Carbon/carbon compositesyb 2 the si 2 o 7 Whisker toughened yb 2 sio 5 Preparation method of composite coating

A carbon composite material and composite coating technology, which is applied in the field of C/C composite materials, can solve the problems of long preparation period, difficult coating, difficult control of coating uniformity, etc., to achieve precise control of coating composition and avoid phase change and brittleness, simple and efficient preparation

Active Publication Date: 2018-02-09
SHAANXI UNIV OF SCI & TECH
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AI Technical Summary

Problems solved by technology

The disadvantage of the embedding method is that the compactness and uniformity of the coating and the thickness of the coating are not easy to control. Many factors (powder ratio, reaction time, temperature and properties of the matrix material, etc.) have an impact on the degree of reaction and diffusion, so it is necessary to It is difficult to prepare dense coatings with few defects
The preparation of C / C composite coatings by supercritical fluid technology needs to be carried out under high temperature and high pressure. This method has high requirements for equipment, and the formed outer coating needs to be heat treated under an inert atmosphere, and the preparation cycle is relatively long [Bemeburg P L ,Krukonis V J.Processing of carbon / carbon composites using supercritical fluid technology[P].United States Patent US 5035921,1991], the coating prepared by the in-situ forming method needs to be treated at a high temperature of 1500°C, and cannot be completed at one time [Huang Jian-Feng, Li He-Jun, Zeng Xie-Rong, Li Ke-Zhi.Surf.coat.Technol.2006,200,5379.], the surface of the outer coating prepared by sol-gel method is easy to dry Cracking and insufficient coating thickness required multiple dipping [Huang Jian-Feng, Zeng Xie-Rong, LiHe-Jun, Xiong Xin-Bo, Sun Guo-ling. Surf.coat. Technol.2005, 190, 255.], melting The disadvantage of the slurry coating method is that the bonding between the coating and the base material is poor, the uniformity of the coating is not easy to control, and the compactness is difficult to meet the requirements.
Although some alloy coatings have been prepared by explosive spraying and ultrasonic spraying, there are still many imperfections in the process, and the prepared high-temperature oxidation resistance needs to be further improved [Terentieva V S, Bogachkova O P, Goriatcheva E V.Method for protecting products made of arefractory material against oxidation,and resulting products[p].US 5677060,1997.]

Method used

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  • Carbon/carbon compositesyb <sub>2</sub> the si <sub>2</sub> o <sub>7</sub> Whisker toughened yb <sub>2</sub> sio <sub>5</sub> Preparation method of composite coating
  • Carbon/carbon compositesyb <sub>2</sub> the si <sub>2</sub> o <sub>7</sub> Whisker toughened yb <sub>2</sub> sio <sub>5</sub> Preparation method of composite coating

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preparation example Construction

[0033] Carbon / carbon composite material Yb of the present invention 2 Si 2 o 7 Whisker toughened Yb 2 SiO 5 The preparation method of composite coating comprises the following steps:

[0034] 1) Choose the purity of commercially available iodine simple substance ≥ 99.7%, the purity of isopropanol ≥ 99.8%;

[0035] 2) Yb 2 Si 2 o 7 The preparation of whiskers comprises the following steps:

[0036] (1) Take Yb(NO) 3 ·5H 2 O, dissolved in absolute ethanol, prepared to a concentration of 0.5 ~ 1mol / L solution C; according to Yb(NO) 3 ·5H 2 O:Si(OC 2 h 5 ) 4 =1:(1~1.5) molar ratio, Si(OC 2 h 5 ) 4 Add it into solution A and stir well to obtain solution D; after drying solution D, obtain powder B, pre-calcine powder B at 200°C, and cool to room temperature to obtain powder C;

[0037] (2) Mix the powder C and the mixed double salt evenly according to the mass ratio of 1:(1~2), and then heat treat at 800~1000°C to obtain the powder D; wherein, the mixed double salt...

