CN104711541A - Zirconia and alumina gradient composite coat and production method thereof - Google Patents
Zirconia and alumina gradient composite coat and production method thereof Download PDFInfo
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- CN104711541A CN104711541A CN201310675873.8A CN201310675873A CN104711541A CN 104711541 A CN104711541 A CN 104711541A CN 201310675873 A CN201310675873 A CN 201310675873A CN 104711541 A CN104711541 A CN 104711541A
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Abstract
The invention relates to a zirconia and alumina gradient composite coat and a production method thereof. The coat comprises composite layers composed of zirconia and alumina according to different mass percentage ratios, and the composite layers composed of zirconia and alumina are laid on a steel substrate. The composite coat can be produced through a metal organic matter chemical vapor deposition technology or a reactive magnetron co-sputtering technology. The zirconia and alumina gradient composite coat combines the hydrogen resistance and penetration characteristics of zirconia and alumina, and the thermal expansion coefficient of the composite coat can be changed by adjusting the proportions of zirconia and alumina in the composite coat to improve the thermal physical matching performance between the composite coat and the substrate, so the thermal cycle use performance of the composite coat is improved.
Description
Technical field
The present invention relates to a kind of zirconium white and aluminum oxide gradient composite coating and preparation method thereof, this compound coating can be applicable to the hydrogen permeation barrier coating relating to steel construction piece in hydrogen field, also can be applicable to wear-resisting, the anti-corrosion coating of steel construction piece.
Background technology
Hydrogen permeation preventing coating is the type coating material hydrogen of structure unit having been permeated to reduction and barrier effect, is the critical material relating to hydrogen and hydrogen isotope Application Areas.As far back as the seventies in last century, the Soviet Union has just carried out the research and development of hydrogen resistance coating SCB glass coating, is applied to the hydrogen infiltration-resistant of TOPAZ space heap heap wall of container.SCB glass possesses good NdFeB permanent magnets, but SiO
2to react with hydrogen at 300 DEG C and cause the embrittlement of glass and break, its application in hydrogen resistance coating is restricted.1991, Forcey etc. proposed to adopt Al/Fe layer as fusion reactor structured material surface resistance tritium coating first, and their research work confirms the application potential of Al/Fe layer as resistance tritium coating, and coating penetration stops that the factor is up to 3-4 the order of magnitude.
In the last few years, investigator had carried out large quantity research to novel hydrogen permeation preventing coating material, such as TiC, SiC, SiO
2, Cr
2o
3, Al
2o
3, Y
2o
3, Er
2o
3, ZrO
2deng.Wherein, Al
2o
3, ZrO
2due to hydrogen infiltration-resistant, high-temperature stability, chemical stability, the wear resisting property of its excellence, receive as hydrogen permeation preventing coating material and study concern widely.In addition, except single coated material, compound coating research was also being carried out in recent years.Compared with single coating, the physics between compound coating and matrix, chemical matched performance are more excellent, and hydrogen permeation barrier, film-substrate cohesion and thermal circulation performance have further raising.CN101469409A discloses the adjustable aluminum oxide of a kind of ratio/Erbium trioxide composite structure hydrogen permeation preventing coating, combine high hydrogen infiltration-resistant and the constitutionally stable advantage of Erbium trioxide of aluminum oxide, compound coating is through room temperature to 500 DEG C repeatedly cold cycling, and coating is without cracking and peeling phenomenon generation.CN101629028A discloses the compound coating of a kind of metal and aluminum oxide alternating deposit, and by the bonding force adding raising compound coating of metal level, this compound coating has excellent high temperature resistant, oxidation resistent susceptibility.
Summary of the invention
The invention provides a kind of zirconium white/aluminum oxide gradient composite coating, for improving the hydrogen infiltration-resistant performance of steel construction piece, the present invention proposes to prepare gradient composite coating in steel matrix, utilizes zirconium white, the difference of aluminum oxide thermal expansivity realizes steel matrix and mate (zirconium white thermal expansivity 11 × 10 with the ermal physics of gradient composite coating
-6k
-1, aluminum oxide 5-6 × 10
-6k
-1), thus the overall thermal improving coating recycles performance.This gradient composite coating combines the hydrogen infiltration-resistant performance of zirconia layer and alumina layer, and coating has the feature of hydrogen infiltration-resistant performance, thermal cycling use properties excellence.
