CN103522627B - The composite coating on a kind of valve sealing element surface and preparation method thereof - Google Patents
The composite coating on a kind of valve sealing element surface and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of composite coating of valve sealing element surface, this coating is matrix with valve sealing element, be by matrix surface stack gradually from bottom to top arrangement Cr layer, by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition.Compared with the CrN coating of existing single structure, the present invention adopts the composite coating of multi-gradient to improve carrying abrasion-resistance and the decay resistance of coating.In addition, the present invention adopts multi sphere ion plating technology to prepare this composite coating, and to deposit successively at matrix surface obtain each layer by controlling argon flow amount, nitrogen flow and sedimentation time, preparation method is simple, batch production can be realized, have a good application prospect.
Description
Technical field
The invention belongs to component of machine surface strengthening treatment technology field, be specifically related to the composite coating on a kind of valve sealing element surface and preparation method thereof.
Background technology
Valve is widely used in the projects such as oil, chemical industry and power plant construction.Valve sealing element is a vitals of valve.In actual applications, require valve sealing element long service life, minimumly can ensure that (general 1 ~ 2 year) valve does not damage within a turn(a)round, run to ensure that whole system safety is normal.Such as, the valve sealing element for nuclear power station requires higher, must ensure safe operation more than 30 years; Some petrochemical pipe privileged sites is also very high to the requirement of valve sealing element, must ensure safety switch more than 100,000 times.
In addition, in use, its seal is in medium valve for a long time, is subject to the corrosion of medium and washes away, and also there is the friction and wear between the sealing pair under seal pressure effect, therefore working condition is quite harsh simultaneously.For improving the performances such as anticorrosive, the heat resistanceheat resistant of seal and anti scuffing, generally the process for treating surface such as built-up welding, thermal spraying is applied in valve sealing element.But the protective layer porosity obtained due to built-up welding and thermal spraying is higher, and corrosive medium easily runs through coating by pin hole and crackle etc. and causes the entirety of coating to be peeled off, and causes seal failure.
At present, the CrN coating utilizing PVD technology to prepare is the protective coating that wear parts mainly adopts.But, the easy corrosion in corrosive medium of traditional CrN coating with columnar crystal structure comes off, and coating fragility is larger, under contact stress effect, holiday (dimpling, Wei Keng, stress raiser etc.) place is easy to crack initiation, causes that coating is improper in early days peels off and the wear out failure that accelerates fatigue.Therefore, the single CrN coating of tradition be difficult to adapt to current and future high mechanical load and corrosive environment in the harsh operating mode Service Environment of valve sealing element and performance requirement, as the low friction under heavy duty, long-life and corrosion resistance etc.
Summary of the invention
Technical purpose of the present invention is the deficiency for above-mentioned existing valve sealing element face coat, and provide a kind of composite coating of valve sealing element surface, this composite coating has higher abrasion resistance properties and decay resistance.
For realizing above-mentioned technical purpose, the present invention adopts following technical scheme: a kind of composite coating of valve sealing element surface, and this coating take valve sealing element as matrix, as shown in Figure 1, this coating by matrix surface stack gradually from bottom to top arrangement Cr layer, by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition.
As preferably, the thickness of described complex gradient coating is 30 μm ~ 50 μm.
As preferably, the thickness of described Cr layer is 1um ~ 2um; Described Cr/Cr
2the thickness of N layer is 8um ~ 12um; Described Cr
2the thickness of N layer is 8um ~ 12um; Described Cr
2the thickness of N/CrN layer is 8um ~ 12um; Described Cr
2the thickness of N layer is 8um ~ 12um.
In order to improve the hardness of matrix, as preferably, first described matrix surface carries out glow discharge nitriding process.
