CN101846498A - Method for determining film thickness and method for manufacturing glass optical element - Google Patents
Method for determining film thickness and method for manufacturing glass optical element Download PDFInfo
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Abstract
Method for determining the film thickness and method for manufacturing a glass optical element. The invention relates to a method for determining the thickness of a film formed on a matrix material. In the method, the thickness of the film for testing is changed, then the following treatment is performed in more than two times: for the film for testing formed on the matrix material for testing with the surface reflectivity (R0) relative to the light with the wavelength (Lamda nanometer), the surface reflectivity (R') of the film for testing relative to the light with the wavelength (Lamda nanometer) is determined, to determine the relation of the thickness of the film for testing and the surface reflectivity change amount (R'-R0), the surface reflectivity (R) of the object relative to the light with the wavelength (Lamda nanometer) is determined, the difference (R-R0) of the surface reflectivity R and the surface reflectivity R0 of the matrix material for testing is taken as the surface reflectivity change amount in the relation, thus the thickness of the film of the object is obtained.
Description
Technical field
The present invention relates to be formed on the film thickness measuring method of the overlay film on the matrix material.
The invention still further relates to the glass optical component manufacture method of using described film thickness measuring method.
Background technology
As the method for making the optical element that lens etc. are made of glass, the known precise punch forming method that has the impact briquetting of utilizing directly to form the optical function face.The precise punch forming method is carried out impact briquetting, thereby is obtained glass optical component by dropping into preformed moulding with glass blank (below, be also referred to as " glass preformed member (glassperform) ") in mould under thermoplastic state.The precise punch forming method is by using precision machined mould, can not need the back processing such as attrition process after the impact briquetting, therefore, can obtain high performance glass lens at an easy rate.
But in the precise punch forming method, the forming surface of glass preformed member and mould is close under the condition of high temperature when impact briquetting, therefore may produce bonding owing to chemical reaction takes place on their interface.
Therefore, in order to prevent the bonding of glass preformed member and mould, proposed to be provided with the technology (with reference to Japanese kokai publication hei 8-217468 communique, Japanese kokai publication hei 8-259241 communique and Japanese kokai publication hei 9-286625 communique) of films such as carbon film on glass preformed member surface.But, at the thickness of described film during, can not fully prevent bonding between glass preformed member and the mould less than predetermined thickness, may crack (crackles of the moulding product that produce during in impact briquetting) on the glass lens of moulding.In addition, when the thickness of described film is blocked up, can have influence on the shrinkage factor of the glass lens of institute's moulding with respect to mould, in other words can have influence on the curvature of glass lens, exist with inferior problem: the shape and the design load deviation of the optical element that obtains by impact briquetting are bigger; And the reactivity of film and glass preformed member sharply uprises, and produces mill flower and outward appearance and significantly worsens.
As mentioned above, we can say in the precise punch forming method that the film that is formed on the glass preformed member is understood the various characteristics that influence the optical element of institute's moulding owing to its thickness largely.In other words, can be by management, estimate the thickness of the film on the glass preformed member, form, come high-quality, obtain the optical element made by precise punch forming at low cost.In addition, be not limited to above-mentioned field, from qualitative control, process management equal angles, the thickness of the overlay film that management, evaluation form on matrix material also is very important.
Usually, as the method for the thickness of estimating (mensuration) film, known have (AtomicForce a Microscope: differential mensuration atomic force microscope), based on XPS (the sub-beam split of X-rayPhotoelectron Spectroscopy:X ray photoelectric) and TOF-SIMS (Time OfFlight-Secondary Ion Mass Spectroscopy: the analysis of spectrum of depth direction flight time type ion microprobe) and based on the optical means of ellipsometer (Ellipsometer) and light transmission based on AFM.In addition, in recent years, also proposed according to the reflectivity spectral in the visible region to as the DLC of carbon-based thin film (Diamond Like Carbon: diamond-like-carbon) thickness of film carry out instrumentation technology (with reference to TOHKEMY 2000-251250 communique), utilize infrared ray absorbing to estimate the technology of the thickness of carbon film (with reference to TOHKEMY 2006-242721 communique), determine the technology (with reference to TOHKEMY 2000-46525 communique) of film thickness according to the reflectivity of the measured value of reflectivity and prediction.
But because surperficial influence, the AFM for curve form and charging property of glass preformed member belongs to destructive inspection, AFM is unfavorable for the thickness that is formed on the lip-deep carbon film of glass preformed member is estimated and managed.In addition, XPS, TOF-SIMS are except existing and the same problem of AFM, and measuring also needs the long time, is not easy method therefore.
Though ellipsometer can non-destructive and carried out instrumentation in short time, same with AFM, XPS, TOF-SIMS, in the restriction of existence in shape of the face of mensuration, this external being seen through under the situation of light as the glass preformed member by film forming face can not be measured thickness.In addition, owing to the absorption of the light of glass preformed member inside, with and the surface be the influence of the lens effect that causes of spherical shape, the light transmission method can not be estimated the thickness of the carbon film that forms on glass preformed member surface.
The method of being put down in writing for above-mentioned TOHKEMY 2000-251250 communique is a relation between minimizing wavelength and the thickness according to the reflectivity in wavelength 330～550 nanometers of resulting reflectivity spectral, calculates the thickness of DLC film.Therefore, in above-mentioned wavelength region may, do not exist under the situation of extreme value of reflectivity, can not measure thickness.
