CN107082651A - A kind of coat of silicon carbide and preparation method thereof - Google Patents
A kind of coat of silicon carbide and preparation method thereof Download PDFInfo
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- CN107082651A CN107082651A CN201710312326.1A CN201710312326A CN107082651A CN 107082651 A CN107082651 A CN 107082651A CN 201710312326 A CN201710312326 A CN 201710312326A CN 107082651 A CN107082651 A CN 107082651A
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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
- C04B41/45—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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- 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
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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
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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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
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
Abstract
The present invention relates to a kind of coat of silicon carbide and preparation method thereof, category inorganic functional coating material field.The preparation method of carborundum includes:First coating slurry and second coating slurry are prepared respectively, wherein it is 3 that the first coating slurry feedstock, which includes weight ratio,:(3~5):Phenolic resin, Si powder and the SiC powder of (0.5~1.5), the second coating slurry are silication slurry;The first coating slurry of preparation is coated to carbonaceous material surface, solidification obtains internal coated layer, then by the silication slurry coating prepared to internal coated layer surface, and solidification obtains outer covering layer;The carbonaceous material for foring outer covering layer is subjected to high-temperature vacuum sintering, coat of silicon carbide is obtained.The internal coated layer and outer covering layer of coat of silicon carbide provided in an embodiment of the present invention can be formed by a high temperature sintering, realize the rapid shaping of high-quality coat of silicon carbide, preparation process significantly simplifies, manufacturing cycle reduction by more than 50%;Adapt to the quick preparation of different structure, different sizes and special-shaped carbonaceous material and its component coating.
Description
Technical field
The present invention relates to a kind of coat of silicon carbide and preparation method thereof, belong to inorganic functional coating material field.
Background technology
Antioxidant coating technology is to realize carbonaceous material (including carbon/carbon compound material, graphite material, carbon/silicon carbide compound
Material etc.) key be on active service in high temperature aerobic environment, being formed on carbonaceous material surface can for the coating of system with resistance to oxidation ceramics
Effectively to stop the contact of ambient oxygen and internal carbonaceous material, so as to play the high-temperature behavior of carbonaceous material.
Method for preparing antioxidant coating is a lot, there is solid phase investment, brushing method, plasma spraying method, chemical vapor deposition
Method, coating sintering method etc., wherein coating sintering method be in recent years exploitation formed, its have different substrate materials Technological adaptability it is good,
It is small to base material damage, easy to realize the advantages of large-size components are prepared, prepared suitable for abnormity component coating, show good
Engineering application value.With coat of silicon carbide prepared by coating sintering method thermostructural composite can be realized in less than 1700 DEG C temperature
Oxidation protection under degree, realizes that the high temperature of Complex Different Shape component is aerobic on the premise of can not damaged ensureing base material mechanical property
It is on active service when long in environment, good application prospect is shown in solar heat protection/load integrated component of new aerospace craft.
, it is necessary to which repeated multiple times coating and sintering process could realize coating when coating sintering method prepares coat of silicon carbide
It is continuous and reach certain thickness requirement, superior in quality effective coating is formed, complex technical process, manufacturing cycle is longer, accordingly
Preparation cost it is also higher.Further, since complex procedures, the antioxidant coating of preparation is easy to be damaged in technical process
Wound, and then add the further perfect cycle of coating.
The content of the invention
It is an object of the invention to prepare the not enough of high-quality coat of silicon carbide for coating sintering method to couple there is provided one kind
The method that coating sintering quickly prepares high-quality coat of silicon carbide, realizes carbonaceous material surface, and especially carbon containing heat structure is combined
It is prepared by the short cycle of the high-quality coat of silicon carbide of material surface, low cost.
