CN112247678B - PBN crucible seed crystal cavity repairing method - Google Patents
PBN crucible seed crystal cavity repairing method Download PDFInfo
- Publication number
- CN112247678B CN112247678B CN202010904396.8A CN202010904396A CN112247678B CN 112247678 B CN112247678 B CN 112247678B CN 202010904396 A CN202010904396 A CN 202010904396A CN 112247678 B CN112247678 B CN 112247678B
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- China
- Prior art keywords
- crucible
- seed crystal
- crystal cavity
- polishing
- repairing
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B49/00—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation
- B24B49/006—Measuring or gauging equipment for controlling the feed movement of the grinding tool or work; Arrangements of indicating or measuring equipment, e.g. for indicating the start of the grinding operation taking regard of the speed
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/002—Crucibles or containers for supporting the melt
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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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
Abstract
The invention discloses a PBN crucible seed crystal cavity repairing method, and relates to the technical field of single crystal growth. The invention relates to a PBN crucible seed crystal cavity repairing method, which is characterized in that an electric polishing pen is adopted to polish and repair the surface of a crucible in a grading manner, and a cleaning step is also included before repairing the crucible, namely, the demolded crucible is cleaned by using a mixed acid solution, then is cleaned by using deionized water, and is naturally dried in the air. The invention discloses a PBN crucible seed crystal cavity repairing method, which improves the repairing efficiency of a crucible, reduces the probability of damaging the crucible, improves the using times of the crucible, ensures that the repaired surface of the crucible is smoother and smoother, and further improves the yield of single crystals.
Description
Technical Field
The invention relates to the technical field of single crystal growth, in particular to a PBN crucible seed crystal cavity repairing method.
Background
When the VGF method is used for growing the indium phosphide single crystal, the PBN crucible used for single crystal charging is reused, the indium phosphide crystal bar can cause desquamation and surface damage of different degrees to the crucible after being demoulded from the PBN crucible, and the crucible is required to be repaired integrally before each reuse, so that the crucible surface is smooth and flat integrally, and has no desquamation and the seed crystal cavity is cylindrical. If the repair is not up to the standard, heterogeneous nucleation can be caused in the crystal growth process, and polycrystal or twin crystal is formed.
In the PBN crucible repairing process, the difficulty of repairing a seed crystal cavity and a corner is the largest, the seed crystal cavity is long and thin, the operating space is limited, the finger operation activity is inconvenient, the corner angle of a cone part and a body part is long and narrow, a common scraper is not easy to be taken off to cause the incapability of repairing, most of the existing repairing methods are places where the seed crystal cavity is poked and peeled by an iron sheet or a ceramic rod refitted by stainless steel tweezers, the force and the direction in a narrow space are not easy to be controlled, deeper pits are easy to poke or the seed crystal cavity is poked/cracked, the repairing method has low efficiency, the crucible is easy to be damaged, the crucible use rate is extremely low, an oil painting knife is selected to repair the corner of the crucible, the oil painting knife is not too soft or too hard, the oil painting knife is not too soft to shovel, the seed crystal cavity is too hard to poke, the edge of the scraper has no radian, the corner cannot be attached, the corner is easy to slide to shovel to the seed crystal cavity to damage, and meanwhile, an interlayer is easy to permeate into a polishing process by using water sand paper, causes impurity contamination, and therefore, in order to improve the crystal growth rate, the use frequency of the crucible, the repair integrity and the repair efficiency, a new method for repairing the seed crystal cavity of the PBN crucible needs to be developed.
Disclosure of Invention
Aiming at the problems, the invention aims to disclose a PBN crucible seed crystal cavity repairing method, which improves the repairing efficiency of a crucible, reduces the probability of damaging the crucible, improves the using times of the crucible, ensures that the repaired surface of the crucible is smoother and smoother, and further improves the yield of single crystals.
In the method for repairing the seed crystal cavity of the PBN crucible, an electric polishing pen is adopted to carry out graded polishing and repairing treatment on the surface of the crucible.
Further, the repairing method specifically comprises the following operations:
1) selecting a 200-mesh straight barrel polishing head for the electric polishing pen, and polishing the part with the step in the crucible seed crystal cavity at the rotating speed of 200r/min until the step is passivated;
2) replacing the electric grinding pen with a 400-mesh straight barrel grinding head, and grinding the peripheral part of the step at the rotating speed of 500r/min until the step and the periphery are completely transited to be flat;
3) replacing an electric polishing pen with a 800-mesh straight barrel polishing head, polishing the whole seed crystal cavity at the rotating speed of 1000r/min until the whole seed crystal cavity is cylindrical in structure, smooth in surface and free of steps, and the color is uniform and free of shadows when the seed crystal cavity is seen under a strong light;
4) and (3) repeating the operation methods of the steps 1) and 3), and replacing the straight-tube polishing head with a conical polishing head to repair the cone part of the corner of the crucible.