The method of being put down in writing for above-mentioned TOHKEMY 2006-242721 communique, the temperature rising unit that is limited to heating arrangements can provide the situation of uniform heat to tabular surface, and its thickness must be more than the tens μ m, therefore can not estimate the thickness from the nano level carbon film of Ya Nami to tens that (mensuration) forms on glass preformed member surface.
On the other hand, in above-mentioned TOHKEMY 2000-46525 communique, as prior art, the method for calculating thickness according to the difference of the reflectivity before and after the film forming is disclosed.Said method according to the reflection of light rate of each wavelength detection at the visible region of shining from Halogen lamp LED, carries out match (fitting) by spectrophotometer.But Halogen lamp LED and spectrophotometric price are higher, therefore in TOHKEMY 2000-46525 communique, as the method for measuring thickness by the device of cheapness, proposed to utilize the light of a plurality of semiconductor light-emitting elements irradiation different wave lengths and detected value has been carried out fitting method.But this method is carried out match between the measured value of a plurality of reflectivity and predicted value, because be to compare with theoretical reflectivity, therefore the thickness difference that is difficult to the logarithm nanometer owing to its error of calculation is discussed.In addition, carry out fitting method and also have such problem, that is, do not knowing under the situation of about thickness, thickness calculates needs the long time.
As mentioned above, there is following problem in existing film thickness measuring method: be difficult to carry out easy mensuration, there is restriction in applicable overlay film, and lacks versatility etc.
Summary of the invention
Under this situation, the object of the present invention is to provide and a kind ofly can measure thickness and the good film thickness measuring method of versatility that is formed on the overlay film on the matrix material easily.
In order to arrive above-mentioned purpose, the inventor has repeated to study intensively, obtained change at the reflection of light rate of single wavelength and matrix material on the thickness of overlay film between good correlationship set up this neodoxy, further repeat research according to this opinion, the result has finished the present invention.
That is, above-mentioned purpose reaches by following means.
[1] a kind of film thickness measuring method that is formed on the overlay film on the matrix material is characterized in that, this method may further comprise the steps:
Change the thickness of testing with overlay film and carry out twice above following processing: have surface reflectivity R at light for the wavelength X nanometer
0Test with forming described test overlay film on the matrix material, measure the surface reflectivity R ' of this test usefulness overlay film for the light of described wavelength X nanometer, derive thus the thickness of described test usefulness overlay film and surface reflectivity variable quantity (R '-R
0) between relational expression; And
Measure the surface reflectivity R of the overlay film of determining film thickness object, in described relational expression, use this surface reflectivity R and described test surface reflectivity R with matrix material for the light of described wavelength X nanometer
0Difference (R-R
0) as described surface reflectivity variable quantity, ask for the thickness of the overlay film of described determining film thickness object thus.
[2] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, use with the overlay film identical materials of described determining film thickness object and use identical one-tenth embrane method, form described test overlay film.
[3] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, described relational expression be described thickness and described surface reflectivity variable quantity (R '-R
0) between, related coefficient is the linear function that the relation more than 0.6 is set up.
[4] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, the matrix material of overlay film that is formed with described determining film thickness object is by constituting with the matrix material identical materials with described test.
[5] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, described wavelength X nanometer is the scope of 400～750 nanometers.
[6] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, described difference (R-R
0) be more than 0.01.
[7] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, the thickness of the overlay film of described determining film thickness object is the scope of 0.4～40 nanometer.
[8] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, the overlay film of described determining film thickness object is to contain carbon film.
[9] according to [8] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, the described carbon content rate that contains carbon film is more than 65% atomic percent.
[10] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, the matrix material that is formed with the overlay film of described determining film thickness object is made of glass.
[11] according to [1] described film thickness measuring method that is formed on the overlay film on the matrix material, wherein, the surface of matrix material that is formed with the overlay film of described determining film thickness object is plane or curve form.
[12] a kind of glass optical component manufacture method, this method are carried out impact briquetting making preformed and have on the surface under the thermoplastic state of glass blank of overlay film, and the forming surface of transfer printing molded mould is characterized in that thus,
Following glass blank is carried out described impact briquetting, about this glass blank, by each described method in 1 to 11 thickness of described overlay film is measured, the thickness of being measured is in predefined reference range.
[13] a kind of glass optical component manufacture method is characterized in that, this method comprises:
Prepare the operation of glass blank batch, this glass blank batch comprises a plurality of preformed and has the glass blank of overlay film on the surface;
From the described batch of operation of extracting at least one glass blank;
Measure the operation of thickness of the overlay film on the described glass blank surface that extracts by each described method in 1 to 11; And
By in thermoplastic carry out impact briquetting under the state of following glass blank, come the operation of the forming surface of transfer printing molded mould, the glass blank of the thickness of this glass blank and described mensuration in predefined reference range is in same batch.
According to the present invention, can non-destructive ground and easily measure the thickness that is formed on the overlay film on the substrate.
Description of drawings
Fig. 1 illustrates the relation between the thickness of the reflectance varies amount of embodiment 1 and carbon film.
Fig. 2 is illustrated in the thickness of the carbon film that calculates among the embodiment 1 and the relation between the film formation time.
Fig. 3 illustrates the relation between the thickness of the reflectance varies amount of embodiment 2 and carbon film.
Fig. 4 is illustrated in the thickness of the carbon film that calculates among the embodiment 2 and based on the relation between the determining film thickness value of AFM.
