CN107321998B - Preparation method of copper-gallium alloy powder - Google Patents
Preparation method of copper-gallium alloy powder Download PDFInfo
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- CN107321998B CN107321998B CN201710605714.9A CN201710605714A CN107321998B CN 107321998 B CN107321998 B CN 107321998B CN 201710605714 A CN201710605714 A CN 201710605714A CN 107321998 B CN107321998 B CN 107321998B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention relates to a preparation method of copper-gallium alloy powder, which is prepared by adopting vacuum high-pressure atomization equipment and comprises the following steps: s1, blending; s2, after vacuumizing, heating and preserving heat under the protection of protective gas to melt and mix the raw materials; s3, atomizing into alloy powder; and S4, naturally cooling to normal temperature to obtain the prepared copper-gallium alloy powder. The preparation method of the copper-gallium alloy powder adopts an atomization powder preparation method to prepare the copper-gallium alloy powder with good flow property, low oxygen content and high purity, and can carry out batching according to the proportioning requirements of the copper-gallium alloy powder according to different application requirements, and the purity of the prepared copper-gallium alloy powder reaches 6N.
Description
Technical Field
The invention relates to the field of preparation of alloy powder, in particular to a preparation method of copper-gallium alloy powder.
Background
Copper indium gallium selenide (CuIn)1-xGaxSe, CIGS) thin-film solar cell has the advantages of low cost, stable performance, strong radiation resistance, wide spectral response range and the like. Currently, there are two main approaches to CIGS preparation: multi-element stepwise evaporation and selenization after metal is placed on the top layer. The realization method mainly comprises the vapor deposition method, the magnetron sputtering, the molecular beam epitaxy technology, the spray pyrolysis and the rapid solidification technology, etc. The magnetron sputtering method has the advantages of controllable components, high utilization rate of raw materials, good compactness of the film, uniform film thickness and the like, and is the most promising method for preparing the CIGS film at present. The CIG precursor film is prepared by sputtering, because indium and gallium are both metals with lower melting points, CIG alloy target materials with stable performance and uniform structure cannot be directly prepared, and therefore, when the CIG precursor film is prepared, a copper-gallium alloy target material and an indium target material or a copper-gallium alloy target material and a copper-indium alloy target material are simultaneously adopted for sputtering deposition. In addition, during sputtering, defects inside the target can cause arcing, which affects the structure and quality of the CIGS absorber film. In order to enable the proportion of gallium in the copper indium gallium selenide thin film to be controllable and reduce the defect of arc discharge caused in the sputtering process, a high-quality copper gallium alloy target material needs to be prepared, the copper gallium alloy powder prepared by the conventional methods such as ball milling at present has poor flow property due to irregular shape and high oxidation content of more than 2000ppm and extremely low production efficiency, and meanwhile, because the copper gallium alloy powder is produced by different devices with multiple processes, alloy components with high purity of 6N and more cannot be produced, the produced copper gallium alloy target material has low relative density which can only reach about 95 percent, the oxygen content in the target material is high, the requirement of the high-quality copper indium gallium selenide thin film on the copper gallium target material cannot be met, and the prepared copper gallium alloy target material has good flow property andhigh-quality copper-gallium alloy powder with high quantity and purity is a key factor for preparing high-quality copper-gallium alloy target materials.
Therefore, it is necessary to design a new method for preparing copper-gallium alloy powder to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a preparation method for preparing high-quality copper-gallium alloy powder with good flow property, low oxygen content and high purity.
In order to achieve the purpose, the invention adopts the following technical scheme: the preparation method of the copper-gallium alloy powder adopts vacuum high-pressure atomization equipment for preparation, the atomization equipment comprises a smelting system, an atomization system, a vacuum pumping system, an air source supply system and an integrated control system, the smelting system comprises a crucible, the atomization system comprises an atomization chamber, an atomization nozzle and a tundish positioned above the atomization nozzle are arranged in the atomization chamber, and the preparation method comprises the following steps:
s1, mixing the high-purity copper and the high-purity gallium according to the mixture ratio, and then putting the raw materials into a crucible of a smelting system;
s2, after vacuumizing, under the protection of protective gas, raising the temperature of the crucible to 1150 ~ 1450 ℃ for 1450 ℃, wherein the temperature raising time is 25 ~ 35min, melting the raw materials in the crucible into a copper-gallium alloy liquid, preserving the heat for 20 ~ 40min, and slowly swinging the crucible to fully and uniformly mix the molten metals;
s3, molten metal is injected into a tundish above an atomizing nozzle, the molten metal flows out from a bottom hole of the tundish, meets high-speed airflow or water flow when passing through the atomizing nozzle and is atomized into fine droplets, and the atomized droplets are rapidly solidified into alloy powder in a closed atomizing chamber;
and S4, naturally cooling to normal temperature, filling protective gas into the atomization equipment to normal pressure, and opening the atomization equipment to obtain the prepared copper-gallium alloy powder.
