CN116606166A - Method for rapidly preparing silicon carbide amorphous coating - Google Patents
Method for rapidly preparing silicon carbide amorphous coating Download PDFInfo
- Publication number
- CN116606166A CN116606166A CN202310460813.8A CN202310460813A CN116606166A CN 116606166 A CN116606166 A CN 116606166A CN 202310460813 A CN202310460813 A CN 202310460813A CN 116606166 A CN116606166 A CN 116606166A
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- workpiece
- amorphous coating
- rapidly preparing
- slurry
- 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 81
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 70
- 238000000576 coating method Methods 0.000 title claims abstract description 60
- 239000011248 coating agent Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 52
- 239000002131 composite material Substances 0.000 claims abstract description 35
- 238000005507 spraying Methods 0.000 claims abstract description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010891 electric arc Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims description 33
- 238000005245 sintering Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 5
- 239000011863 silicon-based powder Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000005253 cladding Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 10
- 239000010703 silicon Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000013081 microcrystal Substances 0.000 abstract description 4
- 239000011268 mixed slurry Substances 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 10
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 7
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 230000001680 brushing effect Effects 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000007613 slurry method Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000010285 flame spraying Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000007581 slurry coating method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
Abstract
The invention relates to the technical field of thermal field material preparation for industrial furnaces, and particularly discloses a method for rapidly preparing a silicon carbide amorphous coating. According to the method, mixed slurry of polycarbosilane and silicon carbide whiskers is used as a silicon source, a voltage-stabilizing and current-stabilizing power supply performs high-voltage arc discharge in a region to be coated of a carbon/carbon composite material workpiece, then the uniformly mixed slurry is deposited on the surface of the workpiece after passing through a high-temperature arc region in an ultrasonic spraying mode, the polycarbosilane is cracked at a high temperature to generate superfine SiC microcrystals, and the microcrystals and the silicon carbide whiskers are sintered and grown on the surface of the workpiece, so that a compact silicon carbide amorphous coating is finally generated. The silicon carbide coating prepared by the method can solve the problems of long production period, high manufacturing cost, poor designability, unstable product quality consistency and the like of the existing coating process. In addition, the SiC coating generated by the preparation process has compact structure, high strength, good combination with a matrix and longer service life.
Description
Technical Field
The invention relates to the technical field of thermal field material preparation for industrial furnaces, and particularly discloses a method for rapidly preparing a silicon carbide amorphous coating.
Background
At present, most of thermal field materials for a monocrystalline silicon drawing furnace adopt carbon material products (such as a crucible, a guide cylinder, a heat preservation cylinder, a heater and the like), and particularly in recent years, as the preparation process of carbon fibers and composite materials thereof is continuously improved, the carbon/carbon composite materials have higher and higher proportion in the selection and use of the thermal field materials by virtue of excellent high-temperature mechanical properties and shape designability. In particular to a crucible and a thermal insulation cylinder, the full replacement of isostatic pressing graphite has been realized. In the actual single crystal silicon drawing process, because the crucible and the heat preservation cylinder are used under the condition of high-temperature silicon steam, the silicon melt at high temperature has extremely strong reactivity, the silicon melt reacts with the quartz crucible to generate SiO and other oxidizing substances and volatilizes from the surface of the melt, the volatilized SiO and other oxidizing substances surround the outer surface of the carbon-carbon composite material, and the outer surface of the carbon-carbon composite material is gradually corroded to form pits until cracking and invalidation are carried out, so that the use effect is influenced, and the service life is shortened. Therefore, how to effectively inhibit the erosion of the carbon material is a key technical problem for prolonging the service life of the carbon/carbon composite material crucible/guide cylinder for the monocrystalline silicon drawing furnace.
Research shows that a layer of compact silicon carbide coating is prepared on the surface of the carbon/carbon crucible/guide cylinder, the surface hole sealing of the composite material is realized through the silicon carbide coating, and the diffusion and permeation of a silicon-containing gas source into the carbon/carbon composite material are inhibited, so that the erosion process of the material at high temperature is further delayed, and the method is an effective means for prolonging the service life of the carbon/carbon composite material crucible/guide cylinder.
