circumference of the yttrium-glass yttrium by the rotation of the laser light source.

According to this configuration, it is possible to easily measure the structure in which the entire circumference of the yttrium oxide glass crucible is in the thickness direction, and it is possible to discriminate the yttrium oxide glass crucible in which the defect cannot be detected over the entire circumference of the yttrium oxide glass crucible.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Example [Embodiment 1]

A flaw measuring device and a weir measuring method according to a first embodiment of the present invention will be described with reference to Figs. 1 to 13 . The figure is a diagram showing an example of the structure of the helium measurement device. 2 to 4 are views showing an example of a state in which a state in which a cerium oxide glass crucible is incident on a laser is measured from the end surface direction. Fig. 5 is a flow chart showing an example of the flow of the 坩埚 measurement method. 6 to 9 are diagrams showing an example of an actual measurement image. Fig. 10 is a view showing internal residual stress of the yttria glass crucible shown in Fig. 6; Fig. 11 is a view showing internal residual stress of the yttria glass crucible shown in Fig. 7; 12 and 13 are diagrams showing an example of a scattering condition when a cross-linear laser is used.

In the present embodiment, a flaw measuring device that measures the scattering state of the laser at each position in the thickness direction inside the side wall portion of the yttria glass crucible having the transparent layer and the bubble-containing layer will be described. In addition, a method of measuring the flaw by the above-described helium measurement device will be described. The crucible measuring device according to the present embodiment is configured to face the oxygen from the inside of the yttrium oxide glass crucible as will be described later. The laser beam is emitted in the thickness direction near the upper end portion of the bismuth glass crucible. Therefore, the xenon measurement device measures the laser scattering state at each position in the thickness direction inside the side wall portion of the yttrium oxide glass crucible by photographing the yttrium oxide glass crucible from the end surface direction. Thereby, as described later, the structure in the thickness direction of the bismuth oxide glass crucible can be grasped. That is, by using the ruthenium measurement device and the ruthenium measurement method described in the present embodiment, it is possible to measure a light-transmitting layer (a region having a transparent layer without defects such as cracks) and a light-scattering layer (including a bubble layer or a transparent layer and having defects such as cracks) Area). As a result, defects such as cracks existing in the transparent layer can be easily found. In addition, the thickness and the like of the light transmitting layer and the light scattering layer can be measured. Further, as described above, by measuring the layer structure in the thickness direction of the cerium oxide glass crucible, it is possible to realize a cerium oxide glass crucible having a reduced possibility of occurrence of a problem in the pulling of the single crystal crucible, and a cerium oxide glass crucible which is less likely to cause cracks.

A photodetector such as an eye, a photodiode, or a photomultiplier can not perceive light if it does not enter the light. For example, even if the laser of the visible region wavelength is visually observed from a direction perpendicular to the direction of travel of the light, the light cannot be seen. . However, in this case, if the reflection/refraction of dust or particles in the air causes the laser to be scattered, the light is allowed to enter the eye or the like by the scattering to see the laser.

As in the air, the laser of the visible region wavelength hardly scatters even in the yttria glass, and thus is not visible from the direction perpendicular to the traveling direction of the light. If the photon of the laser interacts with the atoms that make up the yttrium oxide glass, it will excite the vibration of the electric dipole formed by the atom and release the photons therefrom. The released photons become secondary waves.

In the case where a large number of atoms are scattered and randomly distributed, if these secondary waves are observed in any direction, the intensity becomes the sum of the intensities of the secondary waves from the respective atoms, and generally does not become zero. This is the case of light scattering. On the other hand, when the atoms constituting the yttria glass are dense and the density is uniform, the secondary waves from the respective atoms interfere with each other, and the intensity is zero in a direction other than the specific direction. The secondary wave that does not disappear according to the interference result becomes a reflected wave or a refracted wave.

Light scattering is generally caused by material non-uniformity, and if the laser is scattered due to the presence of voids, bubbles or defects in the uneven yttria glass, the light is seen. Therefore, it is possible to know the existence of voids, bubbles, defects, and boundary of layers, etc., depending on the scattering of the laser.

The cerium oxide glass crucible as the measuring object in the present embodiment has a shape including a cylindrical side wall portion (straight cylindrical portion) having an opening at the upper end; a curved bottom portion; A corner portion that joins the side wall portion and the bottom portion and has a larger curvature than the bottom portion. Further, the upper end surface of the side wall portion of the yttria glass crucible is formed into an annular flat surface. The cerium oxide glass crucible of the present embodiment is produced, for example, by a rotary die method in which a cerium oxide powder layer is arc-melted by depositing cerium oxide powder in a rotating (carbon) mold. Thus, a method of producing a bismuth oxide glass crucible is produced. In addition, since the shape of the vicinity of the opening end portion of the yttrium oxide glass crucible is likely to be irregular, the opening end portion of the yttrium oxide glass crucible manufactured by the rotary die method is cut into a predetermined width, and the shape of the opening end portion is changed. neat.

FIG. 1 is an example of a configuration of a flaw measuring device according to a first embodiment of the present invention. The flaw measuring device includes a laser light source 2 (light emitting portion) that emits a laser beam to the beryllium oxide glass crucible 1 and an imaging device portion 3 (scattering state measuring portion) that photographs from the end surface of the beryllium oxide glass crucible 1 The scattering state of the incident laser in the yttrium oxide glass crucible 1.

The laser light source 2 is, for example, a solid laser light source or a semiconductor laser light source, and is disposed to inject a laser into the thickness direction of the yttrium glass crucible 1. Examples of the laser light source 2 include an AlGaInP (aluminum gallium phosphide) type movable laser light source (output wavelength is around 630 nm). Further, in addition to the laser light source, the light irradiation unit can use a mirror or a laser beam for laser transmission.

As shown in FIG. 1, the laser light source 2 of this embodiment is provided in the inside of the beryllium-tantalum glass crucible 1, and the laser beam is emitted from the inside of the beryllium-glass crucible 1 toward the thickness direction of the beryllium-glass crucible 1. By providing the laser light source 2 in this manner, a laser beam is incident on the yttria glass crucible 1 from the inside toward the outside of the bismuth oxide glass crucible 1.

Further, the laser light source 2 may emit laser light in the thickness direction of the beryllium glass crucible 1, and may be provided not only to be perpendicular to the normal direction of the side wall of the beryllium oxide glass crucible 1, but also to emit laser light in an oblique direction. Further, it is preferable that the laser light source 2 is disposed to enter and transmit the laser light in the vicinity of the end surface of the yttrium-glass iridium 1 (for example, in the vicinity of the upper end portion of the yttrium-glass yttrium from the end surface to a depth of 2 cm or the like).

The laser light emitted from the laser light source 2 passes through the yttrium oxide glass crucible 1 after passing through, for example, air, and is transmitted or partially scattered according to the structure of the yttrium oxide glass crucible 1, thereby indicating various scattering states at various positions in the thickness direction. .

Since yttria glass is amorphous, there is substantially no grain boundary which is a cause of light scattering. In addition, in the visible wavelength range of the wavelength of about 400 nm to 800 nm, the human eye observation can transparently see the yttrium oxide glass. Transparent yttria glass in the visible band means that light in this wavelength region is not absorbed or scattered. This is because, according to the energy gap of the yttria glass, light having a wavelength of about 400 nm or less generates light absorption, but light having a wavelength exceeding the wavelength is not absorbed, and the vibration of the free electron of the yttria glass is irradiated at a wavelength of Light above about 780 nm produces light scattering, so light having a wavelength less than this wavelength is not scattered. Generally, the wavelength range in which the light transmittance of cerium oxide glass is relatively high differs depending on the production method, the raw material, and the like, but is generally about 200 nm to 4000 nm.

