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Preparation process of high temperature oxidation resistant zrnx/(zralfe)n/(zralfem)n composite gradient coating

A technology of anti-oxidation at high temperature and gradient coating, applied in metal material coating process, coating, superimposed layer plating, etc. Maintains stability and mitigates the effect of reduced binding force

Active Publication Date: 2020-07-03
田海军
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It shows that the existing fuel cladding can no longer meet the requirements of accident safety. Therefore, it is urgent to develop new nuclear fuel cladding materials with excellent high temperature oxidation resistance, corrosion resistance, and mechanical properties or to develop surface coating technology for zirconium alloy cladding materials.

Method used

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  • Preparation process of high temperature oxidation resistant zrnx/(zralfe)n/(zralfem)n composite gradient coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] a. Clean the base material:

[0031] Zirconium alloy (Zr 4 Alloy) substrate for grinding and polishing; then use acetone and ethanol as solvents to degrease and degrease and clean in an ultrasonic instrument; then clean with deionized water, dry and put into a vacuum chamber, the vacuum degree is -4 Pa;

[0032] b. Treatment of the substrate before deposition:

[0033] Keep the vacuum chamber vacuum -4 Under the condition of Pa, the reverse sputtering was used for 15 min to clean the zirconium alloy substrate; the reverse sputtering bias voltage was -450 V; the reverse sputtering gas was Ar; the reverse sputtering pressure in the vacuum chamber was 3.5 Pa;

[0034] c. Pre-sputtering:

[0035] Keep the vacuum chamber vacuum -4 Under the condition of Pa, pre-sputtering was used to clean each target for 15 min to remove impurities on the target surface; the pre-sputtering power was 120 W; the pre-sputtering bias was -120 V; the pre-sputtering gas was Ar; The pre-spu...

Embodiment 2

[0040] a. Clean the base material:

[0041] Zirconium alloy (Zr 4 Alloy) substrate for grinding and polishing; then use acetone and ethanol as solvents to degrease and degrease and clean in an ultrasonic instrument; then clean with deionized water, dry and put into a vacuum chamber, the vacuum degree is -4 Pa;

[0042] b. Treatment of the substrate before deposition:

[0043] Keep the vacuum chamber vacuum -4 Under the condition of Pa, the reverse sputtering was used for 15 min to clean the zirconium alloy substrate; the reverse sputtering bias voltage was -450 V; the reverse sputtering gas was Ar; the reverse sputtering pressure in the vacuum chamber was 3.5 Pa;

[0044] c. Pre-sputtering:

[0045] Keep the vacuum chamber vacuum -4 Under the condition of Pa, pre-sputtering was used to clean each target for 15 min to remove impurities on the target surface; the pre-sputtering power was 120 W; the pre-sputtering bias was -120 V; the pre-sputtering gas was Ar; The pre-spu...

Embodiment 3

[0050] a. Clean the base material:

[0051] Zirconium alloy (Zr 4 Alloy) substrate for grinding and polishing; then use acetone and ethanol as solvents to degrease and degrease and clean in an ultrasonic instrument; then clean with deionized water, dry and put into a vacuum chamber, the vacuum degree is -4 Pa;

[0052] b. Treatment of the substrate before deposition:

[0053] Keep the vacuum chamber vacuum -4Under the condition of Pa, the reverse sputtering was used for 15 min to clean the zirconium alloy substrate; the reverse sputtering bias voltage was -450 V; the reverse sputtering gas was Ar; the reverse sputtering pressure in the vacuum chamber was 3.5 Pa;

[0054] c. Pre-sputtering:

[0055] Keep the vacuum chamber vacuum -4 Under the condition of Pa, pre-sputtering was used to clean each target for 15 min to remove impurities on the target surface; the pre-sputtering power was 120 W; the pre-sputtering bias was -120 V; the pre-sputtering gas was Ar; The pre-sputt...

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Abstract

The invention discloses a preparation process of a zirconium alloy surface high-temperature oxidization resistant ZrNx / (ZrAlFe)N / (ZrAlFeM)N composite gradient coating, wherein M is any two kinds of elements in Ti, V and Nb. The concrete process comprises the steps of substrate pretreatment, target material cleaning, ZrNx / (ZrAlFe)N / (ZrAlFeM)N composite coating deposition and the like. The compositecoating preparation is performed in two steps; in the first step, a ZrNx / (ZrAlFe)N gradient transition layer is prepared; firstly, a Zr coating is deposited for 3min on the substrate; then, N2 is gradually introduced at the flow from 0sccm to 6sccm for depositing ZrNx, wherein the flow rate of N2 is 2sccm / min; then, continuous transition is performed to (ZrAlFe)N; in the second step, a (ZrAlFeM)Nmulti-component nitride layer is prepared. In the decomposed (ZrAlFe)N transition layer, the Zr element atom content is in gradient change from 100 at percent to 30 at percent in the thickness direction; the Al and Fe element atom contents are in gradient change from 0 at percent to 35 at percent in the thickness direction; the Zr, Al, Fe and M element atom contents in the decomposed (ZrAlFeM)N multi-component nitride layer are between 10 at percent and 35 at percent; the N element atom content is between 5 at percent and 20 at percent. The process has the characteristics that through the design of a structure with the coating in the gradient change state, the residue stress in the coating can be relieved; the high-temperature oxidization resistance performance is realized; the mechanicalproperty is excellent, and the like.

Description

technical field [0001] The invention belongs to the technical field of reactor nuclear fuel zirconium alloy cladding surface modification technology, and specifically relates to a ZrN with high-temperature oxidation resistance, corrosion resistance and excellent mechanical properties prepared on the surface of zirconium alloy by using multi-target co-sputtering technology x / (ZrAlFe)N / (ZrAlFeM)N composite gradient coating preparation method. Background technique [0002] As an efficient and clean energy, nuclear energy has significant advantages in solving energy crisis and protecting the environment. At present, zirconium alloy has a series of advantages such as good machining performance, small neutron absorption cross section, good corrosion resistance, and good compatibility with uranium fuel, so it is widely used in reactor nuclear fuel cladding tubes and structural materials Wait. Zirconium alloys are easily oxidized with water in a high-temperature steam environment...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/35C23C14/02C23C14/06
CPCC23C14/0036C23C14/022C23C14/025C23C14/0641C23C14/352C23C28/048
Inventor 刘波蒲国林黎蔚
Owner 田海军
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