CN112160032A - Crystal processing method - Google Patents
Crystal processing method Download PDFInfo
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- CN112160032A CN112160032A CN202010914622.0A CN202010914622A CN112160032A CN 112160032 A CN112160032 A CN 112160032A CN 202010914622 A CN202010914622 A CN 202010914622A CN 112160032 A CN112160032 A CN 112160032A
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- crystal
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- magnetized
- crystals
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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
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
- C30B35/007—Apparatus for preparing, pre-treating the source material to be used for crystal growth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- 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
- C30B29/36—Carbides
-
- 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
- C30B29/403—AIII-nitrides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The embodiment of the invention relates to the technical field of crystal processing, and discloses a crystal processing method. The method comprises the following steps: removing particle impurities in the crystal by using ultrasonic; treating the crystal by using a primary magnetized emulsion to remove metal impurities on the surface of the crystal; treating the crystal by using a secondary magnetized emulsion to remove deep particle impurities on the surface of the crystal; the crystals were purged with volatile solvent under nitrogen sparge. And blowing the crystal by using a volatile solvent under the environment of ultrasonic treatment, chemical soaking and medium nitrogen to prepare the ultra-clean seed crystal, thereby providing technical support for the mass production and commercialization of the seed crystal.
Description
Technical Field
The embodiment of the invention relates to the technical field of crystal processing, in particular to a crystal processing method.
Background
The seed crystal is the core material for producing silicon carbide/aluminum nitride single crystal by PVT (physical vapor transport) method, and the cleanliness level of the seed crystal determines the quality of the produced single crystal. Currently, no techniques are reported for systematic processing of seed crystals.
Disclosure of Invention
An object of an embodiment of the present invention is to provide a method for processing a seed crystal, which can greatly improve the seed crystal quality with respect to cleanliness.
In order to solve the above technical problem, an embodiment of the present invention provides a crystal processing method, including:
removing particle impurities in the crystals by using ultrasound;
treating the crystal by using a primary magnetized emulsion to remove metal impurities on the surface of the crystal;
treating the crystal by using a secondary magnetized emulsion to remove deep particle impurities on the surface of the crystal;
purging the crystals with a volatile solvent under nitrogen charging.
Further optionally, the purging the crystals with a volatile solvent comprises:
purging the crystals with ethanol for a first predetermined period of time;
and/or the presence of a gas in the gas,
purging the crystals with acetone for a second predetermined period of time.
Further optionally, the ethanol concentration is 95% to 99.99%, and/or the acetone concentration is 99.99%.
Further optionally, the first preset time period is 20 minutes, and/or the second preset time period is 30 minutes.
Further optionally, the primary magnetized emulsion comprises: one or more of ferroferric oxide, wool acid and deionized water.
Further optionally, the secondary magnetized emulsion comprises: one or more of sodium silicate, deionized water, ZnCl and graphite fluoride.
Further optionally, the step of processing the crystal by using the first-stage magnetized emulsion comprises: and putting the crystal into the primary magnetized emulsion, wherein the temperature of the primary magnetized emulsion is set to be 60 ℃, and emulsifying for 2-4 h.
Further optionally, the processing of the crystals with the secondary magnetized emulsion comprises: and (3) putting the crystal into the secondary magnetized emulsion, and emulsifying for 3-8 h.
Further optionally, the removing of the particle impurities in the crystal by using ultrasound is: fixing the crystal in deionized water at 60 ℃ by using a fixing frame, soaking for 5h, then washing with ultrasonic water, setting the ultrasonic power at 10W-30W, performing ultrasonic treatment for 10min-20min, then taking out, and air-drying until the surface water content is 5%.
Further optionally, the first-stage magnetized emulsion comprises the following components: 5% of ferroferric oxide, 30% of wool acid and 65% of deionized water.
Further optionally, the secondary magnetized emulsion comprises the following components: dispersing 30% sodium silicate into deionized water, adding ZnCl accounting for 10-20% of the total amount of the sodium silicate, and adding graphite fluoride for ultrasonic dispersion for 30 min.
Further optionally, the method further includes:
and (5) conveying the crystals into a sealed tank for storage.
Compared with the prior art, the method provided by the embodiment of the invention has the advantages that the crystal is purged by using the volatile solvent under the environment of ultrasonic treatment, chemical soaking and medium nitrogen, so that the ultra-clean seed crystal is prepared, and the technical support is provided for the mass production and commercialization of the seed crystal.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
One or more embodiments are illustrated by way of example in the accompanying drawings, which correspond to the figures in which like reference numerals refer to similar elements and which are not to scale unless otherwise specified.