To achieve the above object, the present invention provides following technical scheme:
A kind of preparation method of coat of silicon carbide, comprises the following steps:
Step (1):First coating slurry and second coating slurry are prepared respectively, wherein the first coating slurry feedstock bag
It is 3 to include mass ratio:(3~5):Phenolic resin, Si powder and the SiC powder of (0.5~1.5), the second coating slurry are starched for silication
Material;
Step (2):The first coating slurry of preparation is coated to carbonaceous material surface, solidification obtains internal coated layer, then will
The silication slurry prepared is coated to the internal coated layer surface, and solidification obtains outer covering layer;
Step (3):The carbonaceous material for foring outer covering layer is subjected to high-temperature vacuum sintering, coat of silicon carbide is obtained.
In an alternative embodiment, it is 3 that the raw material of the silication slurry, which includes mass ratio,:(2~4):The silicon tree of (1~3)
Fat, Si powder and SiC powder.
In an alternative embodiment, step (1) the first coating slurry feedstock and second coating slurry feedstock also include
Organic solvent, wherein, the organic solvent is one or more kinds of combinations in ethanol, toluene or acetone.
In an alternative embodiment, the quality of the organic solvent of the first coating raw material is total for the first coating raw material
The 10~60% of quality;The quality of the organic solvent of the second coating raw material is the 10 of the total matter content of the second coating raw material
~60%.
In an alternative embodiment, in step (2), the internal coated layer thickness is 50~300 μm, and the outer covering layer thickness is
0.5~3mm.
In an alternative embodiment, the high-temperature vacuum sintering condition described in step (3) is:Temperature is 1300 DEG C~1800
DEG C, pressure is less than 10kPa.
In an alternative embodiment, after step (3) high-temperature vacuum sintering, surface Redundant frame is fallen by deionized water rinsing,
Obtain coat of silicon carbide.
In an alternative embodiment, step (3) also includes:
Overcoating layer surface after sintering prepares glaze layer.
In an alternative embodiment, the density of the carbonaceous material is 1.2g/cm3~2.2g/cm3。
Coat of silicon carbide prepared by the above method.
The advantage of the present invention compared with prior art:
(1) internal coated layer and outer covering layer combination can form continuous carbonization silicon coating by a high temperature sintering, realize
The rapid shaping of high-quality coat of silicon carbide, preparation process significantly simplifies, manufacturing cycle reduction by more than 50%;
(2) by controlling the thickness of internal coated layer and outer covering layer to realize the Effective Regulation of coat of silicon carbide thickness, so that
Realize the preparation of the coat of silicon carbide of different application;
(3) slurry of first coating can realize effective filling on porous substrate surface, it is possible to achieve densification carborundum
The quick preparation of coating;
(4) preparation technology of coating adapts to the quick of different structure, different size and special-shaped carbonaceous material and its component coating
Prepare.
Brief description of the drawings
The coat schematic diagram that Fig. 1 obtains for the preparation method of coat of silicon carbide provided in an embodiment of the present invention;
The knot for the product that Fig. 2 obtains for the preparation method of coat of silicon carbide provided in an embodiment of the present invention after vacuum-sintering
Structure schematic diagram;
Fig. 3 has coat of silicon carbide for what the preparation method of coat of silicon carbide provided in an embodiment of the present invention finally gave
Product structure schematic diagram.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The embodiments of the invention provide a kind of preparation method of coat of silicon carbide, comprise the following steps:
Step (1):First coating slurry and second coating slurry are prepared respectively, wherein the first coating slurry feedstock bag
It is 3 to include mass ratio:(3~5):Phenolic resin, Si powder and the SiC powder of (0.5~1.5), the second coating slurry are starched for silication
Material;
Specifically, the silication slurry can be the coating that is used in traditional coating sintering method coat of silicon carbide preparation technology
Slurry;In the embodiment of the present invention, it is 3 that the raw material of the silication slurry, which includes mass ratio,:(2~4):Silicones, the Si of (1~3)
Powder and SiC powder.Silication formula of size provided in an embodiment of the present invention, coupling painting can be formed by being combined with first coating formula of size
Extra silicon source is provided for first coating in coating, sintering process, the continuous carbon SiClx for promoting first coating formation thickness larger is applied
Layer.
