CN111304736A - Method for eliminating influence of scum on dislocation-free germanium single crystal crystallization - Google Patents
Method for eliminating influence of scum on dislocation-free germanium single crystal crystallization Download PDFInfo
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- CN111304736A CN111304736A CN202010274836.6A CN202010274836A CN111304736A CN 111304736 A CN111304736 A CN 111304736A CN 202010274836 A CN202010274836 A CN 202010274836A CN 111304736 A CN111304736 A CN 111304736A
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- 239000013078 crystal Substances 0.000 title claims abstract description 69
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 50
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000002425 crystallisation Methods 0.000 title claims abstract description 8
- 230000008025 crystallization Effects 0.000 title claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 38
- 239000000725 suspension Substances 0.000 claims abstract description 32
- 238000002844 melting Methods 0.000 claims abstract description 27
- 230000008018 melting Effects 0.000 claims abstract description 27
- 238000010899 nucleation Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 230000000694 effects Effects 0.000 claims abstract description 5
- 238000010309 melting process Methods 0.000 claims abstract description 3
- 230000003746 surface roughness Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 20
- 239000000155 melt Substances 0.000 abstract description 11
- 230000008859 change Effects 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- -1 gallium arsenide compound Chemical class 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- 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
- C30B15/20—Controlling or regulating
-
- 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
- C30B29/08—Germanium
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- 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 invention discloses a method for eliminating the influence of scum on the crystallization of dislocation-free germanium single crystals, which comprises the following steps: putting high-purity germanium ingots into the double-suspension crucible, and vacuumizing; setting heating power and crucible position according to the heating and material melting process and melting germanium material; after the heating and melting are finished, rapidly reducing the heating power, simultaneously raising the position of the crucible relative to the position of the crucible when the melting is heated, and maintaining for 6-12 min; increasing the rotation speed of the crucible and maintaining for 3-10 min; and switching to the required heating power, crucible position and rotating speed parameters for seeding. The invention realizes the effect that the melt at the liquid level part of the melt flows to the inner wall of the crucible by adjusting the temperature, the rotating speed of the crucible and the like, so that the scum flows to the wall of the crucible along with the melt and is attached to the inner wall of the suspended crucible, and the scum can not be brought back to the liquid level by the fluid again under the change of the process ranges of the stages of normal crystal seeding, shouldering, equal diameter and the like, thereby eliminating the influence of the scum on the subsequent growth process of the germanium single crystal.
Description
Technical Field
The invention particularly relates to a method for eliminating influence of scum on dislocation-free germanium single crystal crystallization, and belongs to the technical field of crystal growth.
Background
The germanium single crystal has good infrared performance, high infrared light transmittance and refractive index, low dispersion, good chemical stability, high mechanical strength and the like, and is a preferred material for an infrared light transmission window with a wave band of 3-12 mu m. Germanium single crystals for infrared optical windows are generally antimony-doped n-type germanium single crystals, and the germanium single crystals have high requirements on the magnitude and uniformity of resistivity values and low requirements on crystal defects. Another kind of p-type germanium single crystal with large diameter (more than 4 inches) and heavily doped gallium attracts more and more attention as a substrate material of a photovoltaic cell in the aerospace field, and a gallium arsenide compound multi-junction cell taking a germanium single crystal as a substrate has the advantages of high conversion efficiency, small relative weight and volume, excellent cosmic ray radiation resistance and the like, and completely replaces the traditional silicon cell in an outer space solar power generation system; crystal defects such as dislocation in the germanium single crystal directly influence key performances such as gallium arsenide cell Filling Factor (FF), photoelectric conversion Efficiency (EFF) and cell service life, so that the crystal defects such as dislocation of the germanium single crystal are required to be as few as possible, and the application in the field of foreign aerospace even requires no dislocation. The application in the field of infrared optics and photovoltaics enables the demand of germanium single crystal materials to be continuously increased, and the germanium single crystals have wide market prospects.
The main growth methods of the germanium single crystal comprise a Czochralski method (CZ) and a vertical gradient freezing method (VGF), the two methods are commercially produced, the germanium single crystal produced by the Czochralski method is superior to the vertical gradient freezing method in the aspects of resistivity uniformity and dislocation control in view of the performance of the germanium single crystal, and the VGF method is difficult in growing the germanium single crystal with a larger diameter, so that most manufacturers of the germanium single crystal grow by adopting the Czochralski method at present.
