CN116479525B - Method for producing low-oxygen crystal bar - Google Patents
Method for producing low-oxygen crystal bar Download PDFInfo
- Publication number
- CN116479525B CN116479525B CN202310745487.5A CN202310745487A CN116479525B CN 116479525 B CN116479525 B CN 116479525B CN 202310745487 A CN202310745487 A CN 202310745487A CN 116479525 B CN116479525 B CN 116479525B
- Authority
- CN
- China
- Prior art keywords
- cylinder
- heat preservation
- crucible
- insulation
- heater
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000001301 oxygen Substances 0.000 title claims abstract description 68
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 68
- 239000013078 crystal Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 39
- 238000009413 insulation Methods 0.000 claims description 102
- 238000004321 preservation Methods 0.000 claims description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 49
- 239000010410 layer Substances 0.000 description 41
- 239000007788 liquid Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The embodiment of the application provides a method for producing a low-oxygen crystal bar, and relates to the technical field of single crystal silicon bar production. The method for producing the low-oxygen crystal bar comprises the following steps: the number of layers of the heat-insulating cylinder felts on the upper heat-insulating cylinder is increased, so that the difference of the number of layers of the heat-insulating cylinder felts on the upper heat-insulating cylinder and the lower heat-insulating cylinder is reduced to 2-3 layers, and the number of layers of the heat-insulating cylinder felts on the middle heat-insulating cylinder is increased, so that the number of layers of the heat-insulating cylinder felts on the middle heat-insulating cylinder and the lower heat-insulating cylinder felts is equal, and the oxygen content in the monocrystalline silicon rod can be reduced on the basis of control cost.
Description
Technical Field
The application relates to the technical field of monocrystalline silicon rod production, in particular to a method for producing a low-oxygen crystal rod.
Background
In the process of producing the single crystal silicon rod, oxygen in the single crystal silicon rod is mainly brought in by a quartz crucible, silicon dioxide in the quartz crucible reacts with silicon raw materials to generate SiO gas volatile matters, wherein 99 percent of SiO is volatilized in a gas form, a part of oxygen enters a melt to cause the oxygen content in the single crystal silicon rod to rise, and the higher the temperature is, the more violent the reaction is, and the higher the content of precipitated oxygen is.
At present, the main mode of oxygen reduction is to reform a thermal field part in a single crystal furnace, but the thermal field part is reformed and needs to be reprocessed, so that the labor force is increased, and the production cost is greatly increased due to the fact that a large number of thermal field parts are replaced.
Disclosure of Invention
The object of the present application includes, for example, providing a method for producing a low oxygen ingot, which is capable of reducing the oxygen content in a single crystal silicon rod on the basis of control costs.
Embodiments of the application may be implemented as follows:
the embodiment of the application provides a method for producing a low-oxygen crystal bar, which is applied to a single crystal furnace, wherein the single crystal furnace comprises a furnace body, a crucible, a heater, a guide cylinder, a heat preservation cover, an upper heat preservation cylinder, a middle heat preservation cylinder and a lower heat preservation cylinder, wherein the upper heat preservation cylinder, the middle heat preservation cylinder and the lower heat preservation cylinder are sequentially arranged in the furnace body from top to bottom, the heat preservation cover is arranged at the top of the upper heat preservation cylinder, and the guide cylinder is arranged on the heat preservation cover;
a supporting ring is arranged between the upper heat preservation cylinder and the middle heat preservation cylinder, the crucible is arranged in a cavity surrounded by the upper heat preservation cylinder, the middle heat preservation cylinder and the lower heat preservation cylinder in a lifting manner, the heater is arranged in the furnace body, the top of the heater is lower than the supporting ring, the distance between the top of the heater and the supporting ring is 20-30mm, the bottom of the crucible is provided with a chamfering part, and the chamfering part is lower than the top of the heater; at least one layer of heat insulation felt is arranged on the inner bottom wall of the furnace body, and the lower heat insulation cylinder is supported on the heat insulation felt; and/or the bottom of the heater is provided with a graphite electrode ring; and/or the inner walls of the upper heat preservation cylinder, the middle heat preservation cylinder and the lower heat preservation cylinder are provided with a plurality of layers of heat preservation cylinder felts; the method for producing the low-oxygen crystal bar comprises the following steps:
increasing the number of layers of the insulation cylinder felts on the upper insulation cylinder to reduce the number of layers of the insulation cylinder felts on the upper insulation cylinder and the lower insulation cylinder to 2-3 layers, and increasing the number of layers of the insulation cylinder felts on the middle insulation cylinder to make the number of layers of the insulation cylinder felts on the middle insulation cylinder and the lower insulation cylinder equal;
the crucible rotation is reduced to 4-5 revolutions per minute while pulling the head of the single crystal silicon rod.