At present, three main processes are used for manufacturing the silicon carbide coating:
reaction infiltration method
And (3) placing the carbon/carbon composite material product to be coated in a graphite crucible, embedding the carbon/carbon composite material product with the prepared silicon powder, then placing the graphite crucible in a high-temperature furnace, heating to melt the silicon powder into a liquid state, carrying out in-situ chemical reaction with the silicon carbide coating of the carbon/carbon composite material product, and cooling and taking out the carbon/carbon composite material product with the SiC coating along with the furnace after the reaction is finished, thus obtaining the carbon/carbon composite material sample with the SiC coating.
Second, chemical vapor deposition method
Placing a carbon/carbon composite material product to be coated in a chemical vapor deposition furnace, vacuumizing, raising the furnace temperature to the deposition process temperature, preserving heat for a period of time, then introducing a silicon-containing gas source (such as silicon vapor, trichloromethylsilane, tetrachlorosilane and the like), carrying out in-situ chemical reaction on the silicon-containing gas source and the surface of the carbon/carbon composite material in a high-temperature deposition area to generate a silicon carbide coating, and cooling and taking out the carbon/carbon composite material product with the SiC coating along with the furnace after the reaction is finished, thus obtaining the carbon/carbon composite material sample with the SiC coating.
Third, slurry brushing method
The slurry coating method is to coat slurry containing silicon carbide/simple substance silicon on the surface of a carbon-carbon composite material in a supersonic flame spraying, plasma spraying, explosion spraying, electric arc spraying, manual brushing and the like, then put the carbon-carbon composite material with the slurry coated on the surface into a high-temperature sintering furnace, raise the furnace temperature to the slurry sintering reaction temperature under the protection of vacuum or inert gas, perform reaction sintering for a period of time, generate a silicon carbide coating on the surface of the carbon-carbon composite material, cool the carbon-carbon composite material along with the furnace after the reaction is finished, and take out the carbon-carbon composite material sample with the SiC coating.
The silicon carbide coating is prepared by adopting a reaction infiltration method, and because the preparation temperature is high, the high-temperature Si melt is easy to erode the fiber and the interface, so that the fiber and the interface are easy to damage, and the mechanical property is seriously influenced; and because the reaction infiltration kinetics is controlled, the melted Si is not easy to be completely consumed, and large-size simple substance silicon residues are easy to appear in a product matrix, so that the service life of the material is reduced.
The silicon carbide coating is prepared by adopting a chemical vapor deposition method, so that the cost is high, and the porosity of the prepared composite material is high. And the chemical vapor deposition method is used for preparing the silicon carbide coating in a large-size product, so that the problems of different deposition thicknesses at different positions, different gas phase raw material proportions and the like of the product easily exist, and the coating composition of each part of the product is inconsistent, so that the method is generally not directly used for preparing the silicon carbide coating, but is used for carrying out densification treatment on the coating prepared by other preparation methods.
The slurry brushing method is adopted to prepare the silicon carbide coating, the ceramic powder in the slurry is difficult to be uniformly distributed, so that the silicon carbide coating on the surface of a product is unevenly distributed, the problems of uneven mechanical property and high-temperature property of materials, easy phase separation and the like are caused, in addition, in the process of generating the silicon carbide coating by high-temperature sintering, the slurry method is often required to realize densification of the coating by brushing and sintering for many times due to volatilization of liquid phase components in the slurry, and the slurry method is not suitable for preparing products with complex shapes.
Disclosure of Invention
The invention aims to provide a method for quickly preparing a silicon carbide amorphous coating, which is simple in process, excellent in performance, economical and practical.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for rapidly preparing a silicon carbide amorphous coating, comprising the steps of:
(1) Firstly adding a dispersing agent into an absolute ethanol solvent, then adding silicon carbide whiskers into an ethanol solution, and carrying out ultrasonic dispersion treatment on the suspension added with the silicon carbide whiskers;
(2) Mixing the dispersed suspension with polycarbosilane according to a proportion to prepare slurry, and placing the slurry into a ball mill at room temperature and a rotating speed of 100rpm for ball milling for 24 hours;
(3) Fixing a carbon/carbon composite material workpiece to be coated on a rotatable spraying tool, fixing a graphite electrode of an arc generator at a position 3-8cm away from the surface of the workpiece to be coated, and performing high-voltage arc discharge by adopting a stabilized voltage and stabilized current power supply;
(4) The slurry which is uniformly mixed after ball milling is coated on the surface of a workpiece to be coated by ultrasonic spraying equipment after passing through a high-temperature electric arc zone;
(5) Spraying slurry on the whole inner surface of the workpiece through a rotatable spraying tool under the condition that the relative distance between the surface of the workpiece to be coated and the graphite electrode is kept unchanged;
(6) And carrying out high-temperature sintering treatment on the sprayed carbon/carbon composite material workpiece.
