CN113684460A - Preparation method of accident-resistant cladding Cr/CrN composite coating - Google Patents
Preparation method of accident-resistant cladding Cr/CrN composite coating Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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Abstract
The invention discloses a preparation method of an accident-resistant cladding Cr/CrN composite coating, and belongs to the technical field of functional material preparation. The invention utilizes the gradient reaction magnetron sputtering technology, firstly prepares a Cr layer on a Zr-4 substrate, the matching of two metals is good, the binding force is excellent, and then gradually increases N in a sputtering cabin2Content, first deposition of substoichiometric CrxNyAt the moment, both metal bonds and ion bonds exist in the coating, so that the bonding force is effectively enhanced, and finally N is in the sputtering chamber2When the content of the chromium oxide reaches a certain degree, all sputtered Cr target material particles can generate CrN, the deposition of the CrN on the outer layer is realized, and the obtained composite coating is ensured to haveThe high-temperature oxidation resistance and the wear resistance are better, and simultaneously, the binding force of the coating is greatly improved, and the application requirement of the coating can is met.
Description
Technical Field
The invention relates to a preparation method of an accident-resistant cladding Cr/CrN composite coating, belonging to the technical field of functional material preparation.
Background
At present, cladding of a nuclear reactor is mainly made of Zr alloy, but under the accident condition, the Zr alloy can react with high-temperature water vapor (Zr + 2H)2O＝ZrO2+2H2×) to produce hydrogen and can initiate the explosion, Zr alloy surface protective coating improves Zr alloy's corrosion-resistant, oxidation resistance when the accident takes place for nuclear reactor as one of the research direction of resistant accident cladding to preparation protective coating on current Zr alloy has and makes economic nature good, easily realizes advantages such as commercialization, is the important development direction of resistant accident fuel cladding.
Coating materials such as MAX phase, carbide, oxide, nitride, metallic coatings and composite coatings are currently being investigated to improve performance under accident conditions and normal conditions. Among them, metal Cr has the advantages of high temperature resistance, oxidation resistance, creep resistance, good matching property with Zr alloy, and the like, and is a candidate material of Zr alloy coating with development prospect. However, under normal working conditions, the temperature of the water side in the nuclear reactor reaches 400 ℃, and the hardness and the wear resistance of the metal Cr are reduced at high temperature. In the complex environment of a nuclear reactor, fretting occurs on the water side of the nuclear cladding and the Cr coating may be lost in high pressure flowing water. Therefore, it is necessary to find a material which not only has strong oxidation resistance and good compatibility with Cr coating, but also has strong wear resistance.
The hard nitride coating is widely applied to protection of mechanical parts such as cutters, engine parts and the like due to the advantages of high hardness, good wear resistance, high melting point, good chemical stability, low cost and the like. The excellent mechanical property and oxidation resistance are important basis for the CrN coating to be widely applied to Zr alloy cladding coating materials. However, the CrN coating is brittle due to the high hardness of the CrN coating as a ceramic material, and has poor matching property with Zr metal and low bonding force. In addition, the existing PVD (physical vapor deposition) technologies for preparing the CrN coating, such as magnetron sputtering, only adopt physical adsorption among coatings, are difficult to form bonds, so that the bonding force between the coating and a substrate is weak, and the coating is easy to fall off in a high-temperature environment or a long-time high-pressure water environment.
Therefore, it is necessary to provide a coating with strong oxidation resistance and wear resistance for the Zr alloy cladding.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art, and provides a method for preparing a Cr/CrN composite coating on a zirconium cladding, which improves the binding force between the composite coating and the zirconium cladding on the premise of ensuring better high-temperature oxidation resistance and wear resistance of the coating.
The technical scheme of the invention is as follows:
a preparation method of an accident-resistant cladding Cr/CrN composite coating comprises the following steps:
step 1, pretreatment of a substrate: polishing the oxide layers on the surface and the side surface of the substrate, and then carrying out ultrasonic cleaning treatment;
step 2, preparing a coating: carrying out magnetron sputtering treatment on the pretreated substrate, and plating a Cr/CrN composite coating on two sides of the substrate;
wherein the target material of magnetron sputtering is Cr target, and the sputtering gas is Ar and N2The composition of the mixed gas comprises 100 percent, 90 percent, 80 percent and 70 percent of Ar in the mixed gas in sequence during the magnetron sputtering process.
Further limiting, the polishing operation process in the step 1 is as follows: the wire-cut samples were ground using 100, 400, 1200 and 2000 mesh sandpaper in this order.
Further, the ultrasonic cleaning in step 1 is performed by the following steps: repeatedly ultrasonically cleaning for 3 times by sequentially using absolute ethyl alcohol and deionized water, and finally drying for 1h at 70 ℃.
Further limiting, the magnetron sputtering treatment conditions in the step 2 are as follows: the distance between the substrate and the Cr target is 10-30 cm, and the working air pressure is 5 multiplied by 10-4Pa～1×10-3Pa, magnetron sputtering power of 100W-250W, total gas flow rate of 10 sccm-30 sccm, sputtering gas pressure of 0.5 Pa-1 Pa, sample stage rotation speed of 10 r/min-50 r/min, and deposition timeIs 1-5 h.
Further limiting, the magnetron sputtering treatment conditions in step 2 are as follows: the distance between the substrate and the chromium target is 10cm, and the working air pressure is 5 multiplied by 10-4Pa, the magnetron sputtering power is 200W, the total gas flow rate is 20sccm, the sputtering gas pressure is 0.5Pa, the rotating speed of the sample stage is 20r/min, and the deposition time is 2 h.
Further limiting, starting from magnetron sputtering, for 0min to 30min, wherein the content of Ar in the mixed gas is 100 percent; 30-60 min, wherein Ar accounts for 90% of the mixed gas; 60-90 min, wherein Ar accounts for 80% of the mixed gas; 90-120 min, wherein Ar accounts for 70% of the mixed gas.
Further limited to a Cr target purity of 99.95% and a size of
Further limit, the purity of Ar of sputtering gas is 99.99 percent, and the purity of N of sputtering gas2The purity was 99.99%.
Further defined, the substrate is a Zr-4 alloy sheet material.
The invention has the following beneficial effects: the invention utilizes the gradient reaction magnetron sputtering technology, firstly prepares a Cr layer on a Zr-4 substrate, the matching of two metals is good, the binding force is excellent, and then gradually increases N in a sputtering cabin2Content, first deposition of substoichiometric CrxNyAt the moment, both metal bonds and ion bonds exist in the coating, so that the bonding force is effectively enhanced, and finally N is in the sputtering chamber2When the content of the Cr target material reaches a certain degree, all sputtered Cr target material particles generate CrN, the deposition of the CrN on the outer layer is realized, the obtained composite coating has better high-temperature oxidation resistance and wear resistance, simultaneously, the binding force of the coating is greatly improved, and the application requirement of the coating cladding is met. In addition, the present invention adopts a Cr target and a sputtering gas N2The CrN coating is prepared, so that a target does not need to be replaced in the sputtering process of the two coatings (Cr and CrN), the preparation method is simple, and the method is suitable for commercial application.
Drawings
FIG. 1 is a bar graph comparing the bonding force of the coatings obtained in example 1, comparative example 1 and comparative example 2;
FIG. 2 is a graph of the nano-scratches of the coating obtained in comparative example 1;
FIG. 3 is a graph of the nano-scratches of the coating obtained in example 1;
FIG. 4 is an AFM image of the coating obtained in example 1;
FIG. 5 is a photograph of a sample of a friction test piece and a SEM photograph of a wear area of a coating obtained in example 1 and comparative example 1, wherein a is a photograph of a sample of a friction test piece of a coating obtained in comparative example 1, b is a SEM photograph of a wear area of a coating obtained in comparative example 1, c is a photograph of a sample of a friction test piece of a coating obtained in example 1, and d is a SEM photograph of a wear area of a coating obtained in example 1;
FIG. 6 is a drawing of a sample after a high temperature oxidation test of a Zr-4 base alloy sheet and the coating obtained in example 1, wherein a is the Zr-4 base alloy sheet and b is the coating obtained in example 1;
FIG. 7 is a bar graph comparing weight gain after high temperature oxidation experiments for Zr-4 base alloy sheets and coatings obtained in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
Example 1:
first, pre-treatment of substrate
The plate-shaped Zr-4 alloy was warp-cut into a sheet-shaped substrate sample of 20X 1.4mm in size, and sanded with 100 mesh, 400 mesh, 1200 mesh and 2000 mesh sandpaper in this order. Then repeatedly ultrasonically cleaning for 3 times by sequentially using acetone, absolute ethyl alcohol and deionized water. Finally, the washed sample wafer is dried for 1h in a forced air drying oven with the temperature of 70 ℃.
Preparation of composite coating
(1) Vacuum pumping stage
The mechanical pump and the molecular pump are started to make the vacuum degree in the furnace chamber reach 5 multiplied by 10-4Pa；
(2) Coating deposition phase
And (4) putting the pretreated sample wafer into a deposition chamber of magnetron sputtering to prepare sputtering.
The parameters of sputtering were as follows: the target material of magnetron sputtering is Cr target, and the sputtering gas is Ar and N2The distance between the substrate and the chromium target is 10cm, the magnetron sputtering power is 200W, the total gas flow rate is 20sccm, the sputtering pressure is 0.5Pa, the rotating speed of the sample stage is 20r/min, and the deposition time is 2 h.
Starting sputtering, wherein Ar accounts for 100% in the mixed gas for 0-30 min; 30-60 min, wherein Ar accounts for 90% of the mixed gas; 60-90 min, wherein Ar accounts for 80% of the mixed gas; 90-120 min, wherein Ar accounts for 70% of the mixed gas.
The obtained coating is marked as Cr/CrN composite coating.
Comparative example 1:
this comparative example differs from example 1 in that: and starting sputtering for 0-120 min, wherein the content of Ar in the mixed gas is 100%. The remaining processing and steps are the same as in example 1. The obtained coating was denoted as Cr coating.
Comparative example 2:
this comparative example differs from example 1 in that: at the beginning of sputtering, 0 min-120 min, the proportion of Ar in the mixed gas is 70 percent, and the rest is N2. The remaining processing and steps are the same as in example 1. The coating obtained is denoted as CrN coating.
Example of effects:
(1) and (3) testing the binding force of the coating:
utilize nanometer mar appearance survey Cr/CrN composite coating, the cohesion of Cr coating and CrN coating, nanometer mar appearance passes through the automatic loading function, load 1 ~ 30N's load in succession to the diamond indenter, when the indenter transmits the load to the coating surface, remove the indenter, make the indenter pass the coating surface, the mar length sets up to 3mm, indenter moving speed sets up to 3mm/min, in order to reduce the error, every sample piece mar 3 times take the average value, the test result is as shown in fig. 1 ~ fig. 3. As can be seen from FIG. 1, the Cr/CrN composite coating obtained by controlling the gas flow rate ratio in a gradient manner during sputtering has a bonding force which is obviously higher than that of a CrN coating and slightly higher than that of a Cr coating. As shown in fig. 2, when CrN coating is directly deposited on the substrate, cracking occurs during scratching because the coating is only physically adsorbed to Zr-4 alloy and the coating is easily peeled off by external force. As shown in FIG. 3, the Cr/CrN composite coating has good bonding force, no obvious interface exists between coatings, and the bonding force of the coating is greatly improved compared with that of CrN.
(2) And (3) testing the wear resistance of the coating:
the wear resistance of the coating is measured by a friction resistance tester, the diameter of a grinding material is selected to be 6mm according to the size and the thickness of a film layer in the test process, the grinding material is a 316 stainless steel ball, load is applied in a weight loading mode, and the rotating speed of an objective table is controlled by adjusting the frequency of a motor. The AFM photo is shown in FIG. 4, the surface of the Cr/CrN composite coating has a uniform fine protrusion structure, the structure can provide a larger area physically adhered to CrN, normal locking of the Cr/CrN composite coating and the CrN is facilitated, and the bonding force of the Cr/CrN composite coating can be improved. A physical picture of the friction test sample and an SEM picture of a wear area are shown in FIG. 5. The test results are: the Cr coating is worn out of the substrate after 5 th cycle, and the Cr/CrN composite coating is worn out of the substrate after 11 th cycle, so that the wear resistance of the Cr/CrN composite coating is improved compared with that of the Cr coating.
(3) High temperature oxidation test:
the high temperature oxidation test utilizes a tube furnace to simulate the environment of the accident condition. Weighing a sample sheet to be tested, and then putting the sample sheet into a tubular furnace at room temperature, wherein the parameters of the tubular furnace are as follows: heating to 1000 deg.C within 60min, maintaining at 1000 deg.C for 30min, and naturally cooling. Weighing the sample piece after cooling for the second time, wherein the mass difference of the two times of weighing is the mass increased after oxidation, and the sample piece is used for evaluating the oxidation resistance of the coating, the test result is shown in figures 6-7, and the Zr-4 substrate alloy piece with the Cr/CrN composite coatingZrO with better protection on surface and periphery and no loose cracking2And the generated Cr/CrN composite coating has excellent oxidation resistance.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A preparation method of an accident-resistant cladding Cr/CrN composite coating is characterized by comprising the following steps:
step 1, pretreatment of a substrate: polishing the oxide layers on the surface and the side surface of the substrate, and then carrying out ultrasonic cleaning treatment;
step 2, preparing a coating: carrying out magnetron sputtering treatment on the pretreated substrate, and plating a Cr/CrN composite coating on two sides of the substrate;
wherein the target material of magnetron sputtering is Cr target, and the sputtering gas is Ar and N2The composition of the mixed gas comprises 100 percent, 90 percent, 80 percent and 70 percent of Ar in the mixed gas in sequence during the magnetron sputtering process.
2. The method for preparing the accident-resistant cladding Cr/CrN composite coating according to claim 1, wherein the grinding operation in the step 1 is as follows: the wire-cut samples were ground using 100, 400, 1200 and 2000 mesh sandpaper in this order.
3. The method for preparing the accident-resistant cladding Cr/CrN composite coating according to claim 1, wherein the ultrasonic cleaning in the step 1 comprises the following operation processes: repeatedly ultrasonically cleaning for 3 times by sequentially using acetone, anhydrous ethanol and deionized water, and finally drying for 1h at 70 ℃.
4. The method for preparing the accident-resistant cladding Cr/CrN composite coating according to claim 1, wherein the magnetron sputtering treatment conditions in the step 2 are as follows: base ofThe distance between the bottom and the Cr target is 10 cm-30 cm, and the working air pressure is 5 multiplied by 10-4Pa～1×10-3Pa, magnetron sputtering power of 100W-250W, total gas flow rate of 10 sccm-30 sccm, sputtering gas pressure of 0.5 Pa-1 Pa, sample stage rotation speed of 10 r/min-50 r/min, and deposition time of 1 h-5 h.
5. The method for preparing the accident-resistant cladding Cr/CrN composite coating according to claim 4, wherein the magnetron sputtering treatment conditions in the step 2 are as follows: the distance between the substrate and the chromium target is 10cm, and the working air pressure is 5 multiplied by 10-4Pa, the magnetron sputtering power is 200W, the total gas flow rate is 20sccm, the sputtering gas pressure is 0.5Pa, the rotating speed of the sample stage is 20r/min, and the deposition time is 2 h.
6. The method for preparing the accident-resistant cladding Cr/CrN composite coating according to claim 5, characterized in that, starting from magnetron sputtering, Ar accounts for 100% in the mixed gas for 0-30 min; 30-60 min, wherein Ar accounts for 90% of the mixed gas; 60-90 min, wherein Ar accounts for 80% of the mixed gas; 90-120 min, wherein Ar accounts for 70% of the mixed gas.
7. The method of claim 1, wherein the Cr target has a purity of 99.95% and a size of 99.95%
8. The method for preparing the accident-resistant cladding Cr/CrN composite coating according to claim 1, wherein the Ar purity of the sputtering gas is 99.99%, and the N purity of the sputtering gas2The purity was 99.99%.
9. The method of claim 1, wherein the substrate is a Zr-4 alloy sheet.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115044866A (en) * | 2022-05-16 | 2022-09-13 | 烟台大学 | Multilayer gradient structure coating and preparation method thereof |
| CN116516309A (en) * | 2023-05-10 | 2023-08-01 | 重庆文理学院 | Single-layer Cr-enriched N-doped coating on surface of zirconium alloy for nuclear and preparation method thereof |
| CN117721417A (en) * | 2023-12-18 | 2024-03-19 | 上海交通大学 | Super wear-resistant zirconium alloy cladding surface composite coating and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109972098A (en) * | 2019-05-05 | 2019-07-05 | 大连理工大学 | A kind of preparation method of cladding materials surface C rN thick coating |
| CN113088884A (en) * | 2021-03-09 | 2021-07-09 | 哈尔滨工业大学 | Method for preparing chromium coating with high-temperature oxidation resistance on zirconium cladding |
-
2021
- 2021-07-30 CN CN202110871783.0A patent/CN113684460A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109972098A (en) * | 2019-05-05 | 2019-07-05 | 大连理工大学 | A kind of preparation method of cladding materials surface C rN thick coating |
| CN113088884A (en) * | 2021-03-09 | 2021-07-09 | 哈尔滨工业大学 | Method for preparing chromium coating with high-temperature oxidation resistance on zirconium cladding |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115044866A (en) * | 2022-05-16 | 2022-09-13 | 烟台大学 | Multilayer gradient structure coating and preparation method thereof |
| CN115044866B (en) * | 2022-05-16 | 2024-04-26 | 烟台大学 | Multilayer gradient structure coating and preparation method thereof |
| CN116516309A (en) * | 2023-05-10 | 2023-08-01 | 重庆文理学院 | Single-layer Cr-enriched N-doped coating on surface of zirconium alloy for nuclear and preparation method thereof |
| CN117721417A (en) * | 2023-12-18 | 2024-03-19 | 上海交通大学 | Super wear-resistant zirconium alloy cladding surface composite coating and preparation method thereof |
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