CN106319469A - Preparation method for copper indium gallium alloy target material - Google Patents
Preparation method for copper indium gallium alloy target material Download PDFInfo
- Publication number
- CN106319469A CN106319469A CN201610959814.7A CN201610959814A CN106319469A CN 106319469 A CN106319469 A CN 106319469A CN 201610959814 A CN201610959814 A CN 201610959814A CN 106319469 A CN106319469 A CN 106319469A
- Authority
- CN
- China
- Prior art keywords
- copper
- indium
- heater
- preparation
- carrier gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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 preparation method for a copper indium gallium alloy target material. A low-temperature preparation technique is adopted for mixing and smelting elemental indium and elemental gallium at a lower melting point, the required smelting temperature is low, the volatilization of indium and gallium can be effectively restrained and reduced, the smelting loss of indium and gallium can be reduced, and the component content of the finally prepared target material can meet the design requirement. The preparation method is convenient and simple in operation and is beneficial to the reduction of the production cost of the target material; the elemental copper powder is added into a carrier gas and is directly used as a resource of the copper element in the alloy; the density of the elemental copper powder added into the carrier gas is higher than the density of the pure carrier gas, higher kinetic energy can be formed, and in the process of airflow striking liquid flow, the refining and dispersion of the liquid flow can be realized; the kinetic energy formed by the copper powder striking the liquid flow is also higher, so that the copper is easy to form an alloy compound with indium or gallium, and the uniformity of the component and performance of the finally obtained alloy target material can be guaranteed; and the density of the prepared alloy target material is high, the grain size is small, and the electrical resistivity meets the requirement.
Description
Technical field
The present invention relates to the preparing technical field of magnetic control spattering target, be specifically related to the preparation of a kind of copper and indium gallium alloy target
Method.
Background technology
CIGS thin film solaode, by Cu(copper), In(indium), Ga(gallium) and Se(selenium) four kinds of elements constitute
Chalkopyrite crystalline membrane solaode, when having that light absorpting ability is strong, power generation stability good, transformation efficiency is high, daytime generates electricity
Between long, the many advantages such as generated energy is high, production cost is low and the energy recovery cycle is short, be gradually widely used.At present,
The structure that conventional CIGS thin film solaode is conventional is: glass/Mo electrode layer/CIGS absorbed layer/CdS cushion/intrinsic
ZnO layer/AZO Window layer/surface contact layer.For the manufacture of CIGS hull cell, the preparation of CIGS light absorbing zone is weight
The ring wanted, prepared by the main flow using magnetron sputtering deposition copper and indium gallium (CIG) alloy-layer selenizing again to have become as the industry
Technological means.The magnetron sputtering mode of copper and indium gallium alloy layer generally includes following two: the first is to use CuGa bianry alloy
Target and the mode of In target cosputtering, the second is directly to sputter CuInGa ternary alloy three-partalloy target.Therefore, no matter which kind of is prepared
Mode is required for using the alloy target material of cupric.
High-quality magnetron sputtering plating has a following requirement to target: have high consistency, component uniformly, crystallite dimension
Less and uniform, relatively low resistivity etc..High-compactness is able to ensure that target has good mechanical strength, sputtering stability,
The generation of abnormal discharge can be stoped, it is to avoid the appearance of black dross, extend 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 sedimentation rate of thin film.Target can be divided into planar targets and rotary target material two kinds from form.Plane
The utilization rate of target is relatively low, about about 30 %.And the utilization rate of rotary target material can be up to 80 more than %, owing to spattering
Exit point along with the rotation ceaselessly shift transformation of target pipe, is effectively reduced the dross poisoning of target material surface, and the carrying of cooling effect
Rise the generation that can reduce target crackle, make target as sputter coating process more stable, safer.Therefore, flat with rotary target material replacement
Face target is the development trend in magnetron sputtering plating field, proposes a series of new challenge the most also to target manufacturer.
