CN106319469B - A kind of preparation method of copper and indium gallium alloy target - Google Patents
A kind of preparation method of copper and indium gallium alloy target Download PDFInfo
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- CN106319469B CN106319469B CN201610959814.7A CN201610959814A CN106319469B CN 106319469 B CN106319469 B CN 106319469B CN 201610959814 A CN201610959814 A CN 201610959814A CN 106319469 B CN106319469 B CN 106319469B
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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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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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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
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- B22F2009/0824—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 with a specific atomising 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
- B22F2009/0848—Melting process before atomisation
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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
- B22F2009/088—Fluid nozzles, e.g. angle, distance
Abstract
The invention discloses a kind of preparation methods of copper and indium gallium alloy target, using low-temperature fabrication, by lower melting-point simple substance indium and Metallic Gallium mixed smelting, its required smelting temperature is low, it can effectively inhibit and reduce the volatilization of indium and gallium, the heat waste of indium and gallium is reduced, ensures that the constituent content of the target finally prepared reaches design requirement；The preparation method is easy to operate, simply, contribute to the production cost of reduction target, copper is added in carrier gas by it, directly as the source of copper in alloy, the density for the copper being added in carrier gas is higher than simple carrier gas, higher kinetic energy can be formed, during air-flow hits liquid stream, the refinement and dispersion of liquid stream may be implemented, simultaneously, it is also higher that copper powder shock liquid stream is formed by kinetic energy, copper is set to be easy to form alloy cpd with indium or gallium, ensure the component of finally obtained alloy target material and the uniformity of performance, the alloy target material consistency being prepared is high, crystallite dimension is small, resistivity reaches requirement.
Description
Technical field
The present invention relates to the preparing technical fields of magnetic control spattering target, and in particular to a kind of preparation of copper and indium gallium alloy target
Method.
Background technology
CIGS thin film solar cell is by Cu（Copper）、In（Indium）、Ga（Gallium）And Se（Selenium）What four kinds of elements were constituted
Chalcopyrite crystalline membrane solar cell, with when light absorpting ability is strong, power generation stability is good, transformation efficiency is high, daytime generates electricity
Between the long, many advantages such as generated energy is high, production cost is low and the energy recovery period is short, be gradually widely used.Currently,
Commonly the common structure of CIGS thin film solar cell is：Glass/Mo electrode layers/CIGS absorbed layers/CdS buffer layers/intrinsic
ZnO layer/AZO Window layers/surface contact layer.For the manufacture of CIGS hull cell, the preparation of CIGS light absorbing layers is weight
The ring wanted, using magnetron sputtering deposition copper and indium gallium（CIG）Alloy-layer again selenizing have become the industry a mainstream prepare
Technological means.The magnetron sputtering mode of copper and indium gallium alloy layer generally includes following two：The first is to use CuGa bianry alloys
The mode of target and In target cosputterings, second is direct sputtering CuInGa ternary alloy three-partalloy targets.Therefore, no matter which kind of is prepared
Mode is required for using the alloy target material of cupric.
The magnetron sputtering plating of high quality has following requirement to target：With high consistency, component uniformly, crystallite dimension
Smaller and uniform, lower resistivity etc..High-compactness can ensure that target has good mechanical strength, sputtering stability,
The generation that can prevent abnormal discharge avoids the appearance of black dross, extends target service life；The crystal grain of fine uniform has
Help reduce sputtering power, improve sputter rate and increase the uniformity of plated film；And high conductivity is advantageously implemented quickly
D.c. sputtering deposits, and improves the deposition rate of film.Target can be divided into two kinds of planar targets and rotary target material from form.Plane
The utilization rate of target is relatively low, about 30 % or so.And the utilization rate of rotary target material can be up to 80 % or more, due to splashing
Exit point can effectively reduce the dross poisoning of target material surface with the rotation ceaselessly shift transformation of target pipe, and cooling effect carries
The generation of target crackle can be reduced by rising, and keep target as sputter coating process more stable, safer.Therefore, it is substituted with rotary target material flat
Face target is the development trend in magnetron sputtering plating field, while also proposing a series of new challenges to target manufacturer.