Pulling the head of the monocrystalline silicon rod until the constant diameter length of the head of the monocrystalline silicon rod is more than or equal to 500mm, and lifting the crucible rotation to 7-8 rotations per minute.
And reducing the pressure drop of the furnace body to 9-10torr.
And increasing the flow rate of argon in the furnace body to 90-110slpm.
The crucible-to-heel ratio is adjusted to be 0.06-0.15.
Optionally, a main heating electrode is arranged at the bottom of the furnace body, the heater is connected with the main heating electrode sequentially through a graphite electrode and a copper electrode, and the graphite electrode is formed by sequentially stacking a plurality of graphite electrode rings.
The method for producing the low-oxygen crystal bar has the beneficial effects that: since the more the heater is located closer to the chamfer portion of the crucible during heating of the crucible, the more oxygen is deposited in the chamfer portion, and the higher the oxygen content of the single crystal silicon rod. Therefore, by defining the distance between the top of the heater and the support ring to be 20-30mm, the heater is farther from the chamfer portion within the distance range, the oxygen precipitated from the chamfer portion is reduced, the oxygen content of the single crystal silicon rod is reduced, and the production cost is also controlled because the thermal field components in the single crystal furnace are not modified.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a cross-sectional view of a single crystal furnace in an embodiment of the present application;
FIG. 2 is a flow chart of a method of producing a low oxygen ingot in an embodiment of the application.
Icon: 1-a furnace body; 11-heat preservation felt; 2-a crucible; 21-a chamfer; 3-a heater; 4-a guide cylinder; 5-a heat preservation cover; 6-loading a heat preservation cylinder; 7-a middle heat preservation cylinder; 8-a lower heat preservation cylinder; 9-support ring.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. The components of the embodiments of the present application generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the application, as presented in the figures, is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present application, it should be noted that, if the terms "upper", "lower", "inner", "outer", and the like indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, or the azimuth or the positional relationship in which the inventive product is conventionally put in use, it is merely for convenience of describing the present application and simplifying the description, and it is not indicated or implied that the apparatus or element referred to must have a specific azimuth, be configured and operated in a specific azimuth, and thus it should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, if any, are used merely for distinguishing between descriptions and not for indicating or implying a relative importance.
It should be noted that the features of the embodiments of the present application may be combined with each other without conflict.
The inventor of the application discovers that the main mode of reducing oxygen is to reform a thermal field component in a single crystal furnace at present, but the reformation of the thermal field component needs to be reprocessed to manufacture the thermal field component, so that the labor force is increased, and the production cost is greatly increased due to the fact that the thermal field component is replaced in a large quantity. The embodiment of the application provides a method for producing a low-oxygen crystal bar, which is at least used for solving the technical problem.
Referring to fig. 1, the method for producing a low-oxygen crystal bar provided by the embodiment of the application is applied to a single crystal furnace, the single crystal furnace comprises a furnace body 1, a crucible 2, a heater 3, a guide cylinder 4, a heat insulation cover 5, an upper heat insulation cylinder 6, a middle heat insulation cylinder 7 and a lower heat insulation cylinder 8, wherein the upper heat insulation cylinder 6, the middle heat insulation cylinder 7 and the lower heat insulation cylinder 8 are sequentially arranged in the furnace body 1 from top to bottom, the heat insulation cover 5 is arranged at the top of the upper heat insulation cylinder 6, and the guide cylinder 4 is arranged on the heat insulation cover 5; a supporting ring 9 is arranged between the upper heat preservation cylinder 6 and the middle heat preservation cylinder 7, the crucible 2 is arranged in a cavity surrounded by the upper heat preservation cylinder 6, the middle heat preservation cylinder 7 and the lower heat preservation cylinder 8 in a lifting manner, the heater 3 is arranged in the furnace body 1, the top of the heater 3 is lower than the supporting ring 9, the distance between the top of the heater 3 and the supporting ring 9 is 20-30mm, a chamfer part 21 is arranged at the bottom of the crucible 2, and the chamfer part 21 is lower than the top of the heater 3.
