CN106702491A - Method for extracting GaN single crystal from product of Na flux method - Google Patents
Method for extracting GaN single crystal from product of Na flux method Download PDFInfo
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- CN106702491A CN106702491A CN201510793586.6A CN201510793586A CN106702491A CN 106702491 A CN106702491 A CN 106702491A CN 201510793586 A CN201510793586 A CN 201510793586A CN 106702491 A CN106702491 A CN 106702491A
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- single crystal
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- sodium
- gan single
- gallium
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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
- C30B29/38—Nitrides
-
- 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
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
- C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
- C30B9/10—Metal solvents
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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 invention provides a method for extracting a GaN single crystal from a product of a Na flux method. According to the invention, low-carbon alcohols (including methanol, ethanol, propanol, butanol and isomers thereof) are used to remove metallic sodium; and aqua regia is used to remove a metastable phase which is covered on the surface of the GaN single crystal and composed of gallium/nitrogen elements and a binary alloy constituted by gallium/sodium elements. Under the premise of safe and controllable extraction process, a pure GaN single crystal can be obtained.
Description
Technical field
The present invention relates to technical field of semiconductor, the method that GaN single crystal is extracted in specifically a kind of stream method product from sodium.
Background technology
Nitride with gallium nitride (GaN) as representative is just increasingly becoming photoelectron and the common semi-conducting material of microelectronic.At present, the growing method of GaN crystal mainly has hydride gas-phase epitaxy (Hydride vapor phase epitaxy), high temperature and high pressure method (High nitrogen pressure solution), the hot method of ammonia (Ammothermal growth method) and sodium stream method (Na flux method).Because the growth conditions needed for crystal is moderate, sodium stream method is increasingly becoming the optimization technique for preparing GaN single crystal material.
In sodium stream method, the product after the completion of GaN single crystal growth mainly includes the metastable phase (accessory substance generated in course of reaction) of the bianry alloy (accessory substance generated in course of reaction) of GaN crystal (target product), gallium (remaining excessive raw material), metallic sodium (remaining excessive raw material), gallium/sodium element composition and gallium/nitrogen composition.Wherein, GaN crystal (target product) is needed to retain, and other materials need be removed all.
For gallium, conventional concentrated hydrochloric acid treatment is removed.For metallic sodium, then react and can remove by with water, but, it is well known that metallic sodium is reacted more acutely, if easily being exploded when its amount is big with water, target product GaN crystal, and harm worker safety can be not only destroyed, so being not practicable in the method for extract GaN single crystal.In addition, gallium/itself is more stable for the metastable phase of the bianry alloy of sodium element composition and gallium/nitrogen composition, removal is also a difficult point.
The content of the invention
A kind of method the invention discloses GaN single crystal is extracted in stream method product from sodium, metallic sodium is removed by using low alcohol (including first, second, third, butanol and its isomer) and the metastable phase that the bianry alloy and gallium/nitrogen of the gallium/sodium element composition for being covered in GaN single crystal surface are constituted is eliminated using chloroazotic acid, on the premise of extraction process is safely controllable, more pure GaN single crystal is can obtain.
The method that GaN single crystal is extracted in a kind of stream method product from sodium of the present invention, comprises the following steps：
Step 1, in sodium stream method product, add low alcohol to remove metallic sodium, after bubble-free is emerged, reacted solution is outwelled；
Step 2, to step 1 process after product in add concentrated hydrochloric acid, question response to remove gallium completely after, solution is outwelled；
In step 3, the product after step 2 treatment, add chloroazotic acid to soak more than 2 hours, after removal is covered in the metastable phase of the bianry alloy of the gallium on GaN single crystal surface/sodium element composition and gallium/nitrogen composition, solution is outwelled；
Step 4, using deionized water, be that GaN single crystal is cleaned to the product after step 3 treatment, then dry, obtain required GaN single crystal.
Further, the sodium stream method product in step 1, mainly including the metastable phase of GaN crystal, gallium, metallic sodium, the bianry alloy of gallium/sodium element composition and gallium/nitrogen composition；The low alcohol is one kind or any several combination in methyl alcohol, ethanol, propyl alcohol, butanol and corresponding all isomers；Described low alcohol, concentrated hydrochloric acid and chloroazotic acid, its amount for being added, all be for whole removal reaction it is excessive, it is described it is excessive refer to added low alcohol, concentrated hydrochloric acid and chloroazotic acid the metastable phase of metallic sodium, the bianry alloy of gallium and the gallium/sodium element composition for being covered in GaN single crystal surface and gallium/nitrogen composition that can be enough to remove respectively in the sodium stream method product of amount.
Specific embodiment
For the ease of the understanding of those skilled in the art, below the invention will be further described.
Embodiment one, a kind of method that GaN single crystal is extracted in stream method product from sodium, comprises the following steps：
Step 1, in sodium stream method product, add excessive low alcohol, low alcohol and metallic sodium reaction (2Na+2ROH=2RONa+H in sodium stream method product2↑, ROH represents low alcohol), to remove metallic sodium, after bubble-free is emerged, reacted solution is outwelled；
Step 2, with concentrated hydrochloric acid soaking step 1 process after product, after question response terminates, solution is outwelled.
In step 3, the product after step 2 treatment, chloroazotic acid is added, soaked 2 hours, reacted solution is outwelled；Chloroazotic acid is added again, until after reaction removal completely is covered in the metastable phase of the bianry alloy of the gallium on GaN single crystal surface/sodium element composition and gallium/nitrogen composition, solution is outwelled.
Step 4, using deionized water, be GaN single crystal to the product after step 3 treatment, cleaned, then dry, obtain required GaN single crystal.
Additionally, for above is referred to low alcohol, the one kind being in methyl alcohol, ethanol, propyl alcohol, butanol and corresponding all isomers or any several combination.
It should be noted that the above is not the restriction to technical solution of the present invention, on the premise of creation design of the invention is not departed from, any obvious replacement is within protection scope of the present invention.
Claims (4)
1. a kind of method that GaN single crystal is extracted in stream method product from sodium, it is characterised in that bag
Include following steps：
Step 1, in sodium stream method product, add low alcohol, after bubble-free is emerged, will be anti-
Solution after answering is outwelled；
Step 2, to step 1 process after product in add concentrated hydrochloric acid, question response complete after,
Solution is outwelled；
In step 3, the product after step 2 treatment, chloroazotic acid is added to soak more than 2 hours,
Reacted solution is outwelled；
Step 4, using deionized water, be that GaN single crystal is carried out to the product after step 3 treatment
Cleaning, then dries, and obtains required GaN single crystal.
2. GaN single crystal is extracted in a kind of stream method product from sodium according to claim 1
Method, it is characterised in that the sodium stream method product in step 1, mainly including GaN crystal,
The bianry alloy and gallium of gallium, metallic sodium, gallium/sodium element composition/nitrogen composition
Metastable phase.
3. GaN single crystal is extracted in a kind of stream method product from sodium according to claim 1
Method, it is characterised in that the low alcohol, be methyl alcohol, ethanol, propyl alcohol, butanol and and its
One kind or any several combination in corresponding isomer.
4. GaN single crystal is extracted in a kind of stream method product from sodium according to claim 1
Method, it is characterised in that described low alcohol, concentrated hydrochloric acid and chloroazotic acid its amount for being added,
All it is excessive for whole removal reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510793586.6A CN106702491A (en) | 2015-11-18 | 2015-11-18 | Method for extracting GaN single crystal from product of Na flux method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510793586.6A CN106702491A (en) | 2015-11-18 | 2015-11-18 | Method for extracting GaN single crystal from product of Na flux method |
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| CN106702491A true CN106702491A (en) | 2017-05-24 |
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| CN201510793586.6A Pending CN106702491A (en) | 2015-11-18 | 2015-11-18 | Method for extracting GaN single crystal from product of Na flux method |
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| CN (1) | CN106702491A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680604A (en) * | 2019-10-17 | 2021-04-20 | 丰田合成株式会社 | Method for producing gallium, method for producing sodium, and method for producing gallium nitride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5868837A (en) * | 1997-01-17 | 1999-02-09 | Cornell Research Foundation, Inc. | Low temperature method of preparing GaN single crystals |
| US20010023942A1 (en) * | 2000-03-23 | 2001-09-27 | Samsung Electronics Co., Ltd. | Semiconductor device of heterojunction structure having quantum dot buffer layer |
-
2015
- 2015-11-18 CN CN201510793586.6A patent/CN106702491A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5868837A (en) * | 1997-01-17 | 1999-02-09 | Cornell Research Foundation, Inc. | Low temperature method of preparing GaN single crystals |
| US20010023942A1 (en) * | 2000-03-23 | 2001-09-27 | Samsung Electronics Co., Ltd. | Semiconductor device of heterojunction structure having quantum dot buffer layer |
Non-Patent Citations (1)
| Title |
|---|
| FUMIO KAWAMURA ET AL.: "LPE Growth of Bulk GaN crystal by alkali-metal flux method", 《MATERIALS SCIENCE FORUM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680604A (en) * | 2019-10-17 | 2021-04-20 | 丰田合成株式会社 | Method for producing gallium, method for producing sodium, and method for producing gallium nitride |
| CN112680604B (en) * | 2019-10-17 | 2023-02-17 | 丰田合成株式会社 | Method for producing gallium, method for producing sodium, and method for producing gallium nitride |
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Application publication date: 20170524 |