CN111892419A - High-shock-resistance silicon carbide boat and preparation method thereof - Google Patents
High-shock-resistance silicon carbide boat and preparation method thereof Download PDFInfo
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- CN111892419A CN111892419A CN202010765333.9A CN202010765333A CN111892419A CN 111892419 A CN111892419 A CN 111892419A CN 202010765333 A CN202010765333 A CN 202010765333A CN 111892419 A CN111892419 A CN 111892419A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 84
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 84
- 239000010703 silicon Substances 0.000 claims abstract description 84
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 20
- 230000035939 shock Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 40
- 238000004140 cleaning Methods 0.000 claims description 38
- 238000001035 drying Methods 0.000 claims description 38
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 26
- 239000001257 hydrogen Substances 0.000 claims description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims description 24
- 238000005475 siliconizing Methods 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 16
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003599 detergent Substances 0.000 claims description 10
- 239000004519 grease Substances 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 238000003780 insertion Methods 0.000 claims description 10
- 230000037431 insertion Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000007769 metal material Substances 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011049 filling Methods 0.000 description 3
- 239000011799 hole material Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/673—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere using specially adapted carriers or holders; Fixing the workpieces on such carriers or holders
- H01L21/67313—Horizontal boat type carrier whereby the substrates are vertically supported, e.g. comprising rod-shaped elements
- H01L21/67316—Horizontal boat type carrier whereby the substrates are vertically supported, e.g. comprising rod-shaped elements characterized by a material, a roughness, a coating or the like
Abstract
The invention relates to the technical field of photovoltaics, in particular to a silicon carbide boat with high shock resistance and a preparation method thereof, wherein the transverse size of the silicon carbide boat can be adjusted, the processing yield is improved, a compact silicon carbide coating is formed on the surface of the silicon boat, and the acid and alkali corrosion resistance is improved; including the left side that is the symmetry form place the piece and place the left side with the right side and place the connecting piece that the piece is connected, place and be provided with a plurality of first left standing grooves and a plurality of second left standing groove on the piece on a left side, place and be provided with a plurality of first right standing grooves and a plurality of second right standing groove on the piece on the right side, every first left standing groove of group all with a set of second left standing groove, first right standing groove and second right standing groove are in on same vertical face, the connecting piece includes the connecting block, the front and back end of connecting block left side wall all is provided with left arch, place and be provided with two sets of left recesses with protruding sliding fit in two sets of left on the piece on a left side.
Description
Technical Field
The invention relates to the technical field of photovoltaics, in particular to a silicon carbide boat with high shock resistance and a preparation method thereof.
Background
As is known, a silicon carbide boat is a carrier of a large-scale integrated circuit in the process of ultrahigh temperature processing, plays an important role in the production process of semiconductor wafers, and has the characteristics of high strength, high purity, high heat conductivity, no air holes, acid and alkali corrosion resistance, no pollution at high temperature, no deformation, good thermal shock resistance and the like.
The existing silicon carbide boat with high shock resistance has the following defects: the transverse size of the aluminum alloy can not be adjusted during processing, so that the yield is low, and the aluminum alloy has the defects of more bubbles and poor acid and alkali corrosion resistance.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a silicon carbide boat with high shock resistance, which has adjustable lateral dimensions, improves the yield of the processed products, forms a dense silicon carbide coating on the surface of the silicon boat, and improves the resistance to acid and alkali corrosion.
Another object of the present invention is to provide a method for manufacturing a silicon carbide boat with high shock resistance.
The invention discloses a high-shock-resistance silicon carbide boat which comprises a left placing piece, a right placing piece and a connecting piece, wherein the left placing piece and the right placing piece are symmetrical, the connecting piece is used for connecting the left placing piece and the right placing piece, a plurality of first left placing grooves and a plurality of second left placing grooves are formed in the left placing piece, a plurality of first right placing grooves and a plurality of second right placing grooves are formed in the right placing piece, each group of first left placing grooves and one group of second left placing grooves, each group of first right placing grooves and one group of second right placing grooves are located on the same vertical surface, the connecting piece comprises a connecting block, left protrusions are arranged at the front end and the rear end of the left side wall of the connecting block, two groups of left grooves in sliding fit with the two groups of left protrusions are formed in the left placing piece, right protrusions are arranged at the front end and the rear end of the right side wall of the connecting block, and two groups of right grooves.
According to the silicon carbide boat with high shock resistance, the two groups of left protrusions, the two groups of right protrusions and the connecting block are integrally formed.
The invention relates to a preparation method of a silicon carbide boat with high shock resistance, which comprises the following steps:
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat;
s4, placing the silicon boat in the step S3 in a drying chamber for drying, wherein the temperature of the drying chamber is 100-120 ℃, and the drying time is 15-20 hours;
s5, heating the silicon boat in the S4 to 1800-1900 ℃ for sintering for 0.5-1h, then cooling to 1000-1200 ℃, vacuumizing to 3-5KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating of 20-30um on the surface of the silicon boat;
s6, cooling to 800-;
s7, heating to 1400-1700 ℃, vacuumizing to 100-150Pa, siliconizing the carbon layer by using simple substance silicon as a raw material and adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S8, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
According to the preparation method of the silicon carbide boat with high shock resistance, the cleaning mode in S2 comprises the steps of (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) the silicon impurities generated in the S1 process were cleaned using hydrofluoric acid and pure water as cleaning liquids.
In the preparation method of the silicon carbide boat with high shock resistance, in S3, the insertion depths of the left protrusion and the right protrusion can be adjusted according to needs to adjust the overall size of the silicon boat, and the vacant parts of the left groove and the right groove are filled by filling silicon carbide powder.
According to the preparation method of the silicon carbide boat with high shock resistance, the hydrogen flow in the S5 is 0.03-0.1m3H, argon flow of 0.03-0.4m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
According to the preparation method of the silicon carbide boat with high shock resistance, the flow of methane in S6 is 0.01-0.1m3The nitrogen flow is 0.02-0.2m3/h。
According to the preparation method of the silicon carbide boat with high shock resistance, the purity of the simple substance silicon in the S7 is 99.99%.
Compared with the prior art, the invention has the beneficial effects that: firstly, the silicon boat is preliminarily fixed in a splicing and bonding mode, and the size of the silicon boat can be adjusted in the processing process so as to reduce the processing difficulty and improve the yield; secondly, the silicon carbide coating is plated in advance, carbon is deposited again for filling, and finally a gas phase siliconizing mode is adopted, so that the finally formed silicon carbide coating is compact and has no air holes, and the corrosion resistance is improved.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a cross-sectional view of the left placement member, the first left placement channel and the second left placement channel;
in the drawings, the reference numbers: 1. a left placement member; 2. a right placement member; 3. connecting blocks; 4. a left bulge; 5. a right bulge; 6. a first left placement trough; 7. the second left standing groove.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1:
the method comprises the following steps:
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, placing the silicon boat in the step S3 in a drying chamber for drying, wherein the temperature of the drying chamber is 115 ℃, and drying is carried out for 17 hours;
s5, heating the silicon boat in the S4 to 1800 ℃ for sintering for 1h, then cooling to 1000 ℃, vacuumizing to 5KPa, introducing hydrogen, argon and methyl trichlorosilane, and depositing a silicon carbide coating of 20um on the surface of the silicon boat; the hydrogen flow rate was 0.03m3H, argon flow of 0.03m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
S6, cooling to 1000 ℃, vacuumizing to 1000Pa, continuously introducing methane and nitrogen to form a carbon layer on the surface of the silicon carbide coating, and plugging the exposed part of the silicon carbide coating; the flow rate of methane is 0.1m3H, nitrogen flow 0.2m3/h；
S7, heating to 1700 ℃, vacuumizing to 150Pa, siliconizing the carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material through a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S8, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Example 2:
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, placing the silicon boat in the step S3 in a drying chamber for drying, wherein the temperature of the drying chamber is 100-120 ℃, and the drying time is 15-20 hours;
s5, heating the silicon boat in the S4 to 1900 ℃ for sintering, wherein the sintering time is 0.5h, then cooling to 1200 ℃, vacuumizing to 3KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating of 30um on the surface of the silicon boat; the hydrogen flow rate was 0.1m3H, argon flow of 0.4m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
S6, cooling to 800-; the flow rate of methane is 0.01m3H, nitrogen flow 0.02m3/h；
S7, heating to 1400 ℃, vacuumizing to 100Pa, siliconizing a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S8, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Example 3:
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, drying the silicon boat in the step S3 in a drying chamber at 175 ℃ for 18 hours;
s5, heating the silicon boat in the S4 to 1872 ℃ for sintering, sintering for 0.7h, then cooling to 1194 ℃, vacuumizing to 4.6KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating of 23um on the surface of the silicon boat; the hydrogen flow rate was 0.05m3H, argon flow of 0.16m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
S6, cooling to 915 ℃, vacuumizing to 310Pa, continuously introducing methane and nitrogen to form a carbon layer on the surface of the silicon carbide coating, and plugging the exposed part of the silicon carbide coating; the flow rate of methane is 0.05m3H, nitrogen flow 0.14m3/h；
S7, heating to 1500 ℃, vacuumizing to 112Pa, siliconizing a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S8, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Example 4:
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, drying the silicon boat in the step S3 in a drying chamber at 175 ℃ for 18 hours;
s5, heating the silicon boat in the S4 to 1756 ℃ for sintering for 0.7h, then cooling to 1150 ℃, vacuumizing to 4.6KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating 23um on the surface of the silicon boat; the hydrogen flow rate was 0.05m3H, argon flow of 0.16m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
S6, cooling to 912 ℃, vacuumizing to 310Pa, continuously introducing methane and nitrogen to form a carbon layer on the surface of the silicon carbide coating, and plugging the exposed part of the silicon carbide coating; the flow rate of methane is 0.05m3H, nitrogen flow 0.14m3/h；
S7, heating to 1500 ℃, vacuumizing to 112Pa, siliconizing a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S8, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Comparative example 1:
the difference from example 4 is that: S5-S8;
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, drying the silicon boat in the step S3 in a drying chamber at 175 ℃ for 18 hours;
s5, heating the silicon boat in the S4 to 1756 ℃ for sintering for 0.7h, and then cooling to 1150 ℃;
s6, heating to 1500 ℃,
carrying out siliconizing on a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S7, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Comparative example 2:
the difference from example 3 is that: S5-S8;
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, drying the silicon boat in the step S3 in a drying chamber at 175 ℃ for 18 hours;
s5, heating the silicon boat in the S4 to 1872 ℃ for sintering for 0.7h, and then cooling to 1194 ℃;
s6, heating to 1500 ℃, vacuumizing to 112Pa, siliconizing a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S7, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Comparative example 3:
the difference from example 3 is that: no S6;
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, drying the silicon boat in the step S3 in a drying chamber at 175 ℃ for 18 hours;
s5, heating the silicon boat in the S4 to 1872 ℃ for sintering, sintering for 0.7h, then cooling to 1194 ℃, vacuumizing to 4.6KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating of 23um on the surface of the silicon boat; the hydrogen flow rate was 0.05m3H, argon flow of 0.16m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
S6, heating to 1500 ℃, vacuumizing to 112Pa, siliconizing a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S7, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
Comparative example 4:
the difference from example 4 is that: no S6;
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying; the cleaning mode comprises (1) removing harmful substances such as grease and the like by using a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) cleaning silicon impurities generated in the S1 process by using hydrofluoric acid and pure water as cleaning liquids;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat; the insertion depth of the left bulge and the right bulge can be adjusted according to the requirement to adjust the overall size of the silicon boat, and the left groove are filled with silicon carbide powder;
s4, drying the silicon boat in the step S3 in a drying chamber at 175 ℃ for 18 hours;
s5, heating the silicon boat in the S4 to 1756 ℃ for sintering for 0.7h, then cooling to 1150 ℃, vacuumizing to 4.6KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating 23um on the surface of the silicon boat; the hydrogen flow rate was 0.05m3H, argon flow of 0.16m3The molar mass ratio of hydrogen to monomethyltrichlorosilane is 8: 1.
S6, heating to 1500 ℃, vacuumizing to 112Pa, siliconizing a carbon layer by using simple substance silicon (with the purity of 99.99%) as a raw material by adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S7, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
The following data were obtained from examples 1 to 4 and comparative examples 1 to 4:
from the data, the finally formed silicon carbide coating is compact and has no air holes and the corrosion resistance is improved by plating the silicon carbide coating in advance, depositing carbon for filling and finally adopting a gas phase siliconizing mode.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The silicon carbide boat with high shock resistance is characterized by comprising a left placing piece, a right placing piece and a connecting piece, wherein the left placing piece and the right placing piece are symmetrical, the connecting piece is used for connecting the left placing piece and the right placing piece, the left placing piece is provided with a plurality of first left placing grooves and a plurality of second left placing grooves, the right placing piece is provided with a plurality of first right placing grooves and a plurality of second right placing grooves, each group of the first left placing grooves and the group of the second left placing grooves, the first right placing grooves and the second right placing grooves are positioned on the same vertical plane, the connecting piece includes the connecting block, and the front and back end of connecting block left side wall all is provided with left arch, a left side place on be provided with two sets of left recesses of two sets of left protruding sliding fit, the front and back end of connecting block right side wall all is provided with right arch, the right side place on be provided with two sets of right recesses of two sets of right protruding sliding fit.
2. The silicon carbide boat according to claim 1, wherein the two sets of left protrusions and the two sets of right protrusions are integrally formed with the connecting block.
3. The method for preparing a silicon carbide boat of any of claims 1-2, comprising the steps of:
s1, preparing a left placing piece, a right placing piece and a connecting piece by using the silicon carbide substrate;
s2, washing the left placing piece, the right placing piece and the connecting piece for multiple times and drying;
s3, inserting the left protrusion and the right protrusion on the connecting piece into the left groove of the left placing piece and the right groove of the right placing piece respectively, and bonding the left protrusion and the right protrusion together by a bonding method to form the silicon boat;
s4, placing the silicon boat in the step S3 in a drying chamber for drying, wherein the temperature of the drying chamber is 100-120 ℃, and the drying time is 15-20 hours;
s5, heating the silicon boat in the S4 to 1800-1900 ℃ for sintering for 0.5-1h, then cooling to 1000-1200 ℃, vacuumizing to 3-5KPa, and introducing hydrogen, argon and methyl trichlorosilane to deposit a silicon carbide coating of 20-30um on the surface of the silicon boat;
s6, cooling to 800-;
s7, heating to 1400-1700 ℃, vacuumizing to 100-150Pa, siliconizing the carbon layer by using simple substance silicon as a raw material and adopting a gas phase siliconizing method, and keeping the temperature for 3-6 hours;
and S8, cooling to normal temperature in stages, taking out the silicon boat, and polishing and cleaning.
4. The method of claim 3, wherein the cleaning in S2 comprises (1) removing harmful substances such as grease with a detergent; (2) soaking in aqua regia for 12-24h to remove residual metal material on the surface; (3) the silicon impurities generated in the S1 process were cleaned using hydrofluoric acid and pure water as cleaning liquids.
5. The method of claim 3, wherein in step S3, the insertion depth of the left protrusion and the right protrusion can be adjusted as required to adjust the overall size of the silicon boat, and the empty parts of the left groove and the right groove are filled with silicon carbide powder.
6. The method of claim 3, wherein the hydrogen flow in S5 is 0.03-0.1m3H, argon flow of 0.03-0.4m3H, the molar mass ratio of hydrogen to monomethyltrichlorosilane is8:1。
7. The method of claim 3, wherein the methane flow rate in S6 is 0.01-0.1m3The nitrogen flow is 0.02-0.2m3/h。
8. The method of claim 3, wherein the purity of elemental silicon in S7 is 99.99%.
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