CN112830786A - Preparation method of silicon carbide thin-wall structural member - Google Patents
Preparation method of silicon carbide thin-wall structural member Download PDFInfo
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- CN112830786A CN112830786A CN201911156094.0A CN201911156094A CN112830786A CN 112830786 A CN112830786 A CN 112830786A CN 201911156094 A CN201911156094 A CN 201911156094A CN 112830786 A CN112830786 A CN 112830786A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 34
- 239000010439 graphite Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000012876 topography Methods 0.000 claims description 3
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 230000006872 improvement Effects 0.000 description 6
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a silicon carbide thin-wall structural member, which comprises the following steps: s1, manufacturing a mold by using the graphite substrate; s2, growing silicon carbide on the surface of the graphite substrate by adopting a chemical vapor deposition method; s3, cutting the silicon carbide wrapping part from the edge of the workpiece to expose the graphite substrate inside again; and S4, completely reacting the graphite base material in the workpiece with oxygen to obtain the solid silicon carbide workpiece. The silicon carbide thin-wall structural member has the advantages of higher purity, contribution to avoiding the problems of high temperature, pollution, oxidation, corrosion and the like, and contribution to improving the process capability and stability of equipment.
Description
Technical Field
The invention relates to a preparation method of an internal coating of semiconductor equipment, in particular to a preparation method of a silicon carbide thin-wall structural member.
Background
At present, in the field of semiconductor equipment, because various environments such as corrosive chemical atmosphere, high temperature, ionization, particle deposition and the like exist inside a reaction chamber of equipment, in order to improve the process capability and the process stability of the equipment, 214LD quartz pieces, reactive sintered silicon carbide ceramics and silicon carbide coated graphite are selected materials which are generally applied inside the reaction chamber of the equipment. Because the internal temperature of the reaction cavity of some equipment needs to reach or even exceed 1300 ℃, the traditional 214LD semiconductor grade quartz piece can be softened at high temperature and cannot meet the use requirement; the reactive sintered silicon carbide ceramic is formed by mixing and sintering additive materials such as silicon carbide powder, other binders and the like, the content of metal impurities of the materials is difficult to control, high-precision semiconductor devices are easily polluted, and the yield is caused to be problematic; the silicon carbide coating graphite has high purity and good high-temperature corrosion resistance, but under the impact of temperature rise and temperature drop, the coating is easy to fall off, so that the equipment process is unstable.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a silicon carbide thin-wall structural member, which has higher purity, is beneficial to avoiding the problems of high temperature, pollution, oxidation, corrosion and the like and is beneficial to improving the process capability and stability of equipment.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a silicon carbide thin-wall structural member comprises the following steps:
s1, manufacturing a mold by using the graphite substrate;
s2, growing silicon carbide on the surface of the graphite substrate by adopting a chemical vapor deposition method;
s3, cutting the silicon carbide wrapping part from the edge of the workpiece to expose the graphite substrate inside again;
and S4, completely reacting the graphite base material in the workpiece with oxygen to obtain the solid silicon carbide workpiece.
As a further improvement of the above technical solution: the detailed step of S2 is:
s2.1, placing the graphite substrate into chemical vapor deposition equipment, and vacuumizing the chemical vapor deposition equipment and replacing gas;
s2.2, introducing nitrogen, preheating and heating to 600-800 ℃, wherein the heating rate is 1-15 ℃/min;
s2.3, introducing nitrogen and hydrogen, continuously heating to 1400-1600 ℃, wherein the heating rate is 1-10 ℃/min;
and S2.4, after the temperature field is stabilized, starting to introduce raw material gas, hydrogen and argon, and growing at a rate of 10-200 mu m/h.
As a further improvement of the above technical solution: the detailed step of S2 further includes:
s2.5, cooling when the thickness of the silicon carbide grows to be 200-500 mu m, and rotating and/or inverting the workpiece;
s2.6, repeating the steps S2.1 to S2.5 until the total growth thickness of the silicon carbide reaches the target requirement.
As a further improvement of the above technical solution: in step S2.4, the raw material gas is trichloromethylsilane.
As a further improvement of the above technical solution: and step S4, placing the workpiece into a high-temperature oxidation furnace, heating to 900-1200 ℃, introducing oxygen, reacting the graphite substrate with the oxygen at high temperature, discharging generated carbon dioxide, and obtaining the solid silicon carbide workpiece after the graphite substrate completely reacts.
As a further improvement of the above technical solution: the preparation method of the silicon carbide thin-wall structural member further comprises the following steps: and S5, polishing and grinding the solid silicon carbide workpiece and adjusting the secondary size according to the requirements of the target size and the surface topography.
As a further improvement of the above technical solution: the preparation method of the silicon carbide thin-wall structural member further comprises the following steps: further comprising the steps of: and S6, cleaning by using 10% hydrofluoric acid, and then washing by using ultrasonic waves and deionized water to obtain a finished product.
In step S1 of the method for manufacturing a silicon carbide thin-walled structure, the graphite substrate has a thickness of 2-50 mm and a surface finish of 500-1000nm, and is purified after being processed into a mold.
Compared with the prior art, the invention has the advantages that: the invention discloses a preparation method of a silicon carbide thin-wall structural member, which adopts an all-solid-state deposition silicon carbide material to prepare the structural member, the purity can reach 99.9999 percent, metal impurities such as Fe, Al, Cu, Zn and the like can be reduced to ppb (parts per billion) level, the problems of high temperature, pollution, oxidation, corrosion, material strength and the like can be effectively avoided by combining the material characteristics of silicon carbide, and the method can be widely applied to key parts of SiC oxidation furnace equipment, SiC epitaxial equipment, high-temperature MOCVD equipment and the like, and the process capability and the process stability of the equipment are effectively improved.
Drawings
FIG. 1 is a schematic flow chart of a method for manufacturing a thin-walled silicon carbide structural member according to the present invention.
Fig. 2 is a schematic flow chart of the method for preparing the plane thin-wall structural member.
FIG. 3 is a schematic flow chart of the method for preparing the non-planar special-shaped thin-wall structural member.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples of the specification.
Fig. 1 to 3 show an embodiment of the present invention, and the method for manufacturing a thin-walled silicon carbide structural member of the embodiment includes the following steps:
s1, manufacturing a mold by using the graphite substrate;
planning the size, shape and processing of the graphite mould according to the size of the structural part required to be manufactured, wherein the graphite mould can be a plane equal-thickness thin plate structural part generally or a non-plane special-shaped structural part such as a cylindrical thin-wall tube, a bell-type crucible, an MOCVD (metal organic chemical vapor deposition) tray and the like; the dimension planning of the planar equal-thickness sheet structural member is to obtain two structural members with two reference surfaces symmetrical by respectively taking the surface of the graphite substrate as a reference and taking the outward growth thickness as the structural thickness dimension; the size planning of the non-planar special-shaped thin-wall structural member can be achieved by taking the inner surface or the outer surface of the graphite substrate as a reference and the inward or outward growth thickness as the structural thickness, and taking the structural member growing in the direction of the corresponding reference surface as the final product;
s2, growing silicon carbide on the surface of the graphite substrate by adopting a Chemical Vapor Deposition (CVD) method;
s3, cutting the silicon carbide wrapping part from the edge of the workpiece to expose the graphite substrate inside again;
and S4, completely reacting the graphite base material in the workpiece with oxygen to obtain the solid silicon carbide workpiece.
The preparation method of the silicon carbide thin-wall structural member adopts the all-solid-state deposition silicon carbide material to prepare the structural member, the purity can reach 99.9999 percent, the metal impurities of Fe, Al, Cu, Zn and the like can be reduced to ppb (parts per billion) level, the problems of high temperature, pollution, oxidation, corrosion, material strength and the like can be effectively avoided by combining the material characteristics of silicon carbide, and the method can be widely applied to the key parts of SiC oxidation furnace equipment, SiC epitaxial equipment, high-temperature MOCVD equipment and the like, and the equipment process capability and the process stability are effectively improved.
Further, in this embodiment, the detailed step of S2 is:
s2.1, placing the graphite substrate into chemical vapor deposition equipment, and vacuumizing the chemical vapor deposition equipment and replacing gas;
s2.2, introducing nitrogen, preheating and heating to 600-800 ℃, wherein the heating rate is 1-15 ℃/min;
s2.3, introducing nitrogen and hydrogen, continuously heating to 1400-1600 ℃, wherein the heating rate is 1-10 ℃/min;
s2.4, after the temperature field is stabilized, introducing raw material gases of trichloromethylsilane (or the like), hydrogen and argon, and growing at a rate of 10-200 mu m/h.
Further, in this embodiment, the detailed step of S2 further includes:
s2.5, cooling when the thickness of the silicon carbide grows to be 200-500 mu m, and rotating and/or inverting the workpiece;
s2.6, repeating the steps S2.1 to S2.5 until the total growth thickness of the silicon carbide reaches the target requirement. Namely, a mode of repeated growth is adopted for many times, the workpiece is rotated by a certain angle and inverted after each growth, and the silicon carbide films on the same surface of the workpiece are kept uniform everywhere and the silicon carbide films on the inner surface and the outer surface of the workpiece are kept uniform and consistent.