Step (2):Referring to Fig. 1, the first coating slurry of preparation is coated to the surface of carbonaceous material 1, solidification obtains interior cover
Layer 2, then by the silication slurry coating prepared to the surface of internal coated layer 2, solidification obtains outer covering layer 3;
Specifically, in the embodiment of the present invention long-time dry or heating, drying by way of solidify;
Specifically, the first coating slurry feedstock and second coating slurry feedstock also include organic solvent, by organic
Solvent regulates and controls the mobility of slurry, wherein, the organic solvent is one or more kinds of groups in ethanol, toluene or acetone
Close.
In the embodiment of the present invention, the quality of the organic solvent of the first coating raw material is the total matter of first coating raw material
The 10~60% of amount;The quality of the organic solvent of the second coating raw material for the total matter content of the second coating raw material 10~
60%.
Organic solvent content provided in an embodiment of the present invention, can either ensure that the slurry of allotment effectively fills porous substrate table
Face gap, ensure that slurry has the mobility for meeting technological requirement again.
Specifically, in the embodiment of the present invention, the density of carbonaceous material is in 1.2g/cm3~2.2g/cm3In the range of.
Referring to Fig. 1, in the embodiment of the present invention, internal coated layer 2 and outer covering layer 3 are equal thickness coating, and the thickness of internal coated layer 2 is 50
~300 μm, the thickness of outer covering layer 3 is 0.5~3mm.
Step (3):The carbonaceous material 1 for foring outer covering layer 3 is subjected to high-temperature vacuum sintering, coat of silicon carbide is obtained.
Specifically, in embodiments of the present invention, described high-temperature vacuum sintering condition is:Temperature is 1300 DEG C~1800
DEG C, pressure is less than 10kPa, and sintering time is preferably 0.5-5h.
Specifically, referring to Fig. 2, after high-temperature vacuum sintering, the surface of coat of silicon carbide 5 has Redundant frame 4, it is necessary to remove surface
Redundant frame 4, the embodiment of the present invention falls surface Redundant frame 4 by deionized water rinsing, and obtaining surface has the production of coat of silicon carbide 5
Product, concrete structure is referring to Fig. 3.
In order to improve the antioxygenic property of silicon carbide layer, the coat of silicon carbide surface that can also be formed after sintering prepares glaze
Layer.
Coat of silicon carbide preparation method provided in an embodiment of the present invention, has the advantages that:
(1) internal coated layer and outer covering layer combination can form continuous coat of silicon carbide by a high temperature sintering, realize
The rapid shaping of high-quality coat of silicon carbide, preparation process significantly simplifies, manufacturing cycle reduction by more than 50%;
(2) by controlling the thickness of internal coated layer and outer covering layer to realize the Effective Regulation of coat of silicon carbide thickness, so that
Realize the preparation of the coat of silicon carbide of different application;
(3) slurry of first coating can realize effective filling on porous substrate surface, it is possible to achieve densification carborundum
The quick preparation of coating;
(4) preparation technology of coating adapts to the quick of different structure, different size and special-shaped carbonaceous material and its component coating
Prepare.
The embodiment of the present invention additionally provides a kind of coat of silicon carbide, and the coat of silicon carbide is prepared by above method embodiment
, with above method embodiment identical beneficial effect, will not be repeated here.
It is below several specific embodiments of the present invention:
Embodiment 1:
(1) according to phenolic resin:Si powder:SiC powder:Ethanol=3:4:0.5:3.5 mass ratio weighs each material, will weigh
Phenolic resin, Si powder and SiC powder it is well mixed, regulate and control its viscosity to the degree for being suitable to coating with the ethanol weighed, form master
Body layer slurry;According to silicones:Si powder:SiC powder:Toluene=3:3:1:3 mass ratio weighs each material, by the silicon tree weighed
Fat, Si powder and SiC powder are well mixed, regulate and control its viscosity to the degree for being suitable to coating with toluene with weighing, form silication slurry.