Therefore, in a region where the transparent layer of the yttrium glass yttrium oxide 1 is free from defects such as cracks, the laser light emitted from the laser light source 2 (a laser emitting 630 nm) is not absorbed or scattered, and is transmitted (straight).

On the other hand, in the bubble-containing layer of the yttria glass crucible 1, the laser is scattered at the boundary between the bubble and the yttria glass. Therefore, if the laser light emitted from the laser light source 2 is incident on the bubble containing layer, a part of the laser light is scattered. Further, even in a region where it is visually judged to be transparent (is a transparent layer), when there is a defect such as a crack in the region, a part of the laser is scattered at the defect.

Since cerium oxide glass has a property of interacting with ultraviolet rays or infrared rays, it is preferable that the laser light source 2 emits a laser beam of visible light (a range of about 400 nm to 800 nm). As the laser light source 2 used in the present embodiment, for example, a laser of a red wavelength (for example, about 635 nm, about 650 nm), a laser of a green wavelength (for example, about 532 nm), or a laser of a blue wavelength can be used ( For example, about 410 nm) and the like. Further, in the present embodiment, as the laser light source 2, a laser other than visible light such as a deep ultraviolet laser (for example, 230 nm to 350 nm) may be used.

The aforementioned interaction between the yttria glass and the infrared region light occurs in accordance with the excitation of the vibration between the ions constituting the glass. Since the ions constituting the glass are derived from impurities in the yttrium oxide glass, the less the impurities, the less the absorption of light. Further, the absorption characteristics of light vary depending on the structure of the yttria network in the state at the time of glass production. On the other hand, the interaction of yttrium oxide glass with ultraviolet region light is caused by electron excitation, and thus the interaction with the infrared region light is different. Electron excitation depends on the valence band of the yttrium oxide glass and the band gap of the conduction band, by introducing alkaline gold It is an impurity such that the band gap is small, and the absorption end sometimes spreads to the visible region.

In the present embodiment, for example, the laser light source 2 is measured at a distance of 3 m, and the laser diameter is about 5 nm to 20 mm, and the output is about 0.2 mW to 500 mW. Further, the exit diameter of the laser light source 2 is, for example, about 0.8 mm to 5.5 mm. Further, the laser diameter, output, or exit diameter of the laser light source 2 may be other values than the values exemplified above.

The imaging device unit 3 is a general imaging device, and includes a CCD (Charge Coupled Device) image sensor (CMOS), a CMOS (Complementary Metal Oxide Semiconductor) image sensor, and the like. Photographic elements; and lens parts, etc. The imaging device unit 3 of the present embodiment is configured such that it is provided at an end surface position (that is, an end surface direction) at which the yttrium-glass diaphragm 1 as a measurement object can be imaged, and a ring around the upper end opening of the portion into which the laser beam is incident. In the direction of the end surface, the scattering of the laser beam incident into the yttrium oxide glass crucible 1 by the laser light source 2 in the thickness direction of the side wall portion of the yttrium glass crucible 1 is measured. Specifically, for example, referring to FIG. 1 , in the case where the yttria glass crucible 1 is disposed downward, the imaging device unit 3 is provided on the lower side of the yttrium-glass diaphragm 1 with the lens portion facing upward.

As described above, the laser beam incident on the yttrium oxide glass crucible 1 indicates various scattering states in accordance with the structure of the yttrium oxide glass crucible 1 at each position in the thickness direction of the yttrium oxide glass crucible 1. Therefore, the imaging device unit 3 acquires image data indicating the scattering state of the laser at each position in the thickness direction inside the side wall portion of the yttrium oxide glass crucible by photographing the end surface of the yttrium-glass diaphragm 1 . Thereafter, the imaging device unit 3 displays the acquired image data on, for example, a display unit (not shown).

For example, in the case of observing an object by an optical microscope or a metal microscope, transmitted light or reflected light is utilized. Even in the case of using a laser or the like to observe an object, it is common to use transmitted light or reflected light to observe an object. Therefore, the observation device such as the imaging device unit 3 is generally disposed at a position where the reflected light or the transmitted light can be observed, that is, in the vicinity of the laser light source 2 as the light emitting portion, or in the observation of the oxidation from the laser light source 2 The opposite side position of the side wall portion of the glass crucible 1.

On the other hand, in the invention of the present application, as described above, the imaging device unit 3 is provided at an end surface where the end face of the yttrium oxide glass crucible 1 can be imaged, and the vertical direction is viewed from the laser incident direction (that is, End direction). As described above, in the invention of the present application, by arranging the imaging device unit 3 at a position different from the general position, it is possible to easily acquire an image indicating the scattering state of each of the positions of the yttria glass sheets 1 in the thickness direction without breaking and easily. Data, capable of measuring the layer structure in the thickness direction.

FIG. 2 to FIG. 4 are schematic diagrams of image data acquired by the imaging device unit 3 as a scattering condition of the laser incident into the yttrium oxide glass crucible 1. The scattering state of the laser is represented by two lines, and the intensity of the laser scattering is represented by the interval between the two lines. In Figures 2 to 4, the regions causing more laser scattering are represented by the wider spacing of the two lines, and the regions of less laser scattering are represented by the narrower spacing of the two lines. In addition, the area other than between the two lines indicates that there is no incident or transmission laser, that is, no laser scattering is observed. Therefore, if the dispersion radio frequency is large, the intensity of the scattered light is strong, and conversely, if the dispersion radio frequency is small, the intensity of the scattered light is weak.

Fig. 2 shows that a laser beam is incident from the inner surface of the yttrium-glass iridium 1 and the transparent layer incident on the inner surface side of the laser is transmitted without scattering, but is scattered in the bubble-containing layer.

3 shows a transparent layer on the inner surface side of the yttrium oxide glass crucible 1 in the same manner as in FIG. 2, and a region in which the intensity of the scattering laser is different in the bubble-containing layer. The intensity of the scattered laser is strong near the transparent layer and the bubble-containing layer near the outer side, and the scattering intensity is weak in the middle portion. This is because the bubble-containing layer as the light-scattering layer is composed of a plurality of layers.

4 is the same as FIG. 3, showing that the incident laser is scattered in the bubble-containing layer and scattered in the transparent layer region. This indicates that a defect such as a crack which is a scattering center which cannot be confirmed by visual inspection exists in the transparent layer region, and by measuring the scattered light of the laser, it is possible to find a defect which cannot be visually observed in the transparent layer.

In this way, the imaging device unit 3 acquires image data indicating a state of laser light incident on the cerium oxide glass crucible 1 in accordance with various scattering states such as transmission or partial scattering in the layer structure in the thickness direction of the bismuth glass oxide crucible 1 . By referring to the image data acquired by the imaging device unit 3, it is possible to easily determine the layer structure in the thickness direction of the cerium oxide glass crucible 1 without breaking.

FIG. 5 is a flowchart showing an example of a flow of a flaw measurement method according to the first embodiment.