For achieving the above object, the present invention adopts following technical scheme:
A kind of zirconium white and aluminum oxide gradient composite coating, comprise the composite bed that multilayer (more than two-layer) is made up of zirconium white and the aluminum oxide of different mass per-cent, namely in multiple composite bed, the mass percentage of zirconium white and aluminum oxide is different, and the composite bed of described zirconium white and aluminum oxide composition is laid in steel base.
Described zirconium white and aluminum oxide gradient composite coating, can be made up of the composite bed of multilayer zirconium white and the gradual change of quality of alumina per-cent, can by (100%-x) ZrO of multilayer x value gradual change
2-xAl
2o
3composite bed is formed, and wherein x is Al
2o
3mass percent, 0≤x≤100%; In the composite bed of multilayer zirconium white and the gradual change of quality of alumina per-cent, x value decreasing order or increase progressively; The thickness of gradient composite coating is≤2 microns.
Described zirconium white is single zirconium white, also can be oxide compound stabilizing zirconia, oxide compound be selected from one or more the combination in calcium oxide, magnesium oxide, yttrium oxide, lanthanum trioxide, cerium oxide, Praseodymium trioxide, Neodymium trioxide, promethium oxide, Samarium trioxide, europium sesquioxide, gadolinium sesquioxide, terbium sesquioxide, dysprosium oxide, Holmium trioxide, Erbium trioxide, trioxide, ytterbium oxide, lutecium oxide.In described oxide compound stabilizing zirconia, the content of oxide compound is 4-25wt%.
Described steel base is 304,304L, 316,316L, 410,416,430,431, one in 630 stainless steels.
Present invention also offers the preparation method of above-mentioned zirconium white and aluminum oxide gradient composite coating.
A preparation method for zirconium white and aluminum oxide gradient composite coating, adopts metal-organic chemical vapor deposition equipment method or adopts the preparation of reaction magnetic control co-sputtering method.
Adopt metal-organic chemical vapor deposition equipment method, deposited oxide zirconium/aluminum oxide gradient composite coating in steel base, comprises the steps: that steel base is after acetone, alcohol and deionized water ultrasonic cleaning, puts into reaction chamber; With methyl ethyl diketone zirconium and aluminium acetylacetonate for metal precursor, adopt Ar as carrier gas, O
2as reactant gases; By changing volatilization temperature and the Ar carrier gas flux of methyl ethyl diketone zirconium and aluminium acetylacetonate, regulate the proportion of composing of zirconium white and aluminum oxide in deposition compound coating.As, the volatilization temperature of methyl ethyl diketone zirconium is 150 ~ 180 DEG C, is 10 ~ 30sccm by the Ar carrier gas flux of methyl ethyl diketone zirconium; The volatilization temperature of aluminium acetylacetonate is 120 ~ 125 DEG C, is 10 ~ 30sccm by the Ar carrier gas flux of aluminium acetylacetonate; O
2flow 10 ~ 20sccm, depositing temperature is 500 ~ 600 DEG C, and depositing time is 0.5 ~ 2 hour, and reaction chamber pressure is 1200 ~ 1600Pa.