At present there are three types of the preparation methods of CIG alloy target materials：Smelting process, the cold spraying of controlled atmosphere and particle cold pressing
The method of forming.Chinese patent application 200510011859.3 discloses a kind of method that smelting process prepares copper gallium target, by Metallic Gallium
With elemental copper under gas shield or vacuum state, first it being at the uniform velocity warming up to 800~1100 DEG C, heating rate is 10~50 DEG C/
Then min keeps the temperature 30~90 min, forms uniform alloy liquid, alloy liquid is then cast directly over knockdown target
In material mold, corresponding alloy target material is obtained by controlling cooling.There are some following in this method：The fusing point of Cu
（1084 ℃）With the fusing point of Ga（29.78 ℃）Or the fusing point of In（156.61 ℃）It differs greatly, very to cooling influence
Greatly, ingredient and technique " window " are relatively narrow；It is easy to form interphase, there is higher fusing point, segregation effect, formation " sweat " phase,
Make the reduction of target mechanical strength；Melt cooling shrinkage stress is larger, and between mold there are larger coefficient of thermal expansion not
With property, target cracking is easily led to；The structure and composition of target is difficult to equal control；In addition crystallite dimension is relatively large, is easy to lead
It causes sputter coating uneven, while generating and different degrees of beating arc phenomenon.Cold spraying uses the copper and indium gallium alloy particle of ball milling
For raw material, under the conditions of the protective atmospheres such as argon gas or nitrogen, using carrier gas by alloying pellet high-velocity spray to tube surfaces shape
At certain thickness coating.The forming temperature of this method is relatively low, can tentatively solve alloy target material ingredient caused by smelting process
Problem uneven, oxygen content is higher, but there is also following problems：The utilization rate of powder is relatively low（Generally on the left sides 40~60 %
It is right）, rotary target material can only be prepared, be difficult to the production of planar targets.Particle cold moudling method is the system that developed in the recent period
The new method of standby copper and indium gallium alloy target, common flow are to form alloy by atomization process by after metal simple-substance melting
Grain, then realizes the straight forming of plane or target by way of cold moudling.This method processing is relatively easy, also portion
Divide and solve the problems, such as that ingredient caused by smelting process is uneven, but there is also following problems：Smelting temperature is higher（Higher than the fusing point of copper
1084 ℃）Indium or the gallium volatilization of low melting point can be made serious, do not lead to the alloying component of final particle and designed ingredient not
Match；The inhomogenous aspect of particle diameter distribution of particle causes mobility bad and then influences the promotion of target density, on the other hand also leads
Cause the fluctuation of crystallite dimension.
Invention content
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of copper and indium gallium alloy target
Preparation method.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of preparation side of copper and indium gallium alloy target
Method includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 30~70：20~50：10~30 dispensings, the list
Matter copper powder is made of the copper particle of 1~100 μm of grain size；
（2）Prepare an equipment, which includes smelting furnace and powder feeder, is arranged with and adds around the furnace body of the smelting furnace
The bottom wall of heat coil, the furnace body of the smelting furnace offers fluid hole, and the powder feeder is arranged in the smelting furnace
The lower part of furnace body is equipped with multiple nozzles, furnace body of the multiple nozzle rings around the smelting furnace on the powder feeder
Bottom wall setting；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace, the power supply of heating coil is connected, furnace body is heated,
Simple substance indium and Metallic Gallium melted by heat is set to be flowable melt, after stirring melt, by high-pressure pump to the Liquid Level Pressure of melt,
So that melt is flowed out from fluid hole, form liquid stream, at the same time, powder feeder work is passed through band pressurized carrier gas into powder feeder, described
Carrier gas in added with the copper, the copper is sent by the carrier gas by multiple nozzles
It is interior, so that the copper is sprayed from multiple nozzles together with carrier gas, forms air-flow, described in the air-flow shock of ejection
The appearance of liquid stream, each copper particle is coated by liquid indium gallium melt respectively, forms alloying pellet；
（4）Through compression molding, either 3D printing directly forms planar targets or rotary target material to obtained alloying pellet.
Preferably, the aperture of the fluid hole is 0.5~2 mm.
Preferably, the furnace body of the smelting furnace is up big and down small taper.
Preferably, step（3）In, the heating temperature of furnace body is 30~350 DEG C.
Preferably, step（3）In, after high-pressure pump pressurizes, the liquid level pressure of melt is 0.1~10 MPa, is melted
The flow that body is flowed out from fluid hole is 0.01~5 L/min.
Preferably, step（3）In, the carrier gas for being mixed with the copper is sent to the flows of multiple nozzles and is
0.01~5 L/min.
Preferably, the carrier gas is argon gas or nitrogen, the gas pressure of the carrier gas is 0.8~30 MPa.