The inner diameters of the middle heat preservation cylinder 7 and the lower heat preservation cylinder 8 are equal, the inner diameter of the upper heat preservation cylinder 6 is smaller than the inner diameter of the middle heat preservation cylinder 7, and the upper heat preservation cylinder 6, the middle heat preservation cylinder 7 and the lower heat preservation cylinder 8 are coaxially arranged; the guide cylinder 4 extends downwards to the top of the crucible 2, the liquid level in the crucible 2 gradually drops during the crystal growth process, and the crucible 2 needs to be gradually lifted in order to keep the distance between the liquid level in the crucible 2 and the bottom of the guide cylinder 4 unchanged. The distance between the top of the heater 3 and the support ring 9 is hereinafter referred to as the cap distance.
Since the heater 3 is closer to the chamfer portion 21 of the crucible 2 during heating of the crucible 2, the more oxygen is deposited in the chamfer portion 21, the higher the oxygen content of the single crystal silicon rod. Therefore, by defining the gap of the stopper to be 20-30mm, the heater 3 is farther from the chamfering part 21 within the distance range, oxygen precipitated from the chamfering part 21 is reduced, the oxygen content of the single crystal silicon rod is reduced, and the production cost is also controlled because the thermal field components in the single crystal furnace are not modified.
In practice, the distance between the cover and the support ring 9 should be greater than or equal to 20mm, and if the distance between the cover and the support ring is less than 20mm, the ignition between the heater 3 and the support ring 9 is easily caused.
For example, the cap distance may be 20mm, 25mm or 30mm, it being understood that the distance between the top of the heater 3 and the support ring 9 may be selected within the above ranges depending on the operating conditions.
In an alternative embodiment, at least one layer of heat insulation felt 11 is arranged on the inner bottom wall of the furnace body 1, and the lower heat insulation cylinder 8 is supported on the heat insulation felt 11; and/or the bottom of the heater 3 is provided with a graphite electrode ring; and/or the inner walls of the upper heat preservation cylinder 6, the middle heat preservation cylinder 7 and the lower heat preservation cylinder 8 are provided with a plurality of layers of heat preservation cylinder felts.
It should be noted that, at least one layer of heat insulation felt 11 is arranged on the inner bottom wall of the furnace body 1, and the number of layers of heat insulation felt 11 can be reduced or increased; the graphite electrode ring is arranged at the bottom of the heater 3 and plays a role in raising the heater 3; the layer number of the insulation cylinder felts on the inner walls of the upper insulation cylinder 6, the middle insulation cylinder 7 and the lower insulation cylinder 8 can be adjusted.
In an alternative embodiment, the bottom of the furnace body 1 is provided with a main heating electrode, and the heater 3 is connected with the main heating electrode sequentially through a graphite electrode and a copper electrode, and the graphite electrode is formed by sequentially stacking a plurality of graphite electrode rings.
It should be noted that the heater 3, the graphite electrode, the copper electrode and the main heating electrode are sequentially connected from top to bottom, the graphite electrode is formed by sequentially stacking a plurality of graphite electrode rings, and the number of the graphite electrode rings can be reduced or increased so as to raise or lower the height of the heater 3.
The method for producing the low-oxygen crystal bar provided by the embodiment of the application comprises the following steps:
reducing the number of layers of insulation blanket 11to reduce the distance between heater 3 and support ring 9; and/or adding a graphite electrode ring at the bottom of the heater 3 to raise the heater 3 and reduce the distance between the heater 3 and the support ring 9; and/or increasing the number of layers of the insulation cylinder felts on the upper insulation cylinder 6 so as to reduce the number of layers of the insulation cylinder felts on the upper insulation cylinder 6 and the lower insulation cylinder 8 to 2-3 layers, and increasing the number of layers of the insulation cylinder felts on the middle insulation cylinder 7 so as to make the number of layers of the insulation cylinder felts on the middle insulation cylinder 7 and the lower insulation cylinder 8 equal.