The reaction magnetic control co-sputtering method adopted comprises magnetically controlled DC sputtering, medium frequency magnetron sputtering and radio frequency magnetron sputtering method.Adopt reaction magnetic control co-sputtering method, deposited oxide zirconium/aluminum oxide gradient composite coating in steel base, comprise the steps: adopt metal zirconium (or adopt zirconium/calcium alloy, zirconium/magnesium alloy, zirconium/yittrium alloy, zirconium/lanthanum alloy, zirconium/cerium alloy, zirconium/promethium alloy, zirconium/neodymium alloy, zirconium/promethium alloy, zirconium/samarium alloy, zirconium/europium alloy, zirconium/gadpolinium alloy, zirconium/terbium alloy, zirconium/disprosium alloy, zirconium/holmium alloy, zirconium/erbium alloy, zirconium/thulium alloy, zirconium/ytterbium alloy or zirconium/lutetium alloy), metallic aluminium is target, adopt independently direct current respectively, intermediate frequency and/or radio-frequency power supply are powered, Ar is as build-up of luminance gas, O
2as reactant gases, steel base, after acetone, alcohol and deionized water ultrasonic cleaning, puts into vacuum cavity, when back end vacuum is better than 8 × 10
-3after Pa, in sputtering chamber, clean 15 minutes with Ar plasma bombardment, control Ar/O
2=20/1 ~ 2/1 (throughput ratio), stagnation pressure 0.1 ~ 4Pa, target-cardinal distance 40 ~ 100mm, substrate bias-40 ~-200V, the multi-gradient compound coating of different proportion of composing is obtained by the sputtering power and depositing time adjusting zirconium target and aluminium target.As, be respectively 50 ~ 15000W at the sputtering power of zirconium target and aluminium target, under the condition of 50 ~ 15000W, deposit 5 ~ 200min.
Zirconium white of the present invention/aluminum oxide gradient composite coating, comprises steel matrix and the zirconium white on it/aluminum oxide gradient composite coating.Compared with prior art, the advantage of zirconium white of the present invention/alumina composite gradient cladding is the hydrogen infiltration-resistant characteristic combining zirconium white and aluminum oxide, simultaneously, by regulating zirconium white and aluminum oxide proportion of composing in compound coating, the thermal expansivity of compound coating can be changed, improve the ermal physics matched performance between compound coating and matrix, thus improve the thermal cycling use properties of compound coating.
Embodiment
The present invention further illustrates in conjunction with the following example, but the present invention is not limited to embodiment below.
Embodiment one
Deposited oxide zirconium/aluminum oxide gradient composite coating on 316 stainless steels, adopts metal-organic chemical vapor deposition equipment.316 stainless steels, through acetone, after alcohol and deionized water ultrasonic cleaning, put into reaction chamber.With methyl ethyl diketone zirconium and aluminium acetylacetonate for metal precursor, adopt Ar as carrier gas, O
2as reactant gases.The volatilization temperature of methyl ethyl diketone zirconium is 180 DEG C, is 30sccm by the Ar carrier gas flux of methyl ethyl diketone zirconium.The volatilization temperature of aluminium acetylacetonate is 120 DEG C, is 10sccm by the Ar carrier gas flux of aluminium acetylacetonate.O
2flow 10sccm, depositing temperature is 500 DEG C, and depositing time is 0.5 hour, and reaction chamber pressure is 1200Pa.
By changing volatilization temperature and the Ar carrier gas flux of methyl ethyl diketone zirconium and aluminium acetylacetonate, regulate the proportion of composing of zirconium white and aluminum oxide in deposition compound coating.The volatilization temperature of methyl ethyl diketone zirconium is 150 DEG C, is 30sccm by the Ar carrier gas flux of methyl ethyl diketone zirconium.The volatilization temperature of aluminium acetylacetonate is 125 DEG C, is 10sccm by the Ar carrier gas flux of aluminium acetylacetonate.Depositing temperature is 500 DEG C, and depositing time is 0.5 hour, and reaction chamber pressure is 1600Pa.
The thickness obtaining multi-gradient zirconium white/alumina composite coating is 1.2 microns, and in multi-gradient compound coating, the content of zirconium white and aluminum oxide is 37wt%, 63wt% by 76wt%, 24wt% transition.Carry out hydrogen penetrating quality test to the multi-gradient compound coating style obtained, at 600 DEG C, compound coating reduces the factor to 316 stainless hydrogen infiltrations is 203.