As a further improvement of the invention, the melting system includes a stirring paddle mounted above the crucible.
As a further improvement of the invention, the swinging amplitude of the crucible is +/-60 degrees.
As a further improvement of the invention, the protective gas is an inert gas or nitrogen.
As a further improvement of the invention, the purity of the prepared copper-gallium alloy powder is 6N or more.
As a further improvement of the invention, the purity of the high-purity copper is 5N or more.
As a further improvement of the invention, the purity of the high-purity gallium is 5N or more.
As a further improvement of the invention, the crucible adopts a high-purity graphite crucible or an alumina crucible.
As a further improvement of the invention, the pressure of the atomizing nozzle is 6.8 ~ 10.4.4 MPa.
As a further improvement of the invention, the atomization device also comprises a powder collecting system, a cooling water system and a bracket for supporting the atomization system.
The preparation method of the copper-gallium alloy powder adopts an atomization powder preparation method to prepare the copper-gallium alloy powder with good flow property, low oxygen content and high purity, and can carry out batching according to the proportioning requirements of the copper-gallium alloy powder according to different application requirements, and the purity of the prepared copper-gallium alloy powder reaches 6N.
Drawings
Fig. 1 is a microscopic morphology view of the copper-gallium alloy powder prepared in embodiment 2 of the preparation method of copper-gallium alloy powder of the present invention.
Detailed Description
The technical solutions will be described clearly and completely in the following with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the copper-gallium alloy powder adopts vacuum high-pressure atomization equipment for preparation, the atomization equipment comprises a smelting system, an atomization system, a vacuum pumping system, an air source supply system and an integrated control system, the smelting system comprises a crucible, the atomization system comprises an atomization chamber, an atomization nozzle and a tundish positioned above the atomization nozzle are arranged in the atomization chamber, and in some embodiments of the invention, the atomization equipment further comprises a powder collection system, a cooling water system and a support for supporting the atomization system.
By adopting the atomization equipment, the preparation method of the copper-gallium alloy powder comprises the following steps:
s1, mixing the high-purity copper and the high-purity gallium according to the mixture ratio, and putting the raw materials into a crucible of a smelting system; the high-purity copper is solid and can be in any form of particles, rods, sheets, ingots and the like; the high-purity gallium can be liquid or solid gallium blocks;
s2, after vacuumizing, under the protection of protective gas, raising the temperature of the crucible to 1150 ~ 1450 ℃ for 1450 ℃, wherein the temperature raising time is 25 ~ 35min, melting the raw materials in the crucible into a copper-gallium alloy liquid, preserving the heat for 20 ~ 40min, and slowly swinging the crucible to fully and uniformly mix the molten metals;
s3, molten metal is injected into a tundish above an atomizing nozzle, the molten metal flows out from a bottom hole of the tundish, meets high-speed airflow or water flow when passing through the atomizing nozzle and is atomized into fine droplets, and the atomized droplets are rapidly solidified into alloy powder in a closed atomizing chamber;
and S4, naturally cooling to normal temperature, filling protective gas into the atomization equipment to normal pressure, and opening the atomization equipment to obtain the prepared copper-gallium alloy powder.
In certain embodiments of the invention, the melting system includes a paddle mounted above the crucible for accelerating the uniform mixing of the molten metal.
In some embodiments of the invention, the swinging amplitude of the crucible is +/-60 degrees, the crucible can be continuously swung within +/-60 degrees by hand or driven by a motor, and the stirring paddle can be swung in the melting and heat-preserving process to uniformly stir the molten alloy liquid.
