CN106591952A - Preparation method of SiC wafer - Google Patents
Preparation method of SiC wafer Download PDFInfo
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- CN106591952A CN106591952A CN201611126092.3A CN201611126092A CN106591952A CN 106591952 A CN106591952 A CN 106591952A CN 201611126092 A CN201611126092 A CN 201611126092A CN 106591952 A CN106591952 A CN 106591952A
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- sic
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Classifications
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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
- C30B29/36—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
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
-
- 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
- C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
- C30B31/02—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion materials in the solid state
Abstract
The invention relates to a preparation method of a SiC wafer. The method comprises the following steps that 1, high-purity silicon powder and carbon powder are adopted as raw materials, under the condition of high vacuum, high-purity argon is introduced, the materials are placed in a graphite crucible with a coating for high-temperature synthesis, and high-purity SiC powder low in nitrogen concentration and boron concentration is obtained; 2, under the condition of high vacuum, high-purity argon or a mixed gas of argon and hydrogen is introduced, the SiC powder is placed in the graphite crucible with a coating for high-temperature pretreatment, and doping is conducted through a solid-state source; 3, a grown single crystal is subjected to rolling and orientation treatment, a standard crystal ingot is obtained, and by means of multi-line cutting and grinding and polishing treatment, a semi-insulating SiC polished section is obtained; 4, under the vacuum condition, the wafer is heated and kept for 2-10 h, cooling is conducted for 10-20 h, and the SiC wafer is obtained. The preparation method has the advantages that the prepared SiC crystal is high in electrical resistivity and low in defect, and the quality of the crystal is improved.
Description
Technical field
The present invention relates to a kind of preparation method of the semi-insulating chip of high resistivity low defect, and in particular to a kind of SiC wafer
Preparation method, belong to SiC single crystal growing technology class field.
Background technology
Carborundum（SiC）As third generation semiconductor material with wide forbidden band, with its superior physical characteristics of materials, high temperature,
High frequency, high power electronic field are widely used.Although nearest SiC single crystal diameter and crystal mass aspect have all improved,
A large amount of defects in SiC single crystal hinder its further commercial applications.And the semi-insulating silicon carbide with high resistivity exists
There is relatively low dielectric loss under high frequency, therefore it is microwave GaN base device to prepare high-quality semi insulating silicon carbide silicon substrate
Basis.
For this purpose, how to provide a kind of preparation method of the semi-insulating chip of high resistivity low defect, the crystal matter of the above is solved
Amount problem, is the purpose of present invention research.
The content of the invention
To overcome prior art not enough, the present invention provides a kind of preparation method of SiC wafer, using incorporation deep-level impurity
The mode of vanadium come compensate SiC single crystal growth in all of shallow donor and shallow acceptor energy level, to realize the half insulation of material.
To solve prior art problem, the technical solution adopted in the present invention is：
A kind of preparation method of SiC wafer, comprises the following steps：
Step one, synthesizes high-purity SiC powders:
High-purity silica flour and carbon dust are adopted for raw material, in high vacuum conditions, the mixed of high-purity argon gas or argon gas and hydrogen is passed through
Gas is closed, being placed in the graphite crucible of coating carries out high―temperature nuclei, obtains the high-purity alpha-SiC powder of low nitrogen concentration and boron concentration
Material；
Step 2, the growth of high resistivity semi-insulation SiC crystal:
In high vacuum conditions, the mixed gas of high-purity argon gas or argon gas and hydrogen are passed through, SiC powders has been placed on into coating
Graphite crucible in carry out high temperature pretreatment, and be doped using Solid Source, be grown in being carried out in specific crucible system；
Concentration of the Solid Source concentration more than Nitrogen Impurities；
Step 3, the monocrystalline for growing carries out round as a ball and directional process, obtains the crystal ingot of standard, then through multi-wire saw and grinds
Mill polishing, obtains semi-insulation SiC polished silicon wafer；
Step 4, anneals to semi-insulation SiC polished silicon wafer:
By chip under vacuum, heat, and keep 2-10h, then through temperature fall time 10-20h, obtain and there is high resistance
The semi-insulation SiC chip of rate, low defect.
Further, in described step one, temperature is between 1400-2000 DEG C during high―temperature nuclei.
Further, in described step two, Solid Source adopts vanadium, concentration to select 8 × 1016-1×1017 Individual/cm-3Amount
Level.
Further, in described step two, the concentration of nitrogen impurity is 5 × 1016Individual/cm-3Below.
Further, described step four kind, heating-up temperature is 1600-2000 DEG C.