As shown in FIG. 5, the laser light source 2 is used to oxidize from the inner side of the yttrium oxide glass crucible 1 The laser beam is emitted in the thickness direction of the glass crucible 1 (step S101). Thereby, the cerium oxide glass crucible 1 is incident on the laser. Thereafter, the laser beam incident on the yttrium oxide glass crucible 1 exhibits various scattering conditions such as transmission or partial scattering according to the structure of the yttria glass crucible 1.

Next, the end surface inside the side wall portion of the cerium oxide glass crucible 1 is imaged by the imaging device unit 3. Thereby, the imaging device unit 3 measures the scattering state of the laser at each position in the thickness direction of the yttrium oxide glass crucible 1. In other words, the end surface of the yttrium oxide glass crucible 1 is imaged by the imaging device unit 3, thereby acquiring image data indicating the scattering state of the laser (step S102). Thereafter, the imaging device unit 3 displays the acquired image data on the display device, for example.

Then, the imaging device unit 3 captures the end surface inside the side wall portion of the cerium oxide glass crucible 1 to acquire image data indicating the scattering state of the laser at each position in the thickness direction of the bismuth oxide glass crucible 1 (step S102). Thereafter, the imaging device unit 3 displays the acquired image data on the display device, for example.

In addition, the flaw measuring device of the present embodiment can include an image analyzing unit (not shown) that analyzes the image data acquired by the imaging device unit 3 to determine the iridium oxide glass dome 1 such as a light transmitting layer or a light scattering layer. The layer structure in the thickness direction (the thickness of the light transmitting layer, the light scattering layer, and the light transmitting layer, etc.). Further, the ruthenium measurement method can be configured to analyze the image data to determine the layer structure (the thickness of the light transmission layer, the light scattering layer, and the light transmission layer) in the thickness direction of the yttrium oxide glass crucible 1 .

The image analysis unit is, for example, a general information processing device including an arithmetic unit and a storage device, and the function of analyzing the image data acquired by the imaging device unit 3 is realized by executing the program stored in the storage device by the arithmetic unit. In other words, the image analysis unit determines the layer structure in the thickness direction of the cerium oxide glass crucible 1 based on the image data. Thereby, the layer structure in the thickness direction of the cerium oxide glass crucible 1 can be automatically determined.

Further, in the present embodiment, when the laser beam is incident on the yttria glass crucible 1, the laser may be incident so that the incident angle becomes the Brewster's angle. Further, at this time, a laser beam in which the laser light source 2 emits p-polarized light may be configured. Further, the p-polarized light refers to polarized light in a direction in which the direction of vibration of the electric field is parallel to the incident surface.

With such a configuration, the laser beam emitted from the laser light source 2 can be incident on the interface between the air and the yttrium oxide glass crucible 1 without being reflected. Therefore, it can be used for observation of all layer structures and the like, and can be effectively used. The state of the yttrium oxide glass crucible 1 was observed. Further, when the scattering state of the laser is observed, since the interface between the air and the yttrium oxide glass crucible 1 does not cause reflection, it is possible to detect, for example, a layer structure or a defect in the vicinity of the interface, without being affected by the reflected light.

In addition, the angle of incidence may also be inaccurately a Brewster's angle. By projecting the laser in a manner close to the Brewster angle, a certain degree of effect can be obtained even if it is not an accurate angle.

Since the upper end portion of the yttria glass crucible 1 in which the laser light source 2 is incident on the laser beam has a cylindrical side wall portion, the laser beam is incident on the curved surface, and if the position of the laser light source 2 is deviated, the incident is made. The angle changes and sometimes it cannot become the Brewster angle. Further, as described above, since the yttrium oxide glass crucible 1 is produced by, for example, a rotary die method, the shape of the produced yttrium oxide glass crucible 1 may vary from the design. Therefore, it is necessary to accurately determine the emission position and the incident angle of the laser so that the incident angle becomes the Brewster angle at the determined position, and it is necessary to inject the laser.

For example, regarding a 32-inch yttrium oxide glass crucible having an inner diameter of about 81.3 cm and a mass of 50 kg to 60 kg, with respect to a 40-inch yttria glass crucible having an inner diameter of about 101.6 cm and a mass of 90 kg to 100 kg, Therefore, bismuth oxide glass crucible is a large weight. In order to inject a laser at a desired position and angle at a certain measurement position of such a bismuth oxide glass crucible and observe the scattered light, it is difficult to adjust the set position with high precision by causing the yttrium oxide glass crucible 1 to move itself. And set the angle.

Therefore, for example, a three-dimensional shape (three-dimensional coordinate) of the inner surface of the yttrium oxide glass crucible 1 is measured in advance by a robot or the like, and the position and angle of the emitted laser light with respect to the measurement position are calculated, and the lightning can be changed for each measurement point. Since the position and angle of the light source are measured, it is not necessary to adjust the installation position of the bismuth oxide glass crucible 1 itself.

Further, regarding the three-dimensional shape measurement of the inner surface of the yttrium oxide glass crucible 1, for example, an internal distance measuring portion composed of a laser displacement sensor or the like is provided at the tip end of the manipulator so that the inner distance measuring portion is not along the inner surface of the crucible Move with contact to measure. Specifically, at a plurality of measurement points on the moving path of the internal distance measuring portion, the inner surface of the yttrium glass crucible 1 is irradiated with a laser in an oblique direction, and The reflected light is detected, whereby the three-dimensional shape of the inner surface of the yttrium oxide glass crucible 1 can be measured. Therefore, by utilizing the measurement result, it is possible to easily emit the laser so that the incident angle with respect to the yttrium oxide glass crucible 1 becomes the Brewster's angle.

As described above, according to the flaw measuring device and the measuring method of the present embodiment, the thicknesses of the light transmitting layer and the light scattering layer can be measured. In the case of measuring the thickness of the light transmitting layer and the light scattering layer, if the incident angle is deviated from the normal direction of the incident surface (ie, with respect to the yttrium oxide glass crucible 1 not in the vertical direction but in the oblique direction, the lightning is incident Shot), the error becomes large and cannot be accurately measured. Therefore, it is preferable that the incident angle θ (the angle of the incident surface from the normal direction) of the laser beam emitted from the laser light source 2 is emitted in accordance with the following formula. Further, in the following formula, the wall thickness (thickness of the light transmitting layer and the light scattering layer) of the yttrium oxide glass crucible 1 is represented as T, and the allowable error is expressed as ΔT.

Formula 1 θ=arccos T/(△T+T)

According to the above formula, Table 1 shows the relationship between the wall thickness T of the yttrium oxide glass crucible 1, the allowable difference ΔT, and the incident angle θ. For example, when the wall thickness of the crucible is 10 mm, the allowable laser penetration angle is allowed to be within 8.0° when the difference is 0.1 mm. In this way, the laser light source 2 is controlled so as to have an entrance angle θ corresponding to the wall thickness T of the yttrium oxide glass crucible 1 and the allowable deviation ΔT, whereby the yttrium oxide can be measured within an allowable error range. The wall thickness of the glass crucible 1 (for example, the thickness of the light transmitting layer and the light scattering layer). Further, when the angle θ is controlled, it is preferable to accurately control the angle θ at each point without deviation by using the measurement result of the three-dimensional shape of the inner surface of the yttrium-glass diaphragm 1 by the internal distance measuring unit.

In addition, when measuring the thickness of the light transmitting layer and the light scattering layer, in order to reduce the error, it is preferable to The laser diameter B of the laser (the laser diameter of the portion of the yttrium oxide glass crucible 1) is controlled in such a manner as to satisfy the following formula. Further, in the following formula, the allowable error is expressed as ΔT, the wall thickness of the yttrium oxide glass crucible 1 is represented as T, and the laser diameter is represented as B.