(2) using density as 1.8g/cm3Carbon/carbon compound material be base material, body layer slurry is coated to substrate surface,
Then it solidify to form the internal coated layer of about 100 μm of thickness;Silication slurry is coated in two times and is cured to internal coated layer surface, thickness is formed
About 1.5mm outer covering layer.Form the carbon/carbon compound material for covering coupling coat.
(3) carbon/carbon compound material for coupling coat will be covered in vacuum sintering furnace under 1600 DEG C, 8KPa pressure
After reaction-sintered, the Redundant frame on surface is removed with high pressure water cleaning, obtained after drying be prepared for the oxidation resistant carbon of coat of silicon carbide/
Carbon composite.
Comparative example 1:
Multiple Sintering Method according to traditional coating sintering method prepares coat of silicon carbide, specific as follows:
Coating slurry proportioning is silicones:Si powder:SiC powder=3:3:1 (mass ratio), is coated in two times after being well mixed
1.8g/cm3Carbon/carbon composite material base material surface, thickness about 1.5mm coat is formed, then in 1600 DEG C, 8KPa pressure
Under vacuum sintering furnace in reaction-sintered, the Redundant frame on surface is removed by high pressure water cleaning and above-mentioned painting is repeated after drying
Cover, vacuum-sintering and Redundant frame processing procedure 2 times, obtain the Antioxidated Carbon/carbon Composite Materials for being prepared for coat of silicon carbide.
After tested, the coat of silicon carbide uniformly continuous that embodiment 1 is obtained, about 85 μm of thickness, and the carbon obtained in comparative example 1
SiClx coating also has the feature of uniformly continuous, but only 75 μm or so of thickness after the coating sintering of three times.1200 DEG C of static state
Oxidation examination shows that the oxidation protection ability for the coat of silicon carbide that embodiment 1 is obtained is not less than comparative example.It is carbonized in embodiment 1
The manufacturing cycle of silicon coating is 5 days, and comparative example 1 is 15 days.Therefore, the inventive method prepares high-quality coat of silicon carbide in guarantor
On the basis of having held oxidation protection ability, the characteristics of with short cycle, low cost.
Embodiment 2:
(1) according to phenolic resin:Si powder:SiC powder:Acetone=3:3:1:4 mass ratio weighs each material, by the phenol weighed
Urea formaldehyde, Si powder and SiC powder are well mixed, regulate and control its viscosity to the degree for being suitable to coating with the acetone weighed, obtain body layer
Slurry;According to silicones:Si powder:SiC powder:Ethanol=3:2:1:2 mass ratio weighs each material, by the silicones weighed, Si
Powder and SiC powder are well mixed, regulate and control its viscosity to the degree for being suitable to coating with the ethanol weighed, obtain main body slurry.
(2) using density as 1.5g/cm3Carbon/composite material of silicon carbide be base material, body layer slurry is coated in two times solid
Change the internal coated layer that about 200 μm of thickness is formed to substrate surface;Silication slurry is coated in two times and is cured to internal coated layer surface, shape
Into thickness about 1mm outer covering layer, the carbon/composite material of silicon carbide for covering coupling coat is formed.
(3) carbon/composite material of silicon carbide for covering coupling coat is pressed in vacuum sintering furnace in 1450 DEG C, 5KPa
Under power after reaction-sintered, the Redundant frame on surface is removed with high pressure water cleaning, the antioxygen for being prepared for coat of silicon carbide is obtained after drying
Change carbon/composite material of silicon carbide.
Comparative example 2:
Multiple Sintering Method according to traditional coating sintering method prepares coat of silicon carbide, specific as follows:
Coating slurry proportioning is silicones:Si powder:SiC powder=3:2:1 (mass ratio), is coated in two times after being well mixed
1.5g/cm3Carbon/composite material of silicon carbide substrate surface, form thickness about 1mm coat, then pressed in 1450 DEG C, 5KPa
Reaction-sintered in vacuum sintering furnace under power, removes the Redundant frame on surface by high pressure water cleaning and above-mentioned painting is repeated after drying
Cover, vacuum-sintering and Redundant frame processing procedure 3 times, obtain the oxidation resistant carbon/composite material of silicon carbide for being prepared for coat of silicon carbide.