Preferably, step（3）In, the angle between the liquid stream and the air-flow is 20~90 °.
Preferably, the grain size D50 of the alloying pellet is 5~150 μm.
Compared with the prior art, the advantages of the present invention are as follows：
One, the preparation method of copper and indium gallium alloy target disclosed by the invention will be lower melting-point using low-temperature fabrication
Simple substance indium and Metallic Gallium mixed smelting, required smelting temperature is low, 1084 DEG C of copper is up to without melting fusing point, compared to biography
The high temperature preparation method of system can effectively inhibit and reduce the volatilization of indium and gallium, reduce the heat waste of indium and gallium, ensure final system
The constituent content of standby target reaches design requirement；
Two, preparation method of the present invention, copper is added in carrier gas, directly as the source of copper in alloy,
The preparation method is convenient and simple for operation, contributes to the production cost for reducing target；
Three, the density for the copper being added in carrier gas is higher than simple carrier gas, can form higher kinetic energy, be hit in air-flow
During hitting liquid stream, the refinement and dispersion of liquid stream may be implemented, meanwhile, copper powder hits liquid stream, and to be formed by kinetic energy also higher,
Copper is set to be easy to form alloy cpd with indium or gallium, it is ensured that the component of finally obtained alloy target material and the uniformity of performance,
The alloy target material consistency being prepared is high, and crystallite dimension is small, and resistivity reaches requirement.
Description of the drawings
Fig. 1 is the structural schematic diagram that copper and indium gallium alloy target device therefor is prepared in embodiment.
Specific implementation mode
Below in conjunction with attached drawing embodiment, present invention is further described in detail.
The preparation method of the copper and indium gallium alloy target of embodiment 1, includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 40：40：20 dispensings, copper is by grain size 1~100
μm copper particle 13 form；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 1.0 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 300 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 2.5 MPa of Liquid Level Pressure of melt 12, melt 12 is set to be flowed out from fluid hole 11, shape
At liquid stream 4, the flow of liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressure into powder feeder and carries
Gas 31, carrier gas 31 are argon gas, and the gas pressure of carrier gas 31 is 18 MPa, and carrier gas 31 is interior added with copper, will by carrier gas 31
Copper is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple sprays
It is sprayed in mouth 3, forms air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 45 °, and the air-flow 5 of ejection hits liquid stream 4, each copper
The appearance of grain 13 is coated by liquid indium gallium melt respectively, forms the alloying pellet 6 that grain size D50 is 5~150 μm；
（4）Obtained alloying pellet 6 directly forms planar targets through compression molding.
The preparation method of the copper and indium gallium alloy target of embodiment 2, includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 50：35：15 dispensings, copper is by grain size 1~100
μm copper particle 13 form；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 1.5 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 250 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 2 MPa of Liquid Level Pressure of melt 12, melt 12 is made to be flowed out from fluid hole 11, is formed
The flow of liquid stream 4, liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressurized carrier gas into powder feeder
31, carrier gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 2 MPa, added with copper in carrier gas 31, by carrier gas 31 by simple substance
Copper powder is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple nozzles 3
Middle ejection forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 30 °, and the air-flow 5 of ejection hits liquid stream 4, each copper particle 13
Appearance coated respectively by liquid indium gallium melt, forms grain size D50 as 5~150 μm of alloying pellet 6；
（4）Obtained alloying pellet 6 directly forms planar targets through compression molding.
The preparation method of the copper and indium gallium alloy target of embodiment 3, includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 35：35：30 dispensings, copper by grain size 1~
100 μm of copper particle 13 forms；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 0.5 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 200 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 10 MPa of Liquid Level Pressure of melt 12, melt 12 is made to be flowed out from fluid hole 11, is formed
The flow of liquid stream 4, liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressurized carrier gas into powder feeder
31, carrier gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 25 MPa, and carrier gas 31 is interior added with copper, will be single by carrier gas 31
Matter copper powder is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple nozzles
It is sprayed in 3, forms air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 20 °, and the air-flow 5 of ejection hits liquid stream 4, each copper particle
13 appearance is coated by liquid indium gallium melt respectively, forms the alloying pellet 6 that grain size D50 is 5~150 μm；
（4）Obtained alloying pellet 6 directly forms planar targets through 3D printing.