Embodiment 1

[0051] 1) Choose the purity of commercially available iodine simple substance ≥ 99.7%, the purity of isopropanol ≥ 99.8%;

[0052] 2) Weigh an appropriate amount of Yb 2 SiO 5 Powder and Yb 2 Si 2 o 7 Whiskers (Yb 2 Si 2 o 7 The content of whiskers is 10% of the total mass of the two, Yb 2 SiO 5 The content of powder is 90% of the two total mass) dispersed in 1.5L isopropanol, is mixed with Yb 2 SiO 5 Powder and Yb 2 Si 2 o 7 For a suspension with a total concentration of whiskers of 30 g / L, the suspension was ultrasonically oscillated (ultrasonic power: 800 W) for 30 minutes, then placed on a magnetic stirrer and stirred for 3 hours to obtain suspension A;

[0053] 3) Add elemental iodine to suspension A (control the concentration of elemental iodine to be 4.0g / L) and then vibrate ultrasonically (ultrasonic power is 800W) for 40min, then place it on a magnetic stirrer and stir for 1h (heating and controlling during the stirring process) The heating temperature i...

Embodiment 2

[0059] 1) Choose the purity of commercially available iodine simple substance ≥ 99.7%, the purity of isopropanol ≥ 99.8%;

[0060] 2) Weigh an appropriate amount of Yb 2 SiO 5 Powder and Yb 2 Si 2 o 7 Whiskers (Yb 2 Si 2 o 7 The content of whiskers is 20% of the total mass of the two, Yb 2 SiO 5 The content of powder is 80% of both total mass) is dispersed in the 1.5L isopropanol, is mixed with Yb 2 SiO 5 Powder and Yb 2 Si 2 o 7 For a suspension with a total whisker concentration of 35 g / L, the suspension was ultrasonically oscillated (ultrasonic power: 800 W) for 40 minutes, then placed on a magnetic stirrer and stirred for 4 hours to obtain suspension A;

[0061] 3) Add elemental iodine to the suspension A (control the concentration of elemental iodine to be 4.2g / L) and then vibrate ultrasonically (ultrasonic power is 800W) for 30min, then place it on a magnetic stirrer and stir for 1h (heating and controlling during the stirring process) The heating temperatu...

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Abstract

The invention discloses a preparation method for a carbon/carbon composite Yb2Si2O7 whisker toughened Yb2SiO5 composite coating.The preparation method comprises the following steps that 1, Yb2SiO5 powder and Yb2Si2O7 whiskers are dispersed in isopropanol to prepare a Yb3+ mixture A with the concentration of 30-45 g/L; 2, the mixture A is subjected to ultrasonic concussion and then stirred to prepare suspension liquid A; 3, elementary substance iodine is added into the suspension liquid A to obtain a mixture B, and the mixture B is subjected to ultrasonic concussion for 30-60 min and then stirred while being heated to prepare suspension liquid B; the suspension liquid B is added into a hydrothermal kettle, a graphite electrode serves as an anode, a conductive substrate serves as a cathode, a carbon/carbon composite sample with an SiC inner coating is clamped to the cathode in the hydrothermal kettle, and the hydrothermal kettle is put into an electromagnetic induction heater for a reaction; 5, after the reaction is over, the carbon/carbon composite sample with the SiC inner coating is taken out and dried, and then the carbon/carbon composite Yb2Si2O7 whisker toughened Yb2SiO5 composite coating is prepared.According to the method, the process equipment is simple, the reaction period is short, cost is low, and the method has broad development prospects.

Description

technical field [0001] The invention belongs to the technical field of C / C composite materials, in particular to a carbon / carbon composite material Yb 2 Si 2 o 7 Whisker toughened Yb 2 SiO 5 Preparation method of composite coating. Background technique [0002] Carbon / carbon (C / C) composites have excellent properties such as low thermal expansion coefficient, low density, high temperature resistance, ablation resistance, high strength, high modulus, etc. The excellent performance that the amount increases with the increase of temperature makes it have broad application prospects in the aerospace field. However, C / C composites will be oxidized in an aerobic environment exceeding 450°C. Some active sites in C / C composites are easy to absorb oxygen in the air and oxidize, and the loss of oxidation mass leads to a decrease in its strength, which limits its practical application. Therefore, solving the problem of high-temperature oxidation resistance of C / C composites is t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/89
CPCC04B41/009C04B41/52C04B41/85C04B41/5059C04B41/5024C04B41/4596C04B41/4564C04B35/83
Inventor 曹丽云雍翔周磊黄剑锋李翠艳欧阳海波费杰吴建鹏
Owner SHAANXI UNIV OF SCI & TECH
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