Fig. 5 is the reflectivity spectral that utilizes reference example 1 to obtain.
Fig. 6 is illustrated in the film thickness distribution that is formed on the carbon film on the preformed member among the embodiment 3.
Fig. 7 is illustrated in the film thickness distribution that is formed on the carbon film on the preformed member among the embodiment 4.
Embodiment
[film thickness measuring method]
The present invention relates to be formed on the film thickness measuring method (following also be called " film thickness measuring method " or " assay method ") of the overlay film on the matrix material.
Assay method of the present invention comprises following operation:
(1) changes the thickness of testing with overlay film and carry out twice above following processing: have surface reflectivity R at light at the wavelength X nanometer
0Test with on the matrix material, form described test overlay film, measure this test with the surface reflectivity R ' of overlay film at the light of described wavelength X nanometer, derive thus described test with the thickness of overlay film and surface reflectivity variable quantity (R '-R
0) between relational expression (below be called " relational expression derivation operation "); And
(2) measure the surface reflectivity R of the overlay film (following also be called " determination object overlay film ") of determining film thickness object, in described relational expression, use this surface reflectivity R and described test surface reflectivity R with matrix material at the light of described wavelength X nanometer
0Between difference (R-R
0) as described surface reflectivity variable quantity, ask for the thickness (below be called " thickness calculation process ") of the overlay film of described determining film thickness object thus.
Below, the details of each operation is described successively.
Relational expression derives operation
In this operation, change the thickness of testing with overlay film and carry out twice above following processing: have surface reflectivity R at light at the wavelength X nanometer
0Test with on the matrix material, form described test overlay film, measure this test with the surface reflectivity R ' of overlay film at the light of described wavelength X nanometer.Thus can mark and draw on the curve map more than 2 about the known test of thickness with the thickness of overlay film and surface reflectivity variable quantity (R '-R
0) between relation, therefore can be for example by this curve of least square fitting, thus as linear function try to achieve test with the thickness of overlay film and surface reflectivity variable quantity (R '-R
0) between relational expression.The relational expression of trying to achieve like this can be used as in thickness calculation process described later at the thickness of the overlay film of thickness the unknown and the inspection amount line between the reflectivity.In the method that aforesaid TOHKEMY 2000-46525 communique is put down in writing, need carry out match at each detection of reflected rate of a plurality of wavelength, relative therewith, only use reflection of light rate in the present invention at single wavelength, therefore simpler and easy, and, therefore can carry out the higher mensuration of reliability because error of fitting is considerably less.
Can measure into test matrix material and each test surface reflectivity of overlay film of membrane stage by following apparatus for measuring reflectance, this apparatus for measuring reflectance is the device that can measure reflectivity by the interference light optical spectroscopy, particularly, this apparatus for measuring reflectance has optical projection unit, reflected light light receiving unit and analytic unit thereof, can detect and analyze determined the reflection of light rate characteristic at irradiation.Apparatus for measuring reflectance can utilize object lens to make irradiates light become small luminous point (for example about Φ 60 μ m), even because also reflected illumination light vertically of determined curved surface, no matter therefore how determined shape can both carry out the mensuration of reflectivity, this is desirable.In addition, if can then can only measure determined reflectivity exactly, be preferred therefore by as device from determined reflection of light light (for example back reflected light) in addition.And,, then can carry out high speed and measure if having the device of a flat burnt grating (diffraction grating) and line sensor.As this device, can enumerate the USPM-RU of for example Olympus Corp's manufacturing, the SBFM-R that Shibuya Optical Co., Ltd makes etc.
In the reflectivity spectral that obtains by measuring reflectance, can ask for into the test matrix material and the surface reflectivity of each overlay film of membrane stage by reading the reflectivity of wavelength X nanometer at the light of wavelength X nanometer.Described wavelength X nanometer is not particularly limited, and can particularly, preferably be in the scope of 400～750 nanometers by the visible region of common apparatus for measuring reflectance mensuration but preferably be in.
In order to carry out the high mensuration of reliability, the preferred use and the determination object overlay film identical materials of asking for thickness in thickness calculation process described later forms test and uses overlay film, and use same one-tenth embrane method to carry out in the present invention.Describe filmogen and film build method below in detail.
For derive test with the thickness of overlay film and surface reflectivity variable quantity (R '-R
0) between relational expression, need to mark and draw two points at least.Therefore, in this operation, change the thickness of testing with overlay film and carry out testing with overlay film to the operation of measuring surface reflectivity from forming more than twice.In order to improve the mensuration precision, preferably aforesaid operations is carried out 3～4 times or more.
To be formed on test with the test on the matrix material thickness of overlay film and the relational expression between the surface reflectivity variable quantity in order deriving, to need the value of test with the thickness of overlay film.Though can use the thickness of when film forming, setting as the thickness that is used to derive the above-mentioned relation formula,, preferably test be measured with the thickness of overlay film in order to improve the mensuration precision.Can come test is measured with the thickness of overlay film by known determining film thickness means such as AFM, XPS.As above aforementioned, AFM, XPS etc. is not suitable as the determining film thickness means of the lip-deep overlay film that is formed on curve form.Therefore, in order to carry out determining film thickness by above-mentioned known determining film thickness means, preferred test is the plane with the surface of matrix material.