According to the above formula, Table 2 shows the relationship between the wall thickness T of the yttrium oxide glass crucible 1, the allowable difference ΔT, and the laser diameter B. For example, when the wall thickness of the crucible is 10 mm, the allowable laser diameter becomes 1.4 mm when the tolerance is 0.1 mm. The laser light source 2 is controlled so as to become a laser beam diameter B corresponding to the wall thickness T of the yttria glass crucible 1 shown in Table 2 and the allowable deviation ΔT, thereby measuring within an allowable error range. The wall thickness of the yttrium oxide glass crucible 1 (for example, the thickness of the light transmitting layer and the light scattering layer).

The portion into which the laser is incident is not limited to the inner side of the yttrium glass crucible 1. It is also possible to cause the laser to enter from the outer side toward the inner side in the thickness direction of the yttrium glass crucible 1. Further, the laser may be incident from the end face of the yttria glass crucible 1 and the scattering state of the laser may be measured from the inside of the yttrium oxide glass crucible 1. In this case, the scattering state is measured while moving the position of the laser to be emitted along the thickness direction of the yttria glass crucible 1. Thus, it is possible to grasp that irregularities are formed in the inner transparent layer or the bubble-containing layer of the yttrium oxide glass crucible 1.

Further, the laser light source 2 is rotated at a predetermined predetermined interval (for example, every 2 to 3 degrees, 5 degrees, and 10 degrees, which may be an arbitrary angle) in a state where the laser beam is emitted from the inside of the bismuth oxide glass crucible. This enables the laser to be incident throughout the entire circumference of the yttrium glass crucible 1. At this time, by causing the imaging device unit 3 to move in accordance with the rotation of the laser light source 2, it is possible to measure the laser emission throughout the oxidation. The scattering condition at each position of the entire circumference of the glass crucible 1. As a result, the structure in the thickness direction of the yttrium oxide glass crucible 1 over the entire circumference of the yttrium oxide glass crucible 1 can be measured by an easy method.

Further, by measuring the entire circumference of the yttrium oxide glass crucible 1 as described above, it is possible to measure the thickness distribution and the roundness of each layer when a plurality of layers of concentric circles are present at the upper end portion of the yttrium oxide glass crucible. In addition, it is also possible to measure the roundness of the boundary between the transparent layer and the bubble-containing layer. Since it is also possible to measure the roundness of the inner surface of the yttrium oxide glass crucible 1, it is possible to calculate by using the roundness of the inner surface of the yttrium oxide glass crucible 1 and the roundness of the boundary between the transparent layer and the bubble-containing layer. Whether a transparent layer of the desired thickness of the single crystal crucible is formed. Further, when the single crystal crucible is pulled, if the layer thickness distribution of the cerium oxide glass crucible is uneven, the heat conduction becomes uneven, and the temperature distribution of the cerium solution is uneven. As a result, it is difficult to constantly maintain the position of the contact interface between the single crystal ruthenium and the ruthenium solution, and problems such as misalignment may occur. According to the ruthenium measurement apparatus and the ruthenium measurement method of the present embodiment, the yttrium oxide glass crucible 1 is measured, and it is possible to discriminate the bismuth oxide glass crucible which causes problems such as indexing. Further, when measuring the entire circumference of the yttrium oxide glass crucible 1, it is preferably performed in combination with a horizontal laser to be described later.

In the present embodiment, a case has been described in which a laser light source 2 that is a one-way laser such as a laser pointer is used as the light emitting portion. However, other light emitting portions other than the one-way laser may be used. . For example, the laser light source 2 can be configured to be emitted at a wide angle (for example, by a lens, in which the angle is increased by a predetermined angle with respect to the incident angle of the incident laser (for example, 2 to 4) Double) shot). Alternatively, as the light emitting portion, a linear laser (horizontal laser or vertical laser) or a cross-linear laser may be used. The cross-linear laser emits a laser in the horizontal direction and the vertical direction by passing the emitted laser beam through the cylindrical rod lens after passing through the collimator lens.

In this way, a linear laser or a cross-linear laser is used as the light emitting portion, whereby a wide range of scattering conditions can be measured at one time. For example, by using a linear laser (horizontal laser) in a horizontal direction with the earth's surface, it is possible to measure the layer structure inside the side wall portion of the bismuth oxide glass crucible 1 at a wide range. Thereby, the layer structure can be measured without missing the entire range. In addition, by using a linear laser in the vertical direction (vertical laser: for example, a laser that tilts the horizontal laser by 90 degrees) or a cross-linear laser, it is possible to make a more specific judgment and depth of the layer structure in the bubble-containing layer. Judgment of the layer structure of the direction. In addition, facing the oblique direction (towards the depth of the yttrium glass crucible 1 The direction of the direction of the tilt. The angle can be arbitrarily shot out of the laser, and it is also possible to determine the depth at which the defect is located.

Further, in the case where a cross-linear laser or the like is used as the laser light source 2 in the present embodiment, for example, the distance from the laser light source 2 to the incident object and the incident amount are about 2 mm at a distance of 5 m. The ratio of the line length of the laser when the object is incident on a flat surface is not limited, but it is preferably used in a ratio of about 1:0.3 to 2, for example.

The method for producing a cerium oxide glass crucible according to the present embodiment includes a cerium oxide glass layer forming program and a cerium oxide glass ruthenium inspection program in which cerium oxide powder is melted and then cooled to form a cerium oxide glass layer.

The cerium oxide glass crucible forming program includes the following procedure: (1) depositing a predetermined thickness on the inner surface (bottom and side surfaces) of the inner surface of the inner surface (bottom and side surfaces) of the inner surface (the bottom surface and the side surface) having a predetermined inner surface of the quartz glass crucible a crystalline or amorphous cerium oxide powder to form a cerium oxide powder layer for a cerium oxide glass layer; (2) heating the cerium oxide powder layer to 2000 ° C to 2600 ° C by arc discharge Melting and then solidifying, thereby performing vitrification while cooling immediately; and (3) cutting the open end portion to a predetermined width to make the shape of the open end portion uniform.

The cerium oxide glass ruthenium inspection program includes a procedure for measuring the scattering state at each position in the thickness direction of the above-described cerium oxide glass crucible, and is carried out to the cerium oxide glass crucible subjected to the above-described cerium oxide glass crucible forming procedure. In this inspection procedure, it is possible to manufacture a cerium oxide glass crucible having the above various advantages by discriminating a qualified cerium oxide glass crucible.

FIG. 6 to FIG. 9 are images obtained by actually capturing the scattering state of the laser beam when the laser beam is incident on the alumina glass raft 1 from the inside by the imaging device unit 3.

Fig. 6 shows a state in which a laser beam incident on the yttrium oxide glass crucible 1 is partially scattered by being transmitted from a inside of the yttrium oxide glass crucible 1 to a predetermined position. The yttrium oxide glass crucible 1 has a light transmitting layer (a transparent layer and a layer having no defects) and a light scattering layer (including a bubble layer or the like) which is located outside the light transmitting layer and is scattered by the light transmitting layer, and is determined as The light scattering layer is a single layer structure.

Figure 7 shows that after the incident laser is transmitted from the inside of the yttrium glass yttrium 1 to a predetermined position, After the strong scattering, the scattering becomes weak and the state is strongly scattered again. The yttria glass crucible 1 has a light transmitting layer and a light scattering layer outside the light transmitting layer, and it is determined that the light scattering layer is composed of a plurality of layers.

