CN105000917B - Preparation method of mullite oxidation resistant coating - Google Patents
Preparation method of mullite oxidation resistant coating Download PDFInfo
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- CN105000917B CN105000917B CN201510500693.5A CN201510500693A CN105000917B CN 105000917 B CN105000917 B CN 105000917B CN 201510500693 A CN201510500693 A CN 201510500693A CN 105000917 B CN105000917 B CN 105000917B
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Abstract
The invention relates to a preparation method of a mullite oxidation resistant coating, particularly to a method for preparing a mullite/SiC bilayer-structure oxidation resistant coating on the surface of a carbon/carbon composite material. The preparation method comprises the following steps: pre-calcining mullite powder A and mullite precursor powder B according to the mass ratio of (4-6):1 to prepare pre-calcined mullite powder A and mullite precursor powder B, preparing a coalescing agent and a drying inhibitor according to certain ratio, uniformly mixing the pre-calcined mullite powder A, the pre-calcined mullite precursor powder B, the coalescing agent and the drying inhibitor to obtain a sizing agent, dipping a matrix in the sizing agent, performing sizing agent coating by adopting the dip-coating technology, and after the sizing agent coating, calcining at 1480-1515 DEG C to obtain the mullite oxidation resistant coating. According to the invention, the technology is simple, the raw material is cheap and available, the industrial production is facilitated, and the obtained coating has the advantages of high uniformity and compactness, excellent binding property, and high high-temperature oxidation resistant capacity.
Description
Technical field
The present invention relates to a kind of preparation method of mullite ORC；More particularly to one kind is in carbon/carbon compound material
The method that surface prepares mullite/SiC double-decker ORCs.
Background technology
Carbon/carbon compound material due to possessing low thermal coefficient of expansion, low-density, high heat-conductivity conducting performance, high temperature under it is high-strength
High mould and a series of excellent characteristics such as resistance to ablation, corrosion-resistant, stable friction factor, become one kind and possess great potential
With the high-temperature structural material of broad prospect of application, and obtain widely should in the industrial circles such as Aeronautics and Astronautics, energy petrochemical industry
With.But, because the oxidation onset temperature of carbon/carbon compound material is only 450 DEG C, therefore the oxidation under high temperature oxidation stability atmosphere
Failure just becomes the one of the main reasons of restriction carbon/carbon compound material application development.Improve the antioxidant of carbon/carbon compound material
The key for expanding carbon/carbon compound material range of application can be become.
ORC technology is that a kind of practice proved solves the problems, such as carbon/carbon compound material high-temperature oxidation resistant
Maximally efficient technological approaches.Because the ORC of single layer structure is difficult to meet application requirement, development bilayer or multilamellar
The coating system of structure has become an inexorable trend of ORC technology development.Because mullite ceramic has high temperature
Phase stability is good, excellent in mechanical performance, and anti-thermal shock/thermal cycling capability is strong, the series of advantages such as corrosion resistance environment so as to become
The preferable ORC material system of one class.Further, since the thermal expansion of the thermal coefficient of expansion of mullite ceramic and SiC ceramic
Coefficient is very close, and both are combined can play respective advantage so as to reach preferable protection effect.Therefore with SiC ceramic
For prime coat, mullite ceramic is that external coating is subject in recent years for the Oxidation Resistant Coatings for Carbon/Carbon Composites structure of construction featuress
The extensive concern of researcher.
The technology of preparing of current main mullite coating has plasma spraying method, electro beam physics vapour deposition (EB-
PVD), chemical vapor deposition (CVD) etc..Compare with traditional coating preparation means, sol-gel process mainly has following excellent
Point：First, process equipment is simple, and equipment cost is low；Second, coating prepares speed soon, and production capacity is with the obvious advantage；3rd, Ke Yishi
Now lower preparation temperature, it is to avoid for the hot injury of matrix material in coating preparation process；4th, to material microstructure
Design control ability is strong；5th, low, realization prepares coating on complicated shape matrix of being more convenient for is required base shape.But,
At present traditional sol-gel preparation technology of coating also has many deficiencies, constrains its development and application.Main defect
Have：1) coating is loose porous, and consistency is low,；2) combine between coating and matrix it is poor, coating in drying or sintering process easily
Cracking is peeled off；3) the coating layer thickness upper limit is low, it is difficult to meet the thickness requirement of ORC；4) preparation process need to experience repeatedly painting
Cover-be dried-sintering process, it is difficult to the coating of the even compact of ideal thickness is prepared by single application.
