CN110818421A - Preparation method of compact composite coating based on reactive plasma spraying and laser remelting - Google Patents

Preparation method of compact composite coating based on reactive plasma spraying and laser remelting Download PDF

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CN110818421A
CN110818421A CN201911286393.6A CN201911286393A CN110818421A CN 110818421 A CN110818421 A CN 110818421A CN 201911286393 A CN201911286393 A CN 201911286393A CN 110818421 A CN110818421 A CN 110818421A
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powder
spraying
laser
laser remelting
coating
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马宝霞
徐敦昊
王阳
李金有
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Harbin University of Science and Technology
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Harbin University of Science and Technology
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Abstract

A preparation method of a compact composite coating based on reactive plasma spraying and laser remelting relates to a surface treatment method, in particular to a preparation method of a compact composite coating based on reactive plasma spraying and laser remelting. The method aims to solve the problem of compactness of the in-situ endogenous coating prepared by the existing reactive plasma spraying method. The method comprises the following steps: firstly, mixing the powder, deionized water, ammonium citrate and Arabic gum to obtain slurry, and performing spray granulation on the slurry to obtain mixed spraying powder; secondly, carrying out sand blasting treatment on the surface of the matrix, cleaning and drying; thirdly, the mixed spraying powder is filled into a plasma spray gun and sprayed on the substrate obtained in the second step to obtain a coating; and fourthly, mounting the coating test piece on a workbench of laser equipment for laser remelting. The method can improve the microscopic morphology of the coating, form a uniform and compact laser remelting layer and effectively improve the quality of the coating. The invention is applied to the field of surface pretreatment.

Description

Preparation method of compact composite coating based on reactive plasma spraying and laser remelting
Technical Field
The invention relates to a surface treatment method, in particular to compact ZrB based on reactive plasma spraying and laser remelting2A preparation method of the-SiC-ZrC composite coating.
Background
Zirconium carbide ceramic (ZrC) is one of the most promising high temperature structural candidates due to its ultra-high melting point and hardness, as well as good thermal and electrical conductivity. However, a major problem limiting its engineering applications is its low high temperature oxidation resistance.
ZrB as a typical ultra high temperature ceramic2the-SiC composite ceramic shows excellent oxidation ablation resistance in a long-time loading process with oxyacetylene flame, electric arc or plasma arc as a heat source, and is a promising material in a high-temperature protective coating. In 1998, the American space agency Emms research center is on ZrB2ZrB is prepared by in-situ reaction on the basis of-SiC material2-ZrC-SiC ternary composite ceramics, increasing the oxidation resistance to higher temperatures (2200 ℃).
The Reactive Plasma Spray (RPS) technology for preparing the in-situ endogenetic coating on the surfaces of metals such as aluminum, magnesium, steel and the like and C/C materials has the advantages of high forming speed, no limitation of spraying materials and capability of forming a high-melting-point material coating, so the technology has better application prospect. Currently, the main obstacles limiting the application of reactive plasma spray technology are the typical layered structure of the coating, the porosity and the mechanical bonding of the coating to the substrate. The lack of compactness of such spray coatings may result in cracking or spalling in relatively large pieces when applied in harsh environments such as high bending stress, high temperature and cyclic fatigue.
Disclosure of Invention
The invention aims to solve the problem of compactness of an in-situ endogenous coating prepared by using a conventional reactive plasma spraying method, and provides a preparation method of a compact composite coating based on reactive plasma spraying and laser remelting. The method can obtain a coating with high compactness and high hardness, thereby promoting the application of the coating in high-temperature environment.
