CN107321998A - The preparation method of copper gallium alloy powder - Google Patents
The preparation method of copper gallium alloy powder Download PDFInfo
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- CN107321998A CN107321998A CN201710605714.9A CN201710605714A CN107321998A CN 107321998 A CN107321998 A CN 107321998A CN 201710605714 A CN201710605714 A CN 201710605714A CN 107321998 A CN107321998 A CN 107321998A
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- alloy powder
- gallium alloy
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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
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Abstract
The present invention relates to a kind of preparation method of copper gallium alloy powder, prepared using vacuum high-pressure atomization plant, preparation method comprises the following steps：S1, dispensing；S2, vacuumize after, protective gas protection under, heat up and be incubated cause raw materials melt mixing；S3, atomization are alloyed powder；S4, normal temperature is naturally cooling to, obtains obtained copper gallium alloy powder.The preparation method of copper gallium alloy powder of the present invention prepares the high copper gallium alloy powder of good flowing properties, low oxygen content, purity using powder by atomization method, dispensing can be carried out to the ratio requirement of copper gallium alloy powder according to different application demand, the purity of preparation-obtained copper gallium alloy powder reaches 6N.
Description
Technical field
The present invention relates to a kind of preparation field of alloy powder, more particularly to a kind of preparation method of copper gallium alloy powder.
Background technology
CIGS（CuIn1-xGaxSe, CIGS）Thin-film solar cells has low cost, performance stabilization, radioresistance energy
The advantages of power is strong, spectral response range is wide.Preparing CIGS at present mainly has two kinds of thinkings：Polynary substep evaporation and metal top set
Selenizing after layer.Implementation method mainly has vapour deposition method, magnetron sputtering, molecular beam epitaxy technique, spray pyrolysis and flash set technology
Deng.Wherein magnetically controlled sputter method has the advantages that composition is controllable, raw material availability is high, film compactness is good, uniform film thickness, is mesh
The preceding most promising method for preparing CIGS films.Sputtering prepares CIG precursor thin films, because indium and gallium are all that fusing point is relatively low
Metal, it is impossible to directly prepare that performance is stable, the CIG alloy target materials of even structure, therefore preparing CIG precursor thin films
When, while using copper gallium alloy target and indium target or copper gallium alloy target and copper-indium alloy target sputtering sedimentation.In addition,
During sputtering, the defect inside target can cause arc discharge, and influence CIGS absorbs the structure and quality of layer film.
In order that the proportioning of gallium is controllable in CIGS thin-film and reduction causes the defect of arc discharge, it is necessary to make in sputter procedure
Standby high-quality copper gallium alloy target, the copper gallium alloy powder prepared at present by conventional methods such as ball millings is because pattern is irregular
And poor mobile performance, and amount of oxidation is up to more than 2000ppm, production efficiency is extremely low, simultaneously because being the life of multiple operation distinct device
Production, it is impossible to produce the alloy split of high-purity 6N and the above, so the copper gallium alloy target relative density of production is relatively low, can only achieve
95% or so, oxygen content is higher in target, it is impossible to meets requirement of the high-quality CIGS thin-film to copper gallium target, and prepares stream
It is the key factor for preparing high-quality copper gallium alloy target to move the high high-quality copper gallium alloy powder of good performance, low oxygen content, purity.
Thus, it is necessary to design a kind of preparation method of new copper gallium alloy powder to solve above-mentioned technical problem.
The content of the invention
The high high-quality copper gallium conjunction of good flowing properties, low oxygen content, purity is prepared it is an object of the invention to provide a kind of
The preparation method of bronze.