FIG. 1 is a schematic flow chart of a method for enhancing the processing of a crystal according to an embodiment of the present invention;
fig. 2 is a schematic structural view of a seal pot according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, embodiments of the present invention will be described in detail below with reference to the accompanying drawings. However, it will be appreciated by those of ordinary skill in the art that numerous technical details are set forth in order to provide a better understanding of the present application in various embodiments of the present invention. However, the technical solution claimed in the present application can be implemented without these technical details and various changes and modifications based on the following embodiments. The following embodiments are divided for convenience of description, and should not constitute any limitation to the specific implementation manner of the present invention, and the embodiments may be mutually incorporated and referred to without contradiction.
A first embodiment of the present invention relates to a crystal processing method, the flow of which is shown in fig. 1, and specifically includes the following steps:
101. removing particle impurities in the crystal by using ultrasonic;
102. treating the crystal by using a primary magnetized emulsion to remove metal impurities on the surface of the crystal;
103. treating the crystal by using a secondary magnetized emulsion to remove deep particle impurities on the surface of the crystal;
104. the crystals were purged with volatile solvent under nitrogen sparge.
Compared with the prior art, the method provided by the embodiment of the invention has the advantages that the crystal is purged by using the volatile solvent under the environment of ultrasonic treatment, chemical soaking and medium nitrogen, so that the ultra-clean seed crystal is prepared, and the technical support is provided for the mass production and commercialization of the seed crystal.
Implementation details of the crystal processing method according to the present embodiment are specifically described below, and the following description is provided only for the sake of understanding and is not necessary for implementing the present embodiment.
Purging the crystals with the volatile solvent in step 104 in this embodiment may include, but is not limited to, the following steps:
A. purging the crystals with ethanol for a first predetermined period of time;
and/or the presence of a gas in the gas,
B. purging the crystals with acetone for a second predetermined period of time.
In some alternative embodiments, the concentration of ethanol may be selected from, but not limited to, 95% to 99.99%, and/or the concentration of acetone may be selected from, but not limited to, 99.99%. The implementation proves that the purging time can be shortened by improving the purity of the ethanol and the acetone, and the crystal treatment efficiency is effectively improved.
In some alternative embodiments, the first predetermined period may be selected, but is not limited to, 20 minutes, and/or the second predetermined period may be selected, but is not limited to, 30 minutes.
In some alternative embodiments, the primary magnetized emulsion may include, but is not limited to: one or more of ferroferric oxide, wool acid and deionized water.
In some alternative embodiments, the secondary magnetized emulsion may include, but is not limited to: one or more of sodium silicate, deionized water, ZnCl and graphite fluoride.
In some alternative embodiments, the step 102 of treating the crystals with the primary magnetized emulsion may be: and putting the crystal into the primary magnetized emulsion, setting the temperature of the primary magnetized emulsion at 60 ℃, and emulsifying for 2-4 hours.
In some alternative embodiments, the step 103 of treating the crystals with the secondary magnetized emulsion may be: and putting the crystal into the secondary magnetized emulsion, and emulsifying for 3-8 hours.
In some alternative embodiments, the step 101 of removing the particle-type impurities in the crystals by using ultrasound may be: fixing the crystal in deionized water at 60 ℃ by using a fixing frame, soaking for 5 hours, then washing with ultrasonic water, setting the ultrasonic power between 10W and 30W and the ultrasonic time between 10 minutes and 20 minutes, then taking out, and air-drying until the surface water content is 5%.
In some alternative embodiments, the primary magnetized emulsion may specifically be: 5% of ferroferric oxide, 30% of wool acid and 65% of deionized water.
In some alternative embodiments, the secondary magnetized emulsion may specifically be: dispersing 30% sodium silicate into deionized water, adding ZnCl accounting for 10-20% of the total amount of the sodium silicate, and adding graphite fluoride for ultrasonic dispersion for 30 minutes.
In some alternative embodiments, the crystals are stored in a sealed container after they have been processed by the above steps for good storage.
Referring to fig. 2, the sealed storage tank structure according to the embodiment of the present invention includes: lower box body 1, sealed pad 2, sealed collude 3, spring 4, first round pin axle 5, go up box body 6 and second round pin axle 7.
