CN111235563A - Method for preparing Ta/Al composite anti-irradiation coating by adopting cold spraying - Google Patents

Method for preparing Ta/Al composite anti-irradiation coating by adopting cold spraying Download PDF

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Publication number
CN111235563A
CN111235563A CN202010143441.2A CN202010143441A CN111235563A CN 111235563 A CN111235563 A CN 111235563A CN 202010143441 A CN202010143441 A CN 202010143441A CN 111235563 A CN111235563 A CN 111235563A
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composite
powder
preparing
coating
spraying
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Inventor
熊天英
唐俊榕
杜昊
王吉强
刘晗珲
沈艳芳
杨颖�
毛天亮
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NO.47 INSTITUTE OF CHINA ELECTRONICS TECHNOLOGY Group Corp.
Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C24/00Coating starting from inorganic powder
    • C23C24/02Coating starting from inorganic powder by application of pressure only
    • C23C24/04Impact or kinetic deposition of particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

Abstract

The invention belongs to the field of protective coating preparation, and particularly relates to a method for preparing a Ta/Al composite anti-irradiation coating by adopting cold spraying. The method comprises the following steps: (1) mixing Ta powder and Al powder according to the mass ratio (0.1-20): 1, mixing to prepare composite powder; (2) and spraying the prepared composite powder on the surface of the substrate of the device to be protected by adopting cold air power spraying equipment to form the Ta/Al composite coating. The method can prepare the anti-irradiation coating for the outer surface of the electronic package, and considers different energy ranges of the space irradiation particles.