The preparation method of CIG alloy target material has three kinds at present: smelting process, the cold spray process of controlled atmosphere and granule are colded 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 at the uniform velocity it being warmed up to 800～1100 DEG C, programming rate is 10～50 DEG C/
Min, then insulation 30～90 min, form uniform alloy liquid, then alloy liquid cast directly over knockdown target
In material mould, obtain corresponding alloy target material by controlling cooling.There are some following problems in this method: the fusing point of Cu
(1084 DEG C) differ greatly with the fusing point (29.78 DEG C) of Ga or the fusing point (156.61 DEG C) of In, on the impact cooled down very
Greatly, composition is narrower with technique " window "；Easily form mesophase, there is higher fusing point, segregation effect, formation " sweat " phase,
Target mechanical strength is made to reduce；Liquation cooling shrinkage stress is relatively big, and and mould between not there is bigger thermal coefficient of expansion not
Joining property, is easily caused target cracking；The structure and composition of target is difficult to equal control；Additionally crystallite dimension is relatively large, easily leads
Cause sputter coating is uneven, produce simultaneously in various degree beat arc phenomenon.Cold spray process uses the copper and indium gallium alloy granule of ball milling
For raw material, under the conditions of the protective atmosphere such as argon or nitrogen, utilize carrier gas by alloying pellet high-velocity spray to tube surfaces shape
Become certain thickness coating.The forming temperature ratio of this method is relatively low, can tentatively solve the alloy target material composition that smelting process causes
The problem that uneven, oxygen content is higher, but there is also following problem: the utilization rate of powder body is relatively low (typically left at 40～60 %
Right), rotary target material can only be prepared, be difficult to the production of planar targets.Granule 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 process is by after metal simple-substance melting, forms alloy through atomization process
Grain, then realizes the straight forming of plane or target by the way of cold moudling.The processing of this method is relatively easy, also portion
Divide the problem solving the composition inequality that smelting process causes, but there is also following problem: the higher (fusing point higher than copper of smelting temperature
1084 DEG C) indium of low melting point or gallium volatilization can be made serious, do not cause the alloying component of final granule and designed composition not
Join；On the one hand the particle diameter skewness of granule causes mobility bad and then affects the lifting of target density, on the other hand also leads
Cause the fluctuation of crystallite dimension.
Summary of the invention
The technical problem to be solved is, for the deficiencies in the prior art, it is provided that a kind of copper and indium gallium alloy target
Preparation method.
The present invention solves the technical scheme that above-mentioned technical problem used: the preparation side of a kind of copper and indium gallium alloy target
Method, comprises the following steps:
(1) copper, simple substance indium and Metallic Gallium 30～70:20～50:10～30 dispensing in molar ratio, described elemental copper are taken
Powder is made up of the copper granule of particle diameter 1～100 μm；
(2) preparing an equipment, this equipment includes smelting furnace and powder feeder, is arranged with heater wire around the body of heater of described smelting furnace
Circle, the diapire of the body of heater of described smelting furnace offers liquid outlet, and described powder feeder is arranged on the body of heater of described smelting furnace
Bottom, described powder feeder is provided with multiple nozzle, described multiple nozzle rings are around the end of the body of heater of described smelting furnace
Wall is arranged；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace, connect the power supply of heating coil, body of heater is heated, makes list
Matter indium and Metallic Gallium melted by heat are flowable melt, after stirring melt, by the high-pressure pump Liquid Level Pressure to melt, make to melt
Body flows out from liquid outlet, forms liquid stream, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas, described load in powder feeder
Added with described copper in gas, by described carrier gas by the multiple nozzles described in described copper feeding, make
Described copper sprays from multiple nozzles together with carrier gas, formation air-flow, the liquid stream described in the airflow strikes of ejection,
The appearance of each copper granule is coated with by liquid indium gallium liquation respectively, forms alloying pellet；
(4) alloying pellet obtained prints through compression molding or 3D and directly forms planar targets or rotary target material.
As preferably, the aperture of described liquid outlet is 0.5～2 mm.
As preferably, the body of heater of described smelting furnace is up big and down small taper.
As preferably, in step (3), the heating-up temperature of body of heater is 30～350 DEG C.
As preferably, in step (3), after high-pressure pump pressurizes, the liquid level pressure of melt is 0.1～10 MPa, molten
Body is 0.01～5 L/min from the flow that liquid outlet flows out.
As preferably, in step (3), it is mixed with the carrier gas of described copper and is sent to the flow of described multiple nozzles and be
0.01～5 L/min.
As preferably, described carrier gas is argon or nitrogen, and the gas pressure of described carrier gas is 0.8～30 MPa.
As preferably, in step (3), the angle between described liquid stream and described air-flow is 20～90 °.