Preferably, in the step (1), the addition amount of the dispersing agent is 0.2-2.0wt% of the mass of the silicon carbide whisker.
Preferably, in the step (1), the time of the ultrasonic dispersion treatment is 10-30min.
Preferably, in the step (2), the mass ratio of the dispersed suspension to the polycarbosilane is 1:5.
preferably, in the step (2), high-purity zirconia balls having a diameter of 10mm are used as the grinding medium, and the ball-to-material ratio is 1:1.
Preferably, in the step (3), the voltage of the high-voltage arc discharge is 200-380V, and the current is 5-30A.
Preferably, in the step (4), the slurry spraying amount is 0.5-2g/cm during cladding 2 。
Preferably, in said step (5), the linear velocity of the workpiece relative to the nozzle is 5-10mm/s.
Preferably, in the step (6), the high-temperature sintering temperature is 1500-1800 ℃ and the time is 1-3h.
Preferably, in the step (1), chopped silicon carbide fibers or ultrafine silicon powder are substituted for silicon carbide whiskers.
Preferably, in the step (1), the arc generator is a direct current arc generator or an alternating current arc generator.
Compared with the prior art, the invention has the beneficial effects that:
(1) The silicon carbide coating prepared by combining ultrasonic spraying with high-temperature arc sintering has smaller crystal grains and higher amorphous degree, so that compared with the coating prepared by the prior art, the silicon carbide coating has better mechanical property and higher crack expansion resistance under thermal shock. (2) As the material is doped with the silicon carbide whisker or the silicon carbide chopped fiber reinforced phase, the toughness of the coating is improved, and when defects such as cracks, holes and the like occur, large-area peeling can not occur. (3) Compared with the prior art, the method has the advantages that the problems of uneven thickness and components of different parts are easy to occur when the coating is prepared on a large-size workpiece, and the thickness and the component uniformity of the silicon carbide coating generated in situ by combining spraying and arc sintering are better.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Example 1
A method for rapidly preparing a silicon carbide amorphous coating, comprising the steps of:
(1) Firstly, adding a proper amount of dispersing agent into an absolute ethyl alcohol solvent, wherein the adding amount of the dispersing agent is 0.2wt.% of the mass of the silicon carbide whisker, then adding the silicon carbide whisker into an ethanol solution, and carrying out ultrasonic dispersion treatment on the suspension added with the silicon carbide whisker for 10min.
(2) Mixing the dispersed suspension with polycarbosilane according to a mass ratio of 1:5, mixing and preparing slurry, and ball milling the slurry at 100rpm for 24 hours at room temperature, wherein high-purity zirconia balls with the diameter of 10mm are used as grinding media, and the ball-to-material ratio is 1:1.
(3) The carbon/carbon composite material workpiece to be coated is fixed on a rotatable spraying tool, then a graphite electrode of an arc generator (a direct current arc generator or an alternating current arc generator can be selected) is fixed at a position of 3cm on the surface of the workpiece to be coated, and a stabilized voltage and stabilized current power supply is adopted for high-voltage arc discharge, and the voltage is 200V and the current is 5A.
(4) The slurry which is evenly mixed after ball milling is coated on the surface of a workpiece to be coated by ultrasonic spraying equipment after passing through a high-temperature electric arc zone, and the spraying amount of the slurry is 0.5g/cm 2 。
(5) And (3) spraying slurry on the whole inner surface of the workpiece through a rotatable spraying tool under the condition that the relative distance between the surface of the workpiece to be coated and the graphite electrode is kept unchanged, wherein the linear speed of the workpiece relative to the nozzle is 5mm/s.
(6) And (3) carrying out high-temperature sintering treatment on the sprayed carbon/carbon composite material workpiece, wherein the sintering temperature is 1500 ℃ and the sintering time is 3h.
Example 2
A method for rapidly preparing a silicon carbide amorphous coating, comprising the steps of:
(1) Firstly, adding a proper amount of dispersing agent into an absolute ethyl alcohol solvent, wherein the adding amount of the dispersing agent is 1.1wt.% of the mass of the silicon carbide whisker, then adding the silicon carbide whisker into an ethanol solution, and carrying out ultrasonic dispersion treatment on the suspension added with the silicon carbide whisker for 20min.