After tested, the coat of silicon carbide uniformly continuous that embodiment 2 is obtained, about 160 μm of thickness, and obtained in comparative example 2
Coat of silicon carbide only 85 μm or so of thickness after the coating sintering of four times.1200 DEG C of static oxidation examinations show that embodiment 2 is obtained
The oxidation protection ability of the coat of silicon carbide obtained is better than comparative example 2.The manufacturing cycle of coat of silicon carbide is 5 days in embodiment 2, and
Comparative example is 20 days.Therefore, the characteristics of coat of silicon carbide that prepared by the inventive method not only has short cycle, low cost, oxidation
Protection effect is also improved.
Embodiment 3:
(1) according to phenolic resin:Si powder:SiC powder:Ethanol=3:5:1.5:4 mass ratio weighs each material, by what is weighed
Phenolic resin, Si powder and SiC powder are well mixed, regulate and control its viscosity to the degree for being suitable to coating with the ethanol weighed, form main body
Layer slurry;According to silicones:Si powder:SiC powder:Ethanol=3:4:3:6 mass ratio weighs each material, by the silicones weighed,
Si powder and SiC powder are well mixed, and its viscosity is regulated and controled to the degree for being suitable to coating with ethanol is weighed.
(2) using density as 1.9g/cm3Modifying carbon/carbon composite material be base material, body layer slurry is coated in two times solid
Change the internal coated layer that about 150 μm of thickness is formed to substrate surface;Silication slurry is coated in three times and is cured to internal coated layer surface, shape
Into thickness about 2mm outer covering layer.Form the modifying carbon/carbon composite material for covering coupling coat.
(3) modifying carbon/carbon composite material for covering coupling coat is pressed in vacuum sintering furnace in 1700 DEG C, 3KPa
Under power after reaction-sintered, the Redundant frame on surface is removed with high pressure water cleaning, the antioxygen for being prepared for coat of silicon carbide is obtained after drying
Change modifying carbon/carbon composite material.
Comparative example 3:
Multiple Sintering Method according to traditional coating sintering method prepares coat of silicon carbide, specific as follows:
Coating slurry proportioning is silicones:Si powder:SiC powder=3:4:3 (mass ratioes), are coated in three times after being well mixed
1.9g/cm3Modifying carbon/carbon composite material substrate surface, form thickness about 2mm coat, then pressed in 1700 DEG C, 3KPa
Reaction-sintered in vacuum sintering furnace under power, removes the Redundant frame on surface by high pressure water cleaning and above-mentioned painting is repeated after drying
Cover, vacuum-sintering and Redundant frame processing procedure 2 times, obtain the anti-oxidant modifying carbon/carbon composite material for being prepared for coat of silicon carbide.
After tested, the coat of silicon carbide uniformly continuous that embodiment 3 is obtained, about 120 μm of thickness, and obtained in comparative example 3
Coat of silicon carbide also has the feature of uniformly continuous, but only 80 μm or so of thickness after the coating sintering of three times.1200 DEG C quiet
State oxidation examination shows that the oxidation protection ability for the coat of silicon carbide that embodiment 3 is obtained is higher than comparative example 3.It is carbonized in embodiment 3
The manufacturing cycle of silicon coating is 5 days, and comparative example 3 is 18 days.Therefore, the coat of silicon carbide that prepared by the inventive method not only has
The characteristics of short cycle, low cost, also with more excellent oxidation protection ability.
