CN102392283A - Method for preparing carbon/carbon material zirconium silicate-aluminum phosphate composite antioxidation external coating - Google Patents

Method for preparing carbon/carbon material zirconium silicate-aluminum phosphate composite antioxidation external coating Download PDF

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CN102392283A
CN102392283A CN2011103758046A CN201110375804A CN102392283A CN 102392283 A CN102392283 A CN 102392283A CN 2011103758046 A CN2011103758046 A CN 2011103758046A CN 201110375804 A CN201110375804 A CN 201110375804A CN 102392283 A CN102392283 A CN 102392283A
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solution
carbon
powder
zirconium silicate
water heating
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曹丽云
刘佳
王敦强
黄剑锋
辛宇
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a method for a preparing carbon/carbon material zirconium silicate-aluminum phosphate composite antioxidation external coating. The method comprises the following steps: uniformly mixing ZrSiO4, AlPO4, SiO2 powder to obtain powder A; adding powder A in isopropanol to obtain a solution B; adding iodine in the solution B, carrying out ultrasonic oscillation, magnetically stirring to obtain a solution C; dumping the solution C in a reaction vessel, then clamping the C/C composite material sample with a SiC internal coating on cathode in a hydro-thermal kettle, sealing the hydro-thermal kettle and placing in a microwave generator to carry out arc discharge reaction, naturally cooling to room temperature after finishing the reaction; removing the sample, then placing the sample in a constant temperature drying box for drying to obtain the carbon/carbon material zirconium silicate-aluminum phosphate composite antioxidation external coating. The method employs microwave hydro-thermal arc discharge sedimentation, the reaction is finished in the hydro-thermal kettle once without post heat treatment, the reaction period is short, the cost is low, the prepared coating possesses uniform thickness and no penetrating crackles and millipores, and has strong bonding force with a SiC transition layer.