The method for growing germanium single crystal by Czochralski method is a method for preparing single crystal by pulling a rotating seed crystal from a melt in a crucible, wherein the pulling process is realized in a single crystal furnace. The process of preparing the germanium single crystal by the Czochralski method comprises the steps of vacuumizing, heating and melting materials, removing scum, seeding, shouldering, shoulder rotating, diameter equalizing, ending and the like. In the seeding, shouldering, isometric and other stages of the growth of the germanium single crystal, if scum caused by the introduction of raw materials, the falling of a chamber, the oxidation of chemical materials and other reasons exists on the surface of a melt, the scum is easily adhered to the surface of the crystallized single crystal in the growth process, the heat dissipation and crystallization are influenced, dislocation defects in the single crystal are generated, edge breakage and crystal transformation finally occur, and when the influence of the scum exists, the normal growth of the dislocation-free germanium single crystal cannot be realized.
The technical scheme of the prior scum removing process during the growth of the germanium single crystal comprises the following steps: after heating and melting, soaking seed crystals into the melt for crystallization, quickly pulling the crystal to enable scum to be adhered to crystals, then pulling the crystals to an auxiliary chamber by utilizing an auxiliary chamber structure with a gate valve of a single crystal furnace after judging that the scum is completely adhered to the crystals, closing the gate valve, opening an auxiliary chamber door to cut off the seed crystals after cooling to a proper temperature, taking out the crystals, closing the auxiliary chamber door, vacuumizing and replacing, and then opening the gate valve to enter the next step of process. The prior auxiliary chamber scum removing process has the following problems: (1) the efficiency is low, the process time required for deslagging the auxiliary chamber is too long, and the time of 5-8 hours is required in the processes of growing, cooling, vacuumizing and replacing the auxiliary chamber and the like; (2) the deslagging effect is not ideal, besides scum which is not completely adhered to crystals is removed in the auxiliary chamber, secondary scum generation is possibly caused by slight oxidation caused by the deslagging process, and a small amount of scum still threatens the crystallization of dislocation-free germanium single crystals; (3) the cost is high, the deslagging process of the deslagging method of the auxiliary chamber consumes electric energy, and the crystal adhered with scum is generated to cause the loss of the germanium raw material.
Disclosure of Invention
Aiming at the defects and shortcomings of the existing scum removal process of the secondary chamber, the invention provides a method for eliminating the influence of scum on dislocation-free germanium single crystal formation by combining a double-suspension crucible structure independently designed by the applicant, which replaces the existing scum removal process of the secondary chamber, can eliminate the influence of the scum on dislocation-free germanium single crystal formation, improves the efficiency and reduces the cost.
The invention provides a method for rapidly eliminating the influence of scum on the growth of dislocation-free germanium single crystals by combining the rotation characteristic of a suspension crucible in the growth process of the single crystals, which is described in the independent patent of the applicant (CN 201520815U).
The technical scheme adopted by the invention for solving the technical problems is as follows:
(1) respectively putting high-purity germanium ingots into a single crucible and an inner floating crucible of a double-suspension crucible (disclosed in CN201520815U), and vacuumizing; setting heating power and the integral position of the double-suspension crucible according to a heating and material melting process and melting germanium materials;
(2) after the material heating and melting stage is finished, rapidly reducing the heating power to 5-10% of the total power of the heated and melted material, simultaneously raising the whole position of the double-suspension crucible by 15-25mm relative to the whole position of the double-suspension crucible when the material is heated and melted, and maintaining for 6-12min under the condition;
(3) starting the integral rotating speed of the double-suspension crucible to 2-8 r/min, and maintaining for 3-10 min;
(4) and switching to the heating power required by the seeding stage, the integral position of the double-suspension crucible and the rotating speed parameter for seeding.
After the treatment by the method, the scum on the surface of the melt is adhered around the inner wall of the inner floating crucible of the double-suspension crucible for one circle, and because the subsequent technological process does not allow the technological operation of large temperature rise, and meanwhile, the rotating speed of the whole double-suspension crucible is also maintained at a low speed, the scum can not flow back to the liquid level along with the melt, thereby eliminating the influence of the scum on the subsequent crystal seeding, shouldering, equal-diameter growth processes and the like of the germanium single crystal in the inner floating crucible.
Preferably, in the step (2), the heating power is rapidly reduced to 8% of the total power of the heating material, and the position of the whole double-suspension crucible is raised and maintained for 8-10 min.