Further, the diameter size of the straight tube polishing head is 4-10 mm, and the diameter size of the large end of the conical polishing head is 4-10 mm.
Further, the repairing method also comprises a cleaning step before repairing the crucible, and specifically comprises the following steps: and cleaning the demoulded crucible by using a mixed acid solution, cleaning the crucible by using deionized water, and naturally airing moisture.
Further, the mixed acid solution comprises nitric acid, hydrofluoric acid and deionized water, wherein the volume ratio of the nitric acid to the hydrofluoric acid to the deionized water is 4:2: 1.
Further, after the cleaning step, before the repairing step, a pretreatment step is further included, and the pretreatment step specifically comprises: taking a naturally dried crucible, cleaning the seriously and roughly peeled inner surface by using an oil painting knife, and then polishing the inner surface body to be flat and smooth by using 600-mesh diamond abrasive paper.
The invention has the beneficial effects that:
the invention discloses a PBN crucible seed crystal cavity repairing method, which repairs a crucible seed crystal cavity and a corner position by using a polishing head through an electric polishing pen, and compared with the traditional repairing method, the repairing efficiency is improved by 50 percent, the probability of damaging crucibles is greatly reduced, and the average using times of each crucible is improved; and after the repair, the crucible surface can reach the smooth and flat use standard, the repair effect is better, the probability of generation of polycrystal and twin crystal in the growth process of the single crystal is further reduced, and the yield of the single crystal is improved.
Detailed description of the invention
The present invention will be described in detail with reference to specific examples below:
according to the PBN crucible seed crystal cavity repairing method, the electric polishing pen is adopted to polish and repair the surface of the crucible in a grading manner, compared with the traditional repairing method, the repairing efficiency is better, the effect is better, the damage probability of the crucible can be greatly reduced, and the method specifically comprises the following steps:
examples
Cleaning: respectively taking nitric acid, hydrofluoric acid and deionized water according to the volume ratio of 4:2:1, stirring and mixing uniformly to obtain a mixed acid solution, cleaning the demolded crucible with the mixed acid solution, dissolving residual metal impurities on the surface of the crucible, cleaning with deionized water, and naturally drying in the air.
Pretreatment: the method comprises the steps of taking a naturally dried crucible, cleaning the seriously and roughly peeled inner surface of the crucible by using an oil painting knife, and then polishing the inner surface body part to be flat and smooth by using 600-mesh diamond abrasive paper, wherein the diamond abrasive paper has a single component, so that impurity pollution cannot be brought to the crucible in the polishing process.
Repairing: the grinding head is characterized in that an electric grinding pen is selected to be a straight cylinder grinding head with 200 meshes, the diameter size is 5mm, the length size is 14mm, the part with steps in a crucible seed crystal cavity is ground at the rotating speed of 200r/min until the steps are passivated, the electric grinding pen is replaced by the straight cylinder grinding head with 400 meshes, the part around the steps is ground at the rotating speed of 500r/min until the steps and the periphery are completely transited to be smooth, the electric grinding pen is replaced by the straight cylinder grinding head with 800 meshes, the whole seed crystal cavity is ground at the rotating speed of 1000r/min until the whole seed crystal cavity is cylindrical, the surface is smooth, no steps exist, and the color is uniform and has no shadow under a highlight lamp.
Repeating the operation method, replacing the straight polishing head with the conical polishing head to repair the cone part of the crucible corner, specifically comprising the following steps:
the electric polishing pen is selected to be 200 meshes, the diameter of the large end is 6mm, the length of the electric polishing pen is 15mm, the conical polishing head is used for polishing the part, with the step, of the cone part of the crucible corner at the speed of 200r/min, until the step is passivated, the electric polishing pen is replaced by the conical polishing head with 400 meshes at the speed of 500r/min, the part around the step is polished, the step and the periphery are completely transited to be smooth, the electric polishing pen is replaced by the conical polishing head with 800 meshes, the whole cone part is polished at the speed of 1000r/min, the whole surface of the cone part at the crucible corner is smooth and has no step, the color is uniform and has no shadow under a highlight lamp, and the repair is completed.
Comparative example
The comparative example repairs the crucible seed crystal cavity by adopting the existing repair method, and specifically comprises the following steps:
respectively taking hydrochloric acid and nitric acid according to a volume ratio of 3:1, stirring and mixing uniformly to obtain a aqua regia solution, cleaning a demolded crucible with the aqua regia solution, dissolving residual metal impurities on the surface of the crucible, cleaning with deionized water, naturally drying water, taking the naturally dried crucible, cleaning the seriously peeled and rough part of the inner surface of the corner of a seed crystal cavity by using an oil painting knife, poking the seriously peeled and rough part of the inner surface of the seed crystal cavity by using a ceramic stick or a stainless steel iron sheet, and finally winding waterproof abrasive paper on the surface of the ceramic stick to polish the inner surface of the seed crystal cavity to be flat and smooth as much as possible to finish repairing.