To realize object defined above, the present invention is adopted the following technical scheme that：A kind of preparation method of copper gallium alloy powder, using true
Prepared by outage pressure atomization plant, the atomization plant includes a smelting system, an atomization system, a pumped vacuum systems, a source of the gas
Supply system, an integrated control system, the smelting system include a crucible, and the atomization system includes a spray chamber, described
Spray chamber is built-in with an atomizer and the tundish above atomizer, and preparation method comprises the following steps：
S1, by two kinds of raw materials of high purity copper and high purity gallium according to ratio requirement carry out dispensing after, raw material is put into the earthenware of smelting system
In crucible；
S2, vacuumize after, under protective gas protection so that crucible temperature is warming up to 1150 ~ 1450 DEG C, the heating-up time is 25 ~
Raw materials melt in 35min, crucible is incubated 20 ~ 40min into copper gallium alloy liquid, and crucible is slowly waved so that molten metal is abundant
It is well mixed；
S3, molten metal are injected into the tundish on atomizer, and molten metal is flowed out by tundish bottom leakage eye,
It is atomized by being met during atomizer with high velocity air or current as fine drop, atomized drop is fast in the spray chamber of closing
Speed is frozen into alloy powder；
S4, be naturally cooling to normal temperature, toward atomization plant in be filled with protective gas to normal pressure and can open atomization plant and be made
Copper gallium alloy powder.
As a further improvement on the present invention, the smelting system includes being arranged on the agitating paddle above crucible.
As a further improvement on the present invention, the rocking tendency of the crucible is ± 60 °.
As a further improvement on the present invention, the protective gas is inert gas or nitrogen.
As a further improvement on the present invention, the purity of obtained copper gallium alloy powder be 6N and more than.
As a further improvement on the present invention, the purity of the high purity copper be 5N and more than.
As a further improvement on the present invention, the purity of the high purity gallium be 5N and more than.
As a further improvement on the present invention, the crucible uses high purity graphite crucible or alumina crucible.
As a further improvement on the present invention, the pressure of the atomizer is 6.8 ~ 10.4MPa.
As a further improvement on the present invention, the atomization plant also include a powder collection system, a cooling water system,
A support for supporting atomization system.
The preparation method of copper gallium alloy powder of the present invention prepares good flowing properties, low oxygen content, purity using powder by atomization method
High copper gallium alloy powder, can carry out dispensing according to different application demand to the ratio requirement of copper gallium alloy powder, prepared to obtain
The purity of copper gallium alloy powder reach 6N.
Brief description of the drawings
Fig. 1 is microcosmic for the preparation-obtained copper gallium alloy powder of preparation method embodiment 2 of copper gallium alloy powder of the present invention
Shape appearance figure.
Embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
The preparation method of copper gallium alloy powder of the present invention is prepared using vacuum high-pressure atomization plant, and atomization plant includes a melting
System, an atomization system, a pumped vacuum systems, a source of the gas supply system, an integrated control system, smelting system include an earthenware
Crucible, atomization system includes a spray chamber, and spray chamber is built-in with an atomizer and the tundish above atomizer,
In certain embodiments of the present invention, atomization plant also includes a powder collection system, a cooling water system, for supporting atomization
One support of system.
Using above-mentioned atomization plant, the preparation method of copper gallium alloy powder comprises the following steps：
S1, by two kinds of raw materials of high purity copper and high purity gallium according to ratio requirement carry out dispensing after, raw material is put into smelting system crucible
It is interior；High purity copper is solid-state, can be any forms such as particle, bar-shaped, sheet, ingot shape；High purity gallium can be liquid or Solid Gallium
Block；
S2, vacuumize after, under protective gas protection so that crucible temperature is warming up to 1150 ~ 1450 DEG C, the heating-up time is 25 ~
Raw materials melt in 35min, crucible is incubated 20 ~ 40min into copper gallium alloy liquid, and crucible is slowly waved so that molten metal is abundant
It is well mixed；
S3, molten metal are injected into the tundish on atomizer, and molten metal is flowed out by tundish bottom leakage eye,
It is atomized by being met during atomizer with high velocity air or current as fine drop, atomized drop is fast in the spray chamber of closing
Speed is frozen into alloy powder；
S4, be naturally cooling to normal temperature, toward atomization plant in be filled with protective gas to normal pressure and can open atomization plant and be made
Copper gallium alloy powder.
In certain embodiments of the present invention, smelting system includes being arranged on the agitating paddle above crucible, and agitating paddle is used
In the uniform mixing for accelerating molten metal.
In certain embodiments of the present invention, the rocking tendency of the crucible is ± 60 °, is driven by craft or motor
Crucible can be achieved continuously to wave in the range of ± 60 °, agitating paddle can be shaken during insulation is melted, by the alloy of melting
Liquid stirs.
In certain embodiments of the present invention, the protective gas is inert gas or nitrogen.