Description

The preparation method of a kind of carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating
Technical field
The invention belongs to the C/C technical field of composite materials, be specifically related to the method for a kind of microwave hydrothermal arc-over sedimentation carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating.
Background technology
Carbon/carbon (C/C) matrix material is to can be used for one of advanced material matrix material under the hot environment.Because the carbon/carbon compound material thermal expansivity is low, density is low, anti-ablation, corrosion-resistant, stable friction factor, the heat-conductivity conducting performance is good and characteristics such as HS, high-modulus; The characteristic that particularly goes up not down with temperature rising mechanical property, so it is applied to Aeronautics and Astronautics and civilian industry field.Yet; Its many above-mentioned character is only under inert atmosphere or be lower than under 450 ℃ the condition and could keep; Oxidation weight loss will make the mechanical property of carbon/carbon compound material obviously descend, thereby limit it as the widespread use of high-temperature refractory under oxidizing atmosphere.Therefore, solving carbon/carbon compound material high temperature oxidation protection question is the prerequisite that makes full use of its performance.
At present; The anti-oxidant measure of C/C matrix material mainly contains two types: (1) internal protection; Before the C/C composite material forming, just thomel peace talk matrix being carried out modification handles; Be that he itself has stronger resistance of oxidation, and add the high-temperature oxidation resistance that various inhibitors improve the C/C matrix material.(2) exterior coating prevents that through prepare all kinds of anti-oxidant function gradient claddings at material surface gas contact diffusion from improving the high-temperature oxidation resistance of C/C matrix material.
Up to the present the preparation method of top coating is varied, mainly contains following several kinds: sol-gel method, and entrapping method, chemical vapour deposition, formed in situ, molten slurry applies reaction, water heat electrophoresis deposition method etc.Adopt top coating surface easy of crack and the insufficient shortcoming of coat-thickness [Huang Jian-Feng, Zeng Xie-Rong, Li He-Jun, Xiong Xin-Bo, the Sun Guo-ling.Surf.coat.Technol.2005 of sol-gel method preparation; 190,255.], adopt the coat of silicon carbide of entrapping method preparation that the bigger stress of existence in the surface is arranged, so also occur just face rimose phenomenon [Yulei ZHANG easily; Hejun Li, Qiangang FU, Kezhi LI, Dangshe HOU.J.Mater.Sci.Technol.2008; 24,942.], and the coating of formed in situ method preparation need be 1500 ℃ of following pyroprocessing, and can not once prepare completion [Huang Jian-Feng; LiHe-Jun, Zeng Xie-Rong, Li Ke-Zhi.Surf.coat.Technol.2006,200; 5379.], adopt molten slurry to apply reaction method and prepare coating and still deposit and will repeatedly brush and can not once prepare completion, need heat treated drawback of later stage [Fu Qian-Gang, Li He-Jun; Wang Yong-Jie, Li Ke-Zhi, Tao Jun.Surface&Coating Technology.2010,204; 1832.], the coating that adopts the preparation of water heat electrophoresis deposition method equally is owing to use traditional heating mode, and preparation cycle is grown [Yang Wendong, Huang Jianfeng; Cao Liyun, Xia Changkui. silicate journal .2009,37,1319.].
Zirconium silicate (ZrSiO 4) have a very low oxygen rate of oozing, can be under 1500 ℃ of hot environments stable existence, and do not undergo phase transition, therefore select for use zirconium silicate as top layer material, it is low to have a cost, good effectiveness; Phosphagel phosphaljel is a kind of novel inorganic binder; Have tasteless, nontoxic and advantage such as good high-temperature performance; Aluminum phosphate coatings has stronger viscosifying power; Product that generates after solidifying and coating powder and matrix have good consistency, therefore zirconium silicate are mixed with phosphagel phosphaljel to constitute compound coating, and this coating possesses good antioxidant property.
Summary of the invention
The object of the present invention is to provide a kind of not only preparation cost low, and simple to operate, the short preparation method who does not need heat treated carbon/carbon material zirconium silicate of later stage-phosphagel phosphaljel compound anti-oxidation top coating of preparation cycle.
For achieving the above object, the technical scheme that the present invention adopts is:
1) gets commercially available purity all greater than 99.7% ZrSiO 4, AlPO 4, SiO 2Powder is pressed ZrSiO 4: AlPO 4: SiO 2The mass ratio of=1-5: 5-9: 1-3 mixes, and gets powder A at 80 ℃ of constant temperature dryings with wet ball grinding after 24 hours;
2) get 10-20g powder A and put into Erlenmeyer flask, again the 150-350ml Virahol is poured into magnetic agitation gets solution B in the Erlenmeyer flask;
3) in solution B, add the commercially available purity of 0.5-2.5g greater than 99.8% iodine, shake 10-40min, take out the back and on magnetic stirring apparatus, stir 6-24h with ultrasonic generator, solution C;
4) solution C is poured in the reaction kettle; Compactedness is controlled at 20%-50%, will have then on the negative electrode of the internally coated C/C matrix material of SiC sample holder in water heating kettle, and water heating kettle is sealed and put into microwave generator; Again negative and positive the two poles of the earth of water heating kettle are received on the corresponding the two poles of the earth of constant current power supply; At electric current is 2-9A, and temperature is 200-400 ℃ of following arc-over 2-8min, and question response naturally cools to room temperature after finishing;
5) open water heating kettle, take out sample, then sample is placed 40-80 ℃ the dry carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating that gets of thermostatic drying chamber.
The present invention adopts microwave hydrothermal electrophoretic deposition carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating; Once accomplish owing to be reflected in the water heating kettle, do not need later stage thermal treatment, reaction time is short; Cost is low; And processing unit is simple, and coatings prepared thickness does not evenly have through-wall crack and micropore, with the SiC transition layer stronger bonding force is arranged.The prepared composite coating can be protected C/C matrix materials 500 hours at 1500 ℃ of still airs, and oxidation weight loss is less than 0.8%.
Description of drawings
Fig. 1 for the present invention 200 ℃ of hydrothermal temperatures, arc-over electric current 2A is section surface sweeping Electronic Speculum (SEM) photo of the zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating of preparation down.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) gets commercially available purity all greater than 99.7% ZrSiO 4, AlPO 4, SiO 2Powder is pressed ZrSiO 4: AlPO 4: SiO 2=1: 9: 1 mass ratio mixes, and gets powder A at 80 ℃ of constant temperature dryings with wet ball grinding after 24 hours;
2) get 10g powder A and put into Erlenmeyer flask, again the 150ml Virahol is poured into magnetic agitation gets solution B in the Erlenmeyer flask;
3) in solution B, add the commercially available purity of 0.5g greater than 99.8% iodine, shake 10min, take out the back and on magnetic stirring apparatus, stir 6h with ultrasonic generator, solution C;
4) solution C is poured in the reaction kettle; Compactedness is controlled at 50%, will have then on the negative electrode of the internally coated C/C matrix material of SiC sample holder in water heating kettle, and water heating kettle is sealed and put into microwave generator; Again negative and positive the two poles of the earth of water heating kettle are received on the corresponding the two poles of the earth of constant current power supply; At electric current is 2A, and temperature is 200 ℃ of following arc-over 8min, and question response naturally cools to room temperature after finishing;
5) open water heating kettle, take out sample, then sample is placed 40 ℃ the dry carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating that gets of thermostatic drying chamber.
Embodiment 2:
1) gets commercially available purity all greater than 99.7% ZrSiO 4, AlPO 4, SiO 2Powder is pressed ZrSiO 4: AlPO 4: SiO 2=3: 7: 2 mass ratio mixes, and gets powder A at 80 ℃ of constant temperature dryings with wet ball grinding after 24 hours;
2) get 15g powder A and put into Erlenmeyer flask, again the 250ml Virahol is poured into magnetic agitation gets solution B in the Erlenmeyer flask;
3) in solution B, add the commercially available purity of 1.75g greater than 99.8% iodine, shake 25min, take out the back and on magnetic stirring apparatus, stir 12h with ultrasonic generator, solution C;
4) solution C is poured in the reaction kettle; Compactedness is controlled at 35%, will have then on the negative electrode of the internally coated C/C matrix material of SiC sample holder in water heating kettle, and water heating kettle is sealed and put into microwave generator; Again negative and positive the two poles of the earth of water heating kettle are received on the corresponding the two poles of the earth of constant current power supply; At electric current is 6A, and temperature is 400 ℃ of following arc-over 2min, and question response naturally cools to room temperature after finishing;
5) open water heating kettle, take out sample, then sample is placed 60 ℃ the dry carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating that gets of thermostatic drying chamber.
Embodiment 3:
1) gets commercially available purity all greater than 99.7% ZrSiO 4, AlPO 4, SiO 2Powder is pressed ZrSiO 4: AlPO 4: SiO 2=5: 5: 3 mass ratio mixes, and gets powder A at 80 ℃ of constant temperature dryings with wet ball grinding after 24 hours;
2) get 20g powder A and put into Erlenmeyer flask, again the 350ml Virahol is poured into magnetic agitation gets solution B in the Erlenmeyer flask;
3) in solution B, add the commercially available purity of 2.5g greater than 99.8% iodine, shake 40min, take out the back and on magnetic stirring apparatus, stir 24h with ultrasonic generator, solution C;
4) solution C is poured in the reaction kettle; Compactedness is controlled at 20%, will have then on the negative electrode of the internally coated C/C matrix material of SiC sample holder in water heating kettle, and water heating kettle is sealed and put into microwave generator; Again negative and positive the two poles of the earth of water heating kettle are received on the corresponding the two poles of the earth of constant current power supply; At electric current is 9A, and temperature is 300 ℃ of following arc-over 6min, and question response naturally cools to room temperature after finishing;
5) open water heating kettle, take out sample, then sample is placed 80 ℃ the dry carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating that gets of thermostatic drying chamber.
Can find out that by Fig. 1 the anti-oxidant top coating of prepared load is fine and close and even, combine closely, not have cracking and peels off phenomenon with the SiC undercoat.