Fig. 8 shows that after the incident laser beam is transmitted from the inside of the yttrium glass yttrium 1 to a predetermined position, it is strongly scattered first, and once the scattering is interrupted, the laser scatters. The yttria glass crucible 1 has a light transmitting layer and a light scattering layer outside the light transmitting layer, and it is determined that the light scattering layer is composed of a plurality of layers.

Figure 9 shows the initial scattering of the incident laser, once transmitted, followed by scattering. This yttria glass crucible 1 has a light transmitting layer and a light scattering layer outside the light transmitting layer, and is judged to have a defect (a light scattering layer is formed) in the inner portion of the yttrium oxide glass crucible 1 in the transparent layer.

10 and 11 show the distortion (internal residual stress) of the yttria glass crucible 1 of Figs. 6 and 7. As shown in FIG. 10, in the yttria glass crucible 1 of FIG. 6 (having a light-transmitting layer and a light-scattering layer, the light-scattering layer is determined to be a single-layer structure of yttrium oxide glass), it is judged that although in the light-transmitting layer and light There is a boundary of internal residual stress between the scattering layers, but the internal residual stress in the other portions is slowly changed. Further, since yttria glass has birefringence, if the internal residual stress sharply changes, the refractive index also changes abruptly, and contrast can be observed.

As shown in FIG. 11, in the yttria glass crucible 1 (having a light-transmitting layer and a light-scattering layer, the light-scattering layer is determined to include a plurality of layers), the light-scattering layer is also judged to be in the light-scattering layer. There is a boundary (abrupt change) of internal residual stress inside.

Thus, the correspondence relationship can be observed between the laser scattering state of the yttrium oxide glass crucible 1 and the distortion. It is considered that the yttrium oxide glass is in a state of being compressed or stretched at an atomic level, and the distance (the density of atoms) of the Si-O-Si bonding is not uniform, and the distortion is the same, and the distortion causes scattering of the incident laser.

The distortion inspection is generally performed by destroying the inspection and destroying the bismuth oxide glass crucible 1. Therefore, the distortion test can be easily performed by replacing the distortion test without damaging and simply measuring the laser scattering state of the present invention. In addition, it is also possible to measure the scattering state of the laser, and perform annealing treatment or the like based on the result of the measurement (if necessary).

When polycrystalline germanium is loaded into the interior of the cerium oxide glass crucible 1 in order to manufacture a single crystal germanium, there is a Polycrystalline germanium causes indentation of the inside of the cerium oxide glass crucible 1. In such a case, if the distortion in the yttrium oxide glass crucible 1 is large, the indentation may cause cracks in the yttrium oxide glass crucible 1, but cracks may not occur directly after the indentation is caused. Therefore, there is also a crack in the single crystal 矽 pulling process, especially when the bismuth oxide bismuth 1 is cracked when the ruthenium is being melted, the pulling device is broken, and the raw material is discarded, thereby generating economy. loss. According to the measuring method of the present invention, the distortion measurement of the yttrium oxide glass crucible 1 can be replaced by a non-destructive and easy method, and the above-described loss can be prevented in advance.

12 and 13 are diagrams showing the state of scattering when a cross-linear laser is used. FIG. 12 is a view showing a scattering state in the thickness direction of the yttrium oxide glass crucible 1 when a laser is emitted using a cross-linear laser, and it is understood that light can be discriminated in the entire range of the imaging device unit 3 by using a cross-linear laser. Transmission layer and light scattering layer.

If a cross-linear laser is used, it is possible to measure a wide range of scattering conditions, and in addition to the configuration of the light-transmitting layer and the light-scattering layer, for example, it is possible to determine the processing trace of the edge. In Fig. 13, it is shown that the incident cross-linear laser is also scattered in the region of the transparent layer.

[Embodiment 2]

Next, a second embodiment of the present invention will be described with reference to Figs. 14 to 16 . Fig. 14 shows an example of the configuration of the helium measurement device of the present embodiment. FIG. 15 is a flowchart showing an example of a flow of a flaw measurement method according to the second embodiment. Fig. 16 is a view showing the influence of the distance between the inner surface of the crucible and the illumination portion on the measurement of the scattering condition.

In the present embodiment, a helium measurement device that measures the scattering state of a laser beam incident on the yttria glass crucible 1 under irradiation of light of a predetermined wavelength will be described. In addition, a method of measuring the flaw by the above-described helium measurement device will be described.

As shown in FIG. 14, the xenon measurement device of the present embodiment includes a laser light source 2, an imaging device unit 3, and an illumination unit 4. The configurations of the laser light source 2 and the imaging device unit 3 are the same as those described in the first embodiment. Therefore, the repeated description is omitted.

The illumination unit 4 is configured by, for example, an LED (Light Emitting Diode) or the like, and is configured to emit light having a wavelength corresponding to the wavelength of the laser beam emitted from the laser light source 2. Specifically configured as an example When the laser light source 2 emits a red laser, the illumination unit 4 illuminates the light of the blue wavelength.

Since the illumination in which the hue is close to the laser causes the laser scattering to become unobtrusive, it is preferable to avoid the light (illumination) irradiated by the illumination portion 4. That is, it is preferable that the illumination unit 4 emits light that does not include a wavelength close to the wavelength of the laser beam emitted from the laser light source 2. As an example, when the wavelength of the light emitted from the laser light source 2 is 630 nm, it is preferable to use light illumination that does not include a blue wavelength having a wavelength of around 630 nm. In addition, this is because, when an object is illuminated by white light and the reflected light is red, the object reflects light of a wavelength in a red-visible region of the human eye, and absorbs light of other wavelengths. Therefore, even if the light of the wavelength of the blue visible area of the human eye is illuminated, the object will not see red.

When the laser light source 2 enters the laser beam to the yttria glass crucible 1, the illumination unit 4 performs light irradiation adjusted in accordance with the wavelength of the laser light, and the imaging device unit 3 captures the end surface of the yttrium oxide glass crucible 1 Measure the scattering of the laser. As a result, the layer structure in the thickness direction of the yttrium oxide glass crucible 1 can be measured with higher precision.

Next, an example of a flaw measurement method by the above-described helium measurement device will be described with reference to FIG.

Referring to Fig. 15, first, the laser light source 2 is used to emit a laser beam from the inner side of the beryllium oxide glass crucible 1 in the thickness direction (step S101). Thereby, the cerium oxide glass crucible 1 is incident on the laser. Thereafter, the laser beam incident on the yttrium oxide glass crucible 1 indicates various scattering states such as transmission or partial scattering in accordance with the structure of the yttrium oxide glass crucible 1.

Next, if the illumination unit 4 is used to illuminate the illumination light corresponding to the laser before and after the laser is emitted (S201). Thereby, the laser beam is incident on the iridium oxide glass crucible 1 under the illumination of the illumination unit 4.

Thereafter, the end face of the yttria glass crucible 1 is imaged by the imaging device unit 3. Thereby, the imaging device unit 3 measures the scattering state of the laser at each position in the thickness direction of the yttrium-glass diaphragm 1 under the illumination of the illumination unit 4. In other words, the imaging device unit 3 captures the end surface of the yttrium-glass diaphragm 1 to acquire image data indicating the scattering state of the laser (step S102). Thereafter, the imaging device unit 3 displays the acquired image data on the display device, for example.