Embodiment 4:
(1) according to phenolic resin:Si powder:SiC powder:Acetone=3:3:0.5:2 mass ratio weighs each material, by what is weighed
Phenolic resin, Si powder and SiC powder are well mixed, regulate and control its viscosity to the degree for being suitable to coating with the acetone weighed, form main body
Layer slurry;According to silicones:Si powder:SiC powder:Ethanol=3:4:2:5 mass ratio weighs each material, by the silicones weighed,
Si powder and SiC powder are well mixed, regulate and control its viscosity to the degree for being suitable to coating with the ethanol weighed, form silication slurry.
(2) using density as 1.5g/cm3Graphite material be base material.Body layer slurry is coated to substrate surface, Ran Hougu
Change the internal coated layer for forming about 80 μm of thickness;Silication slurry is coated in two times and is cured to internal coated layer surface, thickness about 1.5mm is formed
Outer covering layer.Form the graphite material for covering coupling coat.
(3) graphite material for coupling coat will be covered in vacuum sintering furnace in reaction under 1800 DEG C, 5KPa pressure
After sintering, the Redundant frame on surface is removed with high pressure water cleaning, the oxidation-resistant graphite material for being prepared for coat of silicon carbide is obtained after drying
Material.
(4) obtained on the coat of silicon carbide surface of acquisition by sol-gel impregnation drying method formation silica glaze layer
The carborundum protective coating of surface glaze layer protection.
Comparative example 4:
Multiple Sintering Method according to traditional coating sintering method prepares coat of silicon carbide, specific as follows:
Coating slurry proportioning is silicones:Si powder:SiC powder=3:4:2 (mass ratioes), are coated in two times after being well mixed
1.5g/cm3Graphite material substrate surface, form thickness about 1.5mm coat, then at 1800 DEG C, 5kPa vacuum is burnt
Reaction-sintered in freezing of a furnace, removes the Redundant frame on surface by high pressure water cleaning and above-mentioned coating, vacuum-sintering is repeated after drying
With Redundant frame processing procedure once, the Anti-oxidized Graphite Material for being prepared for coat of silicon carbide is obtained.In the coat of silicon carbide of acquisition
Surface obtains the carborundum protective coating of surface glaze layer protection by sol-gel impregnation drying method formation silica glaze layer.
After tested, the coat of silicon carbide uniformly continuous that embodiment 4 is obtained, about 70 μm of thickness.The carbonization obtained in comparative example 4
Silicon coating thickness is about 55 μm.1200 DEG C of static state aoxidize examinations and shown, the oxidation protection energy for the coat of silicon carbide that embodiment 4 is obtained
Power is better than comparative example 4.The manufacturing cycle of coat of silicon carbide is 6 days in embodiment 4, and comparative example 4 is 12 days.Therefore, it is of the invention
Method prepare coat of silicon carbide on the basis of oxidation protection ability is maintained, with the short cycle, low cost the characteristics of.
It is described above, it is only the optimal embodiment of the present invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.
Claims (10)
1. a kind of preparation method of coat of silicon carbide, it is characterised in that comprise the following steps:
Step (1):First coating slurry and second coating slurry are prepared respectively, wherein the first coating slurry feedstock includes matter
Amount is than being 3:(3~5):Phenolic resin, Si powder and the SiC powder of (0.5~1.5), the second coating slurry are silication slurry;
Step (2):The first coating slurry of preparation is coated to carbonaceous material surface, solidification obtains internal coated layer, then will prepared
Obtained silication slurry is coated to the internal coated layer surface, and solidification obtains outer covering layer;
Step (3):The carbonaceous material for foring outer covering layer is subjected to high-temperature vacuum sintering, coat of silicon carbide is obtained.
2. a kind of preparation method of coat of silicon carbide according to claim 1, it is characterised in that:
It is 3 that the raw material of the silication slurry, which includes mass ratio,:(2~4):Silicones, Si powder and the SiC powder of (1~3).
3. a kind of preparation method of coat of silicon carbide according to claim 1, it is characterised in that:Step (1) described first
Coating paste raw material and second coating slurry feedstock also include organic solvent, wherein, the organic solvent is ethanol, toluene or third
One or more kinds of combinations in ketone.