(2) Mixing the dispersed suspension with polycarbosilane according to a mass ratio of 1:5, mixing and preparing slurry, and ball milling the slurry at 100rpm for 24 hours at room temperature, wherein high-purity zirconia balls with the diameter of 10mm are used as grinding media, and the ball-to-material ratio is 1:1.
(3) The carbon/carbon composite material workpiece to be coated is fixed on a rotatable spraying tool, then a graphite electrode of an arc generator (a direct current arc generator or an alternating current arc generator can be selected) is fixed at the position of 5cm on the surface of the workpiece to be coated, and a stabilized voltage and stabilized current power supply is adopted to carry out high-voltage arc discharge, and the voltage is 290V and the current is 20A.
(4) The slurry which is evenly mixed after ball milling is coated on the surface of a workpiece to be coated by ultrasonic spraying equipment after passing through a high-temperature electric arc zone, and the spraying amount of the slurry is 1.5g/cm 2 。
(5) And (3) spraying slurry on the whole inner surface of the workpiece through a rotatable spraying tool under the condition that the relative distance between the surface of the workpiece to be coated and the graphite electrode is kept unchanged, wherein the linear speed of the workpiece relative to the nozzle is 5-10mm/s.
(6) And (3) carrying out high-temperature sintering treatment on the sprayed carbon/carbon composite material workpiece, wherein the sintering temperature is 1650 ℃ and the sintering time is 2h.
Example 3
A method for rapidly preparing a silicon carbide amorphous coating, comprising the steps of:
(1) Firstly, adding a proper amount of dispersing agent into an absolute ethyl alcohol solvent, wherein the adding amount of the dispersing agent is 2.0wt.% of the mass of the silicon carbide whisker, then adding the silicon carbide whisker into an ethanol solution, and carrying out ultrasonic dispersion treatment on the suspension added with the silicon carbide whisker for 30min.
(2) Mixing the dispersed suspension with polycarbosilane according to a mass ratio of 1:5, mixing and preparing slurry, wherein the slurry is not uniformly mixed, ball milling is carried out on the slurry at room temperature for 24 hours at a rotating speed of 100rpm, and high-purity zirconia balls with the diameter of 10mm are used as grinding media, wherein the ball-to-material ratio is 1:1.
(3) The carbon/carbon composite material workpiece to be coated is fixed on a rotatable spraying tool, then a graphite electrode of an arc generator (a direct current arc generator or an alternating current arc generator can be selected) is fixed at the position of 8cm on the surface of the workpiece to be coated, and a stabilized voltage and stabilized current power supply is adopted to carry out high-voltage arc discharge, and the voltage is 380V and the current is 30A.
(4) The slurry which is evenly mixed after ball milling is coated on the surface of a workpiece to be coated by ultrasonic spraying equipment after passing through a high-temperature electric arc zone, and the spraying amount of the slurry is 2g/cm 2 。
(5) And (3) spraying slurry on the whole inner surface of the workpiece through a rotatable spraying tool under the condition that the relative distance between the surface of the workpiece to be coated and the graphite electrode is kept unchanged, wherein the linear speed of the workpiece relative to the nozzle is 10mm/s.
(6) And (3) carrying out high-temperature sintering treatment on the sprayed carbon/carbon composite material workpiece, wherein the sintering temperature is 1800 ℃ and the sintering time is 1h.
Example 4
The silicon carbide whiskers in step (1) were replaced with chopped silicon carbide fibers or superfine silicon powder under the other conditions of examples 1-3 described above.
The silicon carbide amorphous coating prepared by the method has smaller crystal grains and higher amorphous degree due to the combination of ultrasonic spraying and high-temperature arc sintering, so that the coating has better mechanical property and higher crack expansion resistance under thermal shock compared with the coating prepared by the prior art.
As the material is doped with the silicon carbide whisker or the silicon carbide chopped fiber reinforced phase, the toughness of the coating is improved, and when defects such as cracks, holes and the like occur, large-area peeling can not occur.
Compared with the prior art, the method has the advantages that the problems of uneven thickness and components of different parts are easy to occur when the coating is prepared on a large-size workpiece, and the thickness and the component uniformity of the silicon carbide coating generated in situ by combining spraying and arc sintering are better.