Wherein, the border of lower box body 1 and the border of last box body 6 are connected through first round pin axle 5, and it is rotatory that last box body 6 can use first round pin axle 5 as the axle center, goes up box body 6 and rotates to different positions, makes box body 1 and last box body 6 be the open or closed state down, and at the closed state, form the holding cavity that is used for placing the crystal down between box body 1 and the last box body 6.
The gasket 2 is disposed at a portion where the lower case 1 and the upper case 6 are coupled for increasing sealability.
Sealed 3 colluding is fixed on last box body 6 through second round pin axle 7, and sealed 3 colluding is close to colluding the sharp position and is connected with second round pin axle 7 through spring 4, and 1 border of lower box body and sealed position of colluding the correspondence are equipped with fixed fastener, and sealed 3 colluding is on fixed fastener through the pulling force card of spring 4.
In order to avoid crystal damage, a soft layer (not shown in the figure) is arranged inside the sealing can, and the outside of the sealing can needs to be sealed in order to avoid damage caused by the external environment.
The crystal processing method provided by the embodiment of the invention comprises the steps of firstly carrying out ultrasonic washing to remove particle impurities, then carrying out primary magnetized emulsion processing to remove metal impurities, then carrying out secondary emulsion processing to add graphite fluoride, removing organic matters by purging with ethanol and acetone under the condition of filling nitrogen, then putting the mixture into a high-temperature-resistant closed storage device, and processing the mixture in a drying box at 150 ℃ to obtain factory ultra-clean seed crystals, thereby effectively improving the cleanliness of the crystals, realizing the preparation of the ultra-clean seed crystals and preparing a crystal packaging device for factory production. The crystal has high cleanliness requirement, and is necessary to be dust-free and sterile, and no commercialized crystal exists at present, so that an ultra-clean crystal commodity can be obtained by the method, the production requirement of a sterile room with high configuration cost of a crystal producer is effectively met, and the method is low in cost, can be applied in an industrial mode and is pollution-free.
The steps of the above methods are divided for clarity, and the implementation may be combined into one step or split some steps, and the steps are divided into multiple steps, so long as the same logical relationship is included, which are all within the protection scope of the present patent; it is within the scope of the patent to add insignificant modifications to the algorithms or processes or to introduce insignificant design changes to the core design without changing the algorithms or processes.
The crystal processing method provided by the embodiment of the invention, the seed crystal processing, can be particularly used for processing the silicon carbide/aluminum nitride seed crystal, and for the convenience of readers to understand the method, the seed crystal is described in detail in the following, specifically as follows:
and 2, putting the silicon carbide/aluminum nitride seed crystals into a primary magnetized emulsion for treatment, setting the temperature of the emulsion at 60 ℃, and emulsifying for 2-4 hours. The metal impurities on the surface of the seed crystal are removed, and the iron on the surface of the seed crystal is mainly removed.
And 3, taking out the seed crystals after the first-stage emulsification treatment, putting the seed crystals into the second-stage emulsification treatment liquid, and emulsifying for 3-8h to remove deep particle impurities in the second-stage emulsification treatment liquid, wherein the deep particle impurities are mainly used for removing organic matters on the surfaces of the seed crystals.
Wherein, the first-stage magnetization emulsification treatment comprises the following components: 5% of ferroferric oxide, 30% of wool acid and 65% of deionized water. Firstly, mixing wool acid and deionized water uniformly, then adding ferroferric oxide, and mixing uniformly by ultrasonic waves.
And 4, blowing the seed crystals after the secondary emulsification in 95 percent ethanol for 20 minutes under the condition of filling nitrogen, and continuously blowing the seed crystals for 30 minutes by using 99.99 percent acetone.
The components of the secondary emulsion are as follows: dispersing 30% sodium silicate into deionized water, then adding ZnCl accounting for 10-20% of the total amount of the sodium silicate, and then adding graphite fluoride for ultrasonic dispersion for 30 min.
And 5, taking out the seed crystals by using the sterile gloves, putting the seed crystals into a designed sealing device, storing the seed crystals, and drying the seed crystals in a high-temperature drying box, wherein the temperature of the high-temperature drying box is set as follows: 150 ℃ for 1.5 h.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.
Claims (12)
1. A method of crystal processing, comprising:
removing particle impurities in the crystal by using ultrasonic;
treating the crystal by using a primary magnetized emulsion to remove metal impurities on the surface of the crystal;
treating the crystal by using a secondary magnetized emulsion to remove deep particle impurities on the surface of the crystal;
purging the crystals with a volatile solvent under nitrogen charging.