Description

Method for preparing Ta/Al composite anti-irradiation coating by adopting cold spraying
Technical Field
The invention belongs to the field of protective coating preparation, and particularly relates to a method for preparing a Ta/Al composite anti-irradiation coating by adopting cold spraying.
Background
The electronic components in space stations and aircraft are exposed to 5 x 10-4~1×10-2In the space irradiation environment with rad (Si)/s radiation dose, various different particle irradiation exists. The energetic particles can cause damage to the electronic device materials. Therefore, it is desirable to protect such electronic components with a coating having radiation resistance.
Tungsten (W) and lead (Pb) have better radiation damage resistance due to the extremely large atomic mass. Recent studies have found that tantalum (Ta) also has a very strong resistance to irradiation by steric protons. In general, for nanomaterials, more grain boundaries inside the material have a further absorbing or hindering effect on defects generated by irradiation damage, but how to retain the nanostructures into the protective coating is extremely challenging. In addition, researches show that the material with larger atomic mass has better effect on protecting the irradiation of the high-energy particles, but has general protection effect on the irradiation particles with smaller energy. The composite material can expand the energy range for protecting the space irradiation particles.
Disclosure of Invention
The invention aims to provide a method for preparing a Ta/Al composite anti-irradiation coating by adopting cold spraying, which can improve the irradiation tolerance of electronic components in space stations and aircrafts.
The technical scheme of the invention is as follows:
a method for preparing a Ta/Al composite anti-irradiation coating by adopting cold spraying comprises the following steps:
(1) mixing Ta powder and Al powder according to the mass ratio (0.1-20): 1, mixing to prepare composite powder;
(2) and spraying the prepared composite powder on the surface of the substrate of the device to be protected by adopting cold air power spraying equipment to form the Ta/Al composite coating.
In the method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying, in the step (1), Ta powder is nano-scale particles, the shape is spherical, and the particle size range is 10-500 nm.
In the method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying, in the step (1), Ta powder is micron-sized particles, the shape is spherical or irregular, and the particle size range is 10-100 mu m.
In the method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying, in the step (1), the shape of Al powder is spherical or spheroidal, and the particle size range is 10-200 mu m.
The method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying comprises the step (1) of selectively doping ceramic particles CeO into composite powder2、ZrO2、Y2O3One or more than two ceramic particles are in nanometer level, the appearance is spherical, and the particle size range is 10-500 nm; the ceramic particles account for 1-20% of the composite powder by mass, and the doped ceramic particles are uniformly distributed.
The method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying comprises the step (1) of preparing composite powder by adopting ball milling or mechanical mixing for 2-8 hours.
The method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying comprises the step (2) that compressed air or nitrogen is used as working gas for cold gas dynamic spraying, the temperature is 180-500 ℃, the pressure is 1.5-4.5 MPa, and the spraying distance is 10-40 mm.
In the method for preparing the Ta/Al composite anti-radiation coating by adopting cold spraying, in the step (2), the substrate of the device to be protected is a metal, ceramic or metal ceramic composite substrate, and the surface of the substrate of the device to be protected is subjected to sand blasting before spraying.
According to the method for preparing the Ta/Al composite anti-irradiation coating by adopting cold spraying, in the step (2), Ta and Al phases of the composite coating are uniformly distributed.
The design idea of the invention is as follows:
aiming at the problem that electronic components in space stations and aircrafts are damaged by irradiation of space particles in different energy ranges, a method for preparing a Ta/Al composite anti-irradiation coating by cold spraying is provided. The existing method adopts a bipolar process to prepare an electronic component so as to improve the radiation resistance, which brings great production cost. And if the anti-radiation coating is prepared on the surface of the packaging material, the production cost and the production time are greatly reduced.
The Ta/Al composite anti-radiation coating is prepared on the packaged metal, ceramic and metal ceramic matrix by adopting cold spraying. Firstly, Al which has better plasticity and is easy to be deposited by cold spraying is added into Ta powder as a binding phase, and the obtained Ta/Al composite coating has good compactness. The design requirement can be met by regulating the proportion of the nano ceramic phase and the nano ceramic phase.
The invention has the advantages and beneficial effects that:
1. the method is simple to operate and is not limited by the shape of the electronic element;
2. the invention effectively avoids the high-temperature condition required by preparing the tantalum coating and the problem of performance reduction such as oxidation and the like caused by the high-temperature condition.
3. The Ta/Al composite coating prepared by the method disclosed by the invention has uniform distribution of Ta, Al and doped ceramic phase.
4. The method can prepare the anti-irradiation coating for the outer surface of the electronic package, and considers different energy ranges of the space irradiation particles.
Drawings
FIG. 1 is a sectional SEM photograph of a micron-sized Ta/Al composite coating: (a) 75% by volume of Ta to 25% of Al, and (b) 50% by volume of Ta to 50% of Al.
FIG. 2 is an SEM photograph of nanoscale Ta/Al composite powder and its coating: (a) composite powder after ball milling, (b) composite powder of electrostatic adsorption, (c) cross section of composite coating.
FIG. 3 is a micron Ta/Al/CeO2/ZrO2Cross-sectional SEM photographs of the composite coating.
FIG. 4 shows a nanoscale Ta/Al/Y2O3Cross-sectional SEM photographs of the composite coating.
Detailed Description
In the specific implementation process, the method for preparing the Ta/Al composite anti-radiation coating by cold spraying is adopted, micron or nano Ta powder and micron Al powder are mixed according to a certain proportion to prepare composite powder, and the prepared composite powder is sprayed on the surface of a metal, ceramic or metal ceramic composite matrix by cold air power spraying equipment under a certain condition to form the Ta/Al composite coating.
The method comprises the following specific steps:
step 1, mixing powder: mixing Ta powder and Al powder according to the mass ratio (0.1-20): 1, mixing to prepare composite powder; preferably, the Ta powder and the Al powder are mixed according to the mass ratio (5-10): 1. wherein a certain amount of CeO may be incorporated2、ZrO2、Y2O3And (3) ceramic particles;
wherein, the Ta powder can be in a nanometer level, the shape is spherical, and the particle size range is 10-500 nm; or micron-sized particles with the shape of sphere or irregular shape and the particle size range of 10-100 mu m. The shape of the Al powder is spherical or spheroidal, and the granularity range is 10-200 mu m. Doped CeO2、ZrO2、Y2O3The ceramic particles are in nanometer level, the appearance is spherical, and the particle size range is 10-500 nm. The composite powder can be prepared by ball milling or mechanical mixing for 2-8 hours.
Step 2, spraying: and spraying the prepared composite powder on the surface of a substrate to be protected by adopting cold air power spraying equipment under a certain condition to form a Ta/Al composite coating, wherein the thickness range of the composite coating is 100-3000 mu m.
The working conditions of the cold spraying equipment are that the temperature is 180-500 ℃, the pressure is 1.5-4.5 MPa, the spraying distance is 10-40 mm, and compressed air or nitrogen is selected as propelling gas. The substrate of the device to be protected is metal, ceramic or metal ceramic, and sand blasting is needed before spraying.
For the cold spraying equipment, refer to a cold air dynamic spraying device mentioned in the Chinese patent of invention (patent No. 01128130.8, granted publication No. CN1161188C) or other commercial cold spraying, dynamic spraying or low pressure cold spraying equipment. The powder is smoothly discharged from the spray gun for a long time in the deposition process without blockage. The Ta and Al phases of the composite coating obtained by deposition are uniformly distributed, and the doped ceramic phase is also uniformly distributed.
The following examples are given for the detailed description of the embodiments of the present invention, and the detailed implementation and specific operation procedures are given on the premise of the technical scheme of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
In the embodiment, irregular Ta powder with the particle size of 10-45 mu m and spherical Al powder with the particle size of 30-40 mu m are mixed for 8 hours in powder mixing equipment; wherein, the volume fraction of the Al powder is 25 percent and 50 percent, and the reduced mass fraction is respectively about 5 percent and 14 percent. The matrix of the device to be protected is an alumina ceramic matrix, the cold spraying operation temperature is 250 ℃, the operation pressure is 2.0MPa, the spraying distance is 20mm, compressed air is selected as working gas, and the spraying time is 20 min. As shown in FIG. 1, the prepared Ta/Al composite coating has a thickness of 250 μm and uniform distribution of Ta and Al phases.
Example 2
In the embodiment, nanometer Ta powder with the particle size of 80nm and micrometer Al powder with the particle size of 30-40 mu m are uniformly mixed (can be subjected to ball milling or simple mechanical mixing); wherein, the volume fraction of the Ta powder is 25 percent, and the reduced mass fraction is 66.5 percent. The matrix of the device to be protected is an alumina ceramic matrix, the cold spraying operation temperature is 200 ℃, the operation pressure is 2.0MPa, the spraying distance is 20mm, compressed air is selected as working gas, and the spraying time is 20 min. As shown in FIG. 2, the thickness of the prepared Ta/Al composite coating is 250 μm, the two phases of Ta and Al are uniformly distributed, and the nano Ta powder is found to be coated around the micron Al powder.
Example 3
In this embodiment, micrometer Ta powder with a particle size of 40-50 μm, micrometer Al powder with a particle size of 40-50 μm, and ceramic CeO particles with a particle size of 100nm are selected2、ZrO2Ball milling for 4 hr to mix homogeneously; wherein, the mass fraction of Ta powder is 80%, the mass fraction of Al powder is 15%, and nano CeO2The mass fraction of (a) is 2.5%, nano ZrO2The mass fraction of (2.5%). The matrix of the device to be protected is an alumina ceramic matrix, the cold spraying operation temperature is 300 ℃, the operation pressure is 3.0MPa, the spraying distance is 30mm, nitrogen is selected as the working gas, and the spraying time is 20 min. As shown in FIG. 3, the prepared Ta/Al composite coating has a thickness of 400 μm, and Ta, Al and ceramic particles of CeO2、ZrO2The distribution is uniform.
Example 4
In the embodiment, nanometer Ta powder with the granularity of 100nm, micrometer Al powder with the granularity of 20-30 mu m and ceramic particles Y with the granularity of 50nm are taken2O3Ball milling for 4 hr to mix homogeneously; wherein, the mass fraction of Ta powder is 75%, the mass fraction of Al powder is 20%, and the mass fraction of ceramic particles Y is2O3Is 5 percent. The matrix of the device to be protected is an alumina ceramic matrix, the cold spraying operation temperature is 400 ℃, the operation pressure is 4.0MPa, the spraying distance is 40mm, nitrogen is selected as the working gas, and the spraying time is 20 min. As shown in FIG. 4, the prepared Ta/Al composite coating had a thickness of 500 μm, Ta, Al, and ceramic particles Y2O3Uniformly distributed, and nanometer Ta and nanometer Y are found2O3The ceramic particles are wrapped around the micron Al powder.
The results of the examples show that the method of the invention has simple operation, saves cost, does not need harsh conditions such as high temperature, high pressure and the like, and does not need to use He or N2The Ta/Al composite coating can be prepared on the ceramic matrix only by using compressed air under the conditions of medium temperature and medium pressure, and two phases in the prepared coating are uniformly distributed.

Claims (9)

1. A method for preparing a Ta/Al composite anti-irradiation coating by adopting cold spraying is characterized by comprising the following steps:
(1) mixing Ta powder and Al powder according to the mass ratio (0.1-20): 1, mixing to prepare composite powder;
(2) and spraying the prepared composite powder on the surface of the substrate of the device to be protected by adopting cold air power spraying equipment to form the Ta/Al composite coating.
2. The method for preparing the Ta/Al composite anti-radiation coating by adopting cold spraying as claimed in claim 1, wherein in the step (1), the Ta powder is nano-scale particles, the morphology is spherical, and the particle size range is 10-500 nm.
3. The method for preparing the Ta/Al composite anti-radiation coating by adopting cold spraying according to claim 1, wherein in the step (1), the Ta powder is micron-sized particles, the morphology is spherical or irregular, and the particle size range is 10-100 μm.
4. The method for preparing the Ta/Al composite anti-radiation coating by adopting cold spraying according to claim 1, wherein in the step (1), the shape of the Al powder is spherical or spheroidal, and the particle size range is 10-200 μm.
5. The method for preparing Ta/Al composite anti-radiation coating by cold spraying as claimed in claim 1, wherein in the step (1), the composite powder is selectively doped with CeO ceramic particles2、ZrO2、Y2O3One or more than two ceramic particles are in nanometer level, the appearance is spherical, and the particle size range is 10-500 nm; the ceramic particles account for 1-20% of the composite powder by mass, and the doped ceramic particles are uniformly distributed.
6. The method for preparing the Ta/Al composite anti-radiation coating by adopting cold spraying according to claim 1, wherein in the step (1), the composite powder is prepared by adopting ball milling or mechanical mixing for 2-8 hours.
7. The method for preparing the Ta/Al composite anti-radiation coating by adopting cold spraying according to claim 1, wherein in the step (2), compressed air or nitrogen is used as a working gas for cold gas dynamic spraying, the temperature is 180-500 ℃, the pressure is 1.5-4.5 MPa, and the spraying distance is 10-40 mm.
8. The method for preparing a Ta/Al composite anti-radiation coating by cold spraying according to claim 1, wherein in the step (2), the substrate of the device to be protected is a metal, ceramic or metal ceramic composite substrate, and the surface of the substrate of the device to be protected is subjected to sand blasting before spraying.
9. The method for preparing a Ta/Al composite anti-radiation coating by cold spraying according to claim 1, wherein in the step (2), the Ta and Al phases of the composite coating are uniformly distributed.
CN202010143441.2A 2020-03-04 2020-03-04 Method for preparing Ta/Al composite anti-irradiation coating by adopting cold spraying Pending CN111235563A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114075664A (en) * 2020-08-17 2022-02-22 中国科学院金属研究所 Method for preparing graphical ceramic copper-clad plate through cold spraying

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