CN1367275A - Preparation method of block silicone carbide monocrystal growth - Google Patents
Preparation method of block silicone carbide monocrystal growth Download PDFInfo
- Publication number
- CN1367275A CN1367275A CN 01105256 CN01105256A CN1367275A CN 1367275 A CN1367275 A CN 1367275A CN 01105256 CN01105256 CN 01105256 CN 01105256 A CN01105256 A CN 01105256A CN 1367275 A CN1367275 A CN 1367275A
- Authority
- CN
- China
- Prior art keywords
- crystal
- preparation
- sic
- monocrystalline
- growth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention provides a preparation method for growing blocky silicon carbide monocrystal. This invention utilizes the preparation of high-purity silicon carbide raw material and inoculating crystal with intact structure; under the precise control of high-temp. high vacuum and crystal growth temp., it utilizes the decomposition and sublimation of SIC material to grow blocky silicon carbide crystal on the inoculating crystal.
Description
The present invention relates to a kind of method of producing single-crystal silicon carbide.
The single-crystal silicon carbide material has excellent physical characteristics and electric property, as wide bandgap material, is applied in high temperature, the width of cloth according to aspects such as, high-power, microwaves, becomes the required high-performance electronic device materials in field such as Aeronautics and Astronautics, radar, communication.Up to now, the domestic single-crystal silicon carbide of not producing as yet.By Siemens at Chinese patents CN1191580A, the method for single-crystal silicon carbide " produce ".The method of the three-dimensional monocrystalline of a kind of SIC of production has been proposed, under ultra-high voltage with SIC powder or other material dissolution in a kind of solvent, and on a nucleus, grow.This method growing silicon carbide single crystal in solvent needs 10 but produce in this way
5Carry out under the Pa pressure, weigh from pressure, this method prepares crystal, the manufacturing of equipment is required high, makes difficulty.
The preparation method who the purpose of this invention is to provide a kind of block silicone carbide monocrystal growth can produce large size, structural integrity, carborundum crystals that defective is few with this method.
The present invention realizes that by following technical scheme its preparation technology is as follows:
(1) preparation of SIC powder:
With high-purity silicon powder and high pure carbon powder, fully admix in proportion, in process furnace, vacuumize, fill high-purity argon gas, heat 1800 ℃-1900 ℃, be incubated 20 hours, be cooled to SIC squamous monocrystalline platelet or polycrystal, then the SIC powder is carried out pickling, remove impurity, dry, become the raw material of SIC monocrystalline.
(2) preparation of seed crystal:
Choice structure is complete, and the crystal that defective is few as growing crystal on (0001) or (0001) natural crystal face, is put into process furnace, uses the PVT method, increases crystal seed one by one, and the seeded growth temperature is 2400 ℃-2600 ℃, vacuum tightness 10
-7モ; axis thermograde 15 ℃/cm in vitellarium with the high-purity argon gas protection, grows into the SIC monocrystalline in process furnace; with this single-crystal wafer; polishing, choice structure is complete again, as seed crystal; put into process furnace again; be prepared into big slightly SIC monocrystalline, carry out so repeatedly, grow up to the large size silicon-carbide monocrystalline.
(3) SIC single crystal preparation:
In the SIC single crystal growth process, the temperature of single crystal growing furnace is 2600 ℃, vacuum tightness 10
-7モ, temperature fluctuation is controlled to be ± 1 ℃ of situation under, by the 15 ℃/cm of thermograde of source and seed crystal, gas flow, vacuum tightness reflects that indoor pressure and growth temperature are mutual relationships such as 2400 ℃-2600 ℃, according to the particular case of crystal growth, there is purpose to regulate and preparation.
The preparation method that the present invention adopts, the blocky SIC monocrystalline of energy production large size, and SIC monocrystalline, colourless, transparent, no wrap, no bubble can be controlled the crystalline process of growth.
Embodiments of the invention:
The preparation technology of silicon carbide monocrystal growth is as follows:
(1) preparation of SIC powder:
Mix with coke with the monocrystalline silica flour, press Si: C=28: 12, put into high temperature high vacuum resistance heading furnace, vacuumizing is 10
-7モ fills high-purity argon gas, and 1800 ℃ of Heating temperatures are incubated 20 hours, after the cooling, becomes SIC squamous monocrystalline platelet or polycrystal, with the SIC powder, puts into hydrochloric acid soln 24 hours, uses deionized water rinsing, removes impurity, oven dry, the raw material of one-tenth preparation SIC monocrystalline.
(2) seed crystal preparation:
In industrial SIC abrasive material, 6 * 8mm crystal that choice structure is complete, defective is few, find out (0001) or (0001) natural crystal face, put into high temperature high vacuum resistance heading furnace, also can use high temperature high vacuum Medium Frequency Induction Heating Furnace,, use the PVT method as the seed crystal that enlarges naturally, crystal growth temperature is 2500 ℃, and vacuum tightness is 10
-7モ; axis gradient 15 ℃/cm in vitellarium with the high-purity argon gas protection, grows into 6H type SIC monocrystalline in high temperature high vacuum resistance heading furnace; with this single-crystal wafer; polishing, choice structure is complete again, as seed crystal; put into high temperature high vacuum resistance heading furnace again; be prepared into big slightly 6H type SIC monocrystalline, so repeat, generate the large size silicon-carbide monocrystalline.
The preparation method of controlled large size silicon-carbide prepares identically with seed crystal, i.e. the section of large size silicon-carbide monocrystalline both can have been made seed crystal (possessing better structural integrity and defective still less) and also can make industrial silicon carbide substrate.The present embodiment block silicone carbide is 40 millimeters of φ, and thick 10 millimeters, microchannel density is 10
-3/ cm
2, dislocation desity 10
-4/ cm
2, 6Hn type SiC.
Claims (2)
1. the preparation method of a block silicone carbide monocrystal growth is characterized in that:
(1) preparation of SIC powder:
With high-purity silicon powder and high pure carbon powder, fully admix in proportion, in process furnace, vacuumize, fill high-purity argon gas, heat 1800 ℃-1900 ℃, be incubated 20 hours, be cooled to SIC squamous monocrystalline platelet or polycrystal, then the SIC powder is carried out pickling, remove impurity, oven dry, become the raw material of SIC monocrystalline
(2) preparation of seed crystal:
Choice structure is complete; the crystal that defective is few as growing crystal on (0001) or (0001) natural crystal face, is put into process furnace; use the PVT method; increase crystal seed one by one, the seeded growth temperature is 2400 ℃-2600 ℃, vacuum tightness 10-7t; 15 ℃/cm of vitellarium axis thermograde; with the high-purity argon gas protection, in process furnace, grow into the SIC monocrystalline, with this single-crystal wafer; polishing; choice structure is complete again, as seed crystal, puts into process furnace again; be prepared into big slightly SIC monocrystalline; carry out so repeatedly, grow up to the large size silicon-carbide monocrystalline
(3) SIC single crystal preparation:
In the SIC single crystal growth process, the temperature of single crystal growing furnace is 2600 ℃, vacuum tightness 10
-7モ, temperature fluctuation is controlled to be ± 1 ℃ of situation under, by the 15 ℃/cm of thermograde of source and seed crystal, gas flow, vacuum tightness reflects that indoor pressure and growth temperature are mutual relationships such as 2400 ℃-2600 ℃, according to the particular case of crystal growth, there is purpose to regulate and preparation.