The invention relates to a preparation method of a compact composite coating based on reactive plasma spraying and laser remelting, which comprises the following steps:
step one, preparing spraying powder:
ball-milling and mixing the powder, deionized water, ammonium citrate and Arabic gum to obtain slurry, and performing spray granulation on the slurry to obtain mixed spraying powder; the powder comprises zirconium powder (Zr) and boron carbide powder (B)4C) And silicon powder (Si);
step two, pretreatment of the base material:
carrying out sand blasting treatment on the surface of the ZrC-SiC matrix, then carrying out ultrasonic cleaning on the ZrC-SiC matrix, and drying to obtain a pretreated ZrC-SiC matrix;
step three, preparing the coating by adopting an RPS technology:
loading the mixed spraying powder obtained in the step one into a plasma spray gun, and spraying the mixed spraying powder on the pretreated ZrC-SiC matrix obtained in the step two to obtain ZrB2-a SiC-ZrC coating;
step four, remelting ZrB by laser2-SiC-based coating:
ZrB prepared in the third step2The SiC-ZrC coating test piece is arranged on a workbench of laser equipment for laser remelting, and the laser remelting process parameters are as follows: the laser power is 0.25-1 kw, the scanning speed is 10-50 mm/S, and the spot size phi is 1-4 mm.
Further, the molar ratio of zirconium powder, boron carbide powder and silicon powder in the first step is 1:0.456: 0.368.
furthermore, in the first step, the mass ratio of the powder material, the deionized water, the ammonium citrate and the Arabic gum is 1 (1.5-2) to 0.4-0.8 to 1-2.
Further, the rotation speed of ball milling mixing in the step one is 300-400 r/min, and the ball milling mixing time is 8-16 hours.
Furthermore, the sand adopted in the sand blasting treatment in the step two is corundum sand.
Further, in the third step, the spraying current is 400-650A.
Further, in the third step, the spraying distance is 70-150 mm.
Further, in the third step, the ion gas is argon (Ar)2) And hydrogen (H)2) Wherein the gas flow of the argon is 35L/min, and the gas flow of the hydrogen is 12L/min.
Further, the flow rate of the powder feeding argon gas sprayed in the third step is 2.5L/min.
And further, in the fourth step, argon is used for blowing along the laser processing direction in the laser remelting process to protect the test piece.
The invention has the beneficial effects that:
1. the invention is a preparation method based on the combination of a reactive plasma technology and a laser remelting technology, wherein the laser remelting is a process of quickly melting and then quickly solidifying the surface of a material by utilizing a high-energy laser beam, most of pores and unfused solid particles on the surface of a coating can be eliminated, the micro-morphology of the coating is improved, a uniform and compact laser remelting layer is formed, and the quality of the coating is effectively improved. ZrB with compact structure, low porosity and good interface bonding can be prepared on the surface of a ZrC-SiC ceramic substrate2-SiC-ZrC coating. Compared with the coating prepared by reactive plasma spraying, ZrB is subjected to laser remelting treatment2The hardness of the-SiC-ZrC coating is improved by 1.2-1.4 times.
2. ZrB is easily caused in the reactive plasma spraying process2The reaction synthesis of the-SiC-ZrC ceramic coating is incomplete, and the secondary heating of laser is utilized to ensure that the reaction in the coating is thorough and complete conversion of reactants is completed.
3. The invention selects ZrC-SiC ceramic as a matrix, ZrB2The thermal expansion coefficient of the-SiC-ZrC ceramic coating is similar to that of the ZrC-SiC matrix, so that the stress caused by thermal mismatch between the coating and the matrix due to thermal impact during laser remelting can be reduced, and the cracking tendency of the coating during laser remelting can be reduced.
4. Reactive plasma spraying involves complex high temperature, rapid, nonlinear, unsteady heat transfer, mass transfer, drive (energy, mass, and momentum transfer), chemical composition, and crystal structure can be in a non-equilibrium state. The laser remelting treatment can improve the structural temperature characteristic of the coating and obtain a stable structure.
Drawings
FIG. 1 shows ZrB before and after laser remelting in example 1 of the present invention2XRD pattern of SiC-ZrC coating.
FIG. 2 shows ZrB prepared by the RPS method before laser remelting in example 1 of the present invention2-microscopic morphology of the surface of the SiC-ZrC coating.
FIG. 3 shows ZrB after laser remelting in example 1 of the present invention2-microscopic morphology of the surface of the SiC-ZrC coating.