The content of the invention
It is an object of the invention to overcome the defect of above-mentioned prior art, by combining dipping-lifting technology and colloidal sol-solidifying
Adhesive process, there is provided it is a kind of once complete coating prepare and without the need for repeatedly circulation and Post isothermal treatment, with preparation cost it is low,
Cycle is short, simple operation and other advantages.
A kind of preparation method of mullite ORC of the present invention, comprises the steps：
Step one
With aluminum soluble salt, esters of silicon acis as raw material, in molar ratio, Al：Si：Organic solvent：Catalyst=(2～3):(1～
1.5):(4～9):(0.3～0.5), carry out after raw material, organic solvent, catalyst back flow reaction and obtain gel with taking；Gained is solidifying
Glue after drying, under an oxygen-containing atmosphere, in 1200-1350 DEG C of calcining, obtains precalcining porzite powder A；
Step 2
With aluminum soluble salt, esters of silicon acis as raw material, in molar ratio, Al：Si：Organic solvent：Catalyst=(2～3):(1～
1.5):(4～9):(0.3～0.5), carry out back flow reaction, Ran Houzai at 60-85 DEG C after raw material, organic solvent, catalyst with taking
Instill deionized water；And be warming up to 80～85 DEG C reaction at least 8 hours after cooling, ageing；After ageing, in 80～120 DEG C of dryings,
Obtain mullite precursor powder material B；
Step 3
In mass ratio, precalcining porzite powder A：Mullite precursor powder material B=4～6:1, with taking precalcining mullite
Powder A, mullite precursor powder material B, then with taking coalescents, drying retarder, solvent；By with the precalcining mullite for taking
Slurry is obtained after powder A, mullite precursor powder material B, coalescents, drying retarder, solvent mix homogeneously, matrix is immersed
In slurry, using Best-Effort request technology slurry coating is carried out；After having coated, in 1480～1515 DEG C of calcinings, obtain mullite and resist
Oxide covering.
A kind of preparation method of mullite ORC of the present invention；In step one,
The one kind of the aluminum soluble salt in nine water aluminum nitrates, six water and aluminum chloride；Required for reacting in step one
Water by aluminium salt water of crystallization provide；
At least one of the esters of silicon acis in tetraethyl orthosilicate, methyl silicate, positive silicic acid propyl ester；
The organic solvent is selected at least one in dehydrated alcohol, absolute methanol；
At least one of the catalyst in glacial acetic acid and Fluohydric acid..
A kind of preparation method of mullite ORC of the present invention；In step one, the back flow reaction is：In 45-75
It is warming up to 80-100 DEG C of reaction 10-14h under DEG C heating in water bath after back flow reaction 3-5h again, obtains gel.
A kind of preparation method of mullite ORC of the present invention；It is dry at 80-120 DEG C after obtaining gel in step one
Dry 8-72 hours；With 150-350rpm after drying, after ball milling 1-4 hours, carry out calcining 2-3 hours at 1200-1350 DEG C, with stove
Room temperature is cooled to, precalcining porzite powder A is obtained.
A kind of preparation method of mullite ORC of the present invention；In step 2；
The aluminum soluble salt is selected from aluminum acetate, Al (NO3)3At least one in 9H2O, anhydrous Aluminum chloride；
At least one of the esters of silicon acis in tetraethyl orthosilicate, methyl silicate, positive silicic acid propyl ester；
The organic solvent is selected at least one in dehydrated alcohol, absolute methanol；
At least one of the catalyst in glacial acetic acid and Fluohydric acid.；
The deionized water for being instilled is 3～7 with the mol ratio of aluminium element in system:6.