Claims (1)

1. the preparation method of carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating is characterized in that:
1) gets commercially available purity all greater than 99.7% ZrSiO 4, AlPO 4, SiO 2Powder is pressed ZrSiO 4: AlPO 4: SiO 2The mass ratio of=1-5: 5-9: 1-3 mixes, and gets powder A at 80 ℃ of constant temperature dryings with wet ball grinding after 24 hours;
2) get 10-20g powder A and put into Erlenmeyer flask, again the 150-350ml Virahol is poured into magnetic agitation gets solution B in the Erlenmeyer flask;
3) in solution B, add the commercially available purity of 0.5-2.5g greater than 99.8% iodine, shake 10-40min, take out the back and on magnetic stirring apparatus, stir 6-24h with ultrasonic generator, solution C;
4) solution C is poured in the reaction kettle; Compactedness is controlled at 20%-50%, will have then on the negative electrode of the internally coated C/C matrix material of SiC sample holder in water heating kettle, and water heating kettle is sealed and put into microwave generator; Again negative and positive the two poles of the earth of water heating kettle are received on the corresponding the two poles of the earth of constant current power supply; At electric current is 2-9A, and temperature is 200-400 ℃ of following arc-over 2-8min, and question response naturally cools to room temperature after finishing;
5) open water heating kettle, take out sample, then sample is placed 40-80 ℃ the dry carbon/carbon material zirconium silicate-phosphagel phosphaljel compound anti-oxidation top coating that gets of thermostatic drying chamber.
CN2011103758046A 2011-11-23 2011-11-23 Method for preparing carbon/carbon material zirconium silicate-aluminum phosphate composite antioxidation external coating Pending CN102392283A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102674900A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of C-AlPO4-mullite composite overcoating for C/C composite material
CN102674890A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of carbon/carbon composite material mullite-C-AlPO4 composite outer coating
CN102674902A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating
CN102674889A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of carbon/carbon material C-AlPO4-mullite-zirconium silicate composite outer coating

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101386552A (en) * 2008-10-29 2009-03-18 陕西科技大学 Method for preparing carbon/carbon compound material silicon carbide/aluminum orthophosphate antioxidizing composite coating
CN101700983A (en) * 2009-10-30 2010-05-05 陕西科技大学 C/C composite material sol/gel-microwave hydrothermal modification method

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101386552A (en) * 2008-10-29 2009-03-18 陕西科技大学 Method for preparing carbon/carbon compound material silicon carbide/aluminum orthophosphate antioxidizing composite coating
CN101700983A (en) * 2009-10-30 2010-05-05 陕西科技大学 C/C composite material sol/gel-microwave hydrothermal modification method

Non-Patent Citations (1)

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Title
刘佳等: "水热沉积电压对ZrSiO4抗氧化涂层显微结构及抗氧化性能的影响", 《无机化学学报》, 31 October 2011 (2011-10-31) *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102674900A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of C-AlPO4-mullite composite overcoating for C/C composite material
CN102674890A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of carbon/carbon composite material mullite-C-AlPO4 composite outer coating
CN102674902A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating
CN102674889A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of carbon/carbon material C-AlPO4-mullite-zirconium silicate composite outer coating
CN102674902B (en) * 2012-05-15 2013-08-28 陕西科技大学 Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating

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Application publication date: 20120328