CN107099775A - The preparation method of CIGS target material metal layer - Google Patents
The preparation method of CIGS target material metal layer Download PDFInfo
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- CN107099775A CN107099775A CN201710289192.6A CN201710289192A CN107099775A CN 107099775 A CN107099775 A CN 107099775A CN 201710289192 A CN201710289192 A CN 201710289192A CN 107099775 A CN107099775 A CN 107099775A
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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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of preparation method of CIGS target material metal layer, step includes：Copper, indium, gallium material are chosen by ratio of weight and the number of copies and be broken into coarse powder and be well mixed；Air-flow is ground；Melting in reactor；Copper-indium-gallium-selenium alloy is made；The copper-indium-gallium-selenium alloy ingot is broken into a diameter of 1~3mm alloy block, is placed in 300~500r/min rotating speed 0.5~1h of ball milling in ball mill, obtains CIGS powder；On the push-down head that graphite bolster plate is placed in hot pressing furnace mould, then copper sheet is placed on graphite bolster plate, groove is processed in the one side of the copper sheet, the groove is located at the central part of the copper sheet, and the area of the groove is not less than the 2/3 of copper sheet area；Obtained CIGS powder is put into groove, seaming chuck is placed into；Hot pressing furnace mould is put into hot pressing furnace and carries out hot pressed sintering；Target is taken out from hot pressing furnace.Cost of the present invention is low, synchronous with target preparation process, substantially reduces production cost.
Description
Technical field
The present invention relates to a kind of preparation method of CIGS target material.
Background technology
CIGS is thin-film solar cells light absorption layer material, strong with capability of resistance to radiation, stable work in work etc.
Advantage, it is necessary to which CIGS target material carries on the back target good contact with copper during CIGS thin-film is prepared, realizes good lead
Electricity, heat-conducting effect.It can realize that the common technology that target is connected with metal has method for brazing, fusing process of intermediate at present.For CIGS
For target, because this target fragility is big, it is easy to volatilize, fusing process of intermediate is not applied to；And method for brazing welding inorganic non-metallic target
When need target surface to metallize, welded with suitable conventional solder.Conventional metallization process has silver paste sintering process, evaporation at present
Method, sputtering method, spraying process etc., the metal layer and matrix combination of these techniques formation are weaker, it is impossible to form metallurgical binding,
The conductive, capacity of heat transmission is poor, it is impossible to meet the process conditions required by solar cell plated film, the film thickness uniformity that plates out and into
Divide lack of homogeneity.The metallurgical binding of target and metal layer is realized, it is necessary to which the element phase counterdiffusion of target and metal layer, reaches
To the purpose of integration.
The content of the invention
The problem of for being previously mentioned, the invention provides a kind of preparation method of CIGS target material metal layer, step
Including：
1) it is 8~10 by ratio of weight and the number of copies：23~26：7~9 choose copper, indium, gallium material, are broken into coarse powder, and mixing is equal
It is even；
2) coarse powder after will be broken carries out air-flow and ground, and powder is made, and the powder size is 4.5~5.5 μm；
3) mixed-powder after air-flow is ground is fitted into reactor, vacuumizes and argon gas is filled with backward reactor, described
The pressure of argon gas is 0.3~0.5MPa, and flow is 30~40cc/min；
4) reactor is warming up to 300~400 DEG C, is incubated 1~3h；
5) reactor is warming up to 600~800 DEG C, is incubated 2~4h；
6) reactor is warming up to 900~1100 DEG C, is incubated 3~5h；
7) reactor is cooled down to 80~100 DEG C, obtains copper and indium gallium alloy；
8) the copper and indium gallium alloy and selenium powder are respectively charged into the two ends of quartz ampoule, and quartz ampoule is carried out to vacuumize behaviour
Make, vacuum reaches 1 × 10-1~1 × 10-4Rear enclosed quartz ampoule；
9) using tube furnace to equipped with copper and indium gallium alloy heating one end to 1050~1100 DEG C, and keeping temperature；
10) heating is equipped with selenium powder one end, described selenium powder one end liter while diamond heating is equipped with copper and indium gallium alloy one end
Temperature is incubated 20~30min to 400~450 DEG C, is then heated to 500~550 DEG C, is incubated 6~9h, is then heated to 800 DEG C,
And keeping temperature；
11) it will be equipped with copper and indium gallium alloy one end and be cooled to 800 DEG C, copper and indium gallium is reacted 20~30h at 800 DEG C with selenium；
12) tube furnace is closed, stops heating, is cooled to room temperature, obtains copper-indium-gallium-selenium alloy ingot；
13) the copper-indium-gallium-selenium alloy ingot is broken into a diameter of 1~3mm alloy block, is placed in ball mill with 300
~500r/min rotating speed 0.5~1h of ball milling, is sieved more than 100 mesh, obtains CIGS powder；
14) thickness is placed on the push-down head of hot pressing furnace mould for 8~13mm graphite bolster plate, is then 18 by thickness
~23mm copper sheet is placed on graphite bolster plate, and the groove that depth is 12~15mm is processed in the one side of the copper sheet, described recessed
Groove is located at the central part of the copper sheet, and the area of the groove is not less than the 2/3 of copper sheet area；
15) CIGS powder made from step 13 is put into groove, places into seaming chuck；
16) hot pressing furnace mould is put into hot pressing furnace and carries out hot pressed sintering, the hot pressing furnace is warming up to 300~400 DEG C,
1~3h is incubated, the hot pressing furnace is warming up to 500~600 DEG C, 2~5h is incubated, the hot pressing furnace is warming up to 650~700
DEG C, safeguard 0.5~1.2h；
17) target is taken out from hot pressing furnace.