In certain embodiments of the invention, the shielding gas is an inert gas or nitrogen.
In some embodiments of the present invention, the purity of the obtained copper-gallium alloy powder is 6N or more.
In certain embodiments of the present invention, the high purity copper has a purity of 5N and above.
In certain embodiments of the present invention, the high purity gallium has a purity of 5N and above.
In certain embodiments of the present invention, the crucible is a high purity graphite crucible or an alumina crucible.
In certain embodiments of the invention, the pressure of the atomizing nozzle is 6.8 ~ 10.4.4 MPa.
Example 1.
Respectively weighing 21kg of 5N copper particles and 7kg of 5N solid gallium according to the mass ratio of copper to gallium of 75:25, putting the 5N copper particles and 7kg of 5N solid gallium into a high-purity graphite crucible of atomization equipment, closing the atomization equipment, starting a vacuumizing system to ensure that the absolute vacuum degree in the atomization equipment is 450Pa, filling 5N high-purity nitrogen to normal pressure, then starting the vacuumizing system again to vacuumize until the absolute vacuum degree of the atomization equipment is 82Pa, starting a medium-frequency induction heating device in a smelting system, raising the smelting temperature in the crucible to 1450 ℃ by slowly adjusting the power of the device, preserving the temperature for 35min, slowly swinging the crucible in the heat preservation process at a swinging angle of +/-60 ℃, discontinuously swinging a stirring paddle to ensure that the alloy liquid is sufficiently and uniformly mixed, setting the pressure of an atomization nozzle to be 10.4MPa after the heat preservation, pouring the molten alloy liquid into a tundish through a drainage groove, and finally contacting the, the molten alloy is atomized into fine droplets and rapidly cooled in an atomization chamber to form alloy powder. And after the materials are completely atomized, closing the atomizing equipment, cooling the atomizing equipment to normal temperature, taking out the alloy powder, screening to obtain 6N spherical copper-gallium alloy powder with different particle size intervals, and detecting and analyzing the oxygen content in the powder to be 142ppm by using an LECO600 oxygen detector.
Example 2.
Respectively weighing 15kg of 6N copper ingot and 18.3kg of 6N liquid gallium according to the mass ratio of the copper to the gallium of 45:55, putting the 6N copper ingot and the 6N liquid gallium into a high-purity graphite crucible of atomization equipment, closing the atomization equipment, starting a vacuumizing system to ensure that the absolute vacuum degree in the atomization equipment is 430Pa, filling 5N high-purity nitrogen to the normal pressure, then starting the vacuumizing system again to vacuumize until the absolute vacuum degree of the atomization equipment is 75Pa, starting a medium-frequency induction heating device in a smelting system, raising the smelting temperature of the crucible to 1150 ℃ by slowly adjusting the power of the device, preserving the temperature for 30min, slowly swinging the crucible in the heat preservation process with the swinging amplitude of +/-45 degrees, continuously stirring paddles during the process to ensure that the alloy liquid is sufficiently and uniformly mixed, starting a high-pressure airflow control system after the heat preservation is finished, setting the pressure of an atomization nozzle to be 6.8MPa, pouring the molten alloy liquid into a, the molten alloy liquid is atomized into fine liquid drops and rapidly cooled to form alloy powder in the atomizing tower chamber. And (3) closing the atomizing equipment after the materials are completely atomized, cooling the atomizing equipment to normal temperature, taking out the alloy powder, screening to obtain 6N spherical copper-gallium alloy powder with different particle size intervals, and detecting and analyzing the oxygen content in the powder to be 129ppm by using an LECO600 oxygen detector, wherein the morphology of the copper-gallium alloy powder is shown in figure 1.
Example 3.