According to more than, use overlay film at each test, asked for the value of thickness and surface reflectivity variable quantity (R '-R
0) value.Next, for example be with the longitudinal axis thickness, transverse axis be the surface reflectivity variable quantity (R '-R
0) chart in mark and draw each value, and carry out match by least square method etc., can be used as thus linear function (particularly, following formula 1) try to achieve test with the thickness of overlay film and surface reflectivity variable quantity (R '-R
0) between relational expression.
(in formula 1, a and b are the constants of obtaining by match respectively.)
Statistically, use the index of related coefficient usually, the following correlation intensity that illustrates at the related coefficient scope as the relevance intensity of two variablees of expression.
0～0.2 is relevant hardly
0.2～0.4 is relevant a little
0.4～0.7 is quite relevant
0.7～1 is relevant strongly
If related coefficient is more than 0.4, then we can say between two variablees to have relevance.Usually, under situation, be judged to be " experimental technique existing problems " mostly by rule of thumb less than 0.6 related coefficient.But " related coefficient is more than 0.6 " is empirical value, from view angle of statistics, even we can say more than 0.4 also no problem.In the present invention, in above-mentioned linear function, thickness and surface reflectivity variable quantity (R '-R
0) between, for example related coefficient is that the relation of (even more than 0.6) more than 0.4 can be set up.
The thickness calculation process
This operation is such operation: will derive the relational expression that obtains in the operation in aforementioned relational expression and measure line as inspection, and ask for the thickness of the overlay film of thickness the unknown by this simple and easy method of measuring reflectance.Can with aforementioned mensuration of similarly carrying out the determination object overlay film at the surface reflectivity R of the light of wavelength X nanometer.And, by derive in the relational expression that derives in the operation surface reflectivity R that application is measured and the described test surface reflectivity R of matrix material in relational expression
0Between difference (R-R
0) as described surface reflectivity variable quantity promptly (R '-R
0), can calculate the thickness of determination object overlay film thus.Described difference (R-R
0) big more, the error of measuring reflectance is more little, can realize high sensitivity more.From this viewpoint, described difference (R-R
0) be preferably more than 0.01, more preferably more than 0.1.Though also depend on the material of determination object overlay film and matrix material, but if the combination of common matrix material and overlay film, if the above thickness of 0.4 nanometer, then can become described preferred difference, therefore preferably apply the present invention to the film thickness measuring method that thickness is the above overlay film of 0.4 nanometer.In addition, from measuring the viewpoint of precision, preferably the overlay film below thickness 40 nanometers is used assay method of the present invention.From the viewpoint of high sensitivity/high-precision measuring, preferred pin is the overlay film of 0.4～20 nanometer to thickness, uses assay method of the present invention.According to assay method of the present invention, can carry out above-mentioned nano level determining film thickness.
In addition, for the matrix material that is formed with the determination object overlay film, preferred pin is identical with matrix material with test to the surface reflectivity of the light of wavelength X nanometer, considers from this respect, and preferred the utilization with test constitutes with the matrix material identical materials.But, use under the different situation of matrix material with test at the surface reflectivity of the light of wavelength X nanometer at the matrix material that forms the determination object overlay film, if in described relational expression, use the corrected value that the difference of surface reflectivity is proofreaied and correct, then can carry out the higher mensuration of reliability.
According to the present invention, can derive operation and thickness calculation process by implementing relational expression discussed above, measure the thickness of the overlay film of the thickness the unknown that is formed on the various matrix materials.
The concrete mode and the optimal way of assay method of the present invention then, are described.
No matter the material of the material of matrix material and shape, overlay film and thickness all can be used assay method of the present invention.For example, the matrix material that constitutes by various materials such as glass, metal, plastics can be enumerated,, various overlay films such as carbon based coating, metal nitride based coating, metal carbide based coating can be enumerated as overlay film as matrix material.The overlay film of determination object can form by one-tenth embrane methods such as vapour deposition method, sputtering method or ion plating methods.In addition, as previously mentioned, from measuring the angle of precision, preferred use with determination object overlay film identical materials with identical become embrane method to form to test use overlay film.Herein, " identical materials " for example is the filmogen with identical component, and " identical one-tenth embrane method " is the one-tenth embrane method of identical type, do not require identical membrance casting condition.But in order to carry out the high mensuration of reliability, the preferred utilization membrance casting condition identical with the determination object overlay film forms the test overlay film.
In measuring reflectance, can carry out mensuration as previously mentioned based on small luminous point.Thus, utilize the assay method of the present invention of measuring reflectance can measure the thickness of the overlay film on the matrix material of different shapes such as being formed on flat shape, curve form.Therefore, according to assay method of the present invention, can measure for AFM, XPS etc. measure difficulty, go up the thickness that contains film such as carbon film that forms at preformed glass blank (glass preformed member).
Below, explanation can be used the glass preformed member of assay method of the present invention and the film on this preformed member.But assay method of the present invention is not limited to mode as described below.
Above-mentioned glass preformed member for example is spherical shape, flat curve form such as spherical or tabular etc., and its shape is not particularly limited as mentioned above.The film on glass preformed member surface can form by one-tenth embrane methods such as vapour deposition method, sputtering method or ion plating methods.