Preferred scheme is：Using the broken copper of hydrogen explosion, indium, gallium material.
Preferred scheme is：5N copper, 5N indiums, 5N galliums and 5N selenium that it is purity 99.999% that elemental copper, indium, gallium, selenium, which are,.
Preferred scheme is：The heating rate is 90~100 DEG C/h.
Preferred scheme is：The reactor is that integral type completely encloses structure.
Preferred scheme is：The reactor is with the degrees second oscillating motion of angular speed 0.8.
The new CIGS target material metal layer preparation method that the present invention is provided has the following advantages that：
1st, conductive, good heat conductivity, due to metal layer and the target matrix formation metallurgical binding of acquisition, target matrix with
Metal layer Percentage bound is close to 100%, and interface resistance is very low, and effectively can export heat from target surface；
2nd, cost is low, synchronous with target preparation process, substantially reduces production cost.
Embodiment
The present invention is described in further detail below, to make those skilled in the art being capable of evidence with reference to specification word
To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or many
The presence or addition of individual other elements or its combination.
Embodiment 1
A kind of preparation method of CIGS target material metal layer is present embodiments provided, step includes：
1) it is 8 by ratio of weight and the number of copies：23：7 choose copper, indium, gallium material, and coarse powder is broken into using hydrogen explosion, are well mixed, single
5N copper, 5N indiums, 5N galliums and 5N selenium that it is purity 99.999% that matter copper, indium, gallium, selenium, which are,；
2) coarse powder after will be broken carries out air-flow and ground, and powder is made, and the powder size is 4.5 μm；
3) mixed-powder after air-flow is ground is fitted into reactor, vacuumizes and argon gas is filled with backward reactor, described
The pressure of argon gas be 0.3MPa, flow is 30cc/min, the reactor be integral type completely enclose structure, the reactor with
The degrees second oscillating motion of angular speed 0.8；
4) reactor is warming up to 300 DEG C, is incubated 1h；
5) reactor is warming up to 600 DEG C, is incubated 2h；
6) reactor is warming up to 900 DEG C, is incubated 3h；
7) reactor is cooled down to 80 DEG C, obtains copper and indium gallium alloy；
8) the copper and indium gallium alloy and selenium powder are respectively charged into the two ends of quartz ampoule, and quartz ampoule is carried out to vacuumize behaviour
Make, vacuum reaches 1 × 10-1~1 × 10-4Rear enclosed quartz ampoule；
9) using tube furnace to equipped with copper and indium gallium alloy heating one end, to 1050 DEG C, heating rate is 90 DEG C/h, and is kept
Temperature；
10) heating is equipped with selenium powder one end, described selenium powder one end liter while diamond heating is equipped with copper and indium gallium alloy one end
Temperature is incubated 20min to 400 DEG C, is then heated to 500 DEG C, is incubated 6h, is then heated to 800 DEG C, and keeping temperature；
11) it will be equipped with copper and indium gallium alloy one end and be cooled to 800 DEG C, copper and indium gallium is reacted 20h at 800 DEG C with selenium；
12) tube furnace is closed, stops heating, is cooled to room temperature, obtains copper-indium-gallium-selenium alloy ingot；
13) the copper-indium-gallium-selenium alloy ingot is broken into a diameter of 1mm alloy block, is placed in ball mill with 300r/min
Rotating speed ball milling 0.5h, more than 100 mesh sieve, obtain CIGS powder；
14) thickness is placed on the push-down head of hot pressing furnace mould for 8mm graphite bolster plate, then by copper of the thickness for 18mm
Piece is placed on graphite bolster plate, and the groove that depth is 12mm is processed in the one side of the copper sheet, and the groove is located at the copper sheet
Central part, the area of the groove is not less than the 2/3 of copper sheet area；
15) CIGS powder made from step 13 is put into groove, places into seaming chuck；
16) hot pressing furnace mould is put into hot pressing furnace and carries out hot pressed sintering, the hot pressing furnace is warming up to 300 DEG C, insulation
1h, 500 DEG C are warming up to by the hot pressing furnace, are incubated 2h, and the hot pressing furnace is warming up into 650 DEG C, safeguard 0.5h；
17) target is taken out from hot pressing furnace.