The method for producing the low-oxygen crystal bar comprises three schemes, wherein the first scheme is that the number of layers of a heat preservation felt 11 is reduced, the upper heat preservation cylinder 6, the middle heat preservation cylinder 7, the lower heat preservation cylinder 8, the guide cylinder 4 and the support ring 9 are all lowered by corresponding distances, the crucible 2 is lowered along with the constant distance between the liquid surface of the crucible 2 and the bottom of the guide cylinder 4, but the height of the heater 3 is constant, the distance between the heater cover and the chamfer part 21 of the crucible 2 is reduced, the distance between the heater 3 and the chamfer part 21 is increased, so that the oxygen precipitated by the chamfer part 21 is reduced, and the oxygen content of the single crystal silicon bar is reduced. On the other hand, the number of layers of the heat insulation felt 11 is reduced, namely, the heat insulation performance of the bottom of the furnace body 1 is reduced, and the chamfer part 21 of the crucible 2 is close to the bottom of the furnace body 1, so that the temperature of the chamfer part 21 of the crucible 2 can be reduced and the precipitation of oxygen can be reduced due to the reduction of the heat insulation performance of the bottom of the furnace body 1.
For example, the thickness of the single-layer insulation blanket 11 is 10mm, and the reduction of one layer of insulation blanket 11 can reduce the gap between the heater 3 and the chamfer 21 of the crucible 2 by 10mm.
The second scheme is that graphite electrode rings are added at the bottom of the heater 3, namely, the number of the graphite electrode rings is increased, and the height of graphite electrodes is increased, so that the heater 3 is lifted, the distance between the heater 3 and the chamfering part 21 of the crucible 2 is increased, the oxygen precipitated by the chamfering part 21 is reduced, and the oxygen content of the monocrystalline silicon rod is reduced.
For example, the height of a single graphite electrode ring is 10mm, and the addition of one graphite electrode ring can reduce the gap between the lids by 10mm, i.e., increase the distance between the heater 3 and the chamfer 21 of the crucible 2 by 10mm.
The third scheme is to increase the layer number of the insulation cylinder felts on the upper insulation cylinder 6 to reduce the layer number difference of the insulation cylinder felts on the upper insulation cylinder 6 and the lower insulation cylinder 8 to 2-3 layers, and increase the layer number of the insulation cylinder felts on the middle insulation cylinder 7 to make the layer number of the insulation cylinder felts on the middle insulation cylinder 7 and the lower insulation cylinder 8 equal, and at this time, the layer number difference of the insulation cylinder felts on the middle insulation cylinder 7 and the lower insulation cylinder 8 is zero.
It should be noted that, the number of layers of the insulation cylinder felts on the original upper insulation cylinder 6 and the number of layers of the insulation cylinder felts on the middle insulation cylinder 7 are different from the number of layers of the insulation cylinder felts on the lower insulation cylinder 8 more, and the difference between the number of layers of the insulation cylinder felts on the upper insulation cylinder 6 and the number of layers of the insulation cylinder felts on the middle insulation cylinder 7 is reduced by increasing the number of layers of the insulation cylinder felts on the upper insulation cylinder 6 and the number of layers of the insulation cylinder felts on the lower insulation cylinder 8, so that the insulation performance of the upper part in a thermal field can be increased, the output power of the heater 3 in the single crystal silicon rod drawing process is reduced, and the baking temperature of the crucible 2 is reduced, and the separation of oxygen is further reduced.
For example, in the case where the number of layers of the insulation cylinder felt on the lower insulation cylinder 8 is 14, the number of layers of the insulation cylinder felt on the upper insulation cylinder 6 can be raised to 12, and the number of layers of the insulation cylinder felt on the insulation cylinder 7 can be raised to 14; or under the condition that the number of layers of the insulation cylinder felts on the lower insulation cylinder 8 is 16, the number of layers of the insulation cylinder felts on the upper insulation cylinder 6 can be increased to 14, and the number of layers of the insulation cylinder felts on the middle insulation cylinder 7 can be increased to 16.