A kind of preparation method of mullite ORC of the present invention；In step 2
A kind of preparation method of mullite ORC of the present invention；In step 2；
4～6h of back flow reaction is carried out at 60-85 DEG C, then deionized water is being instilled；And be warming up to 80～85 DEG C react to
Cooling, ageing after few 8 hours；During ageing, control time is 1～2 month, temperature is 40-65 DEG C；After the completion of ageing, in 100-
After 120 DEG C are dried after 10-14h with 150-350rpm ball milling 1-4 hours, mullite precursor powder material B is obtained.
A kind of preparation method of mullite ORC of the present invention；In step 3, in mass ratio, precalcining mullite powder
Material A：Mullite precursor powder material B=4～6:1, with taking precalcining porzite powder A, mullite precursor powder material B, and matched somebody with somebody
The two kinds of powder gross mass of precalcining porzite powder A and mullite precursor powder material B for taking for solvent for use gross mass 10～
25wt%；By with taking the 0.3-1.5% of precalcining porzite powder A and mullite precursor powder material B gross mass with taking film forming
Auxiliary agent；At least one of the coalescents in polyvinylpyrrolidone, polyvinyl butyral resin；By solvent gross mass
5～8wt%, with taking drying retarder；At least one of the drying retarder in oxalic acid, glycerol；The solvent choosing
At least one from dehydrated alcohol, absolute methanol, acetone.
A kind of preparation method of mullite ORC of the present invention；Its optimization technique technical scheme is comprised the following steps：
Step A
In molar ratio, Al (NO3)3The mol ratio of 9H2O, tetraethyl orthosilicate, dehydrated alcohol and glacial acetic acid is 3：1：5～8：
0.3～0.5, with taking Al (NO3)3·9H2O, tetraethyl orthosilicate, dehydrated alcohol and glacial acetic acid, mix homogeneously, then at 45-75 DEG C
It is warming up to 80-100 DEG C of reaction 10-14h under heating in water bath after back flow reaction 3-5h again, obtains gel；Gained gel is in 80-120
DEG C it is dried 8-72 hours；With 150-350rpm after drying, after ball milling 1-4 hours, carry out calcining 2-3 hours at 1200-1350 DEG C,
Cool to room temperature with the furnace, obtain precalcining porzite powder A；
Step B
In molar ratio, aluminum acetate：Al(NO3)3·9H2O：Anhydrous Aluminum chloride：Tetraethyl orthosilicate=1.8:0.4:0.8:1；Match somebody with somebody
Take aluminum acetate, Al (NO3)3·9H2O, anhydrous Aluminum chloride, tetraethyl orthosilicate；
Then, in molar ratio, glacial acetic acid：Tetraethyl orthosilicate=1～2:5 with taking glacial acetic acid,
By with aluminum acetate, the Al (NO for taking3)3·9H2O, anhydrous Aluminum chloride, tetraethyl orthosilicate, glacial acetic acid are dissolved in dehydrated alcohol
In, in the environment of isolation moisture content, after back flow reaction 3-5h under 60-70 DEG C of heating in water bath, then Deca deionized water, institute's Deca
Deionized water and system in the mol ratio of aluminium element be 3～7:6, then raise temperature to 80-85 DEG C of reaction 8-12h；Reaction terminates
Reaction is obtained gel afterwards is aged 1～2 month at 40-65 DEG C, with 200- after being then dried 10-14h at 100-120 DEG C
Mullite precursor powder material B is obtained after the rotating speed ball milling 1-4h of 300rpm；Aluminum acetate used, Al (NO3)3·9H2O, anhydrous chlorination
Aluminium element and the mol ratio of dehydrated alcohol used are 3 in aluminum：5～8；
Step C
In mass ratio, precalcining porzite powder A：Mullite precursor powder material B=4～6:1st, it is preferably 4.8-5.5:1,
With precalcining porzite powder A, mullite precursor powder material B is taken, then with taking coalescents, drying retarder, solvent；To match somebody with somebody
After the precalcining porzite powder A, mullite precursor powder material B, coalescents, drying retarder, the solvent mix homogeneously that take
To slurry, matrix is immersed in slurry, using Best-Effort request technology slurry coating is carried out；After having coated, at 1480～1515 DEG C
Calcining, obtains mullite ORC；The coalescents are selected from Polyvinylprrilone butyral extremely
Few one kind, the quality of used film forming auxiliary agent is the 0.8- of precalcining porzite powder A and mullite precursor powder material B gross mass
1.2%；The solvent is by dehydrated alcohol and acetone by volume 7:3～5 compositions, and match somebody with somebody the precalcining porzite powder A for taking
With 10～25wt% that two kinds of powder gross mass of mullite precursor powder material B are solvent for use gross mass；；The desiccant is grass
Acid, and consumption of oxalic acid is 5～8wt% of solvent gross mass.