The method of the embodiment and the method of the comparative example are respectively used for repairing the seed crystal cavity of the crucible used for growing the indium phosphide single crystal, the repairing time, the using times of the crucible and the single crystal yield are monitored and recorded, and the results are shown in the following tables 1 and 2:
table 1 examples repair methods crucible usage records
Table 2 comparative example repair method crucible usage record
As can be seen from the comparison of the table 1 and the table 2, by using the PBN crucible seed crystal cavity repairing method, the repairing time of the crucible is obviously shortened from 4h to 2h, the repairing efficiency is doubled, the using times of the crucible are obviously improved, the average using times are improved from 2.9 times to 4.1 times, and the average yield of single crystals is also improved from 24.95% to 31.59%.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (5)
1. A PBN crucible seed crystal cavity repairing method is characterized in that an electric polishing pen is adopted to carry out graded polishing repairing treatment on the surface of a crucible;
the repairing method specifically comprises the following operations:
1) selecting a 200-mesh straight barrel polishing head for the electric polishing pen, and polishing the part with the step in the crucible seed crystal cavity at the rotating speed of 200r/min until the step is passivated;
2) replacing the electric grinding pen with a 400-mesh straight barrel grinding head, and grinding the peripheral part of the step at the rotating speed of 500r/min until the step and the periphery are completely transited to be flat;
3) replacing an electric polishing pen with a 800-mesh straight barrel polishing head, polishing the whole seed crystal cavity at the rotating speed of 1000r/min until the whole seed crystal cavity is cylindrical in structure, smooth in surface and free of steps, and the color is uniform and free of shadows when the seed crystal cavity is seen under a strong light;
4) and (3) repeating the operation methods of the steps 1) and 3), and replacing the straight-tube polishing head with a conical polishing head to repair the cone part of the corner of the crucible.
2. The PBN crucible seed crystal cavity repairing method as claimed in claim 1, wherein the diameter size of the straight tube polishing head is 4-10 mm, and the diameter size of the large end of the conical polishing head is 4-10 mm.
3. The PBN crucible seed crystal cavity repairing method according to claim 1, wherein the repairing method further comprises a cleaning step before repairing the crucible, specifically: and cleaning the demoulded crucible by using a mixed acid solution, cleaning the crucible by using deionized water, and naturally airing moisture.
4. The PBN crucible seed crystal cavity repairing method according to claim 3, wherein the mixed acid solution comprises nitric acid, hydrofluoric acid and deionized water, and the volume ratio of the nitric acid to the hydrofluoric acid to the deionized water is 4:2: 1.
5. The method for repairing a PBN crucible seed crystal cavity as claimed in any one of claims 3 or 4, further comprising a pretreatment step after the cleaning step and before the repairing, wherein the pretreatment step is specifically as follows: taking a naturally dried crucible, cleaning the seriously and roughly peeled inner surface by using an oil painting knife, and then polishing the inner surface body to be flat and smooth by using 600-mesh diamond abrasive paper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010904396.8A CN112247678B (en) | 2020-09-01 | 2020-09-01 | PBN crucible seed crystal cavity repairing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010904396.8A CN112247678B (en) | 2020-09-01 | 2020-09-01 | PBN crucible seed crystal cavity repairing method |
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| Publication Number | Publication Date |
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| CN112247678A CN112247678A (en) | 2021-01-22 |
| CN112247678B true CN112247678B (en) | 2022-04-22 |
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| CN202010904396.8A Active CN112247678B (en) | 2020-09-01 | 2020-09-01 | PBN crucible seed crystal cavity repairing method |
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| CN114737245B (en) * | 2022-04-26 | 2023-10-24 | 广东先导微电子科技有限公司 | PBN crucible maintenance device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101735904A (en) * | 2008-11-20 | 2010-06-16 | Axt公司 | Cleaning solution and cleaning method adopting same |
| CN102776509B (en) * | 2012-08-13 | 2014-04-16 | 北京博宇半导体工艺器皿技术有限公司 | Method for repairing surface of used pyrolytic boron nitride crucible |
| CN104493653B (en) * | 2014-11-29 | 2017-08-15 | 域鑫科技（惠州）有限公司 | A kind of endoporus grinding and polishing device |
| CN107914202A (en) * | 2017-12-18 | 2018-04-17 | 江苏润弛太阳能材料科技有限公司 | A kind of solar energy quartz crucible processing and manufacturing sanding apparatus |
| CN108866630A (en) * | 2018-07-25 | 2018-11-23 | 汉能新材料科技有限公司 | A kind of gallium arsenide polycrystal synthetic method |
| CN210678205U (en) * | 2019-05-08 | 2020-06-05 | 上海澳圣商务有限公司 | Multifunctional polishing pen |
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