As the film on the glass preformed member, known have the carbon film of containing, metal nitride films, a metal carbide film etc.Assay method of the present invention can be applicable to above-mentioned any one film, but for can carry out and the reflectivity of glass surface between the high-precision measuring that differs greatly, preferred carbon containing overlay film.Contain carbon film except carbon, can also comprise other materials such as hydrogen, but from the reflection differences this point of glass surface, preferred carbon content rate is more than 65% atomic percent, more preferably more than 80% atomic percent, 80～100% atomic percents more preferably.In addition, describedly containing that the existence of carbon is not particularly limited in the carbon film, can only be graphitic carbon, can only be agraphitic carbon also, can also be the material that comprises both.As previously mentioned, the above-mentioned thickness that contains carbon film is preferably more than 0.4 nanometer, below 40 nanometers, more preferably the scope of 0.4～20 nanometer.
[manufacture method of glass optical component]
The glass optical component manufacture method of the present invention's first mode (below be called " method for making 1 "), this method is carried out impact briquetting making preformed and have on the surface under the thermoplastic state of glass blank of overlay film, the forming surface of transfer printing molded mould is characterized in that thus
Following glass blank is carried out described impact briquetting, about this glass blank, by assay method of the present invention the thickness of described overlay film is measured, the thickness of being measured is in predefined reference range.
The glass optical component manufacture method of the present invention's second mode (below be called " method for making 2 ") comprises following operation:
Prepare the operation of glass blank batch, this glass blank batch comprises a plurality of preformed and has the glass blank of overlay film on the surface;
From the described batch of operation of extracting at least one glass blank;
Measure the operation of thickness of the overlay film on the described glass blank surface that extracts by assay method of the present invention; And
By in thermoplastic carry out impact briquetting under the state of following glass blank, come the operation of the forming surface of transfer printing molded mould, the glass blank of the thickness of this glass blank and described mensuration in predefined reference range is in same batch.
Below, be called manufacture method of the present invention in conjunction with method for making 1 and method for making 2.
The glass blank that 1 pair of method for making has confirmed to be formed with the overlay film of expectation thickness by assay method of the present invention applies impact briquetting.On the other hand, the glass blank of sampling carries out determining film thickness by assay method of the present invention in 2 pairs from same batch of the method for making, and the glass blank of glass blank in same batch with the overlay film of having confirmed to be formed with the expectation thickness applied impact briquetting.Method for making 1 is the mode of carrying out so-called exhaustive test, and method for making 2 is to carry out the mode that what is called is taken a sample to check.
In any one of method for making 1,2, described overlay film can be the film that forms in order to improve release property.As illustrated before, do not form at the film that is provided with in order to improve release property on the glass blank under the situation of expectation thickness, may bring harmful effect to the various characteristics of the glass optical component of moulding.To this, in any one of method for making 1,2, after having confirmed to be formed with the overlay film of expectation thickness, carry out impact briquetting, so can make high-quality glass optical component.
Below, illustrate in greater detail manufacture method of the present invention.
Described glass blank can be pre-formed as shapes such as ball shape, flat spherical, tabular.But the glass blank that uses in manufacture method of the present invention is not limited to these shapes.In addition, will from melten glass, flow out predetermined weight and hot-forming after the glass blank of above-mentioned shape directly offer impact briquetting, therefore this method is preferred easily and economically.In addition, manufacture method of the present invention is suitable for just can obtaining the precise punch forming method of glass optical component as the grinding step etc. of the shape approximation that need not to be provided with the glass optical component that makes moulding, but also can carry out subsequent handling such as grinding, grinding and obtain glass optical component after impact briquetting.
As the overlay film that is formed on described glass blank surface, preferably contain carbon film.Its details as previously mentioned.
In manufacture method of the present invention, following glass blank is implemented impact briquetting, this glass blank carry out exhaustive test (method for making 1) according to assay method of the present invention or take a sample to check (method for making 2) thus confirmed to be formed with the overlay film of expectation thickness.Here, be used to select the reference range of the thickness of glass blank to be not particularly limited, as long as set according to the shape of the material of glass blank to be formed, impact briquetting condition and optical element to be formed etc.
As the mould that uses when the impact briquetting, can still preferably have abundant thermotolerance and rigidity, careful material is carried out the mould that Precision Machining forms without any restrictedly using the mould that in the moulding of common glass optical component, uses.For example can enumerate metals such as silit, silicon nitride, tungsten carbide, aluminium oxide, titanium carbide, stainless steel, or on these surfaces, cover the mould of mold release film such as carbon, heating resisting metal, precious metal alloys, carbonide, nitride, boride.
Mold release film as the forming surface that covers mould from the angle of release property, preferably contains carbon film.Contain carbon film as this, the preferred use by what the single component layer of noncrystalline and/or crystalline or mixolimnion constituted contains carbon film, contains carbon film by what graphite and/or adamantine single component layer or mixolimnion constituted.This carbon film can use methods such as sputtering method, plasma CVD method, CVD method, ion plating method to come film forming.Assay method of the present invention also is suitable for the film thickness measuring method as the mold release film on this mould forming surface.
Impact briquetting in the manufacture method of the present invention can utilize known approaches to carry out.Be 10 preferably by the viscosity that heats, softens to glass blank
5～10
10The temperature range of dPas is used bed die glass blank is pushed, thereby the forming surface of mould is transferred on the glass blank up and down.Also can in mould, import glass blank, after making glass blank and mould be warmed up to the said temperature scope simultaneously or making glass blank and mould be warmed up to the said temperature scope respectively, glass blank is configured in the mould.In addition, also can adopt following operation: in advance glass blank is heated to respectively and is equivalent to 10
5～10
9The temperature of dPas viscosity, mould is heated to be equivalent to glass viscosity be 10
9～10
12The temperature of dPas, impact briquetting immediately after mould is supplied with glass blank.At this moment, the temperature variation of mould can be smaller, therefore has following effect: can shorten the intensification/cooling cycle of shaped device, and can suppress because the deterioration that the heating of mould causes.No matter which kind of situation preferably, begins to cool down, uses suitable load program when impact briquetting begins or after the beginning, while and be maintained in and lower the temperature being close to of profile and glass blank.Afterwards, the optical element behind the stripping forming can be taken out.Calcining temperature preferably is made as and is equivalent to glass viscosity 10
12.5～10
13.5The temperature of dPas.