As described above, the flaw measurement method of the present embodiment measures the scattering state at each position in the thickness direction of the tantalum oxide glass crucible 1 under irradiation of illumination light. As a result, the layer structure in the thickness direction of the cerium oxide glass crucible 1 can be grasped based on the result of the measurement.

Fig. 16 shows the relationship between the distance between the inner surface (or end surface) of the yttrium oxide glass crucible 1 and the illumination portion 4 and the easiness of measuring the laser scattering condition. Specifically, (A) of FIG. 16 shows a case where the distance between the inner surface of the yttrium oxide glass crucible 1 and the illumination portion 4 is 100 mm, and (B) of FIG. 16 shows the inner surface of the yttrium oxide glass crucible 1 and the illumination portion 4. The distance between them is 300mm. In addition, (C) of FIG. 16 shows a case where the distance between the inner surface of the yttrium oxide glass crucible 1 and the illumination unit 4 is 500 mm.

As shown in FIG. 16, it can be seen that in the laser light source 2 and the illumination unit 4 used, the laser can be measured most clearly when the distance between the inner surface of the yttrium-glass diaphragm 1 and the illumination unit 4 is separated by about 500 mm. Scattering condition. Thus, by adjusting the distance between the inner surface of the yttrium oxide glass crucible 1 and the illuminating portion 4, the scattering state of the incident laser can be more clearly measured. That is, it is preferable that the illumination unit 4 is adjusted such that the distance from the inner surface of the yttrium-glass diaphragm 1 becomes a predetermined predetermined distance (for example, 500 mm). Further, it is considered that an appropriate distance between the yttrium-glass iridium 1 and the illuminating unit 4 can be changed, for example, depending on the intensity of light to be irradiated by the illuminating unit 4 or the like. Therefore, the predetermined predetermined distance described above is a distance that can be adjusted as needed.

The flaw measuring device and the measuring method of the present embodiment are the same as those described in the first embodiment, and various other configurations can be employed. For example, it is also effective to combine the linear laser or the cross-linear laser (light emitting portion) and the illumination portion 4 described above. In particular, for example, by emitting a red laser under the illumination of the blue illumination light of the illumination unit 4, the scattered portion can be measured as purple, and the scattering condition can be measured more clearly.

When the yttrium oxide glass crucible 1 is produced by the rotary die method, it is possible to more easily manufacture and realize preferred oxidation by measuring the scattering state at each position in the thickness direction of the yttrium oxide glass crucible 1 under the illumination of the illumination light.矽 Glass 坩埚 1.

[Embodiment 3]

Next, a third embodiment of the present invention will be described with reference to Figs. 17 to 21 . Figure 17 is the present embodiment An example of the structure of the 坩埚 measuring device. FIG. 18 is a view showing an example of a position at which the sputum measuring device of the present embodiment measures a Raman spectrum. 19 is a flow chart showing an example of a flow of a flaw measurement method according to the third embodiment. 20 and 21 are examples of actually measured Raman spectra.

In the present embodiment, a flaw measuring device that measures the scattering state of the laser beam in the thickness direction of the yttrium oxide glass crucible 1 by measuring the Raman spectrum (measured Raman scattering) will be described. In addition, a method of measuring enthalpy by the above apparatus will be described.

Referring to Fig. 17, the flaw measuring device of the present embodiment includes, for example, a laser portion 21 (light emitting portion) and a Raman spectrometry portion 31 (scattering condition measuring portion). Further, the Raman spectrometry unit 31 includes, for example, a Rayleigh light removing filter 311, a spectroscope 312, and a detector 313.

The laser beam portion 21 is, for example, a semiconductor laser or a solid laser beam, and is configured to emit a single sheet from the end surface direction of the bismuth oxide glass crucible 1 toward the end surface of the bismuth oxide glass crucible 1 in the thickness direction of the bismuth oxide glass crucible 1. Color laser (for example, a green laser at 520 nm). That is, as shown in FIG. 17, the laser beam 21 emits a laser beam toward the end surface of the yttria glass crucible 1 while moving the emission position along the thickness direction of the yttria glass crucible 1. Thereby, the Raman spectrum of each position in the thickness direction of the yttrium oxide glass crucible 1 was measured as follows.

As described above, the Raman spectrometry unit 31 includes the Rayleigh light removing filter 311, the spectroscope 312, and the detector 313.

The Rayleigh light removing filter 311 is a filter for removing Rayleigh scattering, that is, light having the same wavelength as that of the emitted laser light, which is included in the scattered light. The laser beam emitted from the laser beam 21 is incident on the end face of the yttrium oxide glass crucible 1 to generate scattered light. In addition to Raman scattered light (Stokes, Anti-Stokes, which may be one of them), Rayleigh scattered light is included in the scattered light. . Therefore, the Rayleigh light removing filter 31 is used to remove Rayleigh scattered light.

Next, the light passing through the Rayleigh light removing filter 311 is incident on the beam splitter 312. Thereby, the scattered light from which the Rayleigh scattered light is removed is split by the spectroscope 312. Thereafter, the detector 313 detects the split light for each wavelength. With such a configuration, the 本 of the present embodiment The helium measuring device measures the scattering state at each position in the thickness direction of the yttrium oxide glass crucible 1. Further, the detector 313 is connected to, for example, an information processing device (not shown), and the information processing device can calculate a Raman shift value corresponding to the detected light. Thereby, the Raman spectrum can be measured. That is, Raman scattering can be measured.

In addition, the structure for measuring the above Raman spectrum is at most an example. It is also possible to measure the Raman spectrum at each position in the thickness direction of the yttrium oxide glass crucible 1 by using a structure other than the above-described structure.

As described above, the flaw measuring device of the present embodiment includes the laser portion 21 and the Raman spectrometry portion 31. With such a configuration, the Raman spectrum of each position in the thickness direction of the yttrium oxide glass crucible 1 on the end face of the yttrium oxide glass crucible 1 is obtained. In other words, as shown in FIG. 18, the position of the laser portion 21 is adjusted so as to be at each position in the thickness direction of the yttrium-glass glass crucible 1, and the Raman spectrum at each position in the thickness direction of the yttrium-glass iridium 1 is obtained.

Here, it is understood that in the Raman spectrum of the yttrium oxide glass, a plurality of peaks represented by a peak attributed to the planar four-membered ring and a peak attributed to the planar three-membered ring are measured. Therefore, the Raman spectrum at each position in the thickness direction of the end face of the above-described yttrium-tantalum glass crucible 1 also has a plurality of peaks including a peak attributed to the planar four-membered ring and a peak attributed to the planar three-membered ring. On the other hand, if the measurement is actually performed, the value of the Raman shift of each peak may vary at each position in the thickness direction of the yttrium oxide glass crucible 1 . In other words, a plurality of structures may be included in the thickness direction of the yttrium-glass iridium 1 , and as described above, the plurality of structures can be measured by performing Raman measurement at each position in the thickness direction of the yttrium-glass iridium 1 .