A kind of preparation method of mullite ORC of the present invention；When carrying out slurry coating using Best-Effort request technology,
It is 05-3mm/min to control the rate of pulling, and temperature is 40-50 DEG C.
A kind of preparation method of mullite ORC of the present invention；When carrying out slurry coating using Best-Effort request technology,
The nitrogen flow rate for controlling to lift in kettle is 1.0-2L/min, preferably 1.5L/min.
A kind of preparation method of mullite ORC of the present invention；Described matrix is prepared by following proposal：
Step I
First by 60～65wt.%Si, 10～30wt.%SiC, 5～10wt.% powdered carbon, 1～5wt.%Al2O3It is placed in ball
To take out after the rotary speed wet grinding 2-4h of 200-250r/min in grinding jar, it is placed in drying baker and is dried 48- at 80-120 DEG C
72h, sieves, and obtains the embedding powder of -60 mesh；
Step II
After being fitted in graphite tank in embedding powder and C/C composite samples being embedded in embedding powder, burn in vacuum
2-2.5h is incubated after being heated to 1750 DEG C -1800 DEG C in argon gas atmosphere in freezing of a furnace, room temperature is cooled to, sample is taken out, by sample
It is dried after 2-4h at being placed in 80-120 DEG C after being cleaned by ultrasonic totally with dehydrated alcohol and obtains SiC coatings cladding C/C composite samples
Product (as described matrix material).
A kind of preparation method of mullite ORC of the present invention；The mol ratio of aluminum silicon can in gained mullite external coating
To be adjusted according to demand.
A kind of preparation method of mullite ORC of the present invention；The mol ratio of aluminum silicon is excellent in gained mullite external coating
Elect 3 as:1.
Principle and advantage
Present invention achieves the monocycle molding of coating, overcome sol-gel process prepares coating single application thickness it is low,
Easily peel off, the shortcoming of coating-sintering period process need to be repeated several times.
The present invention is designed using rational multicomponent coating slurry formula, will be containing precalcining mullite miropowder, mullite
Presoma powder, coalescents, drying retarder and mixed type solvent by rational composition proportion mixing after be obtained it is new
Coating slurry.The coating slurry can greatly improve the ceramics pyrolysis yield and limit coating thickness of coating slurry, eliminate sintering
During coating cracking phenomenon, fine and close flawless thick coating has been obtained by single application.
The present invention controls the conjunction of mullite precursor by adopting nonaqueous solvent, and the mode of strict isolation environment moisture
Carry out under non-fully hydrolyzed collosol-gelatin route, improve the sintering activity of mullite, control mullite particle pattern
Uniformity, improves coating consistency.
The present invention is realized by coating slurry and matrix surface is realized to be sufficiently impregnated with, and then is greatly improved outside mullite
Combination interface between coating and SiC bottoms, so as to avoid the appearance of disbonding phenomenon.Lifted by precise control simultaneously
The technological parameters such as speed, ambient temperature and gas flow rate, have reached the purpose for improving coating uniformity and control dry rate, change
It has been apt to the uniformity of coating and has avoided cracking phenomenon in dry run.
In a word, the present invention is by cleverly design of components, using precalcining mullite miropowder, mullite precursor powder,
The synergism of coalescents, drying retarder, it is especially mutual between precalcining mullite miropowder, mullite precursor powder
With effect, unexpected effect is achieved.Gained finished product tool coating uniform, densification, binding ability Jing after once lifting coating
It is excellent, the advantage such as high-temperature oxidation resistance is strong.