Manufacture method of the present invention can be effectively applied to make optical elements such as lens, catoptron, grating, prism, lenticule, laminated diffraction optical elements.And, can be applicable to glass types of the present invention and there is no particular restriction.Especially, effectively to be applied to crackly borate-based glass, phosphate-based glass, borophosphate be that glass, fluorophosphate are glass etc. in the present invention.
[embodiment]
Below, further specify the present invention by embodiment, but the invention is not restricted to the mode shown in the embodiment.The USPM-RU that the measuring reflectance of the following stated is to use Olympus Corp to make carries out.
The embodiment of determining film thickness
[embodiment 1]
Relational expression derives operation
At first, on this ground flat of the glass substrate with ground flat, obtain the reflectivity spectral of visible region.
Then, on the ground flat of above-mentioned glass substrate, repeat 4 operations, after each film forming by the DC sputtering method formation carbon film of use argon, reflectivity spectral to the visible region of the carbon film surface after the film forming is measured, and carries out the determining film thickness based on XPS.
From the reflectivity spectral that obtains, read the reflectivity of wavelength 500 nanometers, 600 nanometers, 700 nanometers, calculate under each wavelength and the difference between the reflectivity of the ground flat of glass substrate, as the reflectance varies amount.
Fig. 1 illustrates the relation between the thickness of the reflectance varies amount that obtains by above processing and carbon film.
According to the result of Fig. 1 as can be known, no matter how measure wavelength, linear relation establishment between thickness and the reflectance varies amount.
Therefore, by least square method the data point of Fig. 1 medium wavelength 500 nanometers is carried out match after, obtain following relational expression (formula A ').Similarly, the result who the data point of wavelength 600 nanometers, wavelength 700 nanometers is carried out match by least square method has been expressed on the right side among Fig. 1.
Formula A ' reflectance varies amount=0.4651 * thickness-0.3583
Shown in the right side among Fig. 1 table, each measures thickness on the wavelength and relational expression between the reflectance varies amount, and to become the related coefficient that can judge good correlationship establishment be linear function more than 0.6.
Then, above-mentioned formula A ' is out of shape, obtains following relational expression (formula A).
Formula A thickness (nanometer)=2.15 * reflectance varies amount (point)+0.77
The thickness calculation process
By constituting, carried out to use and above-mentioned (1) identical filmogen on the abrasive surface of glass substrate of identical milled processed with above-mentioned glass substrate identical materials, utilize the DC sputtering method, form the carbon film of different thickness by the change film formation time.At each carbon film, measure reflectivity spectral, on the spectrum that obtains, read the reflectivity of wavelength 500 nanometers.Then, from the reflectivity that reads out, deduct the reflection of light rate on the ground flat of the glass substrate that in above-mentioned (1), determines, calculate difference at wavelength 500 nanometers.The difference that calculates is updated to formula A as " reflectance varies amount ", calculates thickness.Fig. 2 illustrates the thickness that calculated and the relation between the film formation time.
Knownly generally in sputtering method, show as linear relation between thickness and the film formation time.As shown in Figure 2, the thickness that uses formula A to obtain shows as positive correlation with respect to film formation time, when its related coefficient is 0.995, shows as extraordinary value.Can confirm according to this result, can carry out the high determining film thickness of reliability by assay method of the present invention.
In addition, about glass preformed member surface having been carried out the face of plane lapping, carried out determining film thickness and determining film thickness based on reflectivity same as described above based on AFM after, related coefficient performance is good value.
[embodiment 2]
Relational expression derives operation
Except becoming embrane method changes to the vacuum vapour deposition this point from sputtering method, carry out 1 identical operations with embodiment, obtain the reflectance varies amount of carbon film under wavelength 500 nanometers and the relation between the thickness.Fig. 3 illustrates resulting result.As shown in Figure 3, same with the embodiment 1 that uses sputtering method, linear relation is set up between reflectance varies amount and thickness.After by least square method the data point among Fig. 3 being carried out match, obtain following relational expression (formula B ').
Formula B ' reflectance varies amount=0.7194 * thickness-0.2374
As shown in Figure 3, the related coefficient of above-mentioned formula B ' is (a related coefficient: 1), therefore can be judged as correlationship good between thickness and reflectance varies amount and set up more than 0.6.
Then, above-mentioned formula B ' is out of shape, obtains following relational expression (formula B).