The method adopts the mixed slurry of polycarbosilane and silicon carbide whiskers as a silicon source, a voltage-stabilizing and current-stabilizing power supply carries out high-voltage arc discharge in a region to be coated of a carbon/carbon composite material workpiece, then the uniformly mixed slurry is deposited on the surface of the workpiece after passing through a high-temperature arc region in an ultrasonic spraying mode, the polycarbosilane is cracked at high temperature to generate superfine SiC microcrystals, and the microcrystals and the silicon carbide whiskers are sintered and grown on the surface of the workpiece, so that a compact silicon carbide amorphous coating is finally generated. The silicon carbide coating prepared by the method can solve the problems of long production period, high manufacturing cost, poor designability, unstable product quality consistency and the like of the existing coating process. In addition, the SiC coating generated by the preparation process has compact structure, high strength, good combination with a matrix and longer service life.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (11)
1. A method for rapidly preparing a silicon carbide amorphous coating, comprising the steps of:
(1) Firstly adding a dispersing agent into an absolute ethanol solvent, then adding silicon carbide whiskers into an ethanol solution, and carrying out ultrasonic dispersion treatment on the suspension added with the silicon carbide whiskers;
(2) Mixing the dispersed suspension with polycarbosilane according to a proportion to prepare slurry, and placing the slurry into a ball mill at room temperature and a rotating speed of 100rpm for ball milling for 24 hours;
(3) Fixing a carbon/carbon composite material workpiece to be coated on a rotatable spraying tool, fixing a graphite electrode of an arc generator at a position 3-8cm away from the surface of the workpiece to be coated, and performing high-voltage arc discharge by adopting a stabilized voltage and stabilized current power supply;
(4) The slurry which is uniformly mixed after ball milling is coated on the surface of a workpiece to be coated by ultrasonic spraying equipment after passing through a high-temperature electric arc zone;
(5) Spraying slurry on the whole inner surface of the workpiece through a rotatable spraying tool under the condition that the relative distance between the surface of the workpiece to be coated and the graphite electrode is kept unchanged;
(6) And carrying out high-temperature sintering treatment on the sprayed carbon/carbon composite material workpiece.
2. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (1), the addition amount of the dispersing agent is 0.2-2.0wt% of the mass of the silicon carbide whisker.
3. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (1), the ultrasonic dispersion treatment time is 10-30min.
4. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (2), the mass ratio of the dispersed suspension to the polycarbosilane is 1:5.
5. the method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (2), high-purity zirconia balls with the diameter of 10mm are used as grinding media, and the ball-to-material ratio is 1:1.
6. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (3), the voltage of the high-voltage arc discharge is 200-380V, and the current is 5-30A.
7. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (4), the slurry spraying amount is 0.5-2g/cm during cladding 2 。
8. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (5), the linear velocity of the workpiece relative to the nozzle is 5-10mm/s.
9. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (6), the high-temperature sintering temperature is 1500-1800 ℃ and the time is 1-3h.
10. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (1), chopped silicon carbide fibers or superfine silicon powder are substituted for silicon carbide whiskers.
11. The method for rapidly preparing a silicon carbide amorphous coating according to claim 1, wherein: in the step (1), the arc generator is a direct current arc generator or an alternating current arc generator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310460813.8A CN116606166A (en) | 2023-04-26 | 2023-04-26 | Method for rapidly preparing silicon carbide amorphous coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310460813.8A CN116606166A (en) | 2023-04-26 | 2023-04-26 | Method for rapidly preparing silicon carbide amorphous coating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116606166A true CN116606166A (en) | 2023-08-18 |
Family
ID=87673789
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310460813.8A Pending CN116606166A (en) | 2023-04-26 | 2023-04-26 | Method for rapidly preparing silicon carbide amorphous coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116606166A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000185981A (en) * | 1998-12-21 | 2000-07-04 | Tokai Carbon Co Ltd | Porous molded article of silicon carbide and its production |
