CN101033539A - CrN/CrAlN protective coating capable of resisting high temperature corrosion in wide temperature range and preparing method - Google Patents
CrN/CrAlN protective coating capable of resisting high temperature corrosion in wide temperature range and preparing method Download PDFInfo
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- CN101033539A CN101033539A CN 200610045989 CN200610045989A CN101033539A CN 101033539 A CN101033539 A CN 101033539A CN 200610045989 CN200610045989 CN 200610045989 CN 200610045989 A CN200610045989 A CN 200610045989A CN 101033539 A CN101033539 A CN 101033539A
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Abstract
This invention relates to a CrN/CrAlN anti-hot corrosion protection coating in a wide temperature sphere and its preparation method, which applies a mode of DC reaction cosputter to Cr and Al targets to get a CrN/CrAlN coating, in which, the chip temperature is room temperature-300deg.C, Ar and N2 are controlled by mass flowmeter, the flow is 6-20SCCM and 6-20SCCM, the working air pressure is 0.1-0.8Pa, Al content in the coating is controlled by adjusting the power ratio of Cr and Al targets, and 0-150V base negative bias voltage is applied on the base to increase the binding force between the coating and the base, the inner layer of the coating is CrN, the outer is Cr-Al-N with grads distributed Al, and the coating forms a Cr2O3 film with solid solution Al after being oxidized in 800-900deg.C and forms Al oxidation film with rich Al over 1000deg.C and the CrN/CrAlN coating is very good at anti-hot corrosion from hot corrosion experiment.
Description
Technical field
The invention belongs to surface engineering technology, specifically be a kind of in wide temperature range the CrN/CrAlN protective coating and preparation method thereof of resistance to high temperature corrosion.
Background technology
Initial thought source of the present invention is in the notion of the resistance to high temperature corrosion smart coat that is proposed by Britain professor Nicholls the earliest.Promptly in the industrial high temperature corrosive environment, be coated with layer function and can make optimization response or adjustment to environment, so that single coating can have anti-broad variety corrosive ability in broad temperature range or different media in a quasi intelligent mode.Up to the present, the system that clearly is defined as smart coat comprises three classes.Document 1: professor Nicholls has proposed MCrAlY (M=Ni or Co+Ni) smart coat system with chemical ingredients gradient in the material world (Mater.World 4,19, (1996)), makes outer abundant rich Al by oozing Al; Before oozing Al, carry out pre-treatment and make the rich Cr in middle layer.More than 800 ℃, the outer Al that forms
2O
3Film, coating resistance to high temperature oxidation and the thermal etching of I type; At 600-800 ℃, outer shortage protectiveness, and rich Cr middle layer can form the Cr of the faster tool protectiveness of growth
2O
3Film, the oxidation of the anti-lesser temps of coating and the thermal etching of II type.Therefore, above-mentioned MCrAlY coating conforms, and perhaps generates Al
2O
3Film perhaps generates Cr
2O
3Film, thus optimum resistance to high temperature oxidation and molten salt hot corrosion performance is provided, be a kind of smart coat of composition distribution gradient.Document 2:17 fossil energy material nd Annual Meeting collection (17
ThAnnual Conference on Fossil Energy Materials, April 24,2003) in people such as doctor Tortorelli proposes is a kind of Mo-Mo
5SiB
2-Mo
3Si alloy coat system forms silicon oxide or boron silicide in oxidizing atmosphere, have oxidation-resistance; In high-sulfur gesture atmosphere, main formation has anti-sulfurized moly-sulfide.It is anti-oxidant anti-again sulfurized performance requriements that this kind coating can satisfy, and is adapted to such as in combustion of fossil fuel and the energy conversion system.Document 3: the Ir-Al ultrahigh-temperature coating of people's development such as Hosoda in the intermetallic compound (Intermetallics8,1081, (2000)), but form the oxide film Al of the multi-functional layered structure of self-healing during oxidation
2O
3+ Ir/Al
2O
3/ Ir/IrAl.Remove and generate Al
2O
3Outside anti-oxidant, the existence of Ir can be used as the most effective oxygen diffusion barrier.Though the diffusion barrier layer of the Ir oxygen in the coating forms in oxidising process automatically, coating does not experience a response environment and changes the process of reacting, and thinks the not proper smart coat of this kind coating.Integrate and see, point out that as professor Nicholls the smart coat of resistance to high temperature corrosion has been represented the development in future direction, but at present no matter from the system of research still from the degree of depth of research, only be in the starting stage that proposes notion and coating system design.