It should be noted that, according to the actual working conditions, the above three schemes can be adopted at the same time, or only any one or two schemes are adopted, and the oxygen content of the monocrystalline silicon rod can be reduced as long as the distance between the cover and the cover is controlled within the range of 20-30 mm.
Referring to fig. 2, the method for producing a low oxygen ingot further includes:
and S1, when the head part of the monocrystalline silicon rod is pulled, the crucible rotation is reduced to 4-6 rotations per minute.
The segregation coefficient of oxygen in silicon is 1.2, namely the concentration in solid silicon is higher than that in liquid silicon, so that the oxygen content is mainly concentrated at the head of a single crystal silicon rod, and the distribution of the oxygen content in the single crystal silicon is gradually reduced from head to tail, namely, the oxygen content at the head of the single crystal silicon rod is controlled within a qualified range.
The convection is increased by the high crucible transfer crystal pulling, oxygen is increased by the reaction of silicon dioxide and silicon liquid, under the condition that the cover distance is 20-30mm, the heater 3 is far away from the chamfer part 21 of the crucible 2, the oxygen precipitation of the chamfer part 21 is reduced, the crucible 2 is heated by the single crystal furnace to greatly reduce the oxygen content, the head part of a single crystal silicon rod is pulled by the low crucible transfer crystal pulling, the heater 3 is far away from the chamfer part 21 of the crucible 2, the temperature difference between the liquid surface of the crucible 2 and the bottom of the crucible 2 is increased, the possibility of increasing up-and-down convection of melt in the crucible 2 is increased, the crucible transfer is reduced to 4-6 revolutions per minute, the problems that the convection is increased due to the high crucible transfer, the oxygen is increased by the reaction of the silicon dioxide and the silicon liquid are solved, and the like are solved, the oxygen content of the single crystal silicon rod is reduced, the defects such as crystal rod distortion can be further reduced due to the pot transfer reduction, and the quality improvement of the single crystal silicon rod is facilitated.
In practice, the crucible rotation can be reduced from a large rotation speed to 4 rpm, 5 rpm or 6 rpm.
And S2, pulling the head of the monocrystalline silicon rod until the constant diameter length of the head of the monocrystalline silicon rod is greater than or equal to 500mm, and lifting the crucible to 7-9 revolutions per minute.
Because the oxygen content is mainly concentrated at the head part of the monocrystalline silicon rod, the part of the head part of the monocrystalline silicon rod with the constant diameter length within 500mm adopts low crucible rotation crystal pulling of 4-6 rotations per minute to reduce the oxygen content of the head part of the monocrystalline silicon rod; and because the convection current of the crystal pulling from the crucible to the crystal pulling is weaker, the radial temperature gradient is large, the crystal growth is not facilitated, the breakage is easy to occur, the crystal pulling is performed on the head of the monocrystalline silicon rod until the constant diameter length of the head of the monocrystalline silicon rod is more than or equal to 500mm, the crucible is increased to 7-9 revolutions per minute, the convection current is increased, the radial temperature gradient is reduced, and the crystal growth is facilitated.
In actual operation, the crucible rotation can be increased to 7 rpm, 8 rpm or 9 rpm by pulling the head of the single crystal silicon rod until the isodiametric length of the head of the single crystal silicon rod is greater than or equal to 500 mm.
In addition, the method for producing the low-oxygen crystal bar comprises the following steps:
and step S3, reducing the furnace pressure in the furnace body 1to 9-11torr.
In the embodiment of the application, the furnace pressure in the original furnace body 1 is reduced from 12torr to 9-11torr, the furnace pressure is reduced, the oxygen generation can be reduced, the oxygen content in the furnace body 1 is reduced, and the oxygen reduction effect is achieved.
In actual operation, the furnace pressure in the furnace body 1 can be reduced from 12torr to 9torr, 10torr or 11torr.
In addition, the method for producing the low-oxygen crystal bar comprises the following steps:
and S4, increasing the flow of argon in the furnace body 1to 90-110slpm.
In the embodiment of the application, the argon flow in the original furnace body 1 is increased from 80 slpm to 90-110slpm, and the argon with larger flow can take away redundant oxygen in the furnace body 1, so that the oxygen content is reduced, the flow rate is increased, the air flow disturbance is reduced, the temperature difference of a crystal pulling solid-liquid interface is reduced, and the defects of crystal bar distortion and the like are overcome.