As preferably, the particle diameter D50 of described alloying pellet is 5～150 μm.
Compared with prior art, it is an advantage of the current invention that:
One, the preparation method of copper and indium gallium alloy target disclosed by the invention, uses low-temperature fabrication, by simple substance relatively low for fusing point
Indium and Metallic Gallium mixed smelting, needed for it, smelting temperature is low, it is not necessary to melting fusing point is up to the copper of 1084 DEG C, compared to traditional
High temperature preparation method, can effectively suppress and reduce the volatilization of indium and gallium, reduces indium and the heat waste of gallium, it is ensured that final preparation
The constituent content of target reaches to design requirement；
Two, preparation method of the present invention, joins copper in carrier gas, directly as the source of copper in alloy, this system
Preparation Method is convenient and simple for operation, contributes to reducing the production cost of target；
Three, the density of the copper added in carrier gas is higher than simple carrier gas, can form higher kinetic energy, at airflow strikes liquid
During stream, it is possible to achieve the refinement of liquid stream and dispersion, meanwhile, the kinetic energy that copper powder shock liquid stream is formed is the highest, makes copper
It is prone to form alloy cpd with indium or gallium, it is ensured that the component of the alloy target material finally given and the uniformity of performance, preparation
The alloy target material consistency obtained is high, and crystallite dimension is little, and resistivity reaches requirement.
Accompanying drawing explanation
Fig. 1 is the structural representation preparing copper and indium gallium alloy target device therefor in embodiment.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
The preparation method of the copper and indium gallium alloy target of embodiment 1, comprises the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 40:40:20 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 1.0 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 300 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 2.5 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream
4, the flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder,
Carrier gas 31 is argon, and the gas pressure of carrier gas 31 is 18 MPa, added with copper in carrier gas 31, by carrier gas 31 by elemental copper
Powder is sent in multiple nozzles 3 with the flow of 0.01～5 L/min, makes copper together with carrier gas 31 from multiple nozzles 3
Ejection, forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 45 °, and the air-flow 5 of ejection clashes into liquid stream 4, each copper granule 13
Appearance is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained directly forms planar targets through compression molding.
The preparation method of the copper and indium gallium alloy target of embodiment 2, comprises the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 50:35:15 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 1.5 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 250 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 2 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream 4,
The flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder, carries
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 copper
Send in multiple nozzles 3 with the flow of 0.01～5 L/min, make copper spray from multiple nozzles 3 together with carrier gas 31
Going out, form air-flow 5, the angle α between liquid stream 4 and air-flow 5 is 30 °, and the air-flow 5 of ejection clashes into liquid stream 4, outside each copper granule 13
Table is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained directly forms planar targets through compression molding.
The preparation method of the copper and indium gallium alloy target of embodiment 3, comprises the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 35:35:30 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 0.5 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 200 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 10 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream
4, the flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder,
Carrier gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 25 MPa, added with copper in carrier gas 31, by carrier gas 31 by elemental copper
Powder is sent in multiple nozzles 3 with the flow of 0.01～5 L/min, makes copper together with carrier gas 31 from multiple nozzles 3
Ejection, forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 20 °, and the air-flow 5 of ejection clashes into liquid stream 4, each copper granule 13
Appearance is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained prints through 3D and directly forms planar targets.
The preparation method of the copper and indium gallium alloy target of embodiment 4, comprises the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 60:30:10 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 1.2 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 180 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 1.5 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream
4, the flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder,
Carrier gas 31 is argon, and the gas pressure of carrier gas 31 is 15 MPa, added with copper in carrier gas 31, by carrier gas 31 by elemental copper
Powder is sent in multiple nozzles 3 with the flow of 0.01～5 L/min, makes copper together with carrier gas 31 from multiple nozzles 3
Ejection, forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 60 °, and the air-flow 5 of ejection clashes into liquid stream 4, each copper granule 13
Appearance is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained prints through 3D and directly forms rotary target material.
The preparation method of the copper and indium gallium alloy target of embodiment 5, comprises the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 30:50:20 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 1.6 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 350 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 0.5 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream
4, the flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder,
Carrier gas 31 is argon, and the gas pressure of carrier gas 31 is 6 MPa, added with copper in carrier gas 31, by carrier gas 31 by elemental copper
Powder is sent in multiple nozzles 3 with the flow of 0.01～5 L/min, makes copper together with carrier gas 31 from multiple nozzles 3
Ejection, forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 55 °, and the air-flow 5 of ejection clashes into liquid stream 4, each copper granule 13
Appearance is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained prints through 3D and directly forms rotary target material.