Further, when the Raman spectrum is measured, when the Raman shifts at different positions in the thickness direction of the yttrium-glass lanthanum 1 are different, the structure in the thickness direction of the yttrium-glass yttrium 1 is different, and the yttrium oxide glass crucible 1 is used. When the single crystal crucible is pulled, it is easy to cause distortion. On the other hand, the Raman spectrum is measured at each position in the thickness direction of the yttrium-glass iridium 1 and the yttrium oxide glass yt 1 having the same Raman shift (small difference) is discriminated at each position in the thickness direction of the yttrium-glass yttrium 1 Cracked (no crack) yttrium oxide glass 坩埚1. Thus, as one of the methods for determining the bismuth oxide glass crucible 1 which is difficult to crack, measurement of Raman spectroscopy can also be used. In addition, when the Raman spectrum is measured to discriminate the bismuth oxide glass crucible 1 which is difficult to crack, for example, whether the Raman shift is the same in the light transmitting layer or the light scattering layer (which may also be in the transparent layer or the bubble containing layer), or It is confirmed whether or not the Raman shift of the entire thickness direction is the same.

Further, the measurement of the scattering state of the laser described in the first embodiment and the second embodiment and the measurement of the Raman spectrum described in the present embodiment (or laser-based measurement) may be simultaneously performed. The measurement of the scattering condition is used to measure the Raman spectrum (Raman scattering). Specifically, for example, measurement of the scattering state of the laser beam emitted from the inside of the yttrium-glass iridium 1 is performed, and it is determined that the scattering state of the laser is measured for each layer of a different structure by measurement of the scattering state of the laser beam. Laser for medium-irradiation Raman excitation. Thereafter, after the laser for scattering measurement is stopped (when the illumination light is irradiated by the illumination unit 4, the irradiation of the illumination light is also stopped), Raman measurement is performed. In other words, the light transmitting layer and the light scattering layer are grasped based on the measurement result of the scattering state of the laser, and based on the result of the determination, the Raman spectrum is measured for the light transmitting layer or the light scattering layer, the vicinity of the boundary between the light transmitting layer and the light scattering layer, and the like. . By performing measurement by combining these two methods, the layer structure of the yttrium oxide glass crucible 1 in the thickness direction can be easily and accurately grasped. Further, in the laser for scattering measurement (the laser emitted by the laser light source 2) and the laser for Raman measurement (the laser beam emitted by the laser portion 21), it is preferable to use a laser having a different wavelength.

Next, a method of measuring the flaw by the above-described helium measurement device will be described.

Referring to Fig. 19, first, the laser portion 21 emits a laser beam from the end surface direction of the beryllium glass crucible 1 toward the end surface of the beryllium glass crucible 1 (S301). The laser beam emitted from the laser beam 21 is incident on the end face of the yttrium oxide glass crucible 1 to generate scattered light. Therefore, when Rayleigh light is removed, splitting is performed, and the split light is detected for each wavelength. For example, Raman scattering is measured by such a method (S302).

Thereafter, it is confirmed whether or not the exit point of the laser is displaced in the thickness direction of the bismuth glass oxide crucible 1 (S303). In the case where a misalignment occurs, the Raman scattering is measured again (S303, YES), after the projection point of the laser is displaced along the thickness direction of the yttrium glass crucible 1. On the other hand, in the case where there is no misalignment (in the case where the measurement in the thickness direction is ended), the measurement of the Raman scattering is ended (S303, NO).

As described above, the ruthenium measurement method of the present embodiment measures the Raman scattering of each position of the yttria glass crucible 1 in the thickness direction. As a result, based on the result of the measurement, the layer structure in the thickness direction of the yttrium oxide glass crucible 1 can be grasped.

Further, when the yttrium oxide glass crucible 1 is produced by the rotary die method, a preferred bismuth oxide glass crucible 1 can be manufactured and realized even after the procedure for performing the Raman measurement described above. Further, the yttrium oxide glass crucible 1 manufactured by the manufacturing procedure of the yttria glass crucible 1 having the steps of performing the laser measurement and the Raman measurement in the thickness direction can have the same advantageous effects.

20 and 21 are results of actually measuring the Raman spectrum at each position in the thickness direction of the yttrium oxide glass crucible 1. Fig. 20 shows the results of measuring the Raman spectrum at each position in the thickness direction of the yttrium oxide glass crucible 1 on the end faces of the yttrium oxide glass crucible 1 similar to those in Figs. 6 and 10 . Fig. 21 shows the results of measuring the Raman spectrum at each position in the thickness direction of the yttrium oxide glass crucible 1 on the end faces of the yttrium oxide glass crucible 1 similar to those in Figs. 7 and 11 .

The Raman spectrum of Figs. 20 and 21 shows, in order from the bottom to the bottom, the results of the Raman measurement at the inner surface side, the inner surface and the middle boundary, the middle, the intermediate and outer surface side boundaries, and the outer surface side. Further, for easy observation, the results of the Raman spectra of FIGS. 20 and 21 were corrected so that the results did not overlap. Therefore, in the following, only the value of the Raman shift is taken as a problem, and the intensity is not visible.

Referring to Fig. 20, in the peak (the peak near 488 cm ^-1 ) attributed to the planar quaternary ring, the measurement results of the inner surface side and the inner surface and the intermediate boundary, the boundary between the middle, the intermediate and outer surface sides, and the outer surface are known. There are large differences in the measurement results on the side. As shown in FIGS. 6 and 10, the iridium oxide glass crucible 1 after the measurement of FIG. 20 has a light transmitting layer and a light scattering layer, and is a layer which is determined to have a light scattering layer composed of a single layer structure. According to the above configuration, it can be considered that there is a certain correlation between the result of the Raman measurement and the measurement result of the scattering state in the thickness direction of the yttria glass crucible 1. That is, the measurement results of the inner surface side and the inner surface and the intermediate boundary indicate the light transmission layer, and the measurement results of the boundary between the middle, the middle, and the outer surface side and the outer surface side indicate the light scattering layer. As described above, it is understood that the layer structure in the thickness direction of the yttrium oxide glass crucible 1 can be grasped based on the result of the Raman measurement.

Further Similarly, in FIG. 21, seen in the peak attributable to the planar four-membered ring (488cm ^-1 near the peak) and a peak attributed to (602cm ^-1 near the peak) in the three-membered ring plane, each boundary (the The value of the Raman shift of the boundary between the surface and the middle, the boundary between the middle and the outer surface can be observed as a deviation. As shown in FIGS. 7 and 11, the yttria glass crucible 1 after the measurement of FIG. 21 has a light transmitting layer and a light scattering layer, and it is judged that the light scattering layer is composed of a plurality of layers. It is also known from these cases that there is a certain correlation between the results of the Raman measurement and the measurement results of the scattering state in the thickness direction of the yttrium oxide glass.

In addition, Table 2 shows the pulling of the respective points (the inner surface side, the interface 1, the outer side of the inner surface side, the interface 2, and the outer surface side on the inner surface side with the interface 1 as a boundary) having the above-described plurality of interfaces. An example of the results of the measurement performed by the Mann spectrum. In Table 2, an example of the peak (the peak near 488 cm ^-1 ) belonging to the planar quaternary ring and the peak attributed to the planar three-membered ring (the peak near 602 cm ^-1 ) of each of the above points is shown.

Table 3 shows the case of the above-described yttria glass crucible 1, and it is understood that the respective structures on the inner surface side, the intermediate portion, and the outer surface side are different at the respective interfaces (interface 1, interface 2). In other words, it is understood that the yttrium oxide glass crucible 1 has a plurality of layer structures in the thickness direction at the boundary of each interface, and it is understood that the yttrium oxide glass crucible 1 having no cracks is difficult to spread.

Hereinabove, the invention of the present application has been described with reference to the above embodiments, but the invention of the present application is not limited to the above embodiments. The configuration and details of the invention of the present application can be variously modified by those skilled in the art within the scope of the invention of the present application.