In certain embodiments of the present invention, the purity of obtained copper gallium alloy powder be 6N and more than.
In certain embodiments of the present invention, the purity of the high purity copper be 5N and more than.
In certain embodiments of the present invention, the purity of the high purity gallium be 5N and more than.
In certain embodiments of the present invention, the crucible uses high purity graphite crucible or alumina crucible.
In certain embodiments of the present invention, the pressure of the atomizer is 6.8 ~ 10.4MPa.
Embodiment 1.
By copper gallium mass ratio 75:25 weigh the high purity graphite that 5N copper particles 21kg, 5N Solid Gallium 7kg is put into atomization plant respectively
In crucible, close unlatching pumped vacuum systems after atomization plant and make it that Absolute truth reciprocal of duty cycle is 450Pa in atomization plant, is filled with 5N high-purity
Then nitrogen to normal pressure is again turned on pumped vacuum systems and vacuumizes until the Absolute truth reciprocal of duty cycle of atomization plant opens melting to 82Pa
Intermediate frequency induction heating device in system, passes through the power of slow adjusting means so that the smelting temperature in crucible is warming up to
1450 DEG C and 35min is incubated, crucible is slowly waved in insulating process, swing angle is between ± 60 °, and is interrupted shake stirring
Oar, it is ensured that aluminium alloy is full and uniform, after insulation terminates, is set to 10.4MPa by the pressure of atomizer, topples over molten alloy
Liquid, enters tundish by drainage trough, is contacted finally by atomizer with high pressure draught, and molten alloy liquid is atomized to be tiny
Drop and be quickly cooled in spray chamber formation alloy powder.Material closes atomization plant and sets atomization after the completion of being all atomized
It is standby to be cooled to normal temperature, take out and the interval spherical copper gallium alloy powder of 6N of different-grain diameter is can obtain after alloy powder is sieved, lead to
It is 142ppm to cross using oxygen content in LECO600 oxygen analysers detection and analysis powder.
Embodiment 2.
By copper gallium mass ratio 45:55 weigh 6N copper ingots 15kg, 6N liquid gallium 18.3kg respectively is put into the high-purity of atomization plant
In graphite crucible, close unlatching pumped vacuum systems after atomization plant and make it that Absolute truth reciprocal of duty cycle is 430Pa in atomization plant, is filled with 5N
Then high pure nitrogen to normal pressure is again turned on pumped vacuum systems and vacuumizes until the Absolute truth reciprocal of duty cycle of atomization plant is opened to 75Pa
Intermediate frequency induction heating device in smelting system, passes through the power of slow adjusting means so that crucible for smelting temperature is warming up to
1150 DEG C and be incubated 30min, crucible is slowly waved in insulating process, rocking tendency is ± 45 °, during simultaneously uninterrupted shake
Agitating paddle, it is ensured that aluminium alloy is full and uniform, after insulation terminates, opens high pressure draught control system, atomizer pressure is set to
6.8MPa, topples over the aluminium alloy of melting, enters tundish by drainage trough, contacted finally by atomizer with high pressure draught,
Molten alloy liquid is atomized as tiny drop and is quickly cooled in atomisation tower room formation alloy powder.All atomization is completed material
Atomization plant is closed afterwards and atomization plant is cooled to normal temperature, is taken out after alloy powder is sieved and be can obtain different-grain diameter area
Between the spherical copper gallium alloy powder of 6N, by using LECO600 oxygen analysers test and analyze powder in oxygen content be 129ppm, copper gallium
The pattern of alloyed powder is as shown in Figure 1.
Embodiment 3.
