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Preparation method of oxide ceramic coating layer on surface of silicon carbide fiber

A technology of silicon carbide fiber and surface oxide, which is applied in the direction of coating, metal material coating process, gaseous chemical plating, etc., to achieve the effect of precise thickness control, simple reaction mechanism and easy exhaust gas

Inactive Publication Date: 2014-12-17
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to overcome the deficiencies of the existing sol-gel method and chemical vapor deposition method, and provide a method for preparing an oxide ceramic coating on the surface of silicon carbide fiber using atomic layer deposition technology

Method used

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  • Preparation method of oxide ceramic coating layer on surface of silicon carbide fiber
  • Preparation method of oxide ceramic coating layer on surface of silicon carbide fiber
  • Preparation method of oxide ceramic coating layer on surface of silicon carbide fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The example of this embodiment includes the following steps:

[0035] (1) KD- SIC fiber is kept for 30min in a nitrogen atmosphere of 500 ° C for 30 minutes to remove glue, and then placed in acetone for 5 minutes to remove surface dirt and then dry room temperature;

[0036] (2) Put the SIC fiber processed by steps (1) in the ALD reaction chamber, draw vacuum and replace nitrogen three times, the reaction room is heating to 250 ° C, and the reaction room is maintained at 5 TORR pressure;

[0037] (3) The front drive ZR [n (CH 3 Cure 2 ] 4 At the 15SCCM flow rate N 2 Take the lower pulse into the reaction room, adsorb on SIC fiber, the pulse time is 0.4s, and then use 50SCCM N 2 Blow and take away the remaining zr [N (CH 3 Cure 2 ] 4 N 2 The blowing time is 5S, the same H 2 O at 10sccm n 2 The lower pulse enters the reaction room, and ZR [n (CH 3 Cure 2 ] 4 Reaction, generate ZRO 2 The time is 0.1S, and the subsequent excess water and by -products are 50sccm n 2 Blowing th...

Embodiment 2

[0042] The example of this embodiment includes the following steps:

[0043] (1) KD- SIC fiber is kept for 30min in a nitrogen atmosphere of 500 ° C for 30 minutes to remove glue, and then placed in acetone for 5 minutes to remove surface dirt and then dry room temperature;

[0044] (2) Put the SIC fiber processed by steps (1) in the ALD reaction chamber, draw vacuum and replace nitrogen three times, the reaction room is heated to 200 ° C, and the pressure is maintained at 3TORR;

[0045] (3) The front -wheel drive HF [n (CH 3 ) (C 2 H 5 )] 4 At the 20SCCM flow rate N 2 Take the lower pulse into the reaction room, adsorb on SIC fiber, the pulse time is 0.4s, and then use 60SCCM N 2 Blow and take away the remaining HF [N (CH CH 3 ) (C 2 H 5 )] 4 N 2 The blowing time is 5s, and O. 3 In 5SCCM N 2 The lower pulse enters the reaction room, and hf [n (CH 3 ) (C 2 H 5 )] 4 Reaction, generate HFO 2 , Time is 0.02s, subsequent overdose O 3 The by -product is 60SCCM N 2 Blowing the reactio...

Embodiment 3

[0050] The example of this embodiment includes the following steps:

[0051] (1) Put the Hi-NICALON SIC fiber in a 600 ℃ nitrogen atmosphere for 30 minutes to remove the glue, and then clean it in the supraithine for 5 minutes to remove the surface dirt and then dry the room temperature.

[0052] (2) Put the SIC fiber processed by steps (1) in the ALD reaction chamber, draw vacuum and replace nitrogen three times, the reaction room heating to 100 ° C, and the reaction room pressure is maintained at 10TORR;

[0053] (3) The front drive al (CH 3 Cure 3 At the 15SCCM flow rate N 2 Take the lower pulse into the reaction room, adsorb on SIC fiber, the pulse time is 0.02s, and then use 40 SCCM N 2 Blow and take away the remaining al (CH 3 Cure 3 N 2 The blowing time is 10s, and the same ozone generated O. 3 In 5SCCM N 2 The lower pulse enters the reaction room, and AL (CH 3 Cure 3 Reaction, generate al 2 O 3 , Time is 0.02s, subsequent overdose O 3 The by -products are 40 sccm n 2 Blowi...

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Abstract

The invention discloses a preparation method of an oxide ceramic coating layer on a surface of a silicon carbide fiber. The preparation method comprises the following steps: (1) the silicon carbide fiber is removed glue for cleaning; (2) the silicon carbide fiber is put in an ALD reaction chamber to repeatedly vacuumize and replace nitrogen for three times; (3) a reaction precursor is selected according to the type of a deposited oxide coating layer; and the parameters of a deposition process are set; (4) precursor steam is guided in the ALD reaction chamber under the carrying of nitrogen or argon; (5) the reaction chamber is blown by the nitrogen or argon; (6) oxygen source steam is guided in the ALD reaction chamber under the carrying of the nitrogen or argon; (7) the reaction chamber is blown by the nitrogen or argon; (8) the steps (4)-(7) are repeated until the needed thickness of the coating layer is deposited; and (9) the coating layer is put in a high-temperature tube furnace, and is thermally treated under the nitrogen protection. The preparation method can be used for preparing the uniform and compact oxide ceramic coating layer with few impurities and precisely controlled thickness on the surface of the SiC fiber.

Description

Technical field [0001] The invention involves the field of high temperature resistance to the field of anti -oxidation coating, and specifically involves a method of preparing oxide ceramic coating on the surface of silicon carbide fiber on the surface of silicon carbide fiber. Background technique [0002] The silicon carbide (SIC) fiber is not only larger than the intensity, high modeling, and small line expansion coefficients. It also has the characteristics of high temperature resistance, corrosion resistance, creep resistance, and weaving.In high -tech fields such as aviation, aerospace, nuclear industry, and weapons and equipment. [0003] Although silicon carbide fiber has a certain antioxidant performance, oxidation and downgrade will occur when the high -temperature oxidation environment is used for a long time, which will affect its service performance.Oxide ceramics has good antioxidant properties. Therefore, preparing oxide ceramic coating on the surface of silicon ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/44C23C16/40
Inventor 王军曹适意王浩简科王小宙
Owner NAT UNIV OF DEFENSE TECH
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