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Amorphous and nanocrystalline composite coating for zirconium alloy protection and preparation method of amorphous and nanocrystalline composite coating

A nanocrystalline composite and zirconium alloy technology, which is applied in metal material coating technology, coating, ion implantation plating, etc., can solve the problems of affecting the mechanical properties of the coating, low hardness of the coating, and easy peeling and failure of the coating. Achieve good high temperature water vapor corrosion resistance, high hardness and compact structure

Active Publication Date: 2019-02-15
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the hardness of this coating is low, and the range hardness of embodiment record is only 10~15Gpa, and the hardness of coating is low and can affect the mechanical performance of coating, as under long-term stressed state, coating is easy to peel off failure.

Method used

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  • Amorphous and nanocrystalline composite coating for zirconium alloy protection and preparation method of amorphous and nanocrystalline composite coating
  • Amorphous and nanocrystalline composite coating for zirconium alloy protection and preparation method of amorphous and nanocrystalline composite coating

Examples

Experimental program
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Effect test

Embodiment 1

[0049] (1) Substrate cleaning: take the zirconium alloy after polishing as the substrate (surface roughness Ra2 CO 3 Water solution, acetone, absolute ethanol, and deionized water were ultrasonically cleaned for 15 minutes, and then dried in a drying oven at a temperature of 100 °C for 2 hours; the chemically cleaned substrate was placed on the abutment in a vacuum chamber, Below 1×10 -3 After Pa, introduce argon gas and maintain the pressure at 1Pa, then turn on the power supply and apply a negative bias voltage to the substrate at the same time, and use the plasma glow generated by argon to etch and clean it for 10 minutes;

[0050] (2) Connect the power supply: put Cr 61 al 24.5 Si 14.5 The target is connected to a DC power supply, the Cr target is connected to a radio frequency power supply, and the purity of the two targets is greater than 99.99%;

[0051] (3) Coating preparation: put the cleaned zirconium alloy substrate into a vacuum chamber, when the vacuum degree ...

Embodiment 2

[0056] The coating was prepared according to the method described in Example 1, only some parameters in steps (2) and (3) were different.

[0057] Select Cr for use in step (2) 62 al 19 Si 19 target.

[0058] Process parameter difference is in the step (3): the flow ratio of nitrogen and argon is 0.13, Cr 62 al 19 Si 19 The sputtering power density of the target is 3.75W / cm 2 , the power density of the auxiliary plasma Cr target is 3.70W / cm 2 , heating the substrate to 600°C, the composition is Cr 53.5 al 15.3 Si 6.2 N 25 coating.

[0059] The crystal structure of the obtained coating was tested. The coating is a two-phase composite structure of nanocrystalline and amorphous. The TEM high-resolution photos show that the grain size of AlN in the hexagonal phase is 7-12nm. The thickness of the amorphous phase between them is 15-25nm.

[0060] The morphology of the obtained coating was characterized. It can be seen from the cross-sectional SEM topography that the coa...

Embodiment 3

[0063] The coating was prepared according to the method described in Example 1, only some parameters in steps (2) and (3) were different.

[0064] Select Cr for use in step (2) 64.5 al 17 Si 18.5 target.

[0065] Process parameter difference is in step (3): the flow ratio of nitrogen and argon is 0.22, adjusts Cr 64.5 al 17 Si 18.5 The sputtering power density of the target is 4.00W / cm 2 , the power density of the auxiliary plasma Cr target is 3.85W / cm 2 , the substrate is heated to 500°C, and the composition is Cr 54.5 al 15.3 Si 5.3 N 24.9 coating.

[0066]The crystal structure of the obtained coating was tested. The coating is a two-phase composite structure of nanocrystalline and amorphous. As shown in the high-resolution TEM photo, the grain size of AlN in the hexagonal phase is 7-15nm, and the adjacent two nanocrystalline The thickness of the amorphous phase between them is 10-25nm.

[0067] The morphology of the obtained coating was characterized. It can be...

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Abstract

The invention discloses an amorphous and nanocrystalline composite high hardness coating. The coating is composed of Cr<x>Al<y>Si<z>N<100-x-y-z>, wherein 52.0<=x<=55.5, 15.3<=y<=20.2, 3.3<=z<=6.7, thex, y, and z are atomic ratios, the high hardness protective coating is of a hexagonal AlN nanocrystalline and amorphous two-phase composite structure, the thickness of the high hardness protective coating is 8-12 [mu]m, and the density is 4.9-5.7 g / cm<3>; the coating is prepared through physical gas phase magnetron sputtering, when the vacuum degree is 3*10<-5> Pa or the less, the substrate surface is deposited by selecting a target material and adjusting the sputtering power density of the target material and the power density of an auxiliary plasma radio frequency power source, according tothe obtained protective coating, the hardness can reach 18-23 GPa, and can further resist water vapor oxidation at 800-1200 DEG C within a long time period.

Description

technical field [0001] The invention belongs to the field of high-temperature protective coatings, in particular to an amorphous and nanocrystalline composite coating for zirconium alloy protection and a preparation method thereof. Background technique [0002] Zirconium alloys are the only nuclear fuel cladding materials in use today. Zirconium alloys have good corrosion resistance, moderate mechanical properties, and low thermal neutron absorption cross section (zirconium is 0.18 barn) in high temperature, high pressure water and steam at 300-400 ° C, and have good compatibility with nuclear fuel Therefore, it can be used as the core structure material (fuel cladding, pressure tube, bracket and tunnel tube) of light water nuclear reactor. However, when an accident occurs in the cooling system and the surrounding temperature of the cladding material rises above 800°C, the zirconium alloy will react with water vapor to generate hydrogen gas. If it cannot be released or deco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/16C23C14/35C22C27/06C22C45/00
CPCC22C27/06C22C45/006C23C14/0036C23C14/165C23C14/345C23C14/352
Inventor 黄峰祝涵李朋葛芳芳董悦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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