Embodiment two
Deposited oxide zirconium/aluminum oxide gradient composite coating on 304 stainless steels, adopts direct current reaction magnetic control co-sputtering.Independent metal zirconium, aluminium are target, adopt independently DC power supply respectively, Ar as build-up of luminance gas, O
2as reactant gases.304 stainless steels, through acetone, after alcohol and deionized water ultrasonic cleaning, put into vacuum cavity.When back end vacuum is better than 2 × 10
-3after Pa, in sputtering chamber, clean 15 minutes with Ar plasma bombardment.Control Ar/O
2=120/30 (throughput ratio), stagnation pressure 0.4Pa, target-cardinal distance 100mm, substrate bias-80V.The multi-gradient compound coating of different proportion of composing is obtained by the sputtering power and depositing time adjusting zirconium target and aluminium target.Be respectively 3200W at the sputtering power of zirconium target and aluminium target, under the condition of 6000W, deposit 20min.Then the sputtering power of zirconium target and aluminium target is adjusted to 8750W, 12000W respectively, then deposits 20min.
The thickness of the zirconium white/aluminum oxide gradient composite coating obtained is 0.6 micron, and in gradient composite coating, the content of zirconium white and aluminum oxide is by 50wt%, 50wt%, and transition is 59wt%, 41wt%.Carry out hydrogen penetrating quality test to the gradient composite coating style obtained, at 650 DEG C, compound coating reduces the factor to 304 stainless hydrogen infiltrations is 139.
Embodiment three
Deposited oxide zirconium/aluminum oxide gradient composite coating on 304 stainless steels, adopts Radiofrequency muti-hook probe.Independent metal zirconium/yittrium alloy (content of Y is 18wt%), aluminium are target, adopt independently radio-frequency power supply to power respectively, Ar as build-up of luminance gas, O
2as reactant gases.304 stainless steels, through acetone, after alcohol and deionized water ultrasonic cleaning, put into vacuum cavity.When back end vacuum is better than 7 × 10
-3after Pa, substrate cleans 15 minutes with Ar plasma bombardment in sputtering chamber.Control Ar/O
2=50/20 (throughput ratio), stagnation pressure is 1.5Pa, and target-cardinal distance is 50mm, substrate bias-80V.The multi-gradient compound coating of different proportion of composing is obtained by the sputtering power adjusting zirconium/yttrium alloy target and aluminium target.Be respectively 100W at the sputtering power of zirconium target and aluminium target, under the condition of 140W, deposit 90min.Then the sputtering power of zirconium target and aluminium target is adjusted to 80W, 230W respectively, then deposits 90min.
The thickness of the zirconium white/aluminum oxide gradient composite coating obtained is 0.3 micron, and in gradient composite coating, the content of zirconium white and aluminum oxide is 40wt%, 60wt% by 57wt%, 43wt% transition.Carry out hydrogen penetrating quality test to the multi-gradient compound coating style obtained, at 600 DEG C, compound coating reduces the factor to 304 stainless hydrogen infiltrations is 250.
Embodiment four
Deposited oxide zirconium/aluminum oxide gradient composite coating on 316L stainless steel.Independently metal zirconium, aluminium are target, adopt direct supply and intermediate frequency power supply to power respectively.Ar as build-up of luminance gas, O
2as reactant gases.316L stainless steel, through acetone, after alcohol and deionized water ultrasonic cleaning, puts into vacuum cavity.When back end vacuum is better than 5 × 10
-3after Pa, in sputtering chamber, clean 15 minutes with Ar plasma bombardment.Control Ar/O
2=120/15 (throughput ratio), stagnation pressure 1Pa, target-cardinal distance 100mm, substrate bias-80V.The multi-gradient compound coating of different proportion of composing is obtained by the sputtering power and depositing time adjusting zirconium target and aluminium target.Be respectively 3200W at the sputtering power of zirconium target and aluminium target, under the condition of 3000W, deposit 20min.Then the sputtering power of zirconium target and aluminium target is adjusted to 3200W, 8000W respectively, then deposits 20min.Finally the sputtering power of zirconium target and aluminium target is adjusted to 6000W, 3000W respectively, then deposits 20min.
The thickness of the zirconium white/aluminum oxide gradient composite coating obtained is 0.5 micron, and in gradient composite coating, the content of zirconium white and aluminum oxide is 43wt%, 57wt% by 67wt%, 33wt% transition, is finally transitioned into 80%, 20% again.Carry out hydrogen penetrating quality test to the multi-gradient compound coating style obtained, at 600 DEG C, compound coating reduces the factor to the stainless hydrogen infiltration of 316L is 180.