Respectively weighing 9kg of 6N copper ingot and 21kg of 6N liquid gallium according to the mass ratio of the copper to the gallium of 30:70, putting the 6N copper ingot and the 6N liquid gallium into a high-purity graphite crucible of atomization equipment, closing the atomization equipment, starting a vacuumizing system to ensure that the absolute vacuum degree in the atomization equipment is 400Pa, filling 5N high-purity nitrogen to the normal pressure, then starting the vacuumizing system again to vacuumize until the absolute vacuum degree of the atomization equipment is 60Pa, starting a medium-frequency induction heating device in a smelting system, raising the smelting temperature of the crucible to 1250 ℃ by slowly adjusting the power of the device, keeping the temperature for 25min, slowly swinging the crucible in the heat preservation process with the swinging amplitude of +/-25 degrees, continuously swinging a stirring paddle in the process to ensure that alloy liquid is sufficiently and uniformly mixed, starting a high-pressure airflow control system after the heat preservation is finished, setting the pressure of an atomizing nozzle to be 8.0MPa, pouring the molten alloy liquid into, the molten alloy liquid is atomized into fine liquid drops and rapidly cooled to form alloy powder in the atomizing tower chamber. And after the materials are completely atomized, closing the atomizing equipment, cooling the atomizing equipment to normal temperature, taking out the alloy powder, screening to obtain 6N spherical copper-gallium alloy powder with different particle size intervals, and detecting and analyzing the oxygen content in the powder to 133ppm by using an LECO600 oxygen detector.
The preparation method of the copper-gallium alloy powder adopts an atomization powder preparation method to prepare the copper-gallium alloy powder with good flow property, low oxygen content and high purity, and can carry out batching according to the proportioning requirements of the copper-gallium alloy powder according to different application requirements, and the purity of the prepared copper-gallium alloy powder reaches 6N.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (7)
1. A preparation method of copper-gallium alloy powder is characterized by comprising the following steps: the preparation method comprises the following steps of:
s1, mixing the high-purity copper and the high-purity gallium according to the mixture ratio, and then putting the raw materials into a crucible of a smelting system;
s2, after vacuumizing, under the protection of protective gas, raising the temperature of the crucible to 1150-1450 ℃ for 25-35 min, melting the raw materials in the crucible into a copper-gallium alloy liquid, preserving the heat for 20-40 min, and slowly swinging the crucible to fully and uniformly mix the molten metals;
s3, molten metal is injected into a tundish above an atomizing nozzle, the molten metal flows out from a bottom hole of the tundish, meets high-speed airflow or water flow when passing through the atomizing nozzle and is atomized into fine droplets, and the atomized droplets are rapidly solidified into alloy powder in a closed atomizing chamber;
s4, naturally cooling to normal temperature, filling protective gas into the atomization equipment to normal pressure, and opening the atomization equipment to obtain the prepared copper-gallium alloy powder;
the purity of the high-purity copper is 5N or more; the purity of the high-purity gallium is 5N or more; the purity of the obtained copper-gallium alloy powder is 6N or more.
2. The method for producing a copper-gallium alloy powder according to claim 1, characterized in that: the smelting system comprises a stirring paddle arranged above the crucible.
3. The method for producing a copper-gallium alloy powder according to claim 1, characterized in that: the swinging amplitude of the crucible is +/-60 degrees.
4. The method for producing a copper-gallium alloy powder according to claim 1, characterized in that: the protective gas is inert gas or nitrogen.
5. The method for producing a copper-gallium alloy powder according to claim 1, characterized in that: the crucible is a high-purity graphite crucible or an alumina crucible.
6. The method for producing a copper-gallium alloy powder according to claim 1, characterized in that: the pressure of the atomizing nozzle is 6.8-10.4 MPa.
7. The method for producing a copper-gallium alloy powder according to claim 1, characterized in that: the atomization device also comprises a powder collecting system, a cooling water system and a bracket for supporting the atomization system.
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Effective date of registration: 20181127 Address after: 511517 D Workshop of Qingyuan Pioneer Materials Co., Ltd. No. 27-9 Baijia Industrial Park, Qingyuan High-tech Zone, Guangdong Province Applicant after: Pilot film material (Guangdong) Co., Ltd. Address before: 511517 27-9B, Guangdong Qingyuan hi tech Industrial Park Applicant before: Qingyuan Xiandao Materials Co., Ltd. |
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Application publication date: 20171107 Assignee: Pilot film materials Co.,Ltd. Assignor: Leading film materials (Guangdong) Co.,Ltd. Contract record no.: X2021440000141 Denomination of invention: Preparation method of copper gallium alloy powder Granted publication date: 20200107 License type: Common License Record date: 20210730 |