Formula B thickness (nanometer)=1.39 * reflectance varies amount (point)+0.33
The thickness calculation process
On abrasive surface by the glass substrate that constitutes, carried out identical milled processed with the glass substrate identical materials of in above-mentioned (1), carrying out measuring reflectance, use and above-mentioned (1) identical filmogen, utilize vacuum vapour deposition, by changing the carbon film that film formation time forms different thickness.At each carbon film, behind the determining film thickness that has carried out based on AFM, measure reflectivity spectral, on the spectrum that obtains, read the reflectivity of wavelength 500 nanometers.Then, from the reflectivity that reads, deduct in above-mentioned (1) on the ground flat of the glass substrate of measuring, calculate difference at the reflection of light rate of wavelength 500 nanometers.The difference that calculates is updated to formula B as " reflectance varies amount ", calculates thickness.Fig. 4 illustrates the thickness that calculated and based on the relation between the determining film thickness value of AFM.In Fig. 4, transverse axis is based on the determining film thickness value of AFM, and the longitudinal axis is the thickness that through type B calculates.According to Fig. 4 as can be known, 1: 1 relation of between is set up, and its related coefficient is 0.975 o'clock, shows as extraordinary correlationship.Also can confirm according to this result, can carry out the high determining film thickness of reliability by assay method of the present invention.
According to above result as can be known, can be by asking for thickness and any reflectance varies amount under the wavelength in advance, and it is made as inspection amount line, thus utilize the non-contacting method of this non-destruction of measuring reflectance to measure the thickness of various overlay films.In addition, under the normal temperature, even beyond the mensuration face plane, also can carry out measuring reflectance in atmosphere, assay method therefore of the present invention is very useful as easy film thickness measuring.
[reference example]
Fig. 5 illustrates the reflectivity spectral by the visible region of the carbon film with different thickness of sputtering film-forming.In Fig. 5, legend is the thickness by the carbon film of XPS mensuration.According to Fig. 5 as can be known, the reflectivity under each wavelength is according to the thickness of carbon film and difference.In addition, in spectrum shown in Figure 5, in measuring the zone, there is not minimal value, therefore can't carries out determining film thickness by the method for putting down in writing in the aforesaid TOHKEMY 2000-251250 communique.
2. the embodiment that makes of glass optical component
[embodiment 3]
By following method, the manufacturing edge thickness is 0.6 millimeter a male bend moon lens.
As glass material, use boric acid group of the lanthanides glass (the glass model M-LAC 130 that HOYA (Co., Ltd.) makes), by the hot-forming preformed member that is shaped to intended shape made from curved surface.
Different with the making of preformed member, the flat board (glass substrate) that will be made of the glass material identical with preformed member is as the test matrix material, form the carbon film (test use overlay film) of different thickness by sputtering method, utilization and embodiment 1,2 same methods derive the relational expression between thickness and the reflectance varies amount (having estimated the surface reflectivity under wavelength 500 nanometers).In addition, confirmed that test shows as and the surface reflectivity identical value of preformed member surface at the light of wavelength 500 nanometers with the surface reflectivity of matrix material at the light of wavelength 500 nanometers.
Then, use and the test identical filmogen of overlay film, form the carbon film on the preformed member surface that makes by sputtering method.Adjust thickness by changing film formation time, every same film formation time is made 10 preformed members.At each preformed member, by measuring the surface reflectivity under wavelength 500 nanometers, value substitution above-mentioned relation formula that will (surface reflectivity of the surface reflectivity that determines-test usefulness matrix material) calculates the thickness of the carbon film on each preformed member thus.Fig. 6 illustrates the film thickness distribution of carbon film.In addition, the process capability index of the thickness that is calculated according to the thickness scope of the suitable overlay film of thickness calculated value that obtains and said lens is 0.171.
Afterwards, each preformed member of punching press and to make edge thickness be 0.6 millimeter the male bend moon behind the lens is if the thickness of carbon film is less than 2 nanometers then crack on lens, if surpass 5 nanometers then produce the mill flower on the lens that obtain.Therefore, we can say that the thickness that is suitable for the carbon film handled at stamping procedure in the manner is 2～5 nanometers.On the other hand, as shown in Figure 6, the thickness scope of carbon film is 1～6 nanometer.Although each film formation time has been implemented the film forming processing to 10 preformed members, but as shown in Figure 6, the preformed member of thickness 3 nanometers is maximum, and the thickness of carbon film has surpassed the scope that is suitable for handling in stamping procedure for the preformed member of a part, hence one can see that, preferably carried out exhaustive test in the manner before stamping procedure.
Therefore, utilize method same as described above to carry out the thickness calculating (exhaustive test) of the film forming and the use relational expression of the making of preformed member, carbon film, only to select the thickness calculated value be the preformed member of 2～5 nanometers and handle in stamping procedure, as a result, can not observe crackle or mill flower in the lens after which moulding.In order to reference, the preformed member of not selecting is carried out punching press, if thickness less than 2 nanometers then crack and be difficult to continue punching press, produces the mill flower on lens if thickness surpasses 5 nanometers on lens, in order to deliver, need to remove the operation of mill flower as product.
[embodiment 4]
By following method, manufacturing center's thickness is 2.6 millimeters biconvex lens.
As glass material, using borosilicate is glass (the glass model M-BACD 12 that HOYA (Co., Ltd.) makes), by the hot-forming preformed member that is shaped to the intended shape with curved surface of making.
Different with the making of preformed member, the flat board (glass substrate) that will be made of the glass material identical with preformed member is as the test matrix material, form the carbon film (test use overlay film) of different thickness by sputtering method, utilization and embodiment 1,2 same methods derive the relational expression between thickness and the reflectance varies amount (having estimated the surface reflectivity under wavelength 500 nanometers).In addition, confirmed that test shows as and the surface reflectivity identical value of preformed member surface at the light of wavelength 500 nanometers with the surface reflectivity of matrix material at the light of wavelength 500 nanometers.