2. The method of claim 1, wherein the purging the crystal with a volatile solvent comprises:
purging the crystals with ethanol for a first predetermined period of time;
and/or the presence of a gas in the gas,
purging the crystals with acetone for a second predetermined period of time.
3. The method according to claim 2, wherein the ethanol concentration is 95% to 99.99%, and/or the acetone concentration is 99.99%.
4. The method according to claim 2, characterized in that said first preset duration is 20 minutes and/or said second preset duration is 30 minutes.
5. The method of any one of claims 1 to 4, wherein the primary magnetized emulsion comprises: one or more of ferroferric oxide, wool acid and deionized water.
6. The method of any one of claims 1 to 4, wherein the secondary magnetized emulsion comprises: one or more of sodium silicate, deionized water, ZnCl and graphite fluoride.
7. The method according to any one of claims 1 to 4, wherein the treating the crystals with the primary magnetized emulsion is: and putting the crystal into the primary magnetized emulsion, wherein the temperature of the primary magnetized emulsion is set to be 60 ℃, and emulsifying for 2-4 h.
8. The method according to any one of claims 1 to 4, wherein the treating the crystals with the secondary magnetized emulsion is: and (3) putting the crystal into the secondary magnetized emulsion, and emulsifying for 3-8 h.
9. The method according to any one of claims 1 to 4, wherein the removing of the particle-like impurities in the crystals by using ultrasound is: fixing the crystal in deionized water at 60 ℃ by using a fixing frame, soaking for 5h, then washing with ultrasonic water, setting the ultrasonic power at 10W-30W, performing ultrasonic treatment for 10min-20min, then taking out, and air-drying until the surface water content is 5%.
10. The method of any one of claims 1 to 4, wherein the primary magnetized emulsion has a composition of: 5% of ferroferric oxide, 30% of wool acid and 65% of deionized water.
11. The method according to any one of claims 1 to 4, wherein the secondary magnetized emulsion has the following composition: dispersing 30% sodium silicate into deionized water, adding ZnCl accounting for 10-20% of the total amount of the sodium silicate, and adding graphite fluoride for ultrasonic dispersion for 30 min.
12. The method of any of claims 1 to 4, further comprising:
and (5) conveying the crystals into a sealed tank for storage.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010914622.0A CN112160032A (en) | 2020-09-03 | 2020-09-03 | Crystal processing method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010914622.0A CN112160032A (en) | 2020-09-03 | 2020-09-03 | Crystal processing method |
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| CN112160032A true CN112160032A (en) | 2021-01-01 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09309799A (en) * | 1996-05-22 | 1997-12-02 | Sumitomo Metal Ind Ltd | Surface treatment for magnesium oxide single crystal substrate |
| CN101775662A (en) * | 2010-01-26 | 2010-07-14 | 宜昌南玻硅材料有限公司 | Etch-cleaning method for high purity polycrystalline silicon briquette |
| CN102500573A (en) * | 2011-11-08 | 2012-06-20 | 哈尔滨工业大学 | Method for cleaning alpha-Al2O3 monocrystal |
| CN109622503A (en) * | 2018-12-04 | 2019-04-16 | 天津津航技术物理研究所 | A kind of lossless cleaning method after laser gyro cavity optical manufacturing |
| CN109849202A (en) * | 2018-12-28 | 2019-06-07 | 天津洙诺科技有限公司 | A kind of not mulberry brill process for treating surface |
-
2020
- 2020-09-03 CN CN202010914622.0A patent/CN112160032A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09309799A (en) * | 1996-05-22 | 1997-12-02 | Sumitomo Metal Ind Ltd | Surface treatment for magnesium oxide single crystal substrate |
| CN101775662A (en) * | 2010-01-26 | 2010-07-14 | 宜昌南玻硅材料有限公司 | Etch-cleaning method for high purity polycrystalline silicon briquette |
| CN102500573A (en) * | 2011-11-08 | 2012-06-20 | 哈尔滨工业大学 | Method for cleaning alpha-Al2O3 monocrystal |
| CN109622503A (en) * | 2018-12-04 | 2019-04-16 | 天津津航技术物理研究所 | A kind of lossless cleaning method after laser gyro cavity optical manufacturing |
| CN109849202A (en) * | 2018-12-28 | 2019-06-07 | 天津洙诺科技有限公司 | A kind of not mulberry brill process for treating surface |
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Application publication date: 20210101 |