The Cr-Al-N coating system is a kind of ternary nitride coating that develops recently.Document 4: this coating system of report at high temperature has good high temperature oxidation resistance in surface and the coating technology (Surf.Coat.Technol.163-164,57 (2003)).Although to the high temperature oxidation behavior of Cr-Al-N coating system so that preliminary research to be arranged, also not with the Cr-Al-N coating of Al content distribution gradient report as high-temperature protection coating.
Summary of the invention
The object of the present invention is to provide a kind of in wide temperature range the CrN/CrAlN protective coating and the preparation method of resistance to high temperature corrosion, this preparation method is simple, the CrN/CrAlN protective coating of anti-broad variety high temperature corrosion in wide temperature range.
Technical scheme of the present invention is:
Adopt the CrN/CrAlN coating internal layer CrN of the method preparation of magnetron sputtering, and the CrN/CrAlN bilayer structure of outer Al content distribution gradient.And outer Al content x value variation range 0-0.82 is reaching maximum value (Cr near coatingsurface
0.18Al
0.82N).Coating internal layer thickness range is 5-20 μ m, and coating outer layer thickness scope is 5-10 μ m.
The preparation method of described CrN/CrAlN protective coating is to adopt Cr target, the two targets of Al target to spatter altogether, obtains the CrN/CrAlN coating of Al content distribution gradient by the power density of regulating Cr target, Al target.The power density of Cr target, Al target is respectively 1.5-4.2W/cm
2And 0-4.2W/cm
2The flow of nitrogen and argon gas adopts mass flowmeter control, and its flow is respectively 6-20SCCM and 6-20SCCM.Operating pressure is 0.1-0.8Pa, and substrate temperature is-300 ℃ of room temperatures (25 ℃), for the bonding force that improves coating and matrix applies certain matrix negative bias.
The weight purity of described Cr target, Al target is respectively 99.8% and 99.9%, described nitrogen and argon gas bulk purity 〉=99.99%, and the scope of described matrix negative bias is 0--150V.
Advantage of the present invention is:
1, coating has the excellent high-temperature barrier propterty.CrN/CrAlN coating surface when temperature is lower than oxidation in 1000 ℃ of air generates the Cr that solid solution has Al
2O
3Protective membrane can effectively protect low-temperature oxidation and thermal etching.When temperature is higher than 1000 ℃, because the outer rich Al of coating forms when oxidation and can form the Al that at high temperature has excellent protectiveness
2O
3Film.
2 and, when improving the alloy high-temp corrosion resistance, can also improve the mechanics of surface performance of alloy, be highly suitable for not only to need to improve high temperature corrosion property but also surperficial mechanical property had certain requirements and use on the material of industrial environment.Under normal conditions, this is that other kind high temperature corrosion protective coating is unapproachable.
3, technology is simple, and composition is regulated easily.Compare with MCrAlY (M=Ni or Co+Ni) coating system, it is simple in structure.Without the alloys target of melting heterogeneity, the power density that only needs to regulate two sputtering targets just can obtain the coating of Al content distribution gradient during Al content in regulating coating.
4, the present invention is in CrN/CrAlN protective coating anti-oxidant and anti-broad variety high temperature corrosion in wide temperature range of high-temperature alloy surface acquisition, and wide temperature range is 600-1100 ℃.
Description of drawings
The X-ray diffraction spectrum of Fig. 1 CrN/CrAlN coating.
Fig. 2 CrN/CrAlN coating has provided Ti at 800 ℃ constant temperature oxidation kinetics curve simultaneously for its protection effect is described
3Al base alloy and Cr
0.53Al
0.47The kinetic curve of N coating.
Fig. 3 CrN/CrAlN coating has provided Ti at 800 ℃ thermal etching kinetic curve simultaneously for its protection effect is described
3Al base alloy and Cr
0.53Al
0.47The kinetic curve of N coating.
Fig. 4 CrN/CrAlN coating has provided K38G alloy and Cr at 1000-1100 ℃ constant temperature kinetic curve simultaneously for its protection effect is described
0.63Al
0.37The kinetic curve of N coating.
Fig. 5 CrN/CrAlN coating has provided the kinetic curve of K38G alloy at 900 ℃ thermal etching kinetic curve simultaneously for its protection effect is described.
Embodiment
Below by embodiment in detail the present invention is described in detail.
To be of a size of 10 * 20 * 2mm through the surface sand-blasting pre-treatment
3Ti
3Al base alloy substrates is put vacuum coating film equipment into, and being evacuated to the base vacuum degree is 4 * 10
-4Behind the Pa substrate is heated to 300 ℃.Opening intake valve and charge into the nitrogen of 12SCCM and the argon gas of 8SCCM, regulate vacuum tightness to 0.5Pa by the folding degree of regulator plate valve, open the direct supply that is connected on the Cr target subsequently, is 4.2W/cm in power density
2The CrN layer of following sputter individual layer, the time is 5 hours, the CrN layer thickness is 8 μ m.Open the direct supply that is connected on the Al target then, spatter the Cr-Al-N layer altogether with the Cr target, the Cr-Al-N layer thickness is 8 μ m.The power density of Cr target, Al target occurs with following four kinds of matching forms in the process of sputter: 4.2/4.2,3.0/4.2,2.1/4.2,1.5/4.2.And the time of every kind of power density matching form sputter is respectively 1h, 2h, 4h, 6h.After the beginning sputter, give Ti
3Al base alloy substrates applies-the matrix negative bias of 50V.Through X-ray analysis is that coating has the CrN structure, as shown in Figure 1.High-temperature oxidation resistance to the coating that obtained is tested, and 800 ℃ of constant temperature oxidations are after 20 hours, and it is not obvious to increase weight, and the Ti of sample as a comparison
3Al base alloy then increases weight obviously, as shown in Figure 2.Under identical temperature, at 75% weight Na
2SO
4+ 25% weight K
2SO
4Carried out the thermal etching experiment in the fused salt, as shown in Figure 3, the CrN/CrAlN coating can significantly reduce Ti
3The thermal etching speed of Al base alloy.
To be of a size of 10 * 20 * 2mm through surface preparation
3The K38G alloy substrates put vacuum coating film equipment into, being evacuated to the base vacuum degree is 4 * 10
-4Behind the Pa substrate is heated to 250 ℃.Opening intake valve and charge into the nitrogen of 8SCCM and the argon gas of 12SCCM, regulate vacuum tightness to 0.2Pa by the folding degree of regulator plate valve, open the direct supply that is connected on the Cr target subsequently, is 2.1W/cm in power density
2The CrN layer of following sputter individual layer, the time is 10 hours, the CrN layer thickness is 16 μ m.Open the direct supply that is connected on the Al target then, spatter the Cr-Al-N layer altogether with the Cr target, the Cr-Al-N layer thickness is 10 μ m.The power density of Cr target, Al target occurs with following four kinds of matching forms in the process of sputter: 4.2/4.2,3.0/4.2,2.1/4.2,1.5/4.2.And the time of every kind of power density matching form sputter is respectively 1h, 3h, 5h, 7h.Corrosion experiment shows: this coating still has good antioxidant property when temperature is higher than 1000 ℃, as shown in Figure 4, and has good hot corrosion resistance simultaneously, as shown in Figure 5.
Comparative example 1
The power density of different with embodiment 1 is control Cr target and Al target is respectively 1.5W/cm
2And 4.2W/cm
2At Ti
3Al base alloy surface has prepared the Cr of individual layer
0.53Al
0.47The N coating, and carried out 800 ℃ constant temperature oxidation experiment and 800 ℃, 75% weight Na
2SO
4+ 25% weight K
2SO
4The thermal etching experiment of fused salt.As shown in Figure 3, Figure 4, though the Cr of individual layer
0.53Al
0.47The N coating at high temperature has the antioxidant property that is better than the CrN/CrAlN coating slightly, but its hot corrosion resistance is poorer than the CrN/CrAlN coating.
Comparative example 2
The power density of different with embodiment 2 is control Cr target and Al target is respectively 2.1W/cm
2And 4.2W/cm
2The Cr that has prepared individual layer at the K38G alloy surface
0.63Al
0.37The N coating, and carried out 1000-1100 ℃ constant temperature oxidation experiment and 900 ℃, 75% weight Na
2SO
4+ 25% weight K
2SO
4The thermal etching experiment of fused salt.As Fig. 4, shown in Figure 5, though the Cr of individual layer
0.63Al
0.37The N coating at high temperature has the antioxidant property suitable with the CrN/CrAlN coating, but its hot corrosion resistance is poorer than the CrN/CrAlN coating.
By embodiment 1, embodiment 2, comparative example 1, comparative example 2 as seen, the CrN/CrAlN coating not only has the Cr with high Al content
0.63Al
0.37N, Cr
0.53Al
0.47The high-temperature oxidation resistance that the N coating is suitable, and have the hot corrosion resistance that is better than above-mentioned two kinds of coatings.
Claims (5)
1, a kind of in wide temperature range the CrN/CrAlN protective coating of resistance to high temperature corrosion, it is characterized in that: described coating internal layer is CrN, and skin is the Cr-Al-N layer of Al content distribution gradient, and chemical formula is Cr
1-xAl
xN, wherein Al content x value variation range 0-0.82 changes in gradient, is reaching maximum value Cr near coatingsurface
0.18Al
0.82N.
2, according to the described CrN/CrAlN protective coating of claim 1, it is characterized in that: the internal layer thickness range is 5-20 μ m, and the outer layer thickness scope is 5-10 μ m.
3, according to the preparation method of the described CrN/CrAlN protective coating of claim 1, it is characterized in that: adopt Cr target, the Al target mode that two targets spatter altogether in nitrogen and argon gas mixed atmosphere to prepare the CrN/CrAlN coating, operating air pressure is 0.1-0.8Pa, the temperature of matrix is a room temperature-300 ℃, Al content in the coating applies the matrix negative bias to improve the adhesion property of coating and matrix by regulating the power ratio control of Cr target, Al target.
4, according to the preparation method of the described CrN/CrAlN protective coating of claim 3, it is characterized in that: described Cr target weight purity 〉=99.9%, the power density scope is 1.5-4.2W/cm
2Al target weight purity 〉=99%, the power density scope is 0-4.2W/cm
2
5, according to the preparation method of the described CrN/CrAlN protective coating of claim 3, it is characterized in that: the matrix negative bias scope that is applied is 0--150V.
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|---|---|---|---|
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|---|---|---|---|
| CNB2006100459893A CN100482855C (en) | 2006-03-08 | 2006-03-08 | CrN/CrAlN protective coating capable of resisting high temperature corrosion in wide temperature range and preparing method |
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|---|---|
| CN101033539A true CN101033539A (en) | 2007-09-12 |
| CN100482855C CN100482855C (en) | 2009-04-29 |
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| CN101824590A (en) * | 2010-04-29 | 2010-09-08 | 南昌航空大学 | Method for preparing Nb/NbCr2-based high-temperature alloy surface anti-oxidation composite coating |
| CN102400099A (en) * | 2011-11-04 | 2012-04-04 | 四川大学 | Technology for preparing nuclear fission reactor fuel clad surface CrAlSiN gradient coating |
| CN102534490A (en) * | 2010-12-31 | 2012-07-04 | 鸿富锦精密工业（深圳）有限公司 | Covering piece and preparation method thereof |
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| CN101824590A (en) * | 2010-04-29 | 2010-09-08 | 南昌航空大学 | Method for preparing Nb/NbCr2-based high-temperature alloy surface anti-oxidation composite coating |
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| CN102787300A (en) * | 2011-05-18 | 2012-11-21 | 中国核动力研究设计院 | Cr/CrAlN gradient coating technology of supercritical water-cooled reactor fuel can surface |
| CN102400099A (en) * | 2011-11-04 | 2012-04-04 | 四川大学 | Technology for preparing nuclear fission reactor fuel clad surface CrAlSiN gradient coating |
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| CN102676991A (en) * | 2012-06-13 | 2012-09-19 | 东莞理工学院 | Process for preparing superhard nanocomposite laminated coating by PVD (plating vacuum deposition) technology |
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| CN102766846B (en) * | 2012-07-18 | 2014-04-23 | 华南理工大学 | AN/Cr1-xAlxN/Cr30(Al, Y)70N hard gradient coating and its prepn |
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