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Multilayer protective coating with high-temperature steam oxidation resistance and hot water corrosion resistance and preparation method and application

A protective coating and water vapor technology, applied in the coating, metal material coating process, vacuum evaporation plating, etc., can solve the problems of poor hot water corrosion resistance, loss of accident tolerance, coating corrosion, etc. To prevent diffusion, overcome the inability to resist hot water corrosion, and improve the toughness of the coating

Active Publication Date: 2019-11-22
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the typical Cr-Al-Si-N protective coating has a good protective effect in the water vapor environment of 1000 °C under the fault-tolerant working condition, the Al in the coating is easily mixed with water in the hot water environment under the normal working condition. It reacts to form a loose and easily soluble AlO(OH) compound, which makes its hot water corrosion resistance worse, and eventually causes the coating to be corroded and invalid, and loses its accident tolerance

Method used

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  • Multilayer protective coating with high-temperature steam oxidation resistance and hot water corrosion resistance and preparation method and application
  • Multilayer protective coating with high-temperature steam oxidation resistance and hot water corrosion resistance and preparation method and application
  • Multilayer protective coating with high-temperature steam oxidation resistance and hot water corrosion resistance and preparation method and application

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preparation example Construction

[0044] All examples were prepared as figure 2 As shown, when the background vacuum is ≤8×10 -5 Pa, start to heat sample 7 to 600°C and keep it warm for 2 hours, apply a bias voltage of -15V ~ -10V to the substrate, and enter Ar and N respectively through the gas inlet 6 in the chamber 1 2 As a sputtering and reaction gas source, the air pressure of the chamber 1 is adjusted by controlling the opening and closing of the gas outlet 5. In this gas source, 3A targets (Cr a Al b Si 1-a-b target, wherein, 0.5≤a≤0.6, 0.25≤b≤0.3) and 3B target (Cr target) get multi-layer protective coating, 3A target and 3B target are separated by separator 4 (the purpose of isolation is 3A target and 3 B target work independently without interfering with each other, so that the Cr layer and the CrAlSiN layer do not interfere with each other when depositing the Cr layer and the CrAlSiN layer). In the process of sputtering the 3A target and the 3B target, the RF-assisted DC power supply method is u...

Embodiment 1

[0064] This embodiment is prepared by magnetron sputtering method, and the parameters are set as: background vacuum 8×10 -5 Pa; chamber air pressure: 0.5Pa; 3A target components use Cr 0.6 Al 0.3 Si 0.1 target, 3A target power density is 6.2 W / cm 2 ; 3B target power density is 5.2W / cm 2 ; Sputter the 3A target first (the 3B target is closed at this time), and pass in N 2 The flow ratio of Ar gas and Ar gas is 0.13, and the control sample 7 is facing the 3A target, and a 6 μm thick CrAlSiN layer is obtained by sputtering; after that, the 3A target and the N 2 Gas source, start 3B target, start sputtering 3B target and control sample 7 to face 3B target, sputter to get a 4μm thick Cr layer, and do this alternately once to get a Cr / CrAlSiN multilayer protective coating with a periodic layer λ of 1 , one of the periodic layers has a CrAlSiN layer thickness of 6 μm and a Cr layer thickness of 4 μm.

[0065] Structural characterization of the Cr / CrAlSiN (λ=1) multilayer protec...

Embodiment 2

[0071] This embodiment is prepared by magnetron sputtering method, and the parameters are set as: background vacuum 6×10 -5 Pa; chamber air pressure: 0.5Pa; 3A target components use Cr 0.5 Al 0.25 Si 0.25 ; 3A target power density is 6.7 W / cm 2 , 3B target power density is 4.8W / cm 2 ; Sputter the 3A target first (the 3B target is closed at this time), and pass in N 2 The flow ratio of Ar gas and Ar gas is 0.15, and the control sample 7 is facing the 3A target, and a 2.5 μm thick CrAlSiN layer is obtained by sputtering; after that, the 3A target and the N 2 Gas source, start 3B target, start sputtering 3B target and control sample 7 to face 3B target, sputter to get a 2.5μm thick Cr layer, do this twice alternately, get a Cr / CrAlSiN multilayer protective coating with a periodic layer λ of 2 Layers, one of the periodic layers has a CrAlSiN layer thickness of 2.5 μm and a Cr layer thickness of 2.5 μm.

[0072] Structural characterization of the Cr / CrAlSiN (λ=2) multilayer p...

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Abstract

The invention discloses a multilayer protective coating with high-temperature steam oxidation resistance and hot water corrosion resistance. The multilayer protective coating comprises the following components: a Cr layer and a CrAlSiN layer which are periodically and alternately deposited, wherein the most surface layer of the coating is the Cr layer; the cycle number of the alternate depositionis 1-20; the thickness of the Cr layer and the CrAlSiN layer in the unit period is 0.5-10 microns, and the thickness ratio is 2: 3-3: 2. The multilayer protective coating is formed by alternately depositing theCr layer and the CrAlSiN layer on the surface of a zirconium alloy substrate by adopting a magnetron sputtering method. The invention also provides a zirconium alloy covering housing manufactured by the abovementioned method. The multilayer protective coating has the advantages of hot water corrosion resistance under the normal working condition (600-650 DEG C) and high-temperature steamoxidation resistance under the accident fault-tolerant working condition (1000-1200 DEG C), and effectively meets the protection requirements under two working conditions of a light water reactor.

Description

technical field [0001] The invention belongs to the field of ceramic coatings, in particular to a multi-layer protective coating with high temperature water vapor oxidation resistance and hot water corrosion resistance, a preparation method and an application. Background technique [0002] Zirconium alloy has the advantages of radiation resistance and low thermal neutron absorption cross section. It is the cladding material of the mainstream light water reactor fuel at present. Its stable performance and improved life are the keys to ensure the safety and reliability of the nuclear reactor core. However, in the case of coolant failure (LOCA), zirconium alloys are prone to react with high-temperature water vapor to generate a large amount of hydrogen, which can cause an explosion, which is also the main reason for the explosion of the Fukushima nuclear power plant in Japan and the nuclear leak. Therefore, preventing or mitigating the reaction of zirconium alloys with high-tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35C23C14/14C23C14/06C23C14/54
CPCC23C14/0036C23C14/0641C23C14/14C23C14/352C23C14/548
Inventor 黄峰刘海勇李朋葛芳芳祝涵
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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