Description of the drawings
Accompanying drawing 1 is mullite external coating surface SEM photograph prepared by the embodiment of the present invention 1；
Accompanying drawing 2 is the double coating cross sections SEM photographs of mullite/SiC prepared by the embodiment of the present invention 1；
Accompanying drawing 3 is mullite external coating surface XRD spectrum prepared by the embodiment of the present invention 1；
Accompanying drawing 4 is that mullite/SiC duplex coatings prepared by the embodiment of the present invention 1 coat C/C matrixes in 1500 DEG C of air oxygens
Oxidation weight loss curve under changing.
As can be seen from Figure 1 the mullite external coating surface compact flawless obtained by the technique of embodiment 1 is adopted.
As can be seen from Figure 2 using embodiment 1 technique obtained by mullite external coating thickness reach about 180 μm,
And it is well combined with SiC bottoms.
As can be seen from Figure 3 using embodiment 1 technique obtained by mullite external coating mainly by 3/2 mullite and
Cristobalite phase composition.
As can be seen from Figure 4 the mullite obtained by the technique of embodiment 1/SiC cladding C/C composites are adopted to exist
There is excellent antioxygenic property under the conditions of 1500 DEG C of air oxidations.
Specific embodiment
Embodiment 1：
Investment prepares SiC coatings：First by 180g Si powder, 90g SiC powder, 15g powdered carbons, 15g Al2O3It is placed in ball milling
To take out after the rotary speed wet grinding 24h of 200r/min in tank, it is placed in drying baker and 12h is dried at 90 DEG C, then with the sieve of 60 mesh
Net to sieve obtain and embeds powder.
After being fitted in graphite tank in embedding powder and C/C matrix samples being embedded in embedding powder, in vacuum sintering furnace
In 1750 DEG C are heated in argon gas atmosphere after be incubated 2h, sample is taken out after being slowly cooled to room temperature.By sample dehydrated alcohol
It is dried after 2h at being placed in 90 DEG C after being cleaned by ultrasonic totally and obtains SiC coatings cladding C/C composite samples.
Sol-gel process prepares mullite external coating：
1) by 10.4165g tetraethyl orthosilicates and with 56.247gAl (NO3)3·9H2O is dissolved in 14mL ethanol, is added
1.800g glacial acetic acid is warming up to again 80 DEG C of reaction 12h after back flow reaction 4h under 60 DEG C of heating in water bath, subsequently obtains reaction
Gel drying after to be put in Muffle furnace after 250rpm rotating speed ball milling 2h, 5 DEG C/min of heating rate, 1200 DEG C insulation 2h after with
Stove is cooled to room temperature, and precalcining porzite powder A is obtained；
2) by 6.1233g aluminium acetates, 0.1500gAl (NO3)3·9H2O, 12.4000g anhydrous Aluminum chloride and 10.4165g are just
After silester is dissolved in 50mL dehydrated alcohol, add 1.2g glacial acetic acid to stir as after catalyst, treat that solid reagent is completely molten
Solution is slowly added dropwise again into 0.042g under isolation moisture content environment after dehydrated alcohol after back flow reaction 4h under 60 DEG C of heating in water bath
Deionized water, then raises temperature to 80 DEG C of reaction 12h.The gel that reaction obtains reaction after terminating is aged 2 months and is done after 120 DEG C
Obtaining mullite precursor powder material B after 250rpm rotating speed ball milling 2h after dry 12h；
3) by after the acetone mix homogeneously of the dehydrated alcohol of 35mL and 15mL, 0.19g polyvinylpyrrolidones (PVP) are added
Stir to being completely dissolved, be subsequently adding the grass of 15g precalcining porzite powder A, 3.75g mullite precursor powder material Bs and 2.5mL
Acid, after ball milling 4h under 250rpm rotating speeds coating slurry is obtained；4) SiC is coated the sample immersion step 3 of C/C composites)
In the slurry for obtaining, mullite/SiC double-deckers are obtained after 1500 DEG C of sintering 2h in the tube furnace and resisted Jing once lifting to coat
The C/C composite samples of oxide covering cladding.During lifting coating, it is 1mm/min to control the rate of pulling, and lifting ambient temperature is
45 DEG C, it is 1.5L/min to lift the nitrogen flow rate in kettle.Gained coating sample under 1500 DEG C, air ambient after aoxidizing 100h
Its weight-loss ratio is only 0.38%.Its high temperature oxidation resistance is better than from far away like product.