Furthermore, in this embodiment, in step S4, the workpiece is placed in a high temperature oxidation furnace, the temperature is raised to 900 to 1200 ℃, oxygen is introduced to react the graphite substrate with oxygen at a high temperature, carbon dioxide is generated and discharged, and the solid silicon carbide workpiece is obtained after the graphite substrate completely reacts.
Further, in this embodiment, the method for manufacturing a silicon carbide thin-walled structural member further includes the steps of:
and S5, polishing and grinding the solid silicon carbide workpiece and adjusting the secondary size according to the requirements of the target size and the surface topography.
Furthermore, in this embodiment, the method for manufacturing a silicon carbide thin-walled structural member further includes the steps of:
and S6, cleaning by using 10% hydrofluoric acid, and then washing by using ultrasonic waves and deionized water to obtain a finished product.
Further, in this embodiment, in step S1, the graphite substrate has a thickness of 2-50 mm and a surface finish of 500-1000nm, and is processed into a mold and then subjected to a purification treatment, such as a high temperature purification treatment.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (8)
1. A preparation method of a silicon carbide thin-wall structural member is characterized by comprising the following steps: the method comprises the following steps:
s1, manufacturing a mold by using the graphite substrate;
s2, growing silicon carbide on the surface of the graphite substrate by adopting a chemical vapor deposition method;
s3, cutting the silicon carbide wrapping part from the edge of the workpiece to expose the graphite substrate inside again;
and S4, completely reacting the graphite base material in the workpiece with oxygen to obtain the solid silicon carbide workpiece.
2. The method for preparing the silicon carbide thin-walled structure according to claim 1, wherein: the detailed step of S2 is:
s2.1, placing the graphite substrate into chemical vapor deposition equipment, and vacuumizing the chemical vapor deposition equipment and replacing gas;
s2.2, introducing nitrogen, preheating and heating to 600-800 ℃, wherein the heating rate is 1-15 ℃/min;
s2.3, introducing nitrogen and hydrogen, continuously heating to 1400-1600 ℃, wherein the heating rate is 1-10 ℃/min;
and S2.4, after the temperature field is stabilized, starting to introduce raw material gas, hydrogen and argon, and growing at a rate of 10-200 mu m/h.
3. The method for manufacturing a silicon carbide thin-walled structure according to claim 2, wherein: the detailed step of S2 further includes:
s2.5, cooling when the thickness of the silicon carbide grows to be 200-500 mu m, and rotating and/or inverting the workpiece;
s2.6, repeating the steps S2.1 to S2.5 until the total growth thickness of the silicon carbide reaches the target requirement.
4. The method for manufacturing a silicon carbide thin-walled structure according to claim 2, wherein: in step S2.4, the raw material gas is trichloromethylsilane.
5. The method for preparing the silicon carbide thin-walled structure according to claim 1, wherein: and step S4, placing the workpiece into a high-temperature oxidation furnace, heating to 900-1200 ℃, introducing oxygen, reacting the graphite substrate with the oxygen at high temperature, discharging generated carbon dioxide, and obtaining the solid silicon carbide workpiece after the graphite substrate completely reacts.
6. The method for producing a silicon carbide thin-walled structure according to any one of claims 1 to 5, characterized in that: further comprising the steps of:
and S5, polishing and grinding the solid silicon carbide workpiece and adjusting the secondary size according to the requirements of the target size and the surface topography.
7. The method for manufacturing a silicon carbide thin-walled structure according to claim 6, wherein: further comprising the steps of:
and S6, cleaning by using 10% hydrofluoric acid, and then washing by using ultrasonic waves and deionized water to obtain a finished product.
8. The method for producing a silicon carbide thin-walled structure according to any one of claims 1 to 5, characterized in that: in step S1, the graphite substrate has a thickness of 2-50 mm and a surface finish of 500-1000nm, and is purified after being processed into a mold.
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| CN201911156094.0A CN112830786A (en) | 2019-11-22 | 2019-11-22 | Preparation method of silicon carbide thin-wall structural member |
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| EP0899358A2 (en) * | 1997-09-01 | 1999-03-03 | Tokai Carbon Company, Ltd. | Silicon carbide fabrication |
| US6300226B1 (en) * | 1998-02-09 | 2001-10-09 | Tokai Carbon Company, Ltd. | Formed SIC product and manufacturing method thereof |
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