CN112281129A - Preparation process of Ni-Cr corrosion-resistant alloy coating on surface of sintered NdFeB magnet - Google Patents
Preparation process of Ni-Cr corrosion-resistant alloy coating on surface of sintered NdFeB magnet Download PDFInfo
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3471—Introduction of auxiliary energy into the plasma
- C23C14/3478—Introduction of auxiliary energy into the plasma using electrons, e.g. triode sputtering
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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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
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- 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
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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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
- C23C14/06—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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- 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
- C23C14/58—After-treatment
- C23C14/5826—Treatment with charged particles
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Abstract
The invention discloses a preparation process of a Ni-Cr corrosion-resistant alloy coating on the surface of a sintered NdFeB magnet, which comprises the following steps: performing surface pretreatment on the surface of the sintered NdFeB magnet by adopting a plasma etching technology; carrying out double-glow plasma Ni-Cr alloying treatment on the surface of the sintered NdFeB magnet to prepare a Ni-Cr alloy coating; the prepared Ni-Cr alloy coating is subjected to surface micro-nano structure construction by using a plasma etching technology. The Ni-Cr corrosion-resistant alloy coating on the surface of the sintered NdFeB magnet prepared by the invention has the advantages that the internal structure components are distributed in a gradient manner, the contents of Ni and Cr are gradually reduced from the outside to the inside, the interface of the Ni-Cr corrosion-resistant alloy coating and the matrix has a mutual diffusion phenomenon, the coating and the matrix are metallurgically combined, the bonding strength is high, the coating structure is compact, the main component is the nickel-based alloy, the corrosion resistance is good, and the longer corrosion protection can be provided for the sintered NdFeB magnet.
Description
Technical Field
The invention belongs to the field of surface protection and corrosion resistant coatings of magnetic materials, and particularly relates to a preparation process of a Ni-Cr corrosion resistant alloy coating on the surface of a sintered NdFeB magnet.
Background
As a third-generation rare earth permanent magnet material, the sintered NdFeB magnet has the characteristics of excellent coercive force, high remanence, high magnetic energy product and the like, is widely applied to high and new technical fields such as computer hard disks, nuclear magnetic resonance imaging, electric vehicles, wind power generation, magnetic machines, magnetic levitation and the like, and becomes an important basic functional material for the development of industrial science and technology at present. Sintered NdFeB magnets having mainly Nd2Fe14The B main crystal phase and the grain boundary Nd-rich phase are formed, but the Nd element has high chemical activity, and is easy to generate chemical reaction in corrosive media, so that the oxidation resistance and the corrosion resistance of the sintered NdFeB magnet are seriously influenced, and the application of the sintered NdFeB magnet is greatly limited. Therefore, the improvement of the corrosion resistance of the sintered NdFeB magnet has very important scientific significance and social value.
At present, in industrial production, a corrosion-resistant coating is prepared on the surface of a sintered NdFeB magnet mainly through a surface protection technology to improve the corrosion resistance of the sintered NdFeB magnet. In recent years, the surface protection technology of the sintered NdFeB magnet is commonly used in electroplating, electroless plating, organic coating, composite plating, physical vapor deposition, and the like. The slow light blue et al discloses a preparation method combining electroplating and chemical deposition, wherein a nickel-based super-hydrophobic coating is prepared on the surface of a sintered NdFeB magnet, and the corrosion resistance of a matrix is improved. Cao Yu Jie et al prepared a corrosion resistant coating composed of nano zirconia, nano aluminum powder and nano zinc powder on the surface of a sintered NdFeB magnet by using a plasma spraying technique. The Zhuminggang and the like prepare a layer of uniform and compact nano rare earth oxide/epoxy resin composite coating on the surface of the magnet through electrophoretic deposition, and obviously improve the corrosion resistance of the magnet. It should be noted, however, that there is a problem with poor adhesion between the coating and the substrate above. In high temperature or corrosive environment, peeling failure easily occurs, so that the corrosion-resistant coating loses the corrosion protection effect. Although zhanhao et al also discloses a preparation method of a sintered NdFeB coating with high corrosion resistance and high bonding force on the surface, an alloy welding layer is formed on the surface of a sintered NdFeB magnet through plasma arc powder overlaying, so as to improve the adhesion force of the corrosion-resistant coating, rapid heating and cooling treatment in the preparation process enables the internal stress of the corrosion-resistant coating to be larger, and the internal microcracks of the coating to be more.