Embodiment 2：
Investment prepares SiC coatings：First by 260g Si powder, 96g SiC powder, 40g powdered carbons, 4g Al2O3It is placed in ball grinder
In to take out after the rotary speed wet grinding 24h of 200r/min, be placed in drying baker and 12h be dried at 90 DEG C, then with the screen cloth of 60 mesh
Sieves the embedding powder that obtain.
After being fitted in graphite tank in embedding powder and C/C matrix samples being embedded in embedding powder, in vacuum sintering furnace
In 1800 DEG C are heated in argon gas atmosphere after be incubated 2h, sample is taken out after being slowly cooled to room temperature.By sample dehydrated alcohol
It is dried after 2h at being placed in 90 DEG C after being cleaned by ultrasonic totally and obtains SiC coatings cladding C/C composite samples.
Sol-gel process prepares mullite external coating：
1) by 41.666g tetraethyl orthosilicates and with 224.988gAl (NO3)3·9H2O is dissolved in 200mL ethanol, adds 30g
Glacial acetic acid is warming up to again 80 DEG C of reaction 12h, the gel for subsequently obtaining reaction after back flow reaction 4h under 60 DEG C of heating in water bath
To be put in Muffle furnace after 250rpm rotating speed ball milling 2h after drying, 5 DEG C/min of heating rate, furnace cooling after 1200 DEG C of insulation 2h
To room temperature, precalcining porzite powder A is obtained；
2) by 60.6930g aluminium acetates, 3.7498gAl (NO3)3·9H2O, 12.0000g anhydrous Aluminum chloride and 52.0852g
After tetraethyl orthosilicate is dissolved in 200mL dehydrated alcohol, add 20g glacial acetic acid to stir as after catalyst, treat that solid reagent is complete
It is dissolved in after dehydrated alcohol and is slowly added dropwise again into 0.21g after back flow reaction 4h under 60 DEG C of heating in water bath under isolation moisture content environment
Deionized water, then raises temperature to 80 DEG C of reaction 12h.The gel that reaction obtains reaction after terminating is aged 2 months and is done after 120 DEG C
Obtaining mullite precursor powder material B after 250rpm rotating speed ball milling 2h after dry 12h；
3) by after the acetone mix homogeneously of the dehydrated alcohol of 35mL and 15mL, 0.5g polyvinylpyrrolidones (PVP) are added
Stir to being completely dissolved, be subsequently adding the grass of 17g precalcining porzite powder A, 4.25g mullite precursor powder material Bs and 2.5mL
Acid, after ball milling 4h under 250rpm rotating speeds coating slurry is obtained；4) by the immersion step of the sample with SiC coating C/C composites
In the rapid slurry for 3) obtaining, the double-deck knots of mullite/SiC are obtained after 1500 DEG C of sintering 2h in tube furnace Jing once lifting to coat
The C/C composite samples of structure ORC cladding.During lifting coating, the rate of pulling is controlled for 1mm/min, lifting environment temperature
Spend for 45 DEG C, it is 1.5L/min to lift the nitrogen flow rate in kettle.Coating is sintered after 2h at completing 1500 DEG C in the tube furnace
To the C/C composite samples of mullite/SiC double-deckers ORC cladding.Gained coating sample is through 1500 DEG C, sky
It is only 0.45% that its weight-loss ratio after 100h is aoxidized under compression ring border.Its high temperature oxidation resistance is better than from far away like product.