The invention has the beneficial effects as follows：The resistivity of prepared SiC crystal is high, defect is low；Improve the quality of crystal.
Description of the drawings
Fig. 1 is the preparation flow figure of the present invention.
Specific embodiment
In order that those skilled in the art can more understand technical solution of the present invention, with reference to embodiment to the present invention
It is further analyzed.
The method of currently acquired high-purity semi-insulating SiC wafer is physical vapor transport method（PVT）.So-called PVT methods are just
It is that SiC powders are heated to into 2200-2400 °C, because the indoor raw material of growth has certain stable gradient with seed crystal so as to
Distillation is transferred on cold end seed crystal and crystallizes into bulk crystals.The present invention provides a kind of technical scheme for preparing semi-insulation SiC monocrystalline,
All of shallow donor and shallow acceptor energy level in SiC single crystal growth is compensated i.e. using mixing by the way of deep-level impurity vanadium, with reality
The half insulation of existing material, comprises the following steps that：
Step one：The high-purity SiC powders of synthesis.Adopt high-purity silica flour and carbon dust for raw material, in high vacuum conditions, be passed through height
The mixed gas of pure argon or argon gas and hydrogen, being placed in the graphite crucible of coating carries out 1400-2000 DEG C of high temperature
Synthesis, obtains the high-purity alpha-SiC powder of low nitrogen concentration and boron concentration.
Step 2：The growth of high resistivity semi-insulation SiC crystal.In high vacuum conditions, high-purity argon gas or argon are passed through
The mixed gas of gas and hydrogen, SiC powders are placed in the graphite crucible of coating carries out high temperature pretreatment, and vanadium conduct
Solid Source is doped, and is grown in being carried out in specific crucible system.Wherein, the concentration of foreign matter of vanadium is 8 × 1016-1×1017
Individual/cm-3Magnitude, and the concentration of vanadium is greater than the concentration of Nitrogen Impurities, and the concentration of nitrogen impurity can be 5 × 1016Individual/cm-3With
Under.
Step 3：The monocrystalline for growing carries out round as a ball and directional process, the crystal ingot of standard is obtained, then through multi-wire saw
With grinding and polishing process, semi-insulation SiC polished silicon wafer is obtained.
Step 4：Semi-insulation SiC polished silicon wafer is annealed.By chip under vacuum, it is heated to 1600-2000
DEG C, and 2-10h is kept, then through certain temperature fall time 10-20h.
Obtain and there is high resistivity, the semi-insulation SiC chip of low defect.
The method of the invention grows carborundum crystals in SiC single crystal stove using physical vapor transport (PVT methods),
Using high-purity silicon carbide powder, monocrystalline is grown in the high purity graphite earthenware with high vacuum, deep-level impurity vanadium adopts Solid Source
Mode adulterate, and the high temperature anneal is carried out to the chip after polishing, obtain with high resistivity, low defect it is semi-insulating
SiC single crystal piece.
Technical scheme provided herein is described in detail above, embodiment used herein is to the application
Principle and embodiment be set forth, the explanation of above example is only intended to help and understands the present processes and its core
Thought is thought；Simultaneously for one of ordinary skill in the art, according to the thought of the application, in specific embodiment and model is applied
Place and will change, in sum, this specification content should not be construed as the restriction to the application.
Claims (5)
1. a kind of preparation method of SiC wafer, it is characterised in that comprise the following steps：
Step one, synthesizes high-purity SiC powders：
High-purity silica flour and carbon dust are adopted for raw material, in high vacuum conditions, the mixed of high-purity argon gas or argon gas and hydrogen is passed through
Gas is closed, being placed in the graphite crucible of coating carries out high―temperature nuclei, obtains the high-purity alpha-SiC powder of low nitrogen concentration and boron concentration
Material；
Step 2, the growth of high resistivity semi-insulation SiC crystal：
In high vacuum conditions, the mixed gas of high-purity argon gas or argon gas and hydrogen are passed through, SiC powders has been placed on into coating
Graphite crucible in carry out high temperature pretreatment, and be doped using Solid Source, be grown in being carried out in specific crucible system；
Concentration of the Solid Source concentration more than Nitrogen Impurities；
Step 3, the monocrystalline for growing carries out round as a ball and directional process, obtains the crystal ingot of standard, then through multi-wire saw and grinds
Mill polishing, obtains semi-insulation SiC polished silicon wafer；
Step 4, anneals to semi-insulation SiC polished silicon wafer：
By chip under vacuum, heat, and keep 2-10h, then through temperature fall time 10-20h, obtain and there is high resistance
The semi-insulation SiC chip of rate, low defect.