The preparation method of the copper and indium gallium alloy target of embodiment 6, comprises the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 45:25:30 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 0.7 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 280 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 8 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream 4,
The flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder, carries
Gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 1.0 MPa, added with copper in carrier gas 31, by carrier gas 31 by elemental copper
Powder is sent in multiple nozzles 3 with the flow of 0.01～5 L/min, makes copper together with carrier gas 31 from multiple nozzles 3
Ejection, forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 75 °, and the air-flow 5 of ejection clashes into liquid stream 4, each copper granule 13
Appearance is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained 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 comprise the following steps:
(1) taking copper, simple substance indium and Metallic Gallium 70:20:10 dispensing in molar ratio, copper is by particle diameter 1～100 μm
Copper granule 13 form；
(2) preparing an equipment, its structural representation is as it is shown in figure 1, this equipment includes that smelting furnace 1 and powder feeder (do not show in figure
Go out), it is arranged with heating coil 2 around the body of heater of smelting furnace 1, the body of heater of smelting furnace 1 is up big and down small taper, smelting furnace 1
The diapire of body of heater offers liquid outlet 11, and the aperture of liquid outlet 11 is 0.9 mm, and powder feeder is arranged under the body of heater of smelting furnace 1
Portion, powder feeder is provided with multiple nozzle 3, and multiple nozzles 3 are arranged around the diapire of the body of heater of smelting furnace 1；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace 1, connect the power supply of heating coil 2, body of heater is heated, stove
The heating-up temperature of body is 150 DEG C, and making simple substance indium and Metallic Gallium melted by heat is flowable melt 12, after stirring melt 12, logical
Cross high-pressure pump (not shown) Liquid Level Pressure 6 MPa to melt 12, make melt 12 flow out from liquid outlet 11, form liquid stream 4,
The flow of liquid stream 4 is 0.01～5 L/min, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas 31 in powder feeder, carries
Gas 31 is nitrogen, and the gas pressure of carrier gas 31 is 3.5 MPa, added with copper in carrier gas 31, by carrier gas 31 by elemental copper
Powder is sent in multiple nozzles 3 with the flow of 0.01～5 L/min, makes copper together with carrier gas 31 from multiple nozzles 3
Ejection, forms air-flow 5, and the angle α between liquid stream 4 and air-flow 5 is 80 °, and the air-flow 5 of ejection clashes into liquid stream 4, each copper granule 13
Appearance is coated with by liquid indium gallium liquation respectively, forms the alloying pellet 6 that particle diameter D50 is 5～150 μm；
(4) alloying pellet 6 obtained prints through 3D and directly forms planar targets.
Above example uses the planar targets for preparing of low-temperature fabrication or rotary target material, eutectic in preparation process
Indium and the heat waste of gallium of point are few, the constituent content of the target of final preparation reach to design requirement, its component and performance uniformly,
Consistency is high, and crystallite dimension is little, and resistivity reaches requirement.
Claims (9)
1. the preparation method of a copper and indium gallium alloy target, it is characterised in that comprise the following steps:
(1) copper, simple substance indium and Metallic Gallium 30～70:20～50:10～30 dispensing in molar ratio, described elemental copper are taken
Powder is made up of the copper granule of particle diameter 1～100 μm；
(2) preparing an equipment, this equipment includes smelting furnace and powder feeder, is arranged with heater wire around the body of heater of described smelting furnace
Circle, the diapire of the body of heater of described smelting furnace offers liquid outlet, and described powder feeder is arranged on the body of heater of described smelting furnace
Bottom, described powder feeder is provided with multiple nozzle, described multiple nozzle rings are around the end of the body of heater of described smelting furnace
Wall is arranged；
(3) simple substance indium and Metallic Gallium are placed in the body of heater of smelting furnace, connect the power supply of heating coil, body of heater is heated, makes list
Matter indium and Metallic Gallium melted by heat are flowable melt, after stirring melt, by the high-pressure pump Liquid Level Pressure to melt, make to melt
Body flows out from liquid outlet, forms liquid stream, and meanwhile, powder feeder works, and is passed through band pressurized carrier gas, described load in powder feeder
Added with described copper in gas, by described carrier gas by the multiple nozzles described in described copper feeding, make
Described copper sprays from multiple nozzles together with carrier gas, formation air-flow, the liquid stream described in the airflow strikes of ejection,
The appearance of each copper granule is coated with by liquid indium gallium liquation respectively, forms alloying pellet；
(4) alloying pellet obtained prints through compression molding or 3D and directly forms planar targets or rotary target material.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that described liquid outlet
Aperture be 0.5～2 mm.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that described smelting furnace
Body of heater be up big and down small taper.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that in step (3), stove
The heating-up temperature of body is 30～350 DEG C.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that in step (3), warp
After high-pressure pump pressurization, the liquid level pressure of melt is 0.1～10 MPa, and melt is 0.01～5 from the flow that liquid outlet flows out
L/min。
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that in step (3), mixed
It is 0.01～5 L/min that the carrier gas having described copper is sent to the flow of described multiple nozzles.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that described carrier gas is
Argon or nitrogen, the gas pressure of described carrier gas is 0.8～30 MPa.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that in step (3), institute
Angle between the liquid stream stated and described air-flow is 20～90 °.
The preparation method of a kind of copper and indium gallium alloy target the most according to claim 1, it is characterised in that described alloy
The particle diameter D50 of grain is 5～150 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610959814.7A CN106319469B (en) | 2016-10-28 | 2016-10-28 | A kind of preparation method of copper and indium gallium alloy target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610959814.7A CN106319469B (en) | 2016-10-28 | 2016-10-28 | A kind of preparation method of copper and indium gallium alloy target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106319469A true CN106319469A (en) | 2017-01-11 |
| CN106319469B CN106319469B (en) | 2018-08-24 |
Family
ID=57819548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610959814.7A Active CN106319469B (en) | 2016-10-28 | 2016-10-28 | A kind of preparation method of copper and indium gallium alloy target |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106319469B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019024421A1 (en) * | 2017-08-04 | 2019-02-07 | 米亚索乐装备集成（福建）有限公司 | Method for preparing target material and target material |
| CN109763109A (en) * | 2019-03-04 | 2019-05-17 | 中国科学院理化技术研究所 | A kind of liquid metal target and its method for preparing alloy film |
| CN110029309A (en) * | 2017-11-08 | 2019-07-19 | 北京铂阳顶荣光伏科技有限公司 | The system and method for forming selenizing composite metal powder |
| WO2019237545A1 (en) * | 2018-06-15 | 2019-12-19 | 米亚索乐装备集成（福建）有限公司 | Method for preparing copper indium gallium alloy powder |
| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117276A (en) * | 1993-02-06 | 1996-02-21 | 欧斯普瑞金属有限公司 | Production of powder |
| CN2258500Y (en) * | 1995-11-23 | 1997-07-30 | 中南工业大学 | Jet sedimentation device for preparing metal base composite material |
| CN1548257A (en) * | 2003-05-09 | 2004-11-24 | 宝钢集团上海第一钢铁有限公司 | Method and apparatus of adding alloy into liquid metal |
| CN103317124A (en) * | 2013-06-05 | 2013-09-25 | 无锡舒玛天科新能源技术有限公司 | Method for preparing rotary copper, indium and gallium target |
| CN104451563A (en) * | 2013-09-12 | 2015-03-25 | 汉能新材料科技有限公司 | Copper indium gallium selenium target material preparation and application method |
| WO2015114914A1 (en) * | 2014-01-28 | 2015-08-06 | 三菱マテリアル株式会社 | Cu-Ga ALLOY SPUTTERING TARGET AND METHOD FOR PRODUCING SAME |
-
2016
- 2016-10-28 CN CN201610959814.7A patent/CN106319469B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1117276A (en) * | 1993-02-06 | 1996-02-21 | 欧斯普瑞金属有限公司 | Production of powder |
| CN2258500Y (en) * | 1995-11-23 | 1997-07-30 | 中南工业大学 | Jet sedimentation device for preparing metal base composite material |
| CN1548257A (en) * | 2003-05-09 | 2004-11-24 | 宝钢集团上海第一钢铁有限公司 | Method and apparatus of adding alloy into liquid metal |
| CN103317124A (en) * | 2013-06-05 | 2013-09-25 | 无锡舒玛天科新能源技术有限公司 | Method for preparing rotary copper, indium and gallium target |
| CN104451563A (en) * | 2013-09-12 | 2015-03-25 | 汉能新材料科技有限公司 | Copper indium gallium selenium target material preparation and application method |
| WO2015114914A1 (en) * | 2014-01-28 | 2015-08-06 | 三菱マテリアル株式会社 | Cu-Ga ALLOY SPUTTERING TARGET AND METHOD FOR PRODUCING SAME |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019024421A1 (en) * | 2017-08-04 | 2019-02-07 | 米亚索乐装备集成（福建）有限公司 | Method for preparing target material and target material |
| CN110029309A (en) * | 2017-11-08 | 2019-07-19 | 北京铂阳顶荣光伏科技有限公司 | The system and method for forming selenizing composite metal powder |
| WO2019237545A1 (en) * | 2018-06-15 | 2019-12-19 | 米亚索乐装备集成（福建）有限公司 | Method for preparing copper indium gallium alloy 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 |
| CN109763109A (en) * | 2019-03-04 | 2019-05-17 | 中国科学院理化技术研究所 | A kind of liquid metal target and its method for preparing alloy film |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106319469B (en) | 2018-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106319469A (en) | Preparation method for copper indium gallium alloy target material | |
| JP5818139B2 (en) | Cu-Ga alloy target material and method for producing the same | |
| JP2010265544A (en) | Cu-Ga ALLOY SPUTTERING TARGET AND PROCESS FOR MANUFACTURING THEREOF | |
| TWI471442B (en) | Cu-Ga alloy powder, Cu-Ga alloy powder, and Cu-Ga alloy sputtering target manufacturing method and Cu-Ga alloy sputtering target | |
| WO2019024420A1 (en) | Alloy powder and preparation method therefor | |
| CN107876794A (en) | The Mo powder of increasing material manufacturing, the preparation method of Mo alloy spherical powder | |
| CN110117764B (en) | Thermal barrier/high-temperature low-infrared-emissivity integrated coating, metal composite material with coating and preparation method of metal composite material | |
| CN102352483A (en) | Preparation method of silicon-aluminium alloy hollow rotary target for vacuum sputtering coating | |
| CN113005448A (en) | Method for preparing tungsten-copper or molybdenum-copper composite layer on surface of copper alloy through laser cladding | |
| JP4957968B2 (en) | Cu-In-Ga ternary sintered alloy sputtering target and method for producing the same | |
| CN111151764A (en) | Method for preparing CuNiSi spherical powder based on VIGA process | |
| CN104475746A (en) | Rotation centrifugation atomization technology and device for manufacturing small beryllium balls and small beryllium alloy balls | |
| WO2023115929A1 (en) | High-entropy metal oxide coating, preparation method therefor and use thereof | |
| CN102286724A (en) | Copper and gallium alloy rotating target for photovoltaic absorption layer sputtering film coating and preparation method | |
| CN104878342A (en) | Method and device for preparing tungsten powder reinforced aluminum matrix composite | |
| CN208696304U (en) | A kind of device of low-voltage direct plasma gun preparation 3D printing titanium valve | |
| CN103614686A (en) | Method for preparing intermetallic compound composite coating through heterogeneous double-wire spraying and thermal treatment | |
| CN111101043B (en) | CrMoVNbAl high-entropy alloy manufactured by laser additive manufacturing and forming process thereof | |
| CN107999776A (en) | A kind of preparation process of 3D printing metal dust | |
| CN101327515A (en) | Method for processing thick line blank of alloy wire rod made from leadless metal spraying material | |
| CN114990383B (en) | Titanium alloy for improving yield ratio of electrode induction smelting inert gas atomized powder fine powder and preparation method of atomized powder | |
| CN111118437A (en) | Rotary silicon-phosphorus alloy target material and preparation method and application thereof | |
| JP5740891B2 (en) | Cu-Ga alloy sputtering target and method for producing Cu-Ga alloy sputtering target | |
| CN102627472B (en) | Laser near net shaping method of low-porosity titanium alumina ceramic piece | |
| TWI665317B (en) | Cu-ga alloy sputtering target, and method for producing cu-ga alloy sputtering target |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |