CN111533114A - Preparation method of silicon carbide graphene substrate epitaxial material - Google Patents
Preparation method of silicon carbide graphene substrate epitaxial material Download PDFInfo
- Publication number
- CN111533114A CN111533114A CN202010419518.4A CN202010419518A CN111533114A CN 111533114 A CN111533114 A CN 111533114A CN 202010419518 A CN202010419518 A CN 202010419518A CN 111533114 A CN111533114 A CN 111533114A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- graphene
- epitaxial material
- preparing
- graphene substrate
- 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
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 74
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000000463 material Substances 0.000 title claims abstract description 49
- 239000000758 substrate Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 239000011856 silicon-based particle Substances 0.000 claims description 3
- 238000004088 simulation Methods 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims 2
- 230000001105 regulatory effect Effects 0.000 claims 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims 2
- 230000001276 controlling effect Effects 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 20
- 230000004927 fusion Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/188—Preparation by epitaxial growth
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A preparation method of a silicon carbide graphene substrate epitaxial material belongs to the technical field of single crystal material preparation. The invention solves the defect problem existing in the preparation of the silicon carbide graphene substrate epitaxial material at present. The invention provides a preparation method of a silicon carbide graphene substrate epitaxial material, which comprises the steps of growing a silicon carbide substrate layer and a silicon carbide-graphene layer, processing a silicon carbide-graphene composite layer by using special substrate preparation equipment to obtain a silicon carbide graphene epitaxial crystal material, growing graphene on a cut silicon carbide crystal again, processing again to obtain the silicon carbide graphene substrate epitaxial material, and repeating the operations in sequence to obtain the industrial silicon carbide graphene substrate epitaxial material.
Description
Technical Field
The invention relates to a preparation method of a silicon carbide graphene substrate epitaxial material, and belongs to the technical field of single crystal material preparation.
Background
Graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, is considered to be a future revolutionary material, exists in the nature, is difficult to strip out a single-layer structure, is graphite after being laminated, contains about 300 ten thousand layers of graphene in the graphite with the thickness of 1 mm, and can be a base layer or even only one layer of graphene after a pencil is slightly scratched on paper. At present, the common powder production methods of graphene are a mechanical stripping method, an oxidation-reduction method and a silicon carbide epitaxial growth method, and the film production method is a chemical vapor deposition method. The current graphene preparation methods also have the following defects:
1. the redox degree of the redox graphene material which is widely applied at present cannot be accurately controlled, the process is complex, integration is not easy, and industrialization is difficult to realize.
2. The chemical vapor deposition method and the silicon carbide epitaxial growth graphene are still immature in device processing technology, the fusion degree between the silicon carbide and the graphene sheet layer is not high, and a certain amount of pollution can be generated during preparation of the graphene.
In summary, a method for preparing a silicon carbide graphene substrate epitaxial material with low pollution, simple process and high material fusion degree is needed.
Disclosure of Invention
The invention provides a preparation method of a silicon carbide graphene substrate epitaxial material, aiming at solving the problems of low material fusion degree, complex process and difficult industrialization of the existing graphene preparation method.
The technical scheme of the invention is as follows:
a preparation method of a silicon carbide graphene substrate epitaxial material comprises the following steps:
step one, growing a silicon carbide base layer;
growing a silicon carbide-graphene layer;
processing the silicon carbide-graphene composite layer by using special equipment for substrate preparation to obtain a silicon carbide graphene epitaxial crystal material;
and step four, the silicon carbide crystal obtained after cutting is subjected to secondary graphene growth again through the step three, the silicon carbide graphene substrate epitaxial material is obtained after processing again, and the industrial silicon carbide graphene substrate epitaxial material can be obtained through repeated operation in sequence.
Further, the specific implementation steps of the first step are as follows:
step 1: preparing high-purity silicon carbide powder cakes in a high-temperature purification furnace by using high-purity carbon powder and high-purity silicon particles;
step 2: simulating the optimal temperature and pressure for the growth of the silicon carbide crystal by using special simulation software VR-PVT-SiC for the growth of the silicon carbide crystal through a simulation technology;
and step 3: and setting the growth temperature and pressure of the silicon carbide base layer in a high-temperature resistance furnace, introducing nitrogen protective gas, and maintaining the temperature for 115 hours under the conditions to obtain the 300-micron silicon carbide base layer.
Further, the purity of the silicon carbide powder material cake in the step 1 is controlled to be 99.999 percent.
Further, the optimal growth temperature of the silicon carbide base layer in the step 2 is 2300 ℃, and the optimal growth pressure of the silicon carbide base layer is 2.5x104pa。
Further, the concrete implementation steps of the second step are as follows: and (3) putting the silicon carbide crystal taken out in the step one into a high-pressure reaction furnace, adjusting the temperature and the pressure, and slowly evaporating silicon atoms to form the graphene layer with the C-C structure.
Further, in the second step, the temperature of the high-pressure reaction furnace is adjusted to 1650 ℃, and the pressure of the high-pressure reaction furnace is adjusted to 6.7x105pa, by which the silicon atoms are slowly evaporated.
Further, in the third step, the silicon carbide graphene is subjected to rounding, chamfering, cutting, grinding and polishing by using special equipment for substrate preparation.
Further, the processing method in the fourth step is rounding, chamfering, cutting, grinding and polishing.
The invention has the beneficial effects that:
1. the required raw materials are collected and can be repeatedly used, so that the material utilization rate is improved, and the experimental production cost is reduced;
2. the invention avoids the work of chemical coating, etching and the like, has no pollution and simple working procedure;
3. the material obtained by the invention has higher fusion degree, and secondary processing is avoided;
4. the silicon carbide graphene material prepared by the method has good performance.
Drawings
Fig. 1 is a process flow diagram of a preparation method of a silicon carbide graphene substrate epitaxial material.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, which comprises the following steps:
the method comprises the following steps: growing a silicon carbide base layer;
step two: growing a silicon carbide-graphene layer;
step three: processing the silicon carbide-graphene composite layer by using special equipment for preparing the substrate to obtain a silicon carbide graphene epitaxial wafer material;
step four: and (3) growing the graphene again on the cut silicon carbide crystal through the third step, processing the processed silicon carbide graphene substrate epitaxial material again, and repeating the operation in sequence to obtain the industrial silicon carbide graphene substrate epitaxial material.
Example 2
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, and the specific implementation step of the first step is as follows:
step 1: preparing high-purity silicon carbide powder cakes in a high-temperature purification furnace by using high-purity carbon powder and high-purity silicon particles;
step 2: simulating the optimal temperature and pressure for the growth of the silicon carbide crystal by using special simulation software VR-PVT-SiC for the growth of the silicon carbide crystal through a simulation technology;
and step 3: and setting the growth temperature and pressure of the silicon carbide base layer in a high-temperature resistance furnace, introducing nitrogen protective gas, and maintaining the temperature for 115 hours under the conditions to obtain the 300-micron silicon carbide base layer.
Example 3
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, and the purity of the silicon carbide powder cake in the step 1 is controlled to be 99.999%.
Example 4
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, wherein in the step 2, the optimal growth temperature of the silicon carbide base layer is 2300 ℃, and the optimal growth pressure of the silicon carbide base layer is 2.5x104pa。
Example 5
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, and the specific implementation steps of the second step are as follows: and (3) putting the silicon carbide crystal taken out in the step one into a high-pressure reaction furnace, adjusting the temperature and the pressure, and slowly evaporating silicon atoms to form the graphene layer with the C-C structure.
Example 6
In the second step, the temperature of the high-pressure reaction furnace is adjusted to 1650 ℃, and the pressure of the high-pressure reaction furnace is adjusted to 6.7x105pa, by which the silicon atoms are slowly evaporated.
Example 7
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, and in the third step, the silicon carbide graphene is subjected to rounding, chamfering, cutting, grinding and polishing by using special substrate preparation equipment.
Example 8
The embodiment provides a preparation method of a silicon carbide graphene substrate epitaxial material, and the processing method in the fourth step is rounding, chamfering, cutting, grinding and polishing.
Claims (8)
1. A preparation method of a silicon carbide graphene substrate epitaxial material is characterized by comprising the following steps:
the method comprises the following steps: growing a silicon carbide base layer;
step two: growing a silicon carbide-graphene layer;
step three: processing the silicon carbide-graphene composite layer by using special equipment for preparing the substrate to obtain a silicon carbide graphene epitaxial wafer material;
step four: and (3) growing the graphene again on the cut silicon carbide crystal through the third step, processing again to obtain the silicon carbide graphene substrate epitaxial material, and repeating the operation in sequence to obtain the industrial silicon carbide graphene substrate epitaxial material.
2. The method for preparing the silicon nitride graphene substrate epitaxial material according to claim 1, wherein the specific implementation steps of the first step are as follows:
step 1: preparing high-purity silicon carbide powder cakes in a high-temperature purification furnace by using high-purity carbon powder and high-purity silicon particles;
step 2: simulating the optimal temperature and pressure for the growth of the silicon carbide crystal by using special simulation software VR-PVT-SiC for the growth of the silicon carbide crystal through a simulation technology;
and step 3: and setting the growth temperature and pressure of the silicon carbide base layer in a high-temperature resistance furnace, introducing nitrogen protective gas, and maintaining the temperature for 115 hours under the conditions to obtain the 300-micron silicon carbide base layer.
3. The method for preparing the silicon nitride graphene substrate epitaxial material according to claim 2, wherein the method comprises the following steps: and (3) controlling the purity of the silicon carbide powder material cake in the step 1 to be 99.999%.
4. The method for preparing the epitaxial material of the silicon carbide graphene substrate according to claim 2, wherein the method comprises the following steps: in the step 2, the optimal growth temperature of the silicon carbide base layer is 2300 ℃, and the optimal growth pressure of the silicon carbide base layer is 2.5x104pa。
5. The method for preparing the silicon carbide graphene substrate epitaxial material according to claim 1, wherein the concrete implementation steps of the second step are as follows: and (3) putting the silicon carbide crystal taken out in the step one into a high-pressure reaction furnace, adjusting the temperature and the pressure, and slowly evaporating silicon atoms to form the graphene layer with the C-C structure.
6. The method for preparing the epitaxial material of the silicon carbide graphene substrate according to claim 5, wherein the method comprises the following steps: in the second step, the temperature of the high-pressure reaction furnace is regulated to 1650 ℃, and the pressure of the high-pressure reaction furnace is regulated to 6.7x105pa, by which the silicon atoms are slowly evaporated.
7. The method for preparing the epitaxial material of the silicon carbide graphene substrate according to claim 1, wherein the method comprises the following steps: and thirdly, rounding, chamfering, cutting, grinding and polishing the silicon carbide graphene by using special equipment for preparing the substrate.
8. The method for preparing the epitaxial material of the silicon carbide graphene substrate according to claim 1, wherein the method comprises the following steps: the processing method in the fourth step comprises rounding, chamfering, cutting, grinding and polishing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010419518.4A CN111533114A (en) | 2020-05-18 | 2020-05-18 | Preparation method of silicon carbide graphene substrate epitaxial material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010419518.4A CN111533114A (en) | 2020-05-18 | 2020-05-18 | Preparation method of silicon carbide graphene substrate epitaxial material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111533114A true CN111533114A (en) | 2020-08-14 |
Family
ID=71969432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010419518.4A Pending CN111533114A (en) | 2020-05-18 | 2020-05-18 | Preparation method of silicon carbide graphene substrate epitaxial material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111533114A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109137077A (en) * | 2018-10-23 | 2019-01-04 | 台州蓝能新材料科技有限公司 | A kind of preparation facilities and method of high-purity silicon carbide |
| US20190157395A1 (en) * | 2017-11-17 | 2019-05-23 | Infineon Technologies Ag | Method for Forming a Semiconductor Device and a Semiconductor Device |
| US20190330761A1 (en) * | 2018-04-26 | 2019-10-31 | Showa Denko K.K. | SiC SINGLE CRYSTAL GROWTH APPARATUS AND GROWTH METHOD OF SiC SINGLE CRYSTAL |
-
2020
- 2020-05-18 CN CN202010419518.4A patent/CN111533114A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190157395A1 (en) * | 2017-11-17 | 2019-05-23 | Infineon Technologies Ag | Method for Forming a Semiconductor Device and a Semiconductor Device |
| US20190330761A1 (en) * | 2018-04-26 | 2019-10-31 | Showa Denko K.K. | SiC SINGLE CRYSTAL GROWTH APPARATUS AND GROWTH METHOD OF SiC SINGLE CRYSTAL |
| CN109137077A (en) * | 2018-10-23 | 2019-01-04 | 台州蓝能新材料科技有限公司 | A kind of preparation facilities and method of high-purity silicon carbide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11359276B2 (en) | Self-supporting ultra-fine nanocrystalline diamond thick film | |
| CN102102220B (en) | Preparation method of graphene on diamond (111) surface | |
| CN113463192B (en) | Method for splicing and growing diamond single crystal | |
| CN110578171A (en) | Method for manufacturing large-size low-defect silicon carbide single crystal | |
| EP2738140A1 (en) | Polycrystalline diamond, manufacturing method therefor, scribe tool, scribe wheel, dresser, rotary tool, water-jet orifice, wire drawing die, cutting tool, and electron source | |
| CN102296362A (en) | Single-crystal diamond growth base material and method for manufacturing single-crystal diamond substrate | |
| CN114411250B (en) | MPCVD single crystal diamond splicing growth method | |
| CN105839072B (en) | A kind of method that chemical vapor deposition prepares rhenium disulfide film | |
| US20130078424A1 (en) | Hexagonal Boron Nitride Substrate With Monatomic Layer Step, And Preparation Method And Application Thereof | |
| CN108611638B (en) | Micron diamond thick film with high abrasion ratio and high breaking strength and preparation method thereof | |
| CN105579626A (en) | Silicon carbide semiconductor substrate and method for producing same | |
| CN111118471A (en) | Preparation method of high-quality polycrystalline diamond film | |
| CN111733454A (en) | Separation method of CVD homoepitaxy diamond large single crystal based on boron-doped transition layer | |
| CN111533114A (en) | Preparation method of silicon carbide graphene substrate epitaxial material | |
| JPH0556851B2 (en) | ||
| CN114481307B (en) | SiC single crystal substrate and preparation method and application thereof | |
| JPS62101026A (en) | Impurity diffusion source | |
| CN111146146B (en) | Preparation method of high-efficiency heat-dissipation semiconductor substrate with reusable base | |
| CN108892132A (en) | Prepare auxiliary device, the graphene and preparation method thereof of graphene | |
| JP7220844B2 (en) | Manufacturing method of SiC polycrystalline substrate | |
| CN114032613A (en) | Method for improving quality of joint seam of diamond monocrystal grown by splicing method | |
| CN115465856A (en) | Preparation method of patterned graphene | |
| CN113151803A (en) | Preparation method of boron-carbon-nitrogen film | |
| CN111172508A (en) | Method for improving pressure limit of diamond opposite-top anvil | |
| CN105543795A (en) | Growing method for polycrystalline silicon carbide thin film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200814 |