2. the preparation method of a kind of SiC wafer according to claim 1, it is characterised in that：In described step one, high temperature
Temperature is between 1400-2000 DEG C during synthesis.
3. the preparation method of a kind of SiC wafer according to claim 1, it is characterised in that：In described step two, solid-state
Source adopts vanadium, concentration to select 8 × 1016-1×1017 Individual/cm-3Magnitude.
4. the preparation method of a kind of SiC wafer according to claim 1, it is characterised in that：In described step two, azepine
The concentration of matter is 5 × 1016Individual/cm-3Below.
5. the preparation method of a kind of SiC wafer according to claim 1, it is characterised in that：Described step four kind, heating
Temperature is 1600-2000 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611126092.3A CN106591952A (en) | 2016-12-09 | 2016-12-09 | Preparation method of SiC wafer |
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| CN201611126092.3A CN106591952A (en) | 2016-12-09 | 2016-12-09 | Preparation method of SiC wafer |
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| CN106591952A true CN106591952A (en) | 2017-04-26 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974712A (en) * | 2017-11-14 | 2018-05-01 | 山东天岳先进材料科技有限公司 | A kind of preparation method of Semi-insulating silicon carbide mono-crystal |
| CN110919465A (en) * | 2019-11-08 | 2020-03-27 | 中国科学院上海硅酸盐研究所 | Nondestructive high-flatness single crystal silicon carbide planar optical element and preparation method thereof |
| CN111463113A (en) * | 2020-05-25 | 2020-07-28 | 哈尔滨晶创科技有限公司 | Processing method for protecting silicon carbide surface in semi-insulating SiC ion doping annealing process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH061698A (en) * | 1992-06-19 | 1994-01-11 | Sharp Corp | Production of silicon carbide bulk single crystal |
| JPH09142995A (en) * | 1995-11-22 | 1997-06-03 | Nippon Steel Corp | Production of p-type single crystal silicon carbide |
| CN103696012A (en) * | 2013-12-13 | 2014-04-02 | 山东大学 | Preparation method of high-uniformity high-yield semi-insulation silicon carbide substrate |
| CN104805504A (en) * | 2015-05-19 | 2015-07-29 | 山东大学 | Method for quickly growing large-size SiC (Silicon Carbide) single crystal |
| CN105274624A (en) * | 2015-10-09 | 2016-01-27 | 张家港市东大工业技术研究院 | Method for preparation of vanadium doped semi-insulating silicon carbide by microwave irradiation |
| CN105821471A (en) * | 2016-05-10 | 2016-08-03 | 山东大学 | Preparation method of low-stress and high-purity semi-insulating SiC single crystal |
-
2016
- 2016-12-09 CN CN201611126092.3A patent/CN106591952A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH061698A (en) * | 1992-06-19 | 1994-01-11 | Sharp Corp | Production of silicon carbide bulk single crystal |
| JPH09142995A (en) * | 1995-11-22 | 1997-06-03 | Nippon Steel Corp | Production of p-type single crystal silicon carbide |
| CN103696012A (en) * | 2013-12-13 | 2014-04-02 | 山东大学 | Preparation method of high-uniformity high-yield semi-insulation silicon carbide substrate |
| CN104805504A (en) * | 2015-05-19 | 2015-07-29 | 山东大学 | Method for quickly growing large-size SiC (Silicon Carbide) single crystal |
| CN105274624A (en) * | 2015-10-09 | 2016-01-27 | 张家港市东大工业技术研究院 | Method for preparation of vanadium doped semi-insulating silicon carbide by microwave irradiation |
| CN105821471A (en) * | 2016-05-10 | 2016-08-03 | 山东大学 | Preparation method of low-stress and high-purity semi-insulating SiC single crystal |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974712A (en) * | 2017-11-14 | 2018-05-01 | 山东天岳先进材料科技有限公司 | A kind of preparation method of Semi-insulating silicon carbide mono-crystal |
| CN110919465A (en) * | 2019-11-08 | 2020-03-27 | 中国科学院上海硅酸盐研究所 | Nondestructive high-flatness single crystal silicon carbide planar optical element and preparation method thereof |
| CN111463113A (en) * | 2020-05-25 | 2020-07-28 | 哈尔滨晶创科技有限公司 | Processing method for protecting silicon carbide surface in semi-insulating SiC ion doping annealing process |
| CN111463113B (en) * | 2020-05-25 | 2023-04-11 | 哈尔滨晶创科技有限公司 | Processing method for protecting silicon carbide surface in semi-insulating SiC ion doping annealing process |
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Application publication date: 20170426 |