Preferably, in the step (3), the rotating speed of the whole double-suspension crucible is started to 3-5 r/min, and is maintained for 5-8 min.
Preferably, the suspension crucible of the present invention is improved on the basis of the scheme described in "double suspension crucible" (CN201520815U), and the surface roughness of the portion above the liquid level on the inner wall of the inner suspension crucible (e.g., the upper half portion of the inner wall of the inner suspension crucible) is increased during surface processing, so that the adhesion of dross on the inner wall of the crucible can be increased.
Compared with the prior art, the invention has the following advantages:
the method realizes the effect that the melt at the liquid level part of the melt flows to the inner wall of the crucible by adjusting the temperature, the rotating speed of the crucible and the like, so that the scum flows to the wall of the crucible along with the melt and is attached to the inner wall of the suspended crucible, and the scum can not be brought back to the liquid level by the fluid again under the process range change of the stages of normal crystal seeding, shouldering, equal diameter and the like, thereby eliminating the influence of the scum on the subsequent growth process of the germanium single crystal. Compared with the method for removing the scum from the auxiliary chamber, the method has the advantages that the time is greatly shortened, the efficiency is improved, the effect is more remarkable, the raw materials are not lost in the whole process, and the cost is greatly reduced.
Drawings
FIG. 1 is a photomicrograph at 100X of a single crystal test piece grown according to example 1.
FIG. 2 is a photomicrograph at 100X of a test piece of a comparative example grown single crystal.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Putting 80 kg of high-purity germanium ingot into a double-suspension crucible (disclosed in CN201520815U), vacuumizing, setting heating power W, setting the whole position of the crucible to be 0mm, melting materials, rapidly reducing the heating power to 0.05W of the total power of the melting materials after the melting materials are finished, raising the whole position of the crucible to 25mm, and maintaining for 6 minutes under the condition; starting the crucible to rotate at 4 rpm for 10 minutes; and switching to the required heating power, crucible position and crucible rotating speed parameters for seeding. And in the stages of seeding, shouldering and equal diameter, no scum reflows to the liquid level, and the single crystal discharged from the furnace is tested to be dislocation-free germanium single crystal.
Example 2
Putting 80 kg of high-purity germanium ingot into a double-suspension crucible (disclosed in CN201520815U), vacuumizing, setting heating power W, setting the whole position of the crucible to be 0mm, melting materials, rapidly reducing the heating power to 0.1W of the total power of the melting materials after the melting materials are finished, raising the whole position of the crucible to 20mm, and maintaining for 8 minutes under the condition; starting the crucible to rotate at 5 revolutions per minute for 5 minutes; and switching to the required heating power, crucible position and crucible rotating speed parameters for seeding. And in the stages of seeding, shouldering and equal diameter, no scum reflows to the liquid level, and the single crystal discharged from the furnace is tested to be dislocation-free germanium single crystal.
Example 3
Putting 80 kg of high-purity germanium ingot into a double-suspension crucible (disclosed in CN201520815U), vacuumizing, setting heating power W, setting the whole position of the crucible to be 0mm, melting materials, rapidly reducing the heating power to 0.1W of the total power of the melting materials after the melting materials are finished, raising the whole position of the crucible to 25mm, and maintaining for 12 minutes under the condition; starting the crucible to rotate at 3 revolutions per minute for 3 minutes; and switching to the required heating power, crucible position and crucible rotating speed parameters for seeding. And in the stages of seeding, shouldering and equal diameter, no scum reflows to the liquid level, and the single crystal discharged from the furnace is tested to be dislocation-free germanium single crystal.
Example 4
Putting 80 kg of high-purity germanium ingot into a double-suspension crucible (disclosed in CN201520815U), vacuumizing, setting heating power W, setting the whole position of the crucible to be 0mm, melting materials, rapidly reducing the heating power to 0.08W of the total power of the melting materials after the melting materials are finished, raising the whole position of the crucible to 20mm, and maintaining for 10 minutes under the condition; opening the integral rotating speed of the crucible to 2 revolutions per minute for 8 minutes; and switching to the required heating power, crucible position and crucible rotating speed parameters for seeding. And in the stages of seeding, shouldering and equal diameter, no scum reflows to the liquid level, and the single crystal discharged from the furnace is tested to be dislocation-free germanium single crystal.