Claims (10)
1. zirconium white and an aluminum oxide gradient composite coating, is characterized in that: comprise the composite bed that multilayer is made up of zirconium white and the aluminum oxide of different mass per-cent, and the composite bed of described zirconium white and aluminum oxide composition is laid in steel base.
2. zirconium white as claimed in claim 1 and aluminum oxide gradient composite coating, is characterized in that: described gradient composite coating is by (100%-x) ZrO of multilayer x value gradual change
2-xAl
2o
3composite bed is formed, and wherein x is Al
2o
3mass percent.
3. zirconium white as claimed in claim 2 and aluminum oxide gradient composite coating, is characterized in that: thickness≤2 micron of described gradient composite coating.
4. zirconium white as claimed in claim 1 and aluminum oxide gradient composite coating, is characterized in that: described zirconium white is single zirconium white or oxide compound stabilizing zirconia.
5. zirconium white as claimed in claim 4 and aluminum oxide gradient composite coating, it is characterized in that: in described oxide compound stabilizing zirconia, oxide compound is selected from one or more the combination in calcium oxide, magnesium oxide, yttrium oxide, lanthanum trioxide, cerium oxide, Praseodymium trioxide, Neodymium trioxide, promethium oxide, Samarium trioxide, europium sesquioxide, gadolinium sesquioxide, terbium sesquioxide, dysprosium oxide, Holmium trioxide, Erbium trioxide, trioxide, ytterbium oxide and lutecium oxide.
6. zirconium white as claimed in claim 5 and aluminum oxide gradient composite coating, it is characterized in that: in described oxide compound stabilizing zirconia, the content of oxide compound is 4-25wt%.
7. zirconium white as claimed in claim 1 and aluminum oxide gradient composite coating, is characterized in that: described steel base is 304,304L, 316,316L, 410,416,430,431, one in 630 stainless steels.
8. the preparation method of the zirconium white according to any one of claim 1-7 and aluminum oxide gradient composite coating, it is characterized in that: adopt metal-organic chemical vapor deposition equipment method or the preparation of reaction magnetic control co-sputtering method, described reaction magnetic control co-sputtering method comprises magnetically controlled DC sputtering, medium frequency magnetron sputtering and radio frequency magnetron sputtering method.
9. the preparation method of zirconium white as claimed in claim 8 and aluminum oxide gradient composite coating, it is characterized in that: adopt metal-organic chemical vapor deposition equipment method, deposited oxide zirconium/aluminum oxide gradient composite coating in steel base, comprise the steps: that steel base is after acetone, alcohol and deionized water ultrasonic cleaning, puts into reaction chamber; With methyl ethyl diketone zirconium and aluminium acetylacetonate for metal precursor, adopt Ar as carrier gas, O
2as reactant gases; By changing volatilization temperature and the Ar carrier gas flux of methyl ethyl diketone zirconium and aluminium acetylacetonate, regulate the proportion of composing of zirconium white and aluminum oxide in deposition compound coating.
10. the preparation method of zirconium white as claimed in claim 8 and aluminum oxide gradient composite coating, it is characterized in that: adopt magnetron sputtering method, deposited oxide zirconium/aluminum oxide gradient composite coating in steel base, comprise the steps: to adopt metal zirconium, zirconium/calcium alloy, zirconium/magnesium alloy, zirconium/yittrium alloy, zirconium/lanthanum alloy, zirconium/cerium alloy, zirconium/promethium alloy, zirconium/neodymium alloy, zirconium/promethium alloy, zirconium/samarium alloy, zirconium/europium alloy, zirconium/gadpolinium alloy, zirconium/terbium alloy, zirconium/disprosium alloy, zirconium/holmium alloy, zirconium/erbium alloy, zirconium/thulium alloy, zirconium/ytterbium alloy or zirconium/lutetium alloy, and aluminium is target, Ar is as build-up of luminance gas, O
2as reactant gases, steel base, after acetone, alcohol and deionized water ultrasonic cleaning, puts into vacuum cavity, when back end vacuum is better than 8 × 10
-3after Pa, in sputtering chamber, clean 15 minutes with Ar plasma bombardment, control Ar/O
2throughput ratio is 20/1 ~ 2/1, stagnation pressure 0.1 ~ 4Pa, target-cardinal distance 40 ~ 100mm, substrate bias-40 ~-200V, the multi-gradient compound coating of different proportion of composing is obtained by the sputtering power and depositing time adjusting zirconium target and aluminium target.