Present invention also offers a kind of method preparing the composite coating on above-mentioned valve sealing element surface, the method adopts multi sphere ion plating technology, specifically comprises the steps:
Step 1, matrix surface is cleaned, oil removing, surface activation process;
As preferably, ultrasonic wave is utilized to carry out ultrasonic cleaning to matrix surface;
As preferably, described surface activation process is: matrix is placed in filming equipment vacuum cavity and utilizes argon plasma to the matrix surface bombardment activation applying back bias voltage.Further preferably, described vacuum cavity is evacuated to (3 ~ 6) × 10
-3pa, by substrate preheating to 400 DEG C ~ 450 DEG C, passes into work argon gas 100 ~ 350sccm, starts grid bias power supply, with-900 ~-1200V bias voltage bombardment matrix 10 minutes, matrix surface is activated;
Step 2, step 1 is processed after matrix be placed in filming equipment vacuum cavity, select Cr target, Cr target current is 50 ~ 100A, workpiece applies-20 ~-50V back bias voltage, controlling heating-up temperature is 400 DEG C ~ 450 DEG C, passing into argon gas and nitrogen, depositing Cr layer successively, by Cr and Cr by controlling argon flow amount, nitrogen flow and sedimentation time at matrix surface
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition, specific as follows:
(1) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 0sccm, deposits 1 hour ~ 2 hours, obtains Cr layer;
(2) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 20sccm ~ 30sccm, and sedimentation time is 8 hours ~ 12 hours, obtains by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer;
(3) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 45sccm ~ 50sccm, and sedimentation time is 8 hours ~ 12 hours, obtains Cr
2n layer;
(4) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 75sccm ~ 125sccm, and sedimentation time is 8 hours ~ 12 hours, obtains by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer;
(5) argon flow amount remains 0 ~ 100sccm, and nitrogen flow is 200sccm ~ 400sccm, and sedimentation time is 8 hours ~ 12 hours, obtains CrN layer;
As preferably, arrange two groups of Cr targets in described vacuum plant, often group is three Cr targets of upper, middle and lower positioned vertical;
As preferably, described nitrogen selects high-purity 99.95% nitrogen;
After step 3, deposition to be coated, be cooled to less than 220 DEG C under vacuum conditions, then under nitrogen protection atmosphere, be cooled to less than 100 DEG C, finally exit to atmospheric pressure, begin to speak to come out of the stove, namely obtain composite coating at matrix surface.
In order to improve the hardness of matrix self, for follow-up composite coating provides the matrix of high rigidity, as preferably, after described step 1, carrying out matrix surface glow discharge nitriding process, making matrix surface obtain the nitriding layer of high rigidity, then carry out step 2.Further preferably, this Nitrizing Treatment is specially: the matrix after step 1 being processed is placed in filming equipment vacuum cavity, passing into nitrogen flow is 1000 ~ 1200sccm, operating air pressure controls at 8 ~ 10Pa, matrix applies-800 ~-1000V back bias voltage, temperature controls at 450 ~ 500 DEG C, and the Nitrizing Treatment time is 2 ~ 4 hours.
In sum, the coated designs of valve sealing element matrix surface is the composite coating structure of multilayer component gradient change by the present invention, compared with the single CrN coating prepared, has following beneficial effect with existing PVD technology:
(1) adopt the coating structure of multi-gradient, by coating composition by Cr through Cr
2n, gradually to CrN transition, not only reduces the residual stress in coated grains size and lattice, improves the deposit thickness of film, thus significantly improves the carrying abrasion-resistance of coating; And define heterogeneous nanocrystalline and amorphous composite construction, interrupt single crystal orientation growth, effectively can prevent corrosive medium from running through coating and cause coating failure and peel off, improve the decay resistance of coating.
(2) in addition, the present invention adopts multi sphere ion plating technology to prepare this composite coating, to deposit successively obtain Cr layer, Cr/Cr by controlling argon flow amount, nitrogen flow and sedimentation time at matrix surface
2n layer, Cr
2n layer, Cr
2n/CrN layer, and CrN layer, compared with the single CrN coating prepared with existing PVD technology, this preparation method is simple, can realize batch production, can obtain the super thick gradient composite coating of wear-resistant, corrosion-resistant and anti-contact fatigue characteristic.As preferably, after combining with glow discharge nitriding technology, matrix hardness can be strengthened further, obtain the super thick gradient composite coating of high rigidity, wear-resistant, corrosion-resistant and anti-contact fatigue characteristic.
Therefore, composite coating of the present invention can meet the high performance requirements to valve sealing element under bad working environments condition, has a good application prospect in high accuracy aqueous vapor induction system equipment, petrochemical pipe and nuclear power plant equipment etc.
Accompanying drawing explanation
Fig. 1 is the composition structural representation of the composite coating on valve sealing element surface of the present invention;
Fig. 2 to Fig. 8 is the Cross Section Morphology of the coating 1-7 that the embodiment of the present invention 1 adopts different nitrogen flow to generate;
Fig. 9 is the XRD spectra of coating 1-7 obtained in the embodiment of the present invention 1;
Figure 10 (a) and Figure 10 (b) are the XPS spectrum figure of coating 1-7 obtained in the embodiment of the present invention 1;
Figure 11 is the TEM figure of composite coating obtained in the embodiment of the present invention 2.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.
Embodiment 1:
In the present embodiment, matrix selects valve 304 stainless steel spheroid or butterfly valve 316 stainless steel dish plate.Multiple matrix sample is cleaned, oil removal treatment, then multi sphere ion plating technology is utilized respectively at each matrix surface deposited coatings, in the deposition process of each sample, Cr target is selected in ion plating, the electric current of Cr target remains 50 ~ 100A, matrix applies-20 ~-50V back bias voltage, controls heating-up temperature and remain 400 DEG C ~ 450 DEG C in deposition process, the concrete sedimentary condition of different sample is as follows respectively.
(1) sample 1: argon flow amount remains 100sccm, nitrogen flow is 25sccm, and sedimentation time is 4 hours, obtains coating 1;
The Cross Section Morphology of this coating 1 as shown in Figure 2, can find out that the planar thickness of this coating is about 3.3um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer;
(2) sample 2: argon flow amount remains 100sccm, nitrogen flow is 50sccm, and sedimentation time is 4 hours, obtains coating 2;
The Cross Section Morphology of this coating 2 as shown in Figure 3, can find out that the planar thickness of this coating is about 3.75um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is by Cr
2the Cr that N is formed
2n layer;
(3) sample 3: argon flow amount remains 100sccm, nitrogen flow is 75sccm, and sedimentation time is 4 hours, obtains coating 3;
The Cross Section Morphology of this coating 3 as shown in Figure 4, can find out that the planar thickness of this coating is about 4.15um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is by Cr
2the CrN layer that N is formed;
(4) sample 4: argon flow amount remains 100sccm, nitrogen flow is 100sccm, and sedimentation time is 4 hours, obtains coating 4;
The Cross Section Morphology of this coating 4 as shown in Figure 5, can find out that the planar thickness of this coating is about 4.4um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer.
(5) sample 5: argon flow amount remains 100sccm, nitrogen flow is 125sccm, and sedimentation time is 4 hours, obtains coating 5;
The Cross Section Morphology of this coating 5 as shown in Figure 6, can find out that the planar thickness of this coating is about 4.66um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer.
(6) sample 6: argon flow amount remains 100sccm, nitrogen flow is 150sccm, and sedimentation time is 4 hours, obtains coating 6;
The Cross Section Morphology of this coating 6 as shown in Figure 7, can find out that the planar thickness of this coating is about 5.25um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer.
(7) sample 7: argon flow amount remains 100sccm, nitrogen flow is 200sccm, and sedimentation time is 4 hours, obtains coating 7;
The Cross Section Morphology of this coating 7 as shown in Figure 8, can find out that the planar thickness of this coating is about 4.2um, its surfacing.Generate the XRD spectra of coating under different nitrogen flows according to Fig. 3, this coating is the CrN layer formed by CrN.
The XPS spectrum figure of above-mentioned obtained coating 1-7, as shown in Figure 10 (a) Yu Figure 10 (b), can find out by adjustment argon flow amount and nitrogen flow, can generate the coating of heterogeneity.
Embodiment 2:
In the present embodiment, matrix part is valve 304 stainless steel spheroid, the composite coating of this matrix surface be by matrix surface stack gradually from bottom to top arrangement Cr layer, by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition.Wherein, the thickness of this composite coating is 30 μm ~ 50 μm.Wherein, the thickness of Cr layer is 0.3um ~ 1um; Cr/Cr
2the thickness of N layer is 5um ~ 10um; Cr
2the thickness of N/CrN layer is, the thickness of CrN layer is 5um ~ 8um.
Adopt glow discharge nitriding technology and multi sphere ion plating technology to prepare above-mentioned composite coating, concrete preparation process is as follows:
1, carry out blasting treatment to 304 stainless steel spheroids, the technological parameter of blasting treatment is: pressure 0.3MPa, and sand rain size is 320#, and sandblasting distance is 100mm; Then, by the ultrasonic cleaning 20 minutes in acetone soln of 304 stainless steel spheroids, proceed to sodium carbonate 30g/L after air-dry, in sodium phosphate 50g/L mixed solution, process 5 minutes, warm water ultrasonic cleaning at 60 DEG C, nitrogen is air-dry and dry at 80 DEG C; 304 stainless steels are placed in the vacuum chamber of glow discharge nitriding and multi-arc ion coating Integration Equipment, base vacuum is evacuated to 4 × 10 again
-3pa, by substrate preheating to 400 ~ 450 DEG C, utilizes argon plasma to the matrix surface bombardment activation applying back bias voltage, 350sccm flow passes into work argon gas, start grid bias power supply, seal each 2 minutes of enough parts with-900 ,-1100 and the bombardment of-1200V bias voltage respectively, matrix surface is activated.
2, the glow discharge nitriding of matrix surface:
Passing into nitrogen flow is 1200sccm, and operating air pressure controls at 10Pa, and matrix applies-800 ~-1000V back bias voltage, temperature controls at 500 DEG C, the Nitrizing Treatment time is 2-4 hour, obtains the nitriding layer of high rigidity, for follow-up thick coating provides the matrix of high rigidity after completing at matrix surface.
3, the coating CrN of matrix surface
xgradient coating:
Pass into argon gas and high-purity nitrogen (purity is 99.95%), at the compound CrN that matrix surface deposition 30 ~ 50 μm is thick
xgradient coating, in deposition process, ion plating Cr target current is 50 ~ 100A, and matrix applies-20 ~-50V back bias voltage, and controlling heating-up temperature during plated film is 400 DEG C, and concrete deposition process is as follows:
Specific as follows:
(1) argon flow amount remains 100sccm, and nitrogen flow is 0, deposits 1 hour, obtains Cr layer;
(2) argon flow amount remains 100sccm, and nitrogen flow is 25sccm, and sedimentation time is 8 hours, obtains by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer;
(3) argon flow amount remains 100sccm, and nitrogen flow is 50sccm, and sedimentation time is 8 hours, obtains Cr
2n layer;
(4) argon flow amount remains 100sccm, and nitrogen flow is 100sccm, and sedimentation time is 8 hours, obtains by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer;
(5) argon flow amount remains 100sccm, and nitrogen flow is 200sccm, and sedimentation time is 8 hours, obtains CrN layer.
4, after deposition to be coated is formed, be cooled to less than 220 DEG C under vacuum environment, be then filled with protective gas N
2, under protective atmosphere, be cooled to less than 100 DEG C, exit to atmospheric pressure, begin to speak to come out of the stove, finally obtain high rigidity, high abrasion at matrix surface, height is anti-corrosion and the super thick gradient CrN of anti-contact fatigue characteristic
xcomposite coating.
As shown in figure 11, the thickness of this coating is about 35-40um to the TEM figure of above-mentioned obtained composite coating.As can be seen from the figure, this coating be stack gradually from bottom to top from matrix surface arrangement Cr layer, by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition.That is, this coating be composition by Cr through Cr
2n is gradually to the multi-layer composite coatings of CrN gradual transition in gradient.
Just because of this gradient multi-layer compound structure, not only reduce the residual stress in single coating crystallite dimension and lattice, improve the deposit thickness of coating, thus significantly improve the carrying abrasion-resistance of coating; And define heterogeneous nanocrystalline and amorphous composite construction, interrupt single crystal orientation growth, effectively can prevent corrosive medium from running through coating and cause coating failure and peel off, improve the decay resistance of coating.
In addition, above-mentioned composite coating adopts multi sphere ion plating technology combine with nitridation technique and prepare, not only simple, and this can strengthen matrix hardness further, obtains the super thick gradient composite coating of high rigidity, wear-resistant, corrosion-resistant and anti-contact fatigue characteristic.
Embodiment 3:
In the present embodiment, matrix part is butterfly valve 316 stainless steel dish plate, the composite coating of this matrix surface be by matrix surface stack gradually from bottom to top arrangement Cr layer, by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition.Wherein, the thickness of this composite coating is 30 μm ~ 50 μm.Wherein, the thickness of Cr layer is 0.3um ~ 1um; Cr/Cr
2the thickness of N layer is 5um ~ 10um; Cr
2the thickness of N/CrN layer is, the thickness of CrN layer is 5um ~ 8um.
Adopt glow discharge nitriding technology and multi sphere ion plating technology to prepare above-mentioned composite coating, the step 1 in concrete preparation process and step 2 are identical with step 2 with the step 1 in embodiment 2 respectively, and step 3 is as follows with step 4:
3, argon gas and high-purity nitrogen (purity is 99.95%) is passed into, at the CrNx complex gradient coating that matrix surface deposition 30 ~ 50 μm is thick, in deposition process, ion plating Cr target current is 50 ~ 100A, matrix applies-20 ~-50V back bias voltage, controlling heating-up temperature during plated film is 400 DEG C, and concrete deposition process is as follows:
Specific as follows:
(1) argon flow amount remains 100sccm, and nitrogen flow is 0, deposits 2 hours, obtains Cr layer;
(2) argon flow amount remains 100sccm, and nitrogen flow is 25sccm, and sedimentation time is 12 hours, obtains by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer;
(3) argon flow amount remains 100sccm, and nitrogen flow is 50sccm, and sedimentation time is 12 hours, obtains Cr
2n layer;
(4) argon flow amount remains 100sccm, and nitrogen flow is 100sccm, and sedimentation time is 12 hours, obtains by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer;
(5) argon flow amount remains 100sccm, and nitrogen flow is 200sccm, and sedimentation time is 12 hours, obtains CrN layer.
4, after deposition to be coated is formed; less than 220 DEG C are cooled under vacuum environment; then protective gas N2 is filled with; less than 100 DEG C are cooled under protective atmosphere; venting is to atmospheric pressure; begin to speak to come out of the stove, finally obtain high rigidity, high abrasion at matrix surface, height is anti-corrosion and the super thick gradient CrNx composite coating of anti-contact fatigue characteristic.
The TEM of above-mentioned obtained composite coating schemes shown in similar Figure 11, and the thickness of this coating is about 35-45um.As can be seen from the figure, this coating be stack gradually from bottom to top from matrix surface arrangement Cr layer, by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition.That is, this coating be composition by Cr through Cr
2n is gradually to the multi-layer composite coatings of CrN gradual transition in gradient.
Just because of this gradient multi-layer compound structure, not only reduce the residual stress in single coating crystallite dimension and lattice, improve the deposit thickness of coating, thus significantly improve the carrying abrasion-resistance of coating; And define heterogeneous nanocrystalline and amorphous composite construction, interrupt single crystal orientation growth, effectively can prevent corrosive medium from running through coating and cause coating failure and peel off, improve the decay resistance of coating.
In addition, above-mentioned composite coating adopts multi sphere ion plating technology combine with nitridation technique and prepare, not only simple, and this can strengthen matrix hardness further, obtains the super thick gradient composite coating of high rigidity, wear-resistant, corrosion-resistant and anti-contact fatigue characteristic.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all make in spirit of the present invention any amendment, supplement or similar fashion substitute etc., all should be included within protection scope of the present invention.
Claims (7)
1. the composite coating on a valve sealing element surface, this coating take valve sealing element as matrix, it is characterized in that: the thickness of described composite coating is 30 μm ~ 50 μm, the thickness stacking gradually arrangement from bottom to top by matrix surface be 1um ~ 2um Cr layer, by Cr and Cr
2the thickness that N is mixed to form is the Cr/Cr of 8um ~ 12um
2n layer, thickness are the Cr of 8um ~ 12um
2n layer, by Cr
2the thickness that N and CrN is mixed to form is the Cr of 8um ~ 12um
2n/CrN layer, and CrN layer composition;
Adopt multi sphere ion plating technology to prepare the composite coating on described valve sealing element surface, specifically comprise the steps:
Step 1, matrix surface is cleaned, oil removing, surface activation process;
Step 2, step 1 is processed after matrix be placed in filming equipment vacuum cavity, select Cr target, Cr target current is 50 ~ 100A, workpiece applies-20 ~-50V back bias voltage, controlling heating-up temperature is 400 DEG C ~ 450 DEG C, passing into argon gas and nitrogen, depositing Cr layer successively, by Cr and Cr by controlling argon flow amount, nitrogen flow and sedimentation time at matrix surface
2the Cr/Cr that N is mixed to form
2n layer, Cr
2n layer, by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer, and CrN layer composition, specific as follows:
(1) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 0sccm, deposits 1 hour ~ 2 hours, obtains Cr layer;
(2) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 20sccm ~ 30sccm, and sedimentation time is 8 hours ~ 12 hours, obtains by Cr and Cr
2the Cr/Cr that N is mixed to form
2n layer;
(3) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 45sccm ~ 50sccm, and sedimentation time is 8 hours ~ 12 hours, obtains Cr
2n layer;
(4) argon flow amount remains 100sccm ~ 200sccm, and nitrogen flow is 75sccm ~ 125sccm, and sedimentation time is 8 hours ~ 12 hours, obtains by Cr
2the Cr that N and CrN is mixed to form
2n/CrN layer;
(5) argon flow amount remains 0 ~ 100sccm, and nitrogen flow is 200sccm ~ 400sccm, and sedimentation time is 8 hours ~ 12 hours, obtains CrN layer;
After step 3, deposition to be coated, be cooled to less than 220 DEG C under vacuum conditions, then under nitrogen protection atmosphere, be cooled to less than 100 DEG C, finally exit to atmospheric pressure, begin to speak to come out of the stove, namely obtain composite coating at matrix surface.
2. the composite coating on valve sealing element surface as claimed in claim 1, is characterized in that: described matrix is the matrix of surface through glow discharge nitriding process.
3. the composite coating on valve sealing element surface as claimed in claim 1, it is characterized in that: in described step 1, surface activation process is: matrix is placed in filming equipment vacuum cavity, by substrate preheating to 400 DEG C ~ 450 DEG C after vacuumizing, utilize argon plasma to the matrix surface bombardment activation applying back bias voltage.
4. the composite coating on the valve sealing element surface as described in claim 1 or 3, is characterized in that: after described step 1, carry out matrix surface glow discharge nitriding process, then carry out step 2.
5. the composite coating on valve sealing element surface as claimed in claim 4, it is characterized in that: described Nitrizing Treatment is specially: the matrix after step 1 being processed is placed in filming equipment vacuum cavity, passing into nitrogen flow is 1000 ~ 1200sccm, operating air pressure controls at 8 ~ 10Pa, matrix applies-800 ~-1000V back bias voltage, temperature controls at 450 ~ 500 DEG C, and the Nitrizing Treatment time is 2 ~ 4 hours.
6. the composite coating on the valve sealing element surface as described in claim 1 or 3, is characterized in that: arrange two groups of Cr targets in described vacuum plant, and often group is three Cr targets of upper, middle and lower positioned vertical.
7. the composite coating on the valve sealing element surface as described in claim 1 or 3, is characterized in that: described nitrogen selects high-purity 99.95% nitrogen.
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| CN116240512A (en) * | 2023-03-01 | 2023-06-09 | 纳狮新材料有限公司杭州分公司 | Spray cleaning of coating die head and preparation of CrxN lamination on surface of coating die head |
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| KR100295611B1 (en) * | 1996-07-10 | 2001-10-24 | 이구택 | Method for forming rigid film on surface of various metals |
| US20090324937A1 (en) * | 2008-06-30 | 2009-12-31 | Gm Global Technology Operations, Inc. | Layered coating and method for forming the same |
| CN203697597U (en) * | 2013-10-12 | 2014-07-09 | 中国科学院宁波材料技术与工程研究所 | Composite coating on surface of valve sealing element |
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| JP2598878B2 (en) * | 1993-11-12 | 1997-04-09 | 株式会社リケン | piston ring |
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|---|---|---|---|---|
| KR100295611B1 (en) * | 1996-07-10 | 2001-10-24 | 이구택 | Method for forming rigid film on surface of various metals |
| US20090324937A1 (en) * | 2008-06-30 | 2009-12-31 | Gm Global Technology Operations, Inc. | Layered coating and method for forming the same |
| CN203697597U (en) * | 2013-10-12 | 2014-07-09 | 中国科学院宁波材料技术与工程研究所 | Composite coating on surface of valve sealing element |
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