Then, use and the test identical filmogen of overlay film, form the carbon film on the preformed member surface that makes by sputtering method.Adjust thickness by changing film formation time, every same film formation time is made 10 preformed members.At each preformed member,,, calculate the thickness of the carbon film on each preformed member thus with the value substitution above-mentioned relation formula of (surface reflectivity of being measured-test surface reflectivity of matrix material) by measuring the surface reflectivity under wavelength 500 nanometers.Fig. 7 illustrates the film thickness distribution of carbon film.As shown in Figure 7, the film thickness distribution of carbon film is 2～6 nanometers.In addition, the process capability index of the thickness that is calculated according to the thickness scope of the suitable overlay film of thickness calculated value that obtains and said lens is 1.409.
Afterwards, the biconvex lens that each preformed member of punching press and manufacturing center's thickness are 2.6 millimeters, the result can not observe crackle or mill flower in which lens.Like this according to above-mentioned membrance casting condition; can form the carbon film that does not crack and grind colored thickness; process capability index has also surpassed can be judged as 1.33 of the good common reference value of conduct; hence one can see that; taking a sample to check in the manner gets final product, and does not carry out the determining film thickness based on exhaustive test.
Therefore, utilize method same as described above to carry out the making of preformed member and the film forming of carbon film, extract several preformed members from same batch, use the thickness of described relational expression to calculate, confirm to have formed thickness and be after the carbon overlay film of 2～5 nanometers, in stamping procedure, use each preformed member, can not observe crackle or mill flower in the lens after any moulding.
According to the result of embodiment 3 discussed above and 4 as can be known, at the exhaustive test that has carried out overlay film or after taking a sample to check, in stamping procedure, only use certified products, can access the not high-quality glass optical component of mill flower and crackle thus by the present invention.
Utilizability on the industry
The present invention can be used for thickness evaluation and the control of film thickness of film in forming.
Claims (13)
1. a film thickness measuring method that is formed on the overlay film on the matrix material is characterized in that, this method may further comprise the steps:
Change the thickness of testing with overlay film and carry out twice above following processing: have surface reflectivity R at light for the wavelength X nanometer
0Test with forming described test overlay film on the matrix material, measure the surface reflectivity R ' of this test usefulness overlay film for the light of described wavelength X nanometer, derive thus the thickness of described test usefulness overlay film and surface reflectivity variable quantity (R '-R
0) between relational expression; And
Measure the surface reflectivity R of the overlay film of determining film thickness object, in described relational expression, use this surface reflectivity R and described test surface reflectivity R with matrix material for the light of described wavelength X nanometer
0Difference (R-R
0) as described surface reflectivity variable quantity, ask for the thickness of the overlay film of described determining film thickness object thus.
2. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1 wherein, uses with the overlay film identical materials of described determining film thickness object and uses identical one-tenth embrane method, forms described test overlay film.
3. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, described relational expression be described thickness and described surface reflectivity variable quantity (R '-R
0) between, related coefficient is the linear function that the relation more than 0.6 is set up.
4. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, the matrix material of overlay film that is formed with described determining film thickness object is by constituting with the matrix material identical materials with described test.
5. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, described wavelength X nanometer is the scope of 400～750 nanometers.
6. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, described difference (R-R
0) be more than 0.01.
7. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, the thickness of the overlay film of described determining film thickness object is the scope of 0.4～40 nanometer.
8. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, the overlay film of described determining film thickness object is to contain carbon film.
9. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 8, wherein, the described carbon content rate that contains carbon film is more than 65% atomic percent.
10. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, the matrix material that is formed with the overlay film of described determining film thickness object is made of glass.
11. the film thickness measuring method that is formed on the overlay film on the matrix material according to claim 1, wherein, the surface of matrix material that is formed with the overlay film of described determining film thickness object is plane or curve form.
12. a glass optical component manufacture method, this method are carried out impact briquetting making preformed and have on the surface under the thermoplastic state of glass blank of overlay film, the forming surface of transfer printing molded mould is characterized in that thus,
Following glass blank is carried out described impact briquetting, about this glass blank, by each described method in the claim 1 to 11 thickness of described overlay film is measured, the thickness of being measured is in predefined reference range.
13. a glass optical component manufacture method is characterized in that, this method comprises:
Prepare the operation of glass blank batch, this glass blank batch comprises a plurality of preformed and has the glass blank of overlay film on the surface;
From the described batch of operation of extracting at least one glass blank;
Measure the operation of thickness of the overlay film on the described glass blank surface that extracts by each described method in the claim 1 to 11; And
By in thermoplastic carry out impact briquetting under the state of following glass blank, come the operation of the forming surface of transfer printing molded mould, the glass blank of the thickness of this glass blank and described mensuration in predefined reference range is in same batch.
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| JP2009-078163 | 2009-03-27 |
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| CN111895902A (en) * | 2020-07-20 | 2020-11-06 | 苏州大学 | A kind of ultra-thin transparent carbon nanofiber membrane flexible strain sensor and preparation method thereof |
| CN111895902B (en) * | 2020-07-20 | 2022-04-22 | 苏州大学 | Ultrathin transparent carbon nanofiber membrane flexible strain sensor and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2010230472A (en) | 2010-10-14 |
| JP5294938B2 (en) | 2013-09-18 |
| CN101846498B (en) | 2013-01-30 |
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