The double glow plasma surface metallurgy technology is an original surface treatment technology in China, is an environment-friendly treatment technology and has no pollution. Compared with other surface treatment technologies, the internal components of the prepared coating are distributed in a gradient manner, and the coating is metallurgically bonded with a substrate, has high adhesion and good toughness and is not easy to peel off. At present, the double-glow plasma surface metallurgy technology is widely applied to the wear-resistant and corrosion-resistant surface modification of steel materials and titanium alloy materials, but the application to the surface modification of magnetic materials is hardly reported at home and abroad.
Disclosure of Invention
The invention provides a preparation process of a Ni-Cr corrosion-resistant alloy coating on the surface of a sintered NdFeB magnet, aiming at the problem of poor corrosion resistance of the sintered NdFeB magnet, and the Ni-Cr corrosion-resistant alloy coating on the surface of the sintered NdFeB magnet is developed by adopting a dual-glow plasma surface metallurgy technology, so that the sintered NdFeB magnet has high adhesive force and corrosion resistance, and greater economic benefit and social benefit are realized.
In order to achieve the above object, the present invention adopts the following technical solutions. A preparation process of a Ni-Cr corrosion-resistant alloy coating on the surface of a sintered NdFeB magnet comprises the following steps:
1) performing surface pretreatment on the surface of the sintered NdFeB magnet by adopting a plasma etching technology;
2) carrying out double-glow plasma Ni-Cr alloying treatment on the surface of the sintered NdFeB magnet to prepare a Ni-Cr alloy coating;
3) the prepared Ni-Cr alloy coating is subjected to surface micro-nano structure construction by using a plasma etching technology.
Further, the parameters of the plasma etching method in the step 1) are as follows: the voltage is 600V, the current is 1A, the argon pressure is 50 Pa, and the time is 0.5 h.
Further, the Ni-Cr alloy target material adopted in the step 2) comprises the following components in percentage by weight: the atomic percent of Ni in the Ni-Cr alloy target is 80 at percent, and the atomic ratio of Cr in the Ni-Cr alloy target is 20 at percent.
Further, the step of the biglow plasma Ni-Cr alloying treatment is as follows:
(b1) placing the sintered NdFeB magnet and the Ni-Cr alloy target material into a dual-glow plasma surface treatment furnace, wherein the sintered NdFeB magnet is used as a workpiece pole, and the Ni-Cr alloy target material is used as a source electrode;
(b2) vacuum pumping is carried out until the background vacuum degree is 10-3Pa, feeding argon;
(b3) starting a workpiece electrode and a source electrode power supply to perform Ni-Cr alloying treatment, wherein the preparation process of the Ni-Cr alloy coating comprises the following steps: the source voltage is 850-950V; the electrode voltage of the workpiece is 500-600V; the pressure of argon is 20-50 Pa; the distance between the source electrode and the workpiece is 15-25 mm; the treatment time was 3 h.
Further, the parameters of the plasma etching technology in the step 3) are as follows: the voltage is 500V, the current is 0.8A, the argon pressure is 20 Pa, and the time is 0.5 h.
The Ni-Cr corrosion-resistant alloy coating on the surface of the sintered NdFeB magnet prepared by the invention has the advantages that the internal structure components are distributed in a gradient manner, the contents of Ni and Cr are gradually reduced from the outside to the inside, the interface of the Ni-Cr corrosion-resistant alloy coating and the matrix has a mutual diffusion phenomenon, the coating and the matrix are metallurgically combined, the bonding strength is high, the coating structure is compact, the main component is the nickel-based alloy, the corrosion resistance is good, and the longer corrosion protection can be provided for the sintered NdFeB magnet.