Claims (2)
1. a kind of preparation method of mullite ORC, it is characterised in that comprise the following steps：
Step A
In molar ratio, Al (NO3)3·9H2The mol ratio of O, tetraethyl orthosilicate, dehydrated alcohol and glacial acetic acid is 3：1：5～8：0.3
～0.5, with taking Al (NO3)3·9H2O, tetraethyl orthosilicate, dehydrated alcohol and glacial acetic acid, mix homogeneously, then in 45-75 DEG C of water
80-100 DEG C of reaction 10-14h is warming up to again after lower back flow reaction 3-5h of bath heating, obtains gel；Gained gel is at 80-120 DEG C
It is dried 8-72 hours；With 150-350rpm after drying, after ball milling 1-4 hours, in atmosphere, calcined in 1200-1350 DEG C
2-3 hours, cool to room temperature with the furnace, obtain precalcining porzite powder A；
Step B
In molar ratio, aluminum acetate：Al(NO3)3·9H2O：Anhydrous Aluminum chloride：Tetraethyl orthosilicate=1.8:0.4:0.8:1；With taking vinegar
Sour aluminum, Al (NO3)3·9H2O, anhydrous Aluminum chloride, tetraethyl orthosilicate；
Then, in molar ratio, glacial acetic acid：Tetraethyl orthosilicate=1～2:5 with taking glacial acetic acid,
By with aluminum acetate, the Al (NO for taking3)3·9H2O, anhydrous Aluminum chloride, tetraethyl orthosilicate, glacial acetic acid are dissolved in dehydrated alcohol,
In the environment of isolation moisture, after back flow reaction 3-5h under 60-70 DEG C of heating in water bath, then Deca deionized water, institute's Deca
Deionized water is 3～7 with the mol ratio of aluminium element in system:6, then raise temperature to 80-85 DEG C of reaction 8-12h；After reaction terminates
The gel that reaction is obtained is aged 1～2 month at 40-65 DEG C, with 200-300rpm after being then dried 10-14h at 100-120 DEG C
Rotating speed ball milling 1-4h after obtain mullite precursor powder material B；Aluminum acetate used, Al (NO3)3·9H2In O, anhydrous Aluminum chloride
Aluminium element is 3 with the mol ratio of dehydrated alcohol used：5～8；
Step C
In mass ratio, precalcining porzite powder A：Mullite precursor powder material B=4～6:1, with taking precalcining porzite powder
A, mullite precursor powder material B, then with taking coalescents, drying retarder, solvent；By with the precalcining porzite powder for taking
Slurry is obtained after A, mullite precursor powder material B, coalescents, drying retarder, solvent mix homogeneously, matrix is immersed into slurry
In, carry out slurry coating using Best-Effort request technology；After having coated, in 1480～1515 DEG C of calcinings, mullite antioxidation is obtained
Coating；At least one of the coalescents in Polyvinylprrilone butyral, used film forming auxiliary agent
Quality is the 0.8-1.2% of precalcining porzite powder A and mullite precursor powder material B gross mass；The solvent is by anhydrous second
Alcohol and acetone by volume 7:3～5 compositions, and match somebody with somebody two kinds of the precalcining porzite powder A for taking and mullite precursor powder material B
Powder gross mass is 10～25wt% of solvent for use gross mass；The desiccant is oxalic acid, and consumption of oxalic acid is the total matter of solvent
5～8wt% of amount.
2. the preparation method of a kind of mullite ORC according to claim 1；It is characterized in that：Carried using dipping
When pull technology carries out slurry coating, it is 05-3mm/min to control the rate of pulling, and temperature is 40-50 DEG C.
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| CN105967756B (en) * | 2016-05-06 | 2018-06-19 | 陕西科技大学 | A kind of crystal whisker toughened silicate glass antioxidant coating of carbon/carbon composite mullite and preparation method thereof |
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| CN108383132B (en) * | 2018-03-19 | 2021-07-16 | 华南理工大学 | Low-temperature preparation method of superfine mullite powder |
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| CN111233498A (en) * | 2020-03-06 | 2020-06-05 | 中南大学 | Environmental barrier coating and preparation method and application thereof |
| CN115028471B (en) * | 2022-06-10 | 2023-09-26 | 中南大学 | Antioxidant inorganic coating for carbon material product and application thereof |
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| CN101786906A (en) * | 2009-12-14 | 2010-07-28 | 西北工业大学 | Preparation method of anti-oxidation SiC/mullite-Si-Al2O3 composite coating on surface of C/C composite material |
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