The preparation method of the copper and indium gallium alloy target of embodiment 4, includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 60：30：10 dispensings, copper is by grain size 1~100
μm copper particle 13 form；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 1.2 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 180 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 1.5 MPa of Liquid Level Pressure of melt 12, melt 12 is set to be flowed out from fluid hole 11, shape
At liquid stream 4, the flow of liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressure into powder feeder and carries
Gas 31, carrier gas 31 are argon gas, and the gas pressure of carrier gas 31 is 15 MPa, and carrier gas 31 is interior added with copper, will by carrier gas 31
Copper is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple sprays
It is sprayed in mouth 3, forms air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 60 °, and the air-flow 5 of ejection hits liquid stream 4, each copper
The appearance of grain 13 is coated by liquid indium gallium melt respectively, forms the alloying pellet 6 that grain size D50 is 5~150 μm；
（4）Obtained alloying pellet 6 directly forms rotary target material through 3D printing.
The preparation method of the copper and indium gallium alloy target of embodiment 5, includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 30：50：20 dispensings, copper is by grain size 1~100
μm copper particle 13 form；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 1.6 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 350 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 0.5 MPa of Liquid Level Pressure of melt 12, melt 12 is set to be flowed out from fluid hole 11, shape
At liquid stream 4, the flow of liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressure into powder feeder and carries
Gas 31, carrier gas 31 are argon gas, and the gas pressure of carrier gas 31 is 6 MPa, and carrier gas 31 is interior added with copper, will be single by carrier gas 31
Matter copper powder is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple nozzles
It is sprayed in 3, forms air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 55 °, and the air-flow 5 of ejection hits liquid stream 4, each copper particle
13 appearance is coated by liquid indium gallium melt respectively, forms the alloying pellet 6 that grain size D50 is 5~150 μm；
（4）Obtained alloying pellet 6 directly forms rotary target material through 3D printing.
The preparation method of the copper and indium gallium alloy target of embodiment 6, includes the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 45：25：30 dispensings, copper is by grain size 1~100
μm copper particle 13 form；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 0.7 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 280 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 8 MPa of Liquid Level Pressure of melt 12, melt 12 is made to be flowed out from fluid hole 11, is formed
The flow of liquid stream 4, liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressurized carrier gas into powder feeder
31, carrier gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 1.0 MPa, and carrier gas 31 is interior added with copper, will be single by carrier gas 31
Matter copper powder is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple nozzles
It is sprayed in 3, forms air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 75 °, and the air-flow 5 of ejection hits liquid stream 4, each copper particle
13 appearance is coated by liquid indium gallium melt respectively, forms the alloying pellet 6 that grain size D50 is 5~150 μm；
（4）Obtained alloying pellet 6 directly forms planar targets through compression molding.
The preparation method of the copper and indium gallium alloy target of embodiment 7, it is characterised in that include the following steps：
（1）Take copper, simple substance indium and Metallic Gallium in molar ratio 70：20：10 dispensings, copper is by grain size 1~100
μm copper particle 13 form；
（2）Prepare an equipment, structural schematic diagram is as shown in Figure 1, the equipment includes smelting furnace 1 and powder feeder（In figure not
It shows）, heating coil 2 is arranged with around the furnace body of smelting furnace 1, the furnace body of smelting furnace 1 is up big and down small taper, smelting furnace 1
The bottom wall of furnace body offer fluid hole 11, the aperture of fluid hole 11 is 0.9 mm, and the furnace body in smelting furnace 1 is arranged in powder feeder
Lower part is equipped with multiple nozzles 3, bottom wall setting of the multiple nozzles 3 around the furnace body of smelting furnace 1 on powder feeder；
（3）Simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace 1, connect the power supply of heating coil 2, to furnace body plus
The heating temperature of heat, furnace body is 150 DEG C, and it is flowable melt 12, stirring melt 12 to make simple substance indium and Metallic Gallium melted by heat
Afterwards, pass through high-pressure pump（It is not shown in figure）To 6 MPa of Liquid Level Pressure of melt 12, melt 12 is made to be flowed out from fluid hole 11, is formed
The flow of liquid stream 4, liquid stream 4 is 0.01~5 L/min, and at the same time, powder feeder work is passed through band pressurized carrier gas into powder feeder
31, carrier gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 3.5 MPa, and carrier gas 31 is interior added with copper, will be single by carrier gas 31
Matter copper powder is sent into the flow of 0.01~5 L/min in multiple nozzles 3, makes copper together with carrier gas 31 from multiple nozzles
It is sprayed in 3, forms air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 80 °, and the air-flow 5 of ejection hits liquid stream 4, each copper particle
13 appearance is coated by liquid indium gallium melt respectively, forms the alloying pellet 6 that grain size D50 is 5~150 μm；
（4）Obtained alloying pellet 6 directly forms planar targets through 3D printing.