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Cited By (10)
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| CN106567050A (en) * | 2016-10-18 | 2017-04-19 | 四川大学 | Process for low-temperature preparation of Zr-doped alpha-Al2O3 nanometer multilayer tritium barrier coating based on Cr2O3 template |
| CN107012425A (en) * | 2017-03-09 | 2017-08-04 | 电子科技大学 | A kind of thin film sensor composite insulation layer and preparation method thereof |
| CN107475686A (en) * | 2017-06-30 | 2017-12-15 | 湖北大学 | A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane |
| CN108018517A (en) * | 2016-10-31 | 2018-05-11 | 通用电气公司 | Kinds of anti-sulfur corrosion coating, includes its object, and uses its method |
| CN110344024A (en) * | 2018-04-06 | 2019-10-18 | 应用材料公司 | Rare earth oxide ALD and the CVD coating of area's control |
| CN111850557A (en) * | 2020-07-23 | 2020-10-30 | 潍柴动力股份有限公司 | Piston manufacturing method and piston |
| CN112391594A (en) * | 2020-09-30 | 2021-02-23 | 科立视材料科技有限公司 | Platinum channel with zirconia protective coating and preparation method thereof |
| CN113227435A (en) * | 2018-10-25 | 2021-08-06 | 格林特威德科技有限公司 | Plasma resistant multilayer coating and method for making same |
| CN115044868A (en) * | 2022-05-27 | 2022-09-13 | 东北大学 | Oxide ceramic and two-dimensional material composite hydrogen-resistant coating and preparation method thereof |
| CN115784775A (en) * | 2022-12-02 | 2023-03-14 | 中国国检测试控股集团股份有限公司 | Zirconia and alumina gradient composite coating and preparation method thereof |
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| CN107012425A (en) * | 2017-03-09 | 2017-08-04 | 电子科技大学 | A kind of thin film sensor composite insulation layer and preparation method thereof |
| CN107475686A (en) * | 2017-06-30 | 2017-12-15 | 湖北大学 | A kind of preparation method based on ald zirconium oxide corrosion resistance ceramic membrane |
| CN110344024B (en) * | 2018-04-06 | 2022-04-08 | 应用材料公司 | Zone controlled rare earth oxide ALD and CVD coatings |
| CN110344024A (en) * | 2018-04-06 | 2019-10-18 | 应用材料公司 | Rare earth oxide ALD and the CVD coating of area's control |
| CN113227435A (en) * | 2018-10-25 | 2021-08-06 | 格林特威德科技有限公司 | Plasma resistant multilayer coating and method for making same |
| CN111850557A (en) * | 2020-07-23 | 2020-10-30 | 潍柴动力股份有限公司 | Piston manufacturing method and piston |
| WO2022016775A1 (en) * | 2020-07-23 | 2022-01-27 | 潍柴动力股份有限公司 | Piston manufacturing method and piston |
| CN112391594A (en) * | 2020-09-30 | 2021-02-23 | 科立视材料科技有限公司 | Platinum channel with zirconia protective coating and preparation method thereof |
| CN115044868A (en) * | 2022-05-27 | 2022-09-13 | 东北大学 | Oxide ceramic and two-dimensional material composite hydrogen-resistant coating and preparation method thereof |
| CN115044868B (en) * | 2022-05-27 | 2023-08-08 | 东北大学 | Oxide ceramic and two-dimensional material composite hydrogen-resistant coating and preparation method thereof |
| CN115784775A (en) * | 2022-12-02 | 2023-03-14 | 中国国检测试控股集团股份有限公司 | Zirconia and alumina gradient composite coating and preparation method thereof |
| CN115784775B (en) * | 2022-12-02 | 2024-02-20 | 中国国检测试控股集团股份有限公司 | Zirconia and alumina gradient composite coating and preparation method thereof |
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Application publication date: 20150617 |