By copper gallium mass ratio 30:70 weigh the high purity graphite that 6N copper ingots 9kg, 6N liquid gallium 21kg is put into atomization plant respectively
In crucible, close unlatching pumped vacuum systems after atomization plant and make it that Absolute truth reciprocal of duty cycle is 400Pa in atomization plant, is filled with 5N high-purity
Then nitrogen to normal pressure is again turned on pumped vacuum systems and vacuumizes until the Absolute truth reciprocal of duty cycle of atomization plant opens melting to 60Pa
Intermediate frequency induction heating device in system, passes through the power of slow adjusting means so that crucible for smelting temperature is warming up to 1250 DEG C
And be incubated crucible in 25min, insulating process and slowly wave, rocking tendency is ± 25 °, during simultaneously uninterrupted shake stirring
Oar, it is ensured that aluminium alloy is full and uniform, after insulation terminates, opens high pressure draught control system, atomizer pressure is set to
8.0MPa, topples over the aluminium alloy of melting, enters tundish by drainage trough, contacted finally by atomizer with high pressure draught,
Molten alloy liquid is atomized as tiny drop and is quickly cooled in atomisation tower room formation alloy powder.All atomization is completed material
Atomization plant is closed afterwards and atomization plant is cooled to normal temperature, is taken out after alloy powder is sieved and be can obtain different-grain diameter area
Between the spherical copper gallium alloy powder of 6N, by using LECO600 oxygen analysers test and analyze powder in oxygen content be 133ppm.
The preparation method of copper gallium alloy powder of the present invention prepares good flowing properties, low oxygen content, purity using powder by atomization method
High copper gallium alloy powder, can carry out dispensing according to different application demand to the ratio requirement of copper gallium alloy powder, prepared to obtain
The purity of copper gallium alloy powder reach 6N.
Although for example purpose, having been disclosed for the preferred embodiment of the present invention, the ordinary skill people of this area
Member will realize in the case of scope and spirit of the present invention disclosed in not departing from by appended claims, various to change
It is possible for entering, increasing and replacing.
Claims (10)
1. a kind of preparation method of copper gallium alloy powder, it is characterised in that：Prepared using vacuum high-pressure atomization plant, the atomization is set
It is described molten for a smelting system, an atomization system, a pumped vacuum systems, a source of the gas supply system, an integrated control system is included
Refining system includes a crucible, and the atomization system includes a spray chamber, and the spray chamber is built-in with an atomizer and is located at
A tundish above atomizer, preparation method comprises the following steps：
S1, by two kinds of raw materials of high purity copper and high purity gallium according to ratio requirement carry out dispensing after, raw material is put into the earthenware of smelting system
In crucible；
S2, vacuumize after, under protective gas protection so that crucible temperature is warming up to 1150 ~ 1450 DEG C, the heating-up time is 25 ~
Raw materials melt in 35min, crucible is incubated 20 ~ 40min into copper gallium alloy liquid, and crucible is slowly waved so that molten metal is abundant
It is well mixed；
S3, molten metal are injected into the tundish on atomizer, and molten metal is flowed out by tundish bottom leakage eye,
It is atomized by being met during atomizer with high velocity air or current as fine drop, atomized drop is fast in the spray chamber of closing
Speed is frozen into alloy powder；
S4, be naturally cooling to normal temperature, toward atomization plant in be filled with protective gas to normal pressure and can open atomization plant and be made
Copper gallium alloy powder.
2. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The smelting system includes peace
An agitating paddle above crucible.
3. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The rocking tendency of the crucible
For ± 60 °.
4. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The protective gas is inertia
Gas or nitrogen.
5. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：Obtained copper gallium alloy powder
Purity be 6N and more than.
6. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The purity of the high purity copper is
5N and more than.
7. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The purity of the high purity gallium is
5N and more than.
8. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The crucible uses high-purity stone
Black crucible or alumina crucible.
9. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The pressure of the atomizer
For 6.8 ~ 10.4MPa.
10. the preparation method of the copper gallium alloy powder according to claim 1, it is characterised in that：The atomization plant also includes
One powder collection system, a cooling water system, the support for supporting atomization system.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108538532A (en) * | 2018-03-29 | 2018-09-14 | 南京信息工程大学 | A kind of composite magnetic and preparation method thereof |
| CN108962527A (en) * | 2018-06-28 | 2018-12-07 | 南京信息工程大学 | A kind of magnetic material and preparation method thereof |
| CN108962528A (en) * | 2018-06-29 | 2018-12-07 | 南京信息工程大学 | A kind of magnetic material and preparation method thereof with high-temperature stability |
| CN112517917A (en) * | 2020-11-25 | 2021-03-19 | 河南东微电子材料有限公司 | Preparation method of CrTiLa alloy powder for chromium-titanium target material |
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| CN107321998B (en) | 2020-01-07 |
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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 |