Example 5
Putting 80 kg of high-purity germanium ingot into a double-suspension crucible (disclosed in CN201520815U), vacuumizing, setting heating power W, setting the whole position of the crucible to be 0mm, melting materials, rapidly reducing the heating power to 0.1W of the total power of the melting materials after the melting materials are finished, raising the whole position of the crucible to 15mm, and maintaining for 6 minutes under the condition; starting the crucible to rotate at 5 revolutions per minute for 5 minutes; and switching to the required heating power, crucible position and crucible rotating speed parameters for seeding. And in the stages of seeding, shouldering and equal diameter, no scum reflows to the liquid level, and the single crystal discharged from the furnace is tested to be dislocation-free germanium single crystal.
Comparative example
Putting 80 kg of high-purity germanium ingots into a common crucible of a single-crucible system, vacuumizing, setting heating power W, setting the crucible position to be 0mm, melting materials, rapidly reducing the heating power to 0.05W of the total power of the melting materials after the melting materials are finished, raising the crucible position to 25mm, and maintaining for 6 minutes under the condition; starting the crucible to rotate at the speed of 4 revolutions per minute for 10 minutes; and switching to the required heating power, crucible position and crucible rotating speed parameters for seeding. Part of scum reflows to the liquid level in the shouldering stage, and the single crystal after being discharged has dislocation with the dislocation density of 630/cm2。
The above description is only a preferred embodiment of the present invention, and should not be construed as limiting the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (6)
1. A method for eliminating the effect of dross on the crystallization of a dislocation-free germanium single crystal, comprising:
putting high-purity germanium ingots into a double-suspension crucible disclosed in CN201520815U, and vacuumizing; setting heating power and the integral position of the double-suspension crucible according to a heating and material melting process and melting germanium materials;
after the material heating and melting stage is finished, quickly reducing the heating power, and simultaneously raising the integral position of the double-suspension crucible relative to the integral position of the crucible when the material is heated and melted, wherein the integral position is maintained for 6-12min under the condition;
increasing the integral rotating speed of the double-suspension crucible and maintaining for 3-10 min;
and switching to the heating power required by the seeding stage, the integral position of the double-suspension crucible and the rotating speed parameter for seeding.
2. The method as claimed in claim 1, wherein after the material heating stage, the heating power is rapidly reduced to 5-10% of the total material heating power, and the position of the whole double suspension crucible is raised by 15-25mm relative to the position of the whole double suspension crucible when the material is heated, and the heating power is maintained for 6-12 min.
3. The method as claimed in claim 1 or 2, wherein the heating power is rapidly reduced to 8% of the total power of the heated batch while the position of the double suspension crucible as a whole is raised and maintained for 8-10 min.
4. The method as claimed in claim 1 or 2, wherein the rotation speed of the double suspension crucible as a whole is increased to 2-8 rpm and maintained for 3-10 min.
5. The method as claimed in claim 4, wherein the rotating speed of the double suspension crucible is increased to 3-5 r/min and maintained for 5-8 min.
6. The method according to claim 1 or 2, wherein the portion of the inner float crucible inner wall of the double-float crucible above the liquid level increases the surface roughness at the time of surface processing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010274836.6A CN111304736A (en) | 2020-04-09 | 2020-04-09 | Method for eliminating influence of scum on dislocation-free germanium single crystal crystallization |
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| CN202010274836.6A CN111304736A (en) | 2020-04-09 | 2020-04-09 | Method for eliminating influence of scum on dislocation-free germanium single crystal crystallization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113789567A (en) * | 2021-09-17 | 2021-12-14 | 安徽光智科技有限公司 | Large-size germanium single crystal growth method |
| CN116377561A (en) * | 2023-01-03 | 2023-07-04 | 有研国晶辉新材料有限公司 | Method for removing germanium single crystal melt scum and device for removing germanium single crystal melt scum |
-
2020
- 2020-04-09 CN CN202010274836.6A patent/CN111304736A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113789567A (en) * | 2021-09-17 | 2021-12-14 | 安徽光智科技有限公司 | Large-size germanium single crystal growth method |
| CN116377561A (en) * | 2023-01-03 | 2023-07-04 | 有研国晶辉新材料有限公司 | Method for removing germanium single crystal melt scum and device for removing germanium single crystal melt scum |
| CN116377561B (en) * | 2023-01-03 | 2024-02-13 | 有研国晶辉新材料有限公司 | Method for removing germanium single crystal melt scum and device for removing germanium single crystal melt scum |
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Application publication date: 20200619 |