FIG. 4 shows ZrB after laser remelting in EXAMPLE 2 of the present invention2-microscopic morphology of the surface of the SiC-ZrC coating.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the compact composite coating based on reactive plasma spraying and laser remelting comprises the following steps:
step one, preparing spraying powder:
ball-milling and mixing the powder, deionized water, ammonium citrate and Arabic gum to obtain slurry, and performing spray granulation on the slurry to obtain mixed spraying powder; the powder comprises zirconium powder (Zr) and boron carbide powder (B)4C) And silicon powder (Si);
step two, pretreatment of the base material:
carrying out sand blasting treatment on the surface of the ZrC-SiC matrix, then cleaning the ZrC-SiC matrix in an ultrasonic cleaner by using absolute ethyl alcohol, and drying to obtain a pretreated ZrC-SiC matrix;
the ZrC-SiC matrix is prepared by a hot pressing sintering method: mixing ZrC powder and SiC powder by ball milling, and performing vacuum hot pressing sintering to prepare the SiC powder;
step three, preparing the coating by adopting an RPS technology:
mixing the spraying powder obtained in the step onePutting the powder into a plasma spray gun, and spraying the powder on the pretreated ZrC-SiC matrix obtained in the step two to obtain ZrB2-a SiC-ZrC coating;
step four, remelting ZrB by laser2-SiC-based coating:
ZrB prepared in the third step2The SiC-ZrC coating test piece is installed on a workbench of laser equipment for laser remelting, the model of the laser equipment is TruDisk 6002, and the laser remelting process parameters are as follows: the laser power is 0.25-1 kw, the scanning speed is 10-50 mm/S, and the spot size phi is 1-4 mm.
The embodiment combines the reactive plasma technology and the laser remelting technology, the laser remelting is a process of quickly melting the surface of a material by using a high-energy laser beam and then quickly solidifying, most of pores and unfused solid particles on the surface of a coating can be eliminated, the micro-morphology of the coating is improved, a uniform and compact laser remelting layer is formed, and the quality of the coating is effectively improved. ZrB with compact structure, low porosity and good interface bonding can be prepared on the surface of a ZrC-SiC ceramic substrate2-SiC-ZrC coating.
During reactive plasma spraying, some flying powder particles enter a low-temperature region at the edge of plasma arc flow, the powder can be in a partially reacted or unreacted state without obtaining enough heat, and complete conversion of products, namely ZrB is not completed2Reaction synthesis of-SiC-ZrC ceramic coating. The secondary heating of the laser is utilized, so that the reaction in the coating is incomplete and thorough, and the conversion of reactants is completed.
ZrC-SiC ceramic is selected as a matrix, ZrB2The thermal expansion coefficient of the-SiC-ZrC ceramic coating is similar to that of the ZrC-SiC matrix, so that the stress caused by thermal mismatch between the coating and the matrix due to thermal impact during laser remelting can be reduced, and the cracking tendency of the coating during laser remelting can be reduced.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the molar ratio of zirconium powder, boron carbide powder and silicon powder is 1:0.456: 0.368. the rest is the same as the first embodiment.
Ratio of the present embodimentExample resulting Final product ZrB2The SiC content in the-SiC-ZrC is 20 vol.%, and the high-temperature performance of the material is better.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: in the first step, the mass ratio of the powder material to the deionized water to the ammonium citrate to the Arabic gum is 1 (1.5-2) to 0.4-0.8 to 1-2. The rest is the same as the first embodiment.
The mass ratio of the embodiment can be selected to endow the slurry with reasonable viscosity and fluidity, so that the smooth completion of spray granulation is ensured.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the rotation speed of ball milling mixing in the step one is 300-400 r/min, and the ball milling mixing time is 8-16 hours. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: and in the second step, the sand adopted for the sand blasting treatment is corundum sand. The rest is the same as the first embodiment.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: in the third step, the spraying current is 400-650A. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: and in the third step, the spraying distance is 70-150 mm. The rest is the same as the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: in the third step, the ion gas is argon (Ar)2) And hydrogen (H)2) Wherein the gas flow of the argon is 35L/min, and the gas flow of the hydrogen is 12L/min. The rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the flow of the powder feeding gas argon for spraying in the third step is 2.5L/min. The rest is the same as the first embodiment.
In the reactive plasma spraying process, factors such as spraying current, spraying distance, gas flow and the like have interaction, and the factors can influence the temperature, the speed and the like of the sprayed flying particles. The parameters of spraying current, distance and the like selected by the invention can ensure that the spraying powder can obtain reasonable temperature, speed and the like, and the prepared coating can be well combined with a substrate.
The detailed implementation mode is ten: the first difference between the present embodiment and the specific embodiment is: and in the fourth step, argon is used for blowing along the laser processing direction in the laser remelting process to protect the test piece. The rest is the same as the first embodiment.
When the high-energy laser acts on the surface of the coating, the oxidation of the processed surface is well protected.
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1:
the preparation method of the compact composite coating based on reactive plasma spraying and laser remelting comprises the following steps:
firstly, weighing zirconium powder, boron carbide powder and silicon powder according to the molar ratio of 1:0.456:0.368, then mixing the mixed powder, deionized water, ammonium citrate and Arabic gum according to the mass ratio of 1:2:0.8:2, adding zirconia balls, carrying out ball milling for 12 hours, and carrying out spray granulation on the obtained slurry to obtain mixed spraying powder. And (3) vibrating and screening the mixed spraying powder, and selecting the powder with the particle size of 50-120 microns as plasma spraying powder.
And secondly, carrying out sand blasting treatment on the surface of the ZrC-SiC matrix by using corundum sand, then cleaning the surface of the ZrC-SiC matrix in an ultrasonic cleaner by using absolute ethyl alcohol, and drying the surface of the ZrC-SiC matrix for later use.
Thirdly, the obtained plasma spraying powder is filled into a powder feeder of a plasma spray gun, and the plasma gas used for spraying is argon (Ar)2) And hydrogen (H)2) Wherein the gas flow of argon is 35L/min, the gas flow of hydrogen is 12L/min, the gas of powder feeding gas is argon, the gas flow is 2.5L/min, the spraying current is controlled at 600A, the spraying distance is controlled at 100mm, and the powder is naturally cooled to room temperature after the spraying is finished, namelyZrB is prepared on the surface of ZrC-SiC ceramic by reaction spraying2-SiC-ZrC coating.
Fourthly, ZrB2the-SiC-ZrC coating test piece is arranged on a workbench of laser equipment for laser remelting, the laser power is 350W, the spot diameter is 1mm, the scanning speed is 50mm/S, argon is used for blowing in the laser processing direction in the whole remelting process to protect the test piece, and the ZrB with the compact structure is obtained2-SiC-ZrC coated ZrC-SiC ceramic test pieces.
ZrB before and after laser remelting of the example was measured using an X' pert PRO multifunctional X-ray diffractometer2Phase analysis of the-SiC-ZrC coating resulted in FIG. 1 (◆ in FIG. 1 indicates ZrB)2It means SiC, &lttTtransformation = 9632, "& gTt \9632 &/t &gttmeans ZrC, ● means ZrO2). Through comparison, ZrB of in-situ reaction is formed on the surface of the ZrC ceramic material after plasma spraying, namely before laser remelting2-SiC-ZrC ceramic coating, the coating phase consisting essentially of ZrB2SiC and ZrC, and no residual original material component exists, which shows that ZrB is successfully synthesized by the reactive plasma spraying method2-SiC-ZrC coating. Other phases being predominantly ZrO2This oxide phase is mainly formed by oxidation of the SHS powder during plasma spraying. The phase peak of the spray coating is wider (compared with that after laser remelting), which indicates that the crystallization degree of the product phase is not high and the crystal grain is not developed well.
ZrB before and after laser remelting by adopting Apreo C-type scanning electron microscope2The surface topography analysis of the-SiC-ZrC ceramic coating surface is carried out, and the results are shown in FIGS. 2 and 3. As can be seen by comparing the surface morphology after laser remelting, the plasma sprayed coating has a rough surface and relatively loose texture (FIG. 2). The coating after laser remelting had a relatively flat surface and uniform grain size (FIG. 3), indicating that the laser remelting process resulted in ZrB with a dense fine structure2-SiC-ZrC ceramic coating.
Example 2:
the preparation method of the compact composite coating based on reactive plasma spraying and laser remelting comprises the following steps:
firstly, weighing zirconium powder, boron carbide powder and silicon powder according to the molar ratio of 1:0.456:0.368, then mixing the mixed powder, deionized water, ammonium citrate and Arabic gum according to the mass ratio of 1:2:0.8:2, adding zirconia balls, carrying out ball milling for 12 hours, and carrying out spray granulation on the obtained slurry to obtain mixed spraying powder. And (3) vibrating and screening the mixed spraying powder, and selecting the powder with the particle size of 50-120 microns as plasma spraying powder.
And secondly, carrying out sand blasting treatment on the surface of the ZrC-SiC matrix by using corundum sand, then cleaning the surface of the ZrC-SiC matrix in an ultrasonic cleaner by using absolute ethyl alcohol, and drying the surface of the ZrC-SiC matrix for later use.
Thirdly, the obtained plasma spraying powder is filled into a powder feeder of a plasma spray gun, and the plasma gas used for spraying is argon (Ar)2) And hydrogen (H)2) Wherein the gas flow of argon is 35L/min, the gas flow of hydrogen is 12L/min, the gas of powder feeding gas is argon, the gas flow is 2.5L/min, the spraying current is controlled at 600A, the spraying distance is controlled at 100mm, the ZrB ceramic is naturally cooled to room temperature after the spraying is finished, and the ZrB ceramic is prepared on the surface of the ZrC-SiC ceramic by reaction spraying2-SiC-ZrC coating.
Fourthly, ZrB2the-SiC-ZrC coating test piece is arranged on a workbench of laser equipment for laser remelting, the laser power is 300W, the spot diameter is 1.5mm, the scanning speed is 50mm/S, argon is used for blowing in the laser processing direction in the whole remelting process to protect the test piece, and the ZrB with the compact structure is obtained2-SiC-ZrC coated ZrC-SiC ceramic test pieces.
ZrB after laser remelting of this example was performed using an Apreo C-type scanning electron microscope2The surface topography analysis of the-SiC-ZrC ceramic coating surface was carried out, and the results are shown in FIG. 4. The coating after laser remelting has a relatively flat surface and uniform grain size (fig. 4).
ZrB prepared by adopting HXD-1000 microhardness meter to spray reactive plasma2-SiC-ZrC coating and ZrB after reactive plasma spraying + laser remelting treatment of this example2And (3) carrying out a hardness test on the-SiC-ZrC coating, wherein the test result is as follows: reactive plasma spray ZrB2The hardness of the-SiC-ZrC coating is 818HV, and ZrB is formed after laser remelting treatment2The hardness of the-SiC-ZrC coating was 1003HV to 1120HV, and it was found that the coating was subjected to laser remeltingZrB2The hardness of the-SiC-ZrC coating is improved by 1.2-1.4 times. As explained above, the laser remelting treatment can obtain ZrB with a dense fine structure2-SiC-ZrC ceramic coating.

Claims (10)

1. A preparation method of a compact composite coating based on reactive plasma spraying and laser remelting is characterized by comprising the following steps:
step one, preparing spraying powder:
ball-milling and mixing the powder, deionized water, ammonium citrate and Arabic gum to obtain slurry, and performing spray granulation on the slurry to obtain mixed spraying powder; the powder comprises zirconium powder, boron carbide powder and silicon powder;
step two, pretreatment of the base material:
carrying out sand blasting treatment on the surface of the ZrC-SiC matrix, then carrying out ultrasonic cleaning on the ZrC-SiC matrix, and drying to obtain a pretreated ZrC-SiC matrix;
step three, preparing a coating:
loading the mixed spraying powder obtained in the step one into a plasma spray gun, and spraying the mixed spraying powder on the pretreated ZrC-SiC matrix obtained in the step two to obtain ZrB2-a SiC-ZrC coating;
step four, remelting ZrB by laser2-SiC-based coating:
ZrB prepared in the third step2The SiC-ZrC coating test piece is arranged on a workbench of laser equipment for laser remelting, and the laser remelting process parameters are as follows: the laser power is 0.25-1 kw, the scanning speed is 10-50 mm/S, and the spot size phi is 1-4 mm.
2. The method for preparing the compact composite coating based on the reactive plasma spraying and the laser remelting according to claim 1, wherein the molar ratio of the zirconium powder, the boron carbide powder and the silicon powder in the first step is 1:0.456: 0.368.
3. the method for preparing the compact composite coating based on the reactive plasma spraying and the laser remelting as claimed in claim 1 or 2, wherein the mass ratio of the powder, the deionized water, the ammonium citrate and the Arabic gum in the step one is 1 (1.5-2): (0.4-0.8): 1-2.
4. The preparation method of the compact composite coating based on the reactive plasma spraying and the laser remelting as claimed in claim 3, wherein the rotation speed of the ball milling and mixing in the step one is 300-400 r/min, and the ball milling and mixing time is 8-16 hours.
5. The method for preparing a compact composite coating based on reactive plasma spraying and laser remelting according to claim 1 or 2, characterized in that the sand used in the sand blasting in the second step is corundum sand.
6. The preparation method of the compact composite coating based on the reactive plasma spraying and the laser remelting according to claim 1, wherein the spraying current in the third step is 400-650A.
7. The preparation method of the compact composite coating based on the reactive plasma spraying and the laser remelting according to claim 1, wherein the spraying distance in the third step is 70-150 mm.
8. The method for preparing the compact composite coating based on the reactive plasma spraying and the laser remelting as claimed in claim 1, wherein the ion gas in the third step is argon gas and hydrogen gas, wherein the gas flow rate of the argon gas is 35L/min, and the gas flow rate of the hydrogen gas is 12L/min.
9. The method for preparing the compact composite coating based on the reactive plasma spraying and the laser remelting according to the claim 1, 6, 7 or 8, characterized in that the flow of the powder feeding argon gas for spraying in the step three is 2.5L/min.
10. The method for preparing the compact composite coating based on the reactive plasma spraying and the laser remelting as claimed in claim 1, characterized in that in the fourth step, argon gas is used to blow the test piece in the laser processing direction during the laser remelting to protect the test piece.
CN201911286393.6A 2019-12-13 2019-12-13 Preparation method of compact composite coating based on reactive plasma spraying and laser remelting Pending CN110818421A (en)

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CN112408380A (en) * 2020-10-30 2021-02-26 燕山大学 Preparation method for laser in-situ synthesis of submicron spherical graphite
CN113235036A (en) * 2021-05-10 2021-08-10 江苏天沃重工科技有限公司 Preparation method of hard particle reinforced impact wear-resistant coating for machine-made sand
CN113897585A (en) * 2021-10-11 2022-01-07 芜湖映日科技股份有限公司 Silicon-chromium rotary sputtering target material and preparation method thereof

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CN112063960A (en) * 2020-08-24 2020-12-11 电子科技大学 Zirconium boride powder spray granulation method based on atmospheric plasma spraying
CN112408380A (en) * 2020-10-30 2021-02-26 燕山大学 Preparation method for laser in-situ synthesis of submicron spherical graphite
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CN113235036A (en) * 2021-05-10 2021-08-10 江苏天沃重工科技有限公司 Preparation method of hard particle reinforced impact wear-resistant coating for machine-made sand
CN113897585A (en) * 2021-10-11 2022-01-07 芜湖映日科技股份有限公司 Silicon-chromium rotary sputtering target material and preparation method thereof

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