4. a kind of preparation method of coat of silicon carbide according to claim 3, it is characterised in that:The first coating raw material
Organic solvent quality be the first coating raw material gross mass 10~60%;The organic solvent of the second coating raw material
Quality be the second coating raw material gross mass 10~60%.
5. a kind of preparation method of coat of silicon carbide according to claim 1, it is characterised in that:It is described interior in step (2)
Coating thickness is 50~300 μm, and the outer covering layer thickness is 0.5~3mm.
6. a kind of preparation method of coat of silicon carbide according to claim 1, it is characterised in that:Height described in step (3)
Warm vacuum-sintering condition is:Temperature is at 1300 DEG C~1800 DEG C, and pressure is less than 10kPa.
7. a kind of preparation method of coat of silicon carbide according to claim 1, it is characterised in that:Step (3) high-temperature vacuum
After sintering, surface Redundant frame is fallen by deionized water rinsing, coat of silicon carbide is obtained.
8. the preparation method of a kind of coat of silicon carbide according to claim 1, it is characterised in that step (3) also includes:
Overcoating layer surface after sintering prepares glaze layer.
9. a kind of preparation method of coat of silicon carbide according to claim 1, it is characterised in that the carbonaceous material it is close
Spend for 1.2g/cm3~2.2g/cm3。
10. coat of silicon carbide prepared by the method provided by any one of claim 1~9.
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CN110498684A (en) * | 2019-09-11 | 2019-11-26 | 湖南博诚新材料科技有限公司 | A kind of preparation method of coat of silicon carbide |
CN110550962A (en) * | 2019-09-11 | 2019-12-10 | 湖南博诚新材料科技有限公司 | Coating for repairing cured carbon felt and application thereof |
CN111517797A (en) * | 2020-04-23 | 2020-08-11 | 西北工业大学 | Low-temperature normal-pressure sintering preparation method of high-purity SiC ceramic coating capable of realizing mass production |
CN114085081A (en) * | 2021-10-27 | 2022-02-25 | 南通三责精密陶瓷有限公司 | Silicon carbide kiln furniture and manufacturing method thereof |
CN114907145A (en) * | 2022-06-10 | 2022-08-16 | 辽宁奥亿达新材料有限公司 | Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof |
CN115073212A (en) * | 2022-06-02 | 2022-09-20 | 陕西美兰德炭素有限责任公司 | Aluminum silicate-silicon carbide high-temperature-resistant and silicon vapor corrosion-resistant coating and preparation method thereof |
CN116120098A (en) * | 2022-12-29 | 2023-05-16 | 中国科学院长春光学精密机械与物理研究所 | Diamond/silicon carbide-silicon carbide coating, composite material and preparation method thereof |
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CN110498684A (en) * | 2019-09-11 | 2019-11-26 | 湖南博诚新材料科技有限公司 | A kind of preparation method of coat of silicon carbide |
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CN114085081A (en) * | 2021-10-27 | 2022-02-25 | 南通三责精密陶瓷有限公司 | Silicon carbide kiln furniture and manufacturing method thereof |
CN115073212A (en) * | 2022-06-02 | 2022-09-20 | 陕西美兰德炭素有限责任公司 | Aluminum silicate-silicon carbide high-temperature-resistant and silicon vapor corrosion-resistant coating and preparation method thereof |
CN114907145A (en) * | 2022-06-10 | 2022-08-16 | 辽宁奥亿达新材料有限公司 | Silicon carbide coating adhesive on surface of carbon fiber composite material and preparation and use method thereof |
CN116120098A (en) * | 2022-12-29 | 2023-05-16 | 中国科学院长春光学精密机械与物理研究所 | Diamond/silicon carbide-silicon carbide coating, composite material and preparation method thereof |
CN116120098B (en) * | 2022-12-29 | 2023-11-14 | 中国科学院长春光学精密机械与物理研究所 | Diamond/silicon carbide-silicon carbide coating, composite material and preparation method thereof |
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