Above example uses the low-temperature fabrication planar targets or rotary target material that are prepared, eutectic in preparation process
The indium of point and the heat waste of gallium are few, and the constituent content of the target finally prepared reaches design requirement, component and performance uniformly,
Consistency is high, and crystallite dimension is small, and resistivity reaches requirement.
Claims (6)
1. a kind of preparation method of copper and indium gallium alloy target, it is characterised in that include the following steps：
(1) copper, simple substance indium and Metallic Gallium in molar ratio 30~70 is taken：20~50：10~30 dispensings, the elemental copper
Powder is made of the copper particle of 1~100 μm of grain size；
(2) prepare an equipment, which includes smelting furnace and powder feeder, and heater wire is arranged with around the furnace body of the smelting furnace
Circle, the bottom wall of the furnace body of the smelting furnace offer fluid hole, and the furnace body in the smelting furnace is arranged in the powder feeder
Lower part, multiple nozzles, the bottom of furnace body of the multiple nozzle rings around the smelting furnace are installed on the powder feeder
Wall is arranged；
(3) simple substance indium and Metallic Gallium are placed in the furnace body of smelting furnace, connect the power supply of heating coil, furnace body is heated, list is made
Matter indium and Metallic Gallium melted by heat are flowable melt, after stirring melt, by high-pressure pump to the Liquid Level Pressure of melt, make to melt
Body is flowed out from fluid hole, forms liquid stream, and at the same time, powder feeder work is passed through band pressurized carrier gas, the load into powder feeder
Added with the copper in gas, the copper is sent into multiple nozzles by the carrier gas, is made
The copper is sprayed together with carrier gas from multiple nozzles, forms air-flow, and the air-flow of ejection hits the liquid stream,
The appearance of each copper particle is coated by liquid indium gallium melt respectively, forms alloying pellet；
Wherein, after high-pressure pump pressurizes, the liquid level pressure of melt is 0.1~10MPa, the flow that melt is flowed out from fluid hole
For 0.01~5L/min；The carrier gas for being mixed with the copper is sent to the flow of multiple nozzles as 0.01~5L/
min；Angle between the liquid stream and the air-flow is 20~90 °；
(4) through compression molding, either 3D printing directly forms planar targets or rotary target material to the alloying pellet obtained.
2. a kind of preparation method of copper and indium gallium alloy target according to claim 1, it is characterised in that the fluid hole
Aperture be 0.5~2mm.
3. a kind of preparation method of copper and indium gallium alloy target according to claim 1, it is characterised in that the smelting furnace
Furnace body be up big and down small taper.
4. a kind of preparation method of copper and indium gallium alloy target according to claim 1, it is characterised in that in step (3), stove
The heating temperature of body is 30~350 DEG C.
5. a kind of preparation method of copper and indium gallium alloy target according to claim 1, it is characterised in that the carrier gas is
The gas pressure of argon gas or nitrogen, the carrier gas is 0.8~30MPa.
6. a kind of preparation method of copper and indium gallium alloy target according to claim 1, it is characterised in that the alloy
The grain size D50 of grain is 5~150 μm.
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| CN107557737B (en) * | 2017-08-04 | 2019-12-20 | 领凡新能源科技(北京)有限公司 | Method for preparing tubular target material |
| US20190134651A1 (en) * | 2017-11-08 | 2019-05-09 | Beijing Apollo Ding Rong Solar Technology Co., Ltd. | System and method of forming selenized composite metal powder |
| CN110605399A (en) * | 2018-06-15 | 2019-12-24 | 米亚索乐装备集成（福建）有限公司 | Preparation method of copper-indium-gallium alloy powder |
| CN109763109B (en) * | 2019-03-04 | 2022-03-04 | 中国科学院理化技术研究所 | Liquid metal target material and method for preparing alloy film by using same |
| CN113523292A (en) * | 2021-07-16 | 2021-10-22 | 湖南金坤新材料有限公司 | Method for producing aluminum-scandium target material through 3D printing equipment |
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| CN2258500Y (en) * | 1995-11-23 | 1997-07-30 | 中南工业大学 | Jet sedimentation device for preparing metal base composite material |
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