2. the preparation method of block silicone carbide monocrystal growth according to claim 1 is characterized in that the ratio of silica flour material and carbon dust material is Si: C=28: 12.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01105256 CN1367275A (en) | 2001-01-20 | 2001-01-20 | Preparation method of block silicone carbide monocrystal growth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01105256 CN1367275A (en) | 2001-01-20 | 2001-01-20 | Preparation method of block silicone carbide monocrystal growth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1367275A true CN1367275A (en) | 2002-09-04 |
Family
ID=4654341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01105256 Pending CN1367275A (en) | 2001-01-20 | 2001-01-20 | Preparation method of block silicone carbide monocrystal growth |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1367275A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100595144C (en) * | 2008-06-04 | 2010-03-24 | 山东大学 | Artificial synthetic method of high-pure SiC power for semiconductor single-crystal growth |
| CN102021653A (en) * | 2010-12-30 | 2011-04-20 | 北京华进创威电子有限公司 | Method for growing silicon carbide single crystal by using high-density material block |
| CN101163824B (en) * | 2005-04-19 | 2011-10-19 | Ii-Vi有限公司 | Method of and system for forming sic crystals having spatially uniform doping impurities |
| CN102618920A (en) * | 2012-04-25 | 2012-08-01 | 浙江华友电子有限公司 | Heat energy controlling method for melting process of single crystal furnace |
| CN102794281A (en) * | 2012-07-06 | 2012-11-28 | 宁夏隆基硅材料有限公司 | Method for washing graphite piece in thermal field of Czochralski single-crystal furnace |
| CN101932757B (en) * | 2008-01-29 | 2013-03-06 | 丰田自动车株式会社 | Method for growing p-type sic semiconductor single crystal and p-type sic semiconductor single crystal |
| CN104120489A (en) * | 2008-12-08 | 2014-10-29 | Ii-Vi有限公司 | SiC single-crystal crystal ingot in high crystalline quality, and method for forming thereof |
| CN104477917A (en) * | 2014-11-20 | 2015-04-01 | 江苏乐园新材料集团有限公司 | Silicon carbide smelting method |
| CN105603530A (en) * | 2016-01-12 | 2016-05-25 | 台州市一能科技有限公司 | Raw material for high-speed growth of silicon carbide crystals and silicon carbide crystal growing method |
| CN107254715A (en) * | 2010-12-16 | 2017-10-17 | 株式会社电装 | Manufacture the device of single-crystal silicon carbide |
| CN108193282A (en) * | 2017-11-14 | 2018-06-22 | 山东天岳先进材料科技有限公司 | A kind of synthetic method of high-purity silicon carbide raw material and its application |
| CN110042470A (en) * | 2019-04-29 | 2019-07-23 | 南通大学 | A kind of preparation method of more size Mo Sangshi |
| CN113501524A (en) * | 2021-06-10 | 2021-10-15 | 青海圣诺光电科技有限公司 | Preparation method of silicon carbide powder |
-
2001
- 2001-01-20 CN CN 01105256 patent/CN1367275A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101163824B (en) * | 2005-04-19 | 2011-10-19 | Ii-Vi有限公司 | Method of and system for forming sic crystals having spatially uniform doping impurities |
| CN101932757B (en) * | 2008-01-29 | 2013-03-06 | 丰田自动车株式会社 | Method for growing p-type sic semiconductor single crystal and p-type sic semiconductor single crystal |
| CN100595144C (en) * | 2008-06-04 | 2010-03-24 | 山东大学 | Artificial synthetic method of high-pure SiC power for semiconductor single-crystal growth |
| CN104120489B (en) * | 2008-12-08 | 2017-04-26 | Ii-Vi有限公司 | SiC single-crystal crystal ingot in high crystalline quality, and method for forming thereof |
| CN104120489A (en) * | 2008-12-08 | 2014-10-29 | Ii-Vi有限公司 | SiC single-crystal crystal ingot in high crystalline quality, and method for forming thereof |
| CN107254715A (en) * | 2010-12-16 | 2017-10-17 | 株式会社电装 | Manufacture the device of single-crystal silicon carbide |
| CN102021653B (en) * | 2010-12-30 | 2013-06-12 | 北京华进创威电子有限公司 | Method for growing silicon carbide single crystal by using high-density material block |
| CN102021653A (en) * | 2010-12-30 | 2011-04-20 | 北京华进创威电子有限公司 | Method for growing silicon carbide single crystal by using high-density material block |
| CN102618920A (en) * | 2012-04-25 | 2012-08-01 | 浙江华友电子有限公司 | Heat energy controlling method for melting process of single crystal furnace |
| CN102794281B (en) * | 2012-07-06 | 2014-06-18 | 宁夏隆基硅材料有限公司 | Method for washing graphite piece in thermal field of Czochralski single-crystal furnace |
| CN102794281A (en) * | 2012-07-06 | 2012-11-28 | 宁夏隆基硅材料有限公司 | Method for washing graphite piece in thermal field of Czochralski single-crystal furnace |
| CN104477917A (en) * | 2014-11-20 | 2015-04-01 | 江苏乐园新材料集团有限公司 | Silicon carbide smelting method |
| CN105603530A (en) * | 2016-01-12 | 2016-05-25 | 台州市一能科技有限公司 | Raw material for high-speed growth of silicon carbide crystals and silicon carbide crystal growing method |
| CN105603530B (en) * | 2016-01-12 | 2018-02-27 | 台州市一能科技有限公司 | For the raw material of carborundum crystals high-speed rapid growth and the growing method of carborundum crystals |
| CN108193282A (en) * | 2017-11-14 | 2018-06-22 | 山东天岳先进材料科技有限公司 | A kind of synthetic method of high-purity silicon carbide raw material and its application |
| CN110042470A (en) * | 2019-04-29 | 2019-07-23 | 南通大学 | A kind of preparation method of more size Mo Sangshi |
| CN113501524A (en) * | 2021-06-10 | 2021-10-15 | 青海圣诺光电科技有限公司 | Preparation method of silicon carbide powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104805504B (en) | A kind of method of fast-growth large size silicon-carbide monocrystalline | |
| CN1367275A (en) | Preparation method of block silicone carbide monocrystal growth | |
| KR101666596B1 (en) | Sic single crystal and method for producing same | |
| CN102758249B (en) | A kind of preparation method of colourless boule monocrystal | |
| CN104828825B (en) | A kind of method of low cost low temperature synthesizing silicon carbide powder | |
| CN207793475U (en) | A kind of solution edge polycrystalline silicon carbide monocrystal growth device | |
| CN102628184B (en) | Method for growing gem crystals by way of vacuum induction heating and device realizing method | |
| CN103060904B (en) | A kind of method being realized AlN single crystal growing by growth pattern regulation and control | |
| CN110016718A (en) | A kind of processing method for growing silicon carbide crystal with high quality feedstock purification | |
| CN103320851A (en) | Large-size 15R silicon carbide crystal preparation method | |
| CN102978694A (en) | Improved kyropoulos method for sapphire crystal growth | |
| WO2003078703A1 (en) | CdTe SINGLE CRYSTAL AND CdTe POLYCRYSTAL, AND METHOD FOR PREPARATION THEREOF | |
| CN110217796A (en) | A kind of high-pure SiC power and preparation method thereof | |
| CN113264774A (en) | SiC crystal synthesized by seed induced microwave and preparation method thereof | |
| US20080282968A1 (en) | Method of Growing Single Crystals from Melt | |
| CN102021653B (en) | Method for growing silicon carbide single crystal by using high-density material block | |
| CN111962152A (en) | Preparation method of silicon carbide single crystal for reducing crystal defects | |
| CN110284195A (en) | Boron phosphide single crystal and preparation method and application thereof | |
| CN110067024A (en) | Photoelectric functional crystal M3RE(PO4)3And preparation method thereof | |
| CN103205799A (en) | Method for growing C-oriented white stone crystals | |
| CN207608656U (en) | A kind of grower of PVT methods growing large-size Semi-insulating silicon carbide mono-crystal | |
| WO2021244052A1 (en) | High-thickness and low-defect six-inch silicon carbide crystal growth method satisfying industrialization production | |
| CN206244914U (en) | A kind of process units for preparing low boron impurity concentration SiC single crystal | |
| CN106119951B (en) | Fluxing agent for low-temperature high-speed growth of SiC single crystal | |
| CN111411396A (en) | Preparation method of transparent colorful silicon carbide polycrystalline plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |