CN107858656B - Preparation method of CuSe compound rotary target material - Google Patents
Preparation method of CuSe compound rotary target material Download PDFInfo
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- CN107858656B CN107858656B CN201711027535.8A CN201711027535A CN107858656B CN 107858656 B CN107858656 B CN 107858656B CN 201711027535 A CN201711027535 A CN 201711027535A CN 107858656 B CN107858656 B CN 107858656B
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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
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
Abstract
The invention discloses a preparation method of a CuSe compound rotary target, which comprises the following steps: selecting a non-magnetic pipe as a substrate; spraying CuSe powder on the outer surface of the pretreated substrate by using an ultrasonic rapid cold spraying technology, wherein the thickness of a deposited layer is not more than 20 mm; further improving the density under ultrahigh pressure by utilizing a cold isostatic pressing technology; and (3) obtaining a rotary target blank with a corresponding organization structure through high-temperature sintering, and machining to obtain the rotary target. The CuSe material prepared by the method has uniform internal density, is favorable for forming a good coating film, and reduces the defective rate of solar products.
Description
Technical Field
The invention relates to a photoelectric material technology, in particular to a preparation method of a CuSe compound rotary target.
Background
The solar cell has been developed from a silicon crystal system toward a compound thin film through the recent 20 years. The silicon crystal system has a light conversion efficiency of 17% or more, but the manufacturing cost is high. In the early stage of the whole industry, a large amount of energy is consumed for preparing polycrystalline silicon and monocrystalline silicon, and great influence is brought to the environment. In order to better utilize solar energy, a Cu-In-Ga-Se compound thin-film solar cell which is low In manufacturing cost and relatively low In energy consumption and can be produced In batch is developed.
In the process of preparing the Cu-In-Ga-Se compound thin-film solar cell, the CuSe compound is used as one of targets for magnetron sputtering coating, so that the solar cell is simpler to produce, lower In investment cost, lower In production cost and lower In final product cost.
At present, the method for preparing the CuSe target has high cost, relatively nonuniform density and material utilization rate of less than 40 percent.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a CuSe compound rotary target material, the internal density of the CuSe compound rotary target material is uniform, good coating film formation is facilitated, and the defective rate of solar products is reduced.
The technical scheme is as follows:
a method for preparing a CuSe compound rotary target material comprises the following steps:
selecting a non-magnetic pipe as a substrate;
spraying CuSe powder on the outer surface of the pretreated substrate by using an ultrasonic rapid cold spraying technology, wherein the thickness of a deposited layer is not more than 20 mm; further improving the density under ultrahigh pressure by utilizing a cold isostatic pressing technology;
and (3) obtaining a rotary target blank with a corresponding organization structure through high-temperature sintering, and machining to obtain the rotary target.
Further: the non-magnetic pipe is selected from non-magnetic stainless steel pipe, metal copper pipe, metal titanium pipe, nickel-chromium pipe and nickel-aluminum pipe, the two ends of the non-magnetic pipe are processed into connecting screw fasteners according to requirements, and the surface of the matrix is pretreated by sand blasting, cleaning and drying.
Further: the average particle size of the CuSe powder is 1-5 mu m, the purity of the CuSe powder is 99.9-99.999%, the total content of impurities is less than 1000ppm, and the content of single impurity elements is less than 500 ppm.
Further: under the protection atmosphere of helium or nitrogen, CuSe powder is conveyed to an ultrasonic rapid cold spraying technical gun through a powder conveying device, CuSe powder is sprayed on the surface of a substrate layer by layer in a scanning mode through high-speed airflow, each layer is 1-5 mu m until the thickness of a CuSe accumulation layer reaches 5-20 mm, and the CuSe accumulation layer is cooled to room temperature, wherein the gas pressure at a cold spraying inlet is 2-3 MPa, and the gas temperature is 100-200 ℃; heating the working gas to 200-300 ℃, and pressurizing to 3-5 MPa; the spraying distance is 30-55 mm.
Further: coating an anti-seepage material layer on the outer surface of the substrate sprayed with the CuSe accumulation layer, and performing high-pressure treatment in a cold isostatic press, wherein the pressure is not more than 1000 MPa.
Further: in an atmosphere protection furnace, the protection gas is argon or nitrogen, a rotary target blank obtained by high-temperature sintering is heated at 100-300 ℃ for 5 hours, and the relative density of the target is 96-98%.
Further: the rotary target product is cylindrical, the thickness of CuSe is less than 20mm, and the flatness is less than 0.15 mm.
Compared with the prior art, the invention has the technical effects that:
the rotary target material manufactured by the invention has the advantages of high density, no segregation, uniform structure, fine crystal grains, low porosity and the like, and the manufacturing method has the advantages of short process flow, good controllability, low production cost, high production efficiency and the like.
1. The CuSe material has uniform internal density, is favorable for forming a good coating film, and reduces the defective rate of solar products.
2. The material utilization rate of the rotary target material prepared by the invention can exceed 80%. The improvement of the material utilization rate can obviously reduce the production cost and enhance the market competitiveness of the product.
Detailed Description
The technical solution of the present invention will be described in detail with reference to exemplary embodiments. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art.
The preparation method of the CuSe compound rotary target comprises the following specific steps:
step 1: selecting a non-magnetic pipe as a substrate;
the non-magnetic pipe is selected from non-magnetic stainless steel pipe, metal copper pipe, metal titanium pipe, nickel-chromium pipe and nickel-aluminum pipe, the non-magnetic pipe is processed to a size meeting the use requirement, two ends of the non-magnetic pipe are processed into connecting screw fasteners according to the requirement, and the surface of the non-magnetic pipe is pretreated by sand blasting, cleaning, drying and the like.
Step 2: spraying CuSe powder on the outer surface of the pretreated substrate by using an ultrasonic rapid cold spraying technology, wherein the thickness of a deposited layer is not more than 20 mm; further improving the density under ultrahigh pressure by utilizing a cold isostatic pressing technology;
under the protection atmosphere of helium or nitrogen, CuSe powder is conveyed to an ultrasonic rapid cold spraying technical gun through a powder conveying device, CuSe powder is sprayed on the surface of a substrate layer by layer in a scanning mode through high-speed airflow, each layer is 1-5 mu m until the thickness of a CuSe accumulation layer reaches 5-20 mm, and the CuSe accumulation layer is cooled to room temperature, wherein the gas pressure at a cold spraying inlet is 2-3 MPa, and the gas temperature is 100-200 ℃; heating the working gas to 200-300 ℃, and pressurizing to 3-5 MPa; the spraying distance is 30-55 mm.
Coating an anti-seepage material layer on the outer surface of the substrate sprayed with the CuSe accumulation layer, and performing high-pressure treatment in a cold isostatic press, wherein the pressure is not more than 1000 MPa.
CuSe powder with a particle size of less than 1 μm is removed by sieving. The average particle size of the CuSe powder is 1-5 mu m, the purity of the CuSe powder is 99.9-99.999%, other elements are impurities, the total content of the impurities is less than 1000ppm, and the content of single impurity elements is less than 500 ppm.
And step 3: and (3) obtaining a rotary target blank with a corresponding organization structure through high-temperature sintering, and machining to obtain the rotary target.
In an atmosphere protection furnace, the protection gas is argon or nitrogen, a rotary target blank with a corresponding organization structure is obtained by high-temperature sintering, the temperature is 100-300 ℃, the heating treatment time is 5 hours, and the relative density of the target is 96-98%; and (4) machining the formed rotary target blank, and cleaning and drying the machined rotary target blank to obtain the rotary target. The rotary target product is cylindrical, the thickness of CuSe is less than 20mm, and the flatness is less than 0.15 mm.
Example 1:
a preparation method of a CuSe compound rotary target material specifically comprises the following steps:
(1) preparing a non-magnetic stainless steel pipe, processing the size of the non-magnetic stainless steel pipe to meet the use requirement, processing two ends of the non-magnetic stainless steel pipe into connecting screw fasteners according to the requirement, and performing pretreatment such as sand blasting, cleaning, drying and the like on the surface of the non-magnetic stainless steel pipe; screening out CuSe powder with the particle size of less than 1 mu m for later use;
(2) under the nitrogen protection atmosphere, a powder feeding device feeds CuSe powder to an ultrasonic rapid cold spraying technical gun, under the condition that a nonmagnetic stainless steel pipe keeps rotating, CuSe powder is sprayed on the surface of a base body layer by high-speed airflow in a scanning mode, each layer is 2 micrometers until the accumulation of the CuSe layer reaches 7mm, and the CuSe layer is cooled to room temperature, wherein the gas pressure at a cold spraying inlet is 2MPa, and the gas temperature is 100 ℃; heating the working gas to 200 ℃, and pressurizing to 3 MPa; the spraying distance is 30-55 mm;
(3) coating an anti-seepage material layer on the outer surface of the liner pipe sprayed with the CuSe accumulation layer, and performing high-pressure treatment in a cold isostatic press at the pressure of 300 MPa;
(4) in an argon protection furnace, high-temperature sintering is carried out to obtain a rotary target blank with a corresponding organization structure, the temperature is 100 ℃, the heating treatment time is 5 hours, and the relative density of the target is 96 percent;
(5) and (4) machining the formed rotary target blank, and cleaning and drying the machined rotary target blank to obtain a finished rotary target product.
Example 2:
a preparation method of a CuSe compound rotary target material specifically comprises the following steps:
(1) preparing a metal copper pipe, processing the size of the metal copper pipe to meet the use requirement, processing two ends of the metal copper pipe into connecting screw fasteners according to the requirement, and performing pretreatment such as sand blasting, cleaning, drying and the like on the surface of the metal copper pipe; screening out CuSe powder with the particle size of less than 1 mu m for later use;
(2) under the protective atmosphere of helium, a powder feeding device feeds CuSe powder to an ultrasonic rapid cold spraying technical gun, under the condition that a metal copper pipe keeps rotating, CuSe powder is sprayed on the surface of a base body layer by high-speed airflow in a scanning mode, each layer is 4 micrometers until the accumulation of the CuSe layer reaches 11mm, and the CuSe layer is cooled to room temperature, wherein the gas pressure at a cold spraying inlet is 3MPa, and the gas temperature is 150 ℃; heating the working gas to 200 ℃, and pressurizing to 4 MPa; the spraying distance is 30-55 mm;
(3) coating an anti-seepage material layer on the outer surface of the substrate sprayed with the CuSe accumulation layer, and performing high-pressure treatment in a cold isostatic press at the pressure of 500 MPa;
(4) in a nitrogen protection furnace, high-temperature sintering is carried out to obtain a rotary target blank with a corresponding organization structure, the temperature is 200 ℃, the heating treatment time is 5 hours, and the relative density of the target is 97 percent;
(5) and (4) machining the formed rotary target blank, and cleaning and drying the machined rotary target blank to obtain a finished rotary target product.
Example 3:
a preparation method of a CuSe compound rotary target material specifically comprises the following steps:
(1) preparing a metal titanium pipe, processing the size of the metal titanium pipe to meet the use requirement, processing two ends of the metal titanium pipe into connecting screw fasteners according to the requirement, and performing pretreatment such as sand blasting, cleaning, drying and the like on the surface of the metal titanium pipe; screening out CuSe powder with the particle size of less than 1 mu m for later use;
(2) under the protective atmosphere of helium, a powder feeding device feeds CuSe powder to an ultrasonic rapid cold spraying technical gun, under the condition that a metal copper pipe keeps rotating, CuSe powder is sprayed on the surface of a base body layer by high-speed airflow in a scanning mode, each layer is 5 micrometers until the accumulation of the CuSe layer reaches 15mm, and the CuSe layer is cooled to room temperature, wherein the gas pressure at a cold spraying inlet is 3MPa, and the gas temperature is 200 ℃; heating the working gas to 300 ℃, and pressurizing to 5 MPa; the spraying distance is 30-55 mm;
(3) coating a layer of anti-seepage material on the outer surface of the substrate sprayed with the CuSe accumulation layer, and performing high-pressure treatment in a cold isostatic press at the pressure of 700 MPa;
(4) in an argon protection furnace, high-temperature sintering is carried out to obtain a rotary target blank with a corresponding organization structure, the temperature is 280 ℃, the heating treatment time is 5 hours, and the relative density of the target is 98 percent;
(4) and (4) machining the formed rotary target blank, and cleaning and drying the machined rotary target blank to obtain a finished rotary target product.
The terminology used herein is for the purpose of description and illustration, rather than of limitation. As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the meets and bounds of the claims, or equivalences of such meets and bounds are therefore intended to be embraced by the appended claims.
Claims (2)
1. A method for preparing a CuSe compound rotary target material comprises the following steps:
selecting a non-magnetic pipe as a substrate;
spraying CuSe powder on the outer surface of the pretreated substrate by using an ultrasonic rapid cold spraying technology, wherein the thickness of a deposited layer is not more than 20 mm; the average particle size of the CuSe powder is 1-5 mu m, the purity is 99.9-99.999%, the total content of impurities is less than 1000ppm, and the content of single impurity elements is less than 500 ppm;
under the protection atmosphere of helium or nitrogen, CuSe powder is conveyed to an ultrasonic rapid cold spraying technical gun through a powder conveying device, CuSe powder is sprayed on the surface of a substrate layer by layer in a scanning mode through high-speed airflow, each layer is 1-5 mu m until the thickness of a CuSe accumulation layer reaches 5-20 mm, and the CuSe accumulation layer is cooled to room temperature, wherein the gas pressure at a cold spraying inlet is 2-3 MPa, and the gas temperature is 100-200 ℃; heating the working gas to 200-300 ℃, and pressurizing to 3-5 MPa; the spraying distance is 30-55 mm; coating a layer of anti-seepage material on the outer surface of the substrate sprayed with the CuSe accumulation layer, performing high-pressure treatment in a cold isostatic press, wherein the pressure is not more than 1000MPa, and further improving the density under ultrahigh pressure;
in an atmosphere protection furnace, the protection gas is argon or nitrogen, a rotary target blank with a corresponding organization structure is obtained through high-temperature sintering, the temperature is 100-300 ℃, the heating treatment time is 5 hours, the rotary target is obtained through machining, and the relative density of the rotary target is 96-98%; the shape of the target material product is cylindrical, the thickness of CuSe is less than 20mm, and the flatness is less than 0.15 mm.
2. The method for preparing the CuSe compound rotary target material as claimed in claim 1, wherein: the non-magnetic pipe is selected from non-magnetic stainless steel pipe, metal copper pipe, metal titanium pipe, nickel-chromium pipe and nickel-aluminum pipe, the two ends of the non-magnetic pipe are processed into connecting screw fasteners according to requirements, and the surface of the matrix is pretreated by sand blasting, cleaning and drying.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102103959A (en) * | 2009-12-17 | 2011-06-22 | 通用电气公司 | Apparatus for X-ray generation and method of making same |
| CN103930591A (en) * | 2011-10-14 | 2014-07-16 | 株式会社爱发科 | Target assembly and production method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102103959A (en) * | 2009-12-17 | 2011-06-22 | 通用电气公司 | Apparatus for X-ray generation and method of making same |
| CN103930591A (en) * | 2011-10-14 | 2014-07-16 | 株式会社爱发科 | Target assembly and production method therefor |
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