In actual operation, the argon flow in the original furnace body 1 can be increased from 80 slpm to 90slpm, 100 slpm or 110slpm.
In addition, the method for producing the low-oxygen crystal bar further comprises the following steps:
and S5, adjusting the crucible-to-heel ratio to be 0.06-0.15.
It should be noted that the crucible-to-crucible ratio is the ratio of crucible elevation to crystal elevation, during the crystal growth process, as the material in the crucible 2 decreases, the liquid level of the crucible 2 decreases, and the crucible 2 needs to rise upward along with the crucible-to-crucible ratio, so that the distance between the liquid level of the crucible 2 and the bottom of the guide cylinder 4 is kept unchanged, the chamfer portion 21 of the crucible 2 gradually approaches the heating area of the heater 3, and when the rod is drawn, the crucible 2 reaches the highest position, at this time, the chamfer portion 21 is located in the heating area of the heater 3, and oxygen precipitation of the chamfer portion 21 is aggravated.
For example, the crucible-to-heel ratio may be 0.078, 0.096 or 0.137, and in practice, the crucible-to-heel ratio may be reasonably adjusted within the above-described range.
By controlling the crucible-to-heel ratio in the range of 0.06-0.15, the raising speed of the crucible 2 is not excessively high at this time, thereby reducing the increase of oxygen precipitation caused by excessively high raising of the crucible 2, and reducing the oxygen content of the ingot.
Wherein, step S3, step S4 and step S5 may be performed in synchronization with step S1.
In summary, the embodiment of the application provides a method for producing a low-oxygen crystal bar, wherein the distance between the cover and the heater 3 is 20-30mm structurally through the limiter, and the distance is far from the chamfering part 21, so that the oxygen precipitated from the chamfering part 21 is reduced, and the oxygen content of the monocrystalline silicon bar is reduced; by reducing the number of layers of the insulation blanket 11 and/or increasing the number of graphite electrode rings so that the gap between the cover and the chamfer 21 of the crucible 2 is reduced to a range of 20-30mm, the distance between the heater 3 and the chamfer 21 is increased, and thus the oxygen deposited at the chamfer 21 is reduced. By limiting the crucible rotation from the process, when the head part of the monocrystalline silicon rod is pulled, the crucible rotation is reduced to 4-6 rotations per minute; limiting the furnace pressure, and reducing the furnace pressure in the furnace body 1to 9-11torr; limiting the flow of argon, and lifting the flow of the argon in the furnace body 1to 90-110slpm; and limiting the crucible-to-heel ratio, and adjusting the crucible-to-heel ratio to 0.06-0.15 can achieve the effect of reducing the oxygen content of the crystal bar.
The foregoing is merely illustrative of the present application, and the present application is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present application should be included in the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (2)
1. The method for producing the low-oxygen crystal bar is characterized by being applied to a single crystal furnace, wherein the single crystal furnace comprises a furnace body, a crucible, a heater, a guide cylinder, a heat preservation cover, an upper heat preservation cylinder, a middle heat preservation cylinder and a lower heat preservation cylinder, the upper heat preservation cylinder, the middle heat preservation cylinder and the lower heat preservation cylinder are sequentially arranged in the furnace body from top to bottom, the heat preservation cover is arranged at the top of the upper heat preservation cylinder, and the guide cylinder is arranged on the heat preservation cover;
a supporting ring is arranged between the upper heat preservation cylinder and the middle heat preservation cylinder, the crucible is arranged in a cavity surrounded by the upper heat preservation cylinder, the middle heat preservation cylinder and the lower heat preservation cylinder in a lifting manner, the heater is arranged in the furnace body, the top of the heater is lower than the supporting ring, the distance between the top of the heater and the supporting ring is 20-30mm, the bottom of the crucible is provided with a chamfering part, and the chamfering part is lower than the top of the heater; at least one layer of heat insulation felt is arranged on the inner bottom wall of the furnace body, and the lower heat insulation cylinder is supported on the heat insulation felt; and/or the bottom of the heater is provided with a graphite electrode ring; and/or the inner walls of the upper heat preservation cylinder, the middle heat preservation cylinder and the lower heat preservation cylinder are provided with a plurality of layers of heat preservation cylinder felts;
the method for producing the low-oxygen crystal bar comprises the following steps:
increasing the number of layers of the insulation cylinder felts on the upper insulation cylinder to reduce the number of layers of the insulation cylinder felts on the upper insulation cylinder and the lower insulation cylinder to 2-3 layers, and increasing the number of layers of the insulation cylinder felts on the middle insulation cylinder to make the number of layers of the insulation cylinder felts on the middle insulation cylinder and the lower insulation cylinder equal;
when the head of the monocrystalline silicon rod is pulled, the crucible rotation is reduced to 4-5 rotations per minute;
pulling the head of the monocrystalline silicon rod until the isodiametric length of the head of the monocrystalline silicon rod is more than or equal to 500mm, and lifting the crucible rotation to 7-8 rotations per minute;
reducing the furnace pressure in the furnace body to 9-10torr;
the argon flow in the furnace body is increased to 90-110slpm;
the crucible-to-heel ratio is adjusted to be 0.06-0.15.
2. The method for producing a low-oxygen crystal ingot according to claim 1, wherein a main heating electrode is provided at the bottom of the furnace body, the heater is connected to the main heating electrode sequentially through a graphite electrode and a copper electrode, and the graphite electrode is formed by sequentially stacking a plurality of graphite electrode rings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310745487.5A CN116479525B (en) | 2023-06-25 | 2023-06-25 | Method for producing low-oxygen crystal bar |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310745487.5A CN116479525B (en) | 2023-06-25 | 2023-06-25 | Method for producing low-oxygen crystal bar |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116479525A CN116479525A (en) | 2023-07-25 |
| CN116479525B true CN116479525B (en) | 2023-09-15 |
Family
ID=87221827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310745487.5A Active CN116479525B (en) | 2023-06-25 | 2023-06-25 | Method for producing low-oxygen crystal bar |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116479525B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101922040A (en) * | 2009-06-10 | 2010-12-22 | 江国庆 | Device of oxygen control growth in single crystal furnace |
| CN102002753A (en) * | 2010-12-13 | 2011-04-06 | 天津市环欧半导体材料技术有限公司 | Processing method of phi 8-inch <110> czochralski silicon and thermal system thereof |
| CN102628178A (en) * | 2012-05-10 | 2012-08-08 | 江苏聚能硅业有限公司 | Method for decreasing oxygen content of solar 8-inch monocrystalline silicon wafers |
| CN110552058A (en) * | 2019-08-22 | 2019-12-10 | 宁夏隆基硅材料有限公司 | Crystal pulling method, device and equipment |
| CN216738634U (en) * | 2021-10-19 | 2022-06-14 | 宇泽半导体(云南)有限公司 | Thermal field for single crystal furnace |
| CN115404541A (en) * | 2022-10-18 | 2022-11-29 | 四川晶科能源有限公司 | A crystal pulling method |
| CN218262821U (en) * | 2022-10-27 | 2023-01-10 | 宇泽半导体(云南)有限公司 | Thermal field capable of reducing oxygen content of single crystal |
| CN115821367A (en) * | 2022-12-07 | 2023-03-21 | 西安奕斯伟材料科技有限公司 | Crucible device, single crystal furnace device and working method thereof |
| CN219044980U (en) * | 2022-12-05 | 2023-05-19 | 乐山市京运通新材料科技有限公司 | Czochralski monocrystalline silicon oxygen reduction thermal field device and monocrystalline furnace |
-
2023
- 2023-06-25 CN CN202310745487.5A patent/CN116479525B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101922040A (en) * | 2009-06-10 | 2010-12-22 | 江国庆 | Device of oxygen control growth in single crystal furnace |
| CN102002753A (en) * | 2010-12-13 | 2011-04-06 | 天津市环欧半导体材料技术有限公司 | Processing method of phi 8-inch <110> czochralski silicon and thermal system thereof |
| CN102628178A (en) * | 2012-05-10 | 2012-08-08 | 江苏聚能硅业有限公司 | Method for decreasing oxygen content of solar 8-inch monocrystalline silicon wafers |
| CN110552058A (en) * | 2019-08-22 | 2019-12-10 | 宁夏隆基硅材料有限公司 | Crystal pulling method, device and equipment |
| CN216738634U (en) * | 2021-10-19 | 2022-06-14 | 宇泽半导体(云南)有限公司 | Thermal field for single crystal furnace |
| CN115404541A (en) * | 2022-10-18 | 2022-11-29 | 四川晶科能源有限公司 | A crystal pulling method |
| CN218262821U (en) * | 2022-10-27 | 2023-01-10 | 宇泽半导体(云南)有限公司 | Thermal field capable of reducing oxygen content of single crystal |
| CN219044980U (en) * | 2022-12-05 | 2023-05-19 | 乐山市京运通新材料科技有限公司 | Czochralski monocrystalline silicon oxygen reduction thermal field device and monocrystalline furnace |
| CN115821367A (en) * | 2022-12-07 | 2023-03-21 | 西安奕斯伟材料科技有限公司 | Crucible device, single crystal furnace device and working method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116479525A (en) | 2023-07-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11851784B2 (en) | Apparatus and method for growing high-purity semi-insulating silicon carbide crystal | |
| JP5904079B2 (en) | Silicon single crystal growing apparatus and silicon single crystal growing method | |
| US7299658B2 (en) | Quartz glass crucible for the pulling up of silicon single crystal | |
| CN105531406A (en) | Silicon single crystal puller | |
| JP2007230846A (en) | Crucible for single crystal manufacturing equipment | |
| US8268077B2 (en) | Upper heater, single crystal production apparatus, and method for producing single crystal | |
| JP5008695B2 (en) | Silica glass crucible and silicon single crystal pulling method using quartz glass crucible | |
| CN114232070B (en) | Double-cavity structure and method for growing gallium oxide crystal by Czochralski method | |
| JP2009161363A (en) | Silica glass crucible for pulling silicon single crystals | |
| JP4717771B2 (en) | Silica glass crucible | |
| KR102253607B1 (en) | Heat shield member, single crystal pulling device, and single crystal silicon ingot manufacturing method | |
| CN116479525B (en) | Method for producing low-oxygen crystal bar | |
| KR102038960B1 (en) | Silicon single crystal manufacturing method | |
| JP6033650B2 (en) | Single crystal manufacturing apparatus and single crystal manufacturing method | |
| JP6855358B2 (en) | Quartz glass crucible for pulling silicon single crystal | |
| JP2018052783A (en) | Heater insulation structure, and single crystal production apparatus | |
| CN109415842A (en) | The manufacturing method of monocrystalline silicon | |
| CN103553052B (en) | Device and method for reverse solidification of polysilicon | |
| CN114293256B (en) | Thermal field and growth process for growing dislocation-free germanium single crystal by Czochralski method | |
| CN104178813A (en) | Kyropoulos-process sapphire single-crystal growth furnace thermal-insulation side screen | |
| CN221028784U (en) | Crystal growth apparatus | |
| JP3777983B2 (en) | Method for manufacturing glass article | |
| CN114616361A (en) | Method for producing silicon single crystal | |
| CN221421277U (en) | Single crystal furnace variable wall thickness heater capable of reducing crystal oxygen content | |
| JP7150250B2 (en) | Quartz glass crucible and method for manufacturing quartz glass crucible |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231226 Address after: 663000 Xiban area of the Industrial Demonstration Park in Guangnan County, Wenshan Zhuang and Miao Autonomous Prefecture, Yunnan Province Patentee after: Yuze Semiconductor (Wenshan) Co.,Ltd. Address before: G3-2401, No. 88, Jinjihu Avenue, Suzhou Industrial Park, Suzhou Pilot Free Trade Zone, China (Jiangsu) 215000 Patentee before: Suzhou Chenhui Intelligent Equipment Co.,Ltd. |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 663300 Xiban area of the Industrial Demonstration Park in Guangnan County, Wenshan Zhuang and Miao Autonomous Prefecture, Yunnan Province Patentee after: Yuze New Energy (Wenshan) Co.,Ltd. Country or region after: China Address before: 663000 Xiban area of the Industrial Demonstration Park in Guangnan County, Wenshan Zhuang and Miao Autonomous Prefecture, Yunnan Province Patentee before: Yuze Semiconductor (Wenshan) Co.,Ltd. Country or region before: China |