| CN101654778A (en) * | 2008-08-21 | 2010-02-24 | 北京盘天新技术有限公司 | Method for preparing insulating heat conducting ceramic coating from polymer precursor |
| CN102822985A (en) * | 2010-04-06 | 2012-12-12 | 高菲欧股份有限公司 | Epitaxial structures, methods of forming the same, and devices including the same |
| CN104264455A (en) * | 2014-09-24 | 2015-01-07 | 中国人民解放军国防科学技术大学 | Low-cost preparation method of fiber surface silicon carbide coating |
| CN109721377A (en) * | 2019-01-30 | 2019-05-07 | 湖南兴晟新材料科技有限公司 | Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof |
| WO2020199681A1 (en) * | 2019-04-02 | 2020-10-08 | 安徽弘昌新材料有限公司 | Method for preparing high-performance silicon carbide coating on surface of carbon/carbon composite thermal insulation material |
-
2023
- 2023-04-26 CN CN202310460813.8A patent/CN116606166A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000185981A (en) * | 1998-12-21 | 2000-07-04 | Tokai Carbon Co Ltd | Porous molded article of silicon carbide and its production |
| CN101654778A (en) * | 2008-08-21 | 2010-02-24 | 北京盘天新技术有限公司 | Method for preparing insulating heat conducting ceramic coating from polymer precursor |
| CN102822985A (en) * | 2010-04-06 | 2012-12-12 | 高菲欧股份有限公司 | Epitaxial structures, methods of forming the same, and devices including the same |
| CN104264455A (en) * | 2014-09-24 | 2015-01-07 | 中国人民解放军国防科学技术大学 | Low-cost preparation method of fiber surface silicon carbide coating |
| CN109721377A (en) * | 2019-01-30 | 2019-05-07 | 湖南兴晟新材料科技有限公司 | Ceramic Matrix Composites Reinforced by Carbon Fibers and preparation method thereof |
| WO2020199681A1 (en) * | 2019-04-02 | 2020-10-08 | 安徽弘昌新材料有限公司 | Method for preparing high-performance silicon carbide coating on surface of carbon/carbon composite thermal insulation material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107814591B (en) | Preparation method of boride modified silicon-based antioxidant coating on surface of carbon material | |
| TWI722531B (en) | Boroncarbide sintered body and etch apparatus comprising the same | |
| CN110643929B (en) | Anti-sticking coating on surface of hard alloy sintered boat and preparation method thereof | |
| JP3657800B2 (en) | Molybdenum disilicide-based composite ceramic heating element and manufacturing method thereof | |
| Zhou et al. | Microstructural evolution of SiC coating on C/C composites exposed to 1500° C in ambient air | |
| CN100537485C (en) | Method for preparing silicon carbide nano-wire | |
| CN105967759A (en) | Rare earth oxide modified Si-Mo-O gradient anti-oxidation coating layer and production method thereof | |
| CN107056334A (en) | A kind of ZrC ceramic material surfaces ZrB2The preparation method of SiC composite coatings | |
| CN112592207A (en) | Self-healing ZrB2-SiC-Y2O3Coating and application thereof to SiC-embedded carbon-carbon composite material | |
| CN116332678B (en) | Method for preparing tantalum carbide coating on surface of carbon material | |
| Li et al. | Sealing role of Ti-rich phase in HfC-ZrC-TiC coating for C/C composites during ablation above 2100° C | |
| CN110590404A (en) | HfB on surface of carbon-based material2Preparation method of-SiC oxidation resistant coating | |
| CN105350294B (en) | A kind of chopped carbon fiber of applying silicon carbide layer and preparation method thereof | |
| CN107244944B (en) | Carbon/carbon composite material with antioxidant coating and preparation method and application thereof | |
| Wang et al. | Enhanced oxidation resistance of Mo-modified Si-SiC coating on C/C composites by laser-inducing | |
| CN107675120A (en) | A kind of method for preparing silication molybdenum coating in molybdenum or molybdenum alloy surface | |
| CN111662085B (en) | Preparation method of tungsten carbide ceramic containing diamond based on non-contact flash firing technology | |
| CN116606166A (en) | Method for rapidly preparing silicon carbide amorphous coating | |
| CN108504980B (en) | High-temperature-resistant ablation-resistant composite coating and preparation method thereof | |
| Zou et al. | Enhanced ablative resistance of C/C composites with densified ZrB2-based ceramics by incorporation of Mo as interface layer | |
| CN115894085B (en) | Composite ceramic coating material and preparation method and application thereof | |
| RU2471751C1 (en) | Method of producing protective coating and composition of protective coating mixture | |
| CN114455969B (en) | High-density C/C-SiC composite material crucible containing alumina coating | |
| CN114455963B (en) | A composition containing alpha-Al 2 O 3 Coated carbon/carbon-silicon carbide composite crucible | |
| CN106892684B (en) | Preparation method of ZrC coating on surface of C/C composite material |
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 |