Drawings
FIG. 1 is a sectional view of Ni-Cr corrosion-resistant alloy coating on the surface of a sintered NdFeB magnet according to the present invention;
FIG. 2 is a sectional EDS composition distribution diagram of the Ni-Cr corrosion-resistant alloy coating on the surface of the sintered NdFeB magnet according to the invention;
FIG. 3 is a graph of open circuit potential versus time for a Ni-Cr corrosion resistant alloy coating on the surface of a sintered NdFeB magnet in accordance with the present invention;
wherein: electrolyte solution: 3.5% NaCl solution;
FIG. 4 is a Tafel plot of the Ni-Cr corrosion resistant alloy coating on the surface of a sintered NdFeB magnet according to the present invention;
wherein: electrolyte solution: 3.5% NaCl solution; scanning rate: 2 mV/s.
Detailed Description
The invention is further illustrated by the following figures and examples.
Example 1:
a preferred preparation method of the invention is as follows:
(1) 4 pieces of Ni-Cr alloy plates are adopted to form a grid-shaped target material, the size of the Ni-Cr alloy plate is 80 mm multiplied by 20 mm multiplied by 5 mm, the distance between every two Ni-Cr alloy plates is 10 mm, and the adopted Ni-Cr alloy target material comprises the following components in percentage by weight: the atomic percent of Ni in the Ni-Cr alloy target is 80 at percent, and the atomic ratio of Cr in the Ni-Cr alloy target is 20 at percent.
(2) The substrate material was a sintered NdFeB magnet having dimensions of 15 mm × 15 mm × 5 mm. Before surface treatment, 0#, 1#, 3#, 4# and 5# metallographic abrasive paper are used for grinding in sequence, then diamond grinding paste with the granularity of 2.5 mu m is used for polishing, and then acetone solution is used for ultrasonic cleaning, and drying is carried out for later use.
(3) The surface of the sintered NdFeB magnet is cleaned by adopting a plasma etching method, and the process parameters are as follows: the voltage is 600V, the current is 1A, the argon pressure is 50 Pa, and the time is 0.5 h.
(4) By utilizing a dual-glow plasma surface metallurgy technology, a Ni-Cr alloy target material is used as a source electrode, a sintered NdFeB magnet is used as a workpiece electrode, Ni-Cr alloying treatment is carried out on the surface of the sintered NdFeB magnet, and a Ni-Cr corrosion-resistant alloy coating is prepared on the surface of the sintered NdFeB magnet. The preparation process parameters of the Ni-Cr alloy coating are as follows: the source voltage is 900V; the electrode voltage of the workpiece is 600V; the argon pressure is 20 Pa; the distance between the source electrode and the workpiece is 15 mm; the treatment time was 3 h.
(5) Adopting a plasma etching method to construct a micro-nano structure on the surface of the Ni-Cr corrosion-resistant alloy coating, wherein the process parameters are as follows: the voltage is 500V, the current is 0.8A, the argon pressure is 20 Pa, and the time is 0.5 h.
FIG. 1 is the cross-sectional shape of the prepared Ni-Cr corrosion resistant alloy coating, from which it can be seen that the Ni-Cr alloy coating has a dense structure and is well combined with the substrate.
FIG. 2 shows the EDS component distribution of the cross section of the prepared Ni-Cr corrosion-resistant alloy coating, and it can be seen from the EDS component distribution that Ni and Cr alloy elements are distributed in a gradient manner in the coating, the content of the Ni and Cr alloy elements is gradually reduced from the outside to the inside, and the content of the Fe element is gradually increased, which shows that the Ni-Cr corrosion-resistant alloy coating is metallurgically bonded with a sintered NdFeB substrate.
The Ni-Cr corrosion-resistant alloy coating prepared by the method is subjected to electrochemical corrosion resistance test in a standard three-electrode system, a working electrode is the porous high-entropy alloy prepared by the method, a reference electrode is a saturated calomel electrode, and a counter electrode is a Pt electrode.
Fig. 3 is an open circuit potential-time curve of the Ni-Cr corrosion-resistant alloy coating and the sintered NdFeB magnet, and it can be seen that the open circuit potential of the sintered NdFeB magnet after the Ni-Cr alloying treatment on the surface of the double glow plasma is significantly shifted forward, indicating that the Ni-Cr corrosion-resistant alloy coating on the surface of the sintered NdFeB magnet is more difficult to corrode than the substrate.
Fig. 4 is a Tafel curve of the Ni-Cr corrosion-resistant alloy coating and the sintered NdFeB magnet, and it can be seen that the Ni-Cr corrosion-resistant alloy coating has a higher corrosion potential and a lower corrosion circuit density, indicating that the Ni-Cr corrosion-resistant alloy coating has good corrosion resistance.
Example 2:
the preparation method of the invention is further preferably as follows:
(1) the Ni-Cr alloy target with the diameter of 100 mm is adopted, and the adopted Ni-Cr alloy target comprises the following components in percentage by weight: the atomic percent of Ni in the Ni-Cr alloy target is 80 at percent, and the atomic ratio of Cr in the Ni-Cr alloy target is 20 at percent.
(2) The substrate material was a sintered NdFeB magnet having dimensions of 15 mm × 15 mm × 5 mm. Before surface treatment, 0#, 1#, 3#, 4# and 5# metallographic abrasive paper are used for grinding in sequence, then diamond grinding paste with the granularity of 2.5 mu m is used for polishing, and then acetone solution is used for ultrasonic cleaning, and drying is carried out for later use.
(3) The surface of the sintered NdFeB magnet is cleaned by adopting a plasma etching method, and the process parameters are as follows: the voltage is 600V, the current is 1A, the argon pressure is 50 Pa, and the time is 0.5 h.
(4) By utilizing a dual-glow plasma surface metallurgy technology, a Ni-Cr alloy target material is used as a source electrode, a sintered NdFeB magnet is used as a workpiece electrode, Ni-Cr alloying treatment is carried out on the surface of the sintered NdFeB magnet, and a Ni-Cr corrosion-resistant alloy coating is prepared on the surface of the sintered NdFeB magnet. The preparation process parameters of the Ni-Cr alloy coating are as follows: the source voltage is 950V; the electrode voltage of a workpiece is 650V; the argon pressure is 20 Pa; the distance between the source electrode and the workpiece is 20 mm; the treatment time was 3 h.
(5) Adopting a plasma etching method to construct a micro-nano structure on the surface of the Ni-Cr corrosion-resistant alloy coating, wherein the process parameters are as follows: the voltage is 500V, the current is 0.8A, the argon pressure is 20 Pa, and the time is 0.5 h.
Example 3:
the invention also discloses a preparation method which comprises the following steps:
(1) 4 pieces of Ni-Cr alloy plates are adopted to form a grid-shaped target material, the size of the Ni-Cr alloy plate is 80 mm multiplied by 20 mm multiplied by 5 mm, the distance between every two Ni-Cr alloy plates is 10 mm, and the adopted Ni-Cr alloy target material comprises the following components in percentage by weight: the atomic percent of Ni in the Ni-Cr alloy target is 80 at percent, and the atomic ratio of Cr in the Ni-Cr alloy target is 20 at percent.
(2) The substrate material was a sintered NdFeB magnet having dimensions of 15 mm × 15 mm × 5 mm. Before surface treatment, 0#, 1#, 3#, 4# and 5# metallographic abrasive paper are used for grinding in sequence, then diamond grinding paste with the granularity of 2.5 mu m is used for polishing, and then acetone solution is used for ultrasonic cleaning, and drying is carried out for later use.
(3) The surface of the sintered NdFeB magnet is cleaned by adopting a plasma etching method, and the process parameters are as follows: the voltage is 600V, the current is 1A, the argon pressure is 50 Pa, and the time is 0.5 h.
(4) By utilizing a dual-glow plasma surface metallurgy technology, a Ni-Cr alloy target material is used as a source electrode, a sintered NdFeB magnet is used as a workpiece electrode, Ni-Cr alloying treatment is carried out on the surface of the sintered NdFeB magnet, and a Ni-Cr corrosion-resistant alloy coating is prepared on the surface of the sintered NdFeB magnet. The preparation process parameters of the Ni-Cr alloy coating are as follows: the source voltage is 850-950V; the electrode voltage of the workpiece is 500-600V; the argon pressure is 50 Pa; the distance between the source electrode and the workpiece is 20 mm; the treatment time was 3 h.
(5) Adopting a plasma etching method to construct a micro-nano structure on the surface of the Ni-Cr corrosion-resistant alloy coating, wherein the process parameters are as follows: the voltage is 500V, the current is 0.8A, the argon pressure is 20 Pa, and the time is 0.5 h.
Claims (5)
1. A preparation process of a Ni-Cr corrosion-resistant alloy coating on the surface of a sintered NdFeB magnet is characterized by comprising the following steps of:
1) performing surface pretreatment on the surface of the sintered NdFeB magnet by adopting a plasma etching technology;
2) carrying out double-glow plasma Ni-Cr alloying treatment on the surface of the sintered NdFeB magnet to prepare a Ni-Cr alloy coating;
3) the prepared Ni-Cr alloy coating is subjected to surface micro-nano structure construction by using a plasma etching technology.
2. The method for sintering the Ni-Cr corrosion-resistant alloy coating on the surface of the magnet according to claim 1, wherein the parameters of the plasma etching method in the step 1) are as follows: the voltage is 600V, the current is 1A, the argon pressure is 50 Pa, and the time is 0.5 h.
3. The method for sintering the Ni-Cr corrosion-resistant alloy coating on the surface of the magnet according to claim 1, wherein the Ni-Cr alloy target material adopted in the step 2) comprises the following components in percentage by weight: the atomic percent of Ni in the Ni-Cr alloy target is 80 at percent, and the atomic ratio of Cr in the Ni-Cr alloy target is 20 at percent.
4. The method for sintering Ni-Cr corrosion resistant alloy coating on the surface of magnet according to claim 1, wherein the step of the bi-glow plasma Ni-Cr alloying treatment is as follows:
(b1) placing the sintered NdFeB magnet and the Ni-Cr alloy target material into a dual-glow plasma surface treatment furnace, wherein the sintered NdFeB magnet is used as a workpiece pole, and the Ni-Cr alloy target material is used as a source electrode;
(b2) vacuum pumping is carried out until the background vacuum degree is 10-3Pa, feeding argon;
(b3) starting a workpiece electrode and a source electrode power supply to perform Ni-Cr alloying treatment, wherein the preparation process of the Ni-Cr alloy coating comprises the following steps: the source voltage is 850-950V; the electrode voltage of the workpiece is 500-600V; the pressure of argon is 20-50 Pa; the distance between the source electrode and the workpiece is 15-25 mm; the treatment time was 3 h.
5. The method for sintering the Ni-Cr corrosion-resistant alloy coating on the surface of the magnet according to claim 1, wherein the parameters of the plasma etching technique in the step 3) are as follows: the voltage is 500V, the current is 0.8A, the argon pressure is 20 Pa, and the time is 0.5 h.
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CN114150271A (en) * | 2021-12-08 | 2022-03-08 | 西北有色金属研究院 | NiCr anti-oxidation coating for stainless steel container of space nuclear reactor and preparation method thereof |
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Cited By (1)
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CN114150271A (en) * | 2021-12-08 | 2022-03-08 | 西北有色金属研究院 | NiCr anti-oxidation coating for stainless steel container of space nuclear reactor and preparation method thereof |
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