1‧‧‧Oxide glass

2‧‧‧Laser light source

3‧‧‧Photographing Department

Claims (24)

An apparatus for measuring a flaw, comprising: a light emitting portion that emits a laser beam to a beryllium oxide glass crucible to be measured, the tantalum glass crucible having a cylindrical straight portion having an opening at an upper end; a bottom portion; and a corner portion connecting the side wall portion and the bottom portion and having a larger curvature than the bottom portion, wherein an upper end of the straight cylindrical portion is formed flat; and a scattering condition measuring portion that measures oxidation to the light emitting portion The scattering state of the laser beam incident in the glass crucible in the thickness direction inside the side wall portion of the cerium oxide glass crucible, wherein the scattering state measuring portion is configured to measure the scattering state at each position in the thickness direction of the yttrium oxide glass crucible . The flaw measuring device according to claim 1, wherein the light emitting portion is configured to emit the laser beam from the inner side of the yttrium-glass diaphragm to the thickness direction of the yttrium-glass diaphragm, and the scattering state measuring unit is configured to The direction of the thickness of the laser inside the side wall portion of the yttrium oxide glass crucible is measured from the direction of the annular end surface of the portion of the upper end opening of the portion where the light exit portion is incident on the laser beam. Scattering condition. The flaw measuring device according to claim 1 or 2, wherein the illuminating unit irradiates the yttrium oxide glass crucible with light of a predetermined wavelength corresponding to a wavelength of a laser beam emitted from the light emitting portion, the scattering state The measuring unit is configured to measure the scattering state of the laser light under the illumination of the illumination unit. The flaw measuring device according to any one of claims 1 to 3, wherein the light emitting portion is configured to emit a horizontal laser as the laser. The flaw measuring device according to any one of claims 1 to 4, wherein the light emitting portion is configured to emit a vertical laser as the laser. The flaw measuring device according to any one of claims 1 to 5, wherein the light emitting portion is configured to obliquely emit the laser toward a depth direction of the bismuth glass crucible. The flaw measuring device according to any one of claims 1 to 6, wherein the light emitting portion is configured to emit a laser at a predetermined predetermined interval over a entire circumference of the bismuth oxide glass crucible, the scattering condition measurement The portion is configured to respectively measure the laser corresponding to the light emitted from the light emitting portion The scattering condition of the laser. The flaw measuring device according to any one of claims 1 to 7, wherein the light emitting portion is configured to emit a laser beam of visible light. The flaw measuring device according to any one of claims 1 to 8, wherein the light emitting portion is configured to emit p-polarized light to the yttrium oxide glass so that the incident angle is a Brewster angle. The p-polarized light is polarized light whose direction of vibration of the electric field is parallel to the incident surface. The flaw measuring device according to claim 9, wherein the inner surface shape measuring portion includes a three-dimensional shape of an inner surface of the yttrium oxide glass crucible, and the light emitting portion is based on a measurement result of the inner surface shape measuring portion The angle at which the angle of incidence becomes Brewster's angle is to illuminate the cerium oxide glass. The flaw measuring device according to any one of claims 1 to 10, wherein the light emitting portion is configured to emit a laser beam at each position in a thickness direction of the bismuth oxide glass crucible from an end surface direction of the bismuth oxide glass crucible. The scattering condition measuring unit measures Raman scattering corresponding to the laser beam emitted from the light emitting unit at each of the positions as a scattering state of the laser. A measuring method in which a laser beam is emitted from a yttrium oxide glass crucible as a measuring object, and a scattering state of a laser beam incident into the yttrium oxide glass crucible at each position in a thickness direction inside a side wall portion of the yttrium glass yttrium is measured, Wherein the yttria glass crucible has a cylindrical straight portion having an opening at an upper end; a curved bottom portion; and a corner portion that connects the side wall portion and the bottom portion and has a larger curvature than the bottom portion. The upper end of the straight cylindrical portion is formed flat. The measuring method according to claim 12, wherein the laser is emitted from the inner side of the yttrium oxide glass crucible toward the thickness direction of the yttrium oxide glass crucible, and is incident on the laser from the yttrium oxide glass crucible as a measuring object. The scattering direction of the laser inside the side wall portion of the yttrium oxide glass crucible was measured in the direction of the annular end surface around the upper opening portion. The measuring method according to claim 12 or 13, wherein the yttrium oxide glass ray is irradiated with illumination light of a predetermined wavelength corresponding to a wavelength of the emitted laser light, and the scattering of the laser light is measured under irradiation of the illumination light situation. The measuring method according to any one of claims 12 to 14, wherein a horizontal laser is emitted to the yttrium oxide glass crucible, and each of the horizontal lasers injected into the yttrium oxide glass crucible is measured in the thickness direction of the yttrium oxide glass crucible. The scattering condition at the location. The measuring method according to any one of claims 12 to 15, wherein a vertical laser is emitted from the yttrium oxide glass crucible, and each of the vertical lasers injected into the yttrium oxide glass crucible is measured in the thickness direction of the yttrium oxide glass crucible. The scattering condition at the location. The measuring method according to any one of claims 12 to 16, wherein the laser is obliquely emitted toward a depth direction of the bismuth oxide glass crucible, and the laser incident into the yttrium oxide glass crucible is measured in the yttrium oxide glass. The scattering condition at each position of the thickness direction of the crucible. The measuring method according to any one of claims 12 to 17, wherein the laser is emitted over the entire circumference of the yttrium-glass diaphragm at a predetermined predetermined interval, and the laser corresponding to the emitted laser is separately measured. Scattering condition. The measuring method according to any one of claims 12 to 18, wherein the laser that emits visible light to the yttrium oxide glass crucible measures the laser beam incident on the visible light in the yttrium oxide glass crucible in the thickness direction of the yttrium oxide glass crucible Scattering conditions at various locations. The measuring method according to any one of claims 12 to 19, wherein the three-dimensional shape of the inner surface of the cerium oxide glass crucible is measured, and based on the measurement result, the cerium oxide glass is formed in such a manner that the incident angle becomes the Brewster angle. This shot the laser. The measuring method according to any one of claims 12 to 20, wherein p-polarized light is emitted from the yttrium oxide glass in such a manner that the incident angle becomes the Brewster angle, and the p incident into the yttrium oxide glass crucible is measured. The scattering state of the polarized light at each position in the thickness direction of the bismuth oxide glass crucible, which is the polarized light in the direction in which the vibration direction of the electric field is parallel to the incident surface. The measuring method according to any one of claims 12 to 21, wherein a laser beam is emitted from each end position in the thickness direction of the bismuth oxide glass crucible from an end surface direction of the bismuth oxide glass crucible, and the respective positions are measured at the respective positions. The Raman scattering correspondingly generated by the emitted laser is used as the scattering condition of the laser. The enthalpy measurement method according to any one of claims 12 to 22, wherein the laser is emitted from the inner side of the yttrium oxide glass crucible toward the thickness direction of the yttrium oxide glass yttrium, from the yttrium oxide glass yttrium as a measuring object. Measuring the scattering state of the laser inside the side wall portion of the yttrium oxide glass crucible in the direction of the annular end surface around the upper end opening of the portion of the laser beam, and measuring the pulling based on the measurement result of the scattering condition Man scattering. A method for producing a cerium oxide glass crucible, wherein: The inspection procedure described in any one of claims 12 to 23 is performed.