Metal layer is more than 98% with metal layer Percentage bound, can had with target matrix formation metallurgical binding, target matrix
Effect exports heat from target surface.
Embodiment 2
A kind of preparation method of CIGS target material metal layer is present embodiments provided, step includes：
1) it is 10 by ratio of weight and the number of copies：26：9 choose copper, indium, gallium material, and coarse powder is broken into using hydrogen explosion, are well mixed,
5N copper, 5N indiums, 5N galliums and 5N selenium that it is purity 99.999% that elemental copper, indium, gallium, selenium, which are,；
2) coarse powder after will be broken carries out air-flow and ground, and powder is made, and the powder size is 5.5 μm；
3) mixed-powder after air-flow is ground is fitted into reactor, vacuumizes and argon gas is filled with backward reactor, described
The pressure of argon gas be 0.5MPa, flow is 40cc/min, the reactor be integral type completely enclose structure, the reactor with
The degrees second oscillating motion of angular speed 0.8；
4) reactor is warming up to 400 DEG C, is incubated 3h；
5) reactor is warming up to 800 DEG C, is incubated 4h；
6) reactor is warming up to 1100 DEG C, is incubated 5h；
7) reactor is cooled down to 100 DEG C, obtains copper and indium gallium alloy；
8) the copper and indium gallium alloy and selenium powder are respectively charged into the two ends of quartz ampoule, and quartz ampoule is carried out to vacuumize behaviour
Make, vacuum reaches 1 × 10-1~1 × 10-4Rear enclosed quartz ampoule；
9) using tube furnace to equipped with copper and indium gallium alloy heating one end, to 1100 DEG C, heating rate is 100 DEG C/h, and is kept
Temperature；
10) heating is equipped with selenium powder one end, described selenium powder one end liter while diamond heating is equipped with copper and indium gallium alloy one end
Temperature is incubated 30min to 450 DEG C, is then heated to 550 DEG C, is incubated 9h, is then heated to 800 DEG C, and keeping temperature；
11) it will be equipped with copper and indium gallium alloy one end and be cooled to 800 DEG C, copper and indium gallium is reacted 30h at 800 DEG C with selenium；
12) tube furnace is closed, stops heating, is cooled to room temperature, obtains copper-indium-gallium-selenium alloy ingot；
13) the copper-indium-gallium-selenium alloy ingot is broken into a diameter of 3mm alloy block, is placed in ball mill with 500r/min
Rotating speed ball milling 1h, more than 100 mesh sieve, obtain CIGS powder；
14) thickness is placed on the push-down head of hot pressing furnace mould for 13mm graphite bolster plate, then by thickness be 18~
23mm copper sheet is placed on graphite bolster plate, and the groove that depth is 15mm is processed in the one side of the copper sheet, and the groove is located at
The central part of the copper sheet, the area of the groove is not less than the 2/3 of copper sheet area；
15) CIGS powder made from step 13 is put into groove, places into seaming chuck；
16) hot pressing furnace mould is put into hot pressing furnace and carries out hot pressed sintering, the hot pressing furnace is warming up to 400 DEG C, insulation
3h, 600 DEG C are warming up to by the hot pressing furnace, are incubated 2~5h, and the hot pressing furnace is warming up into 700 DEG C, safeguard 1.2h；
17) target is taken out from hot pressing furnace.
Metal layer is more than 98.5%, energy with target matrix formation metallurgical binding, target matrix with metal layer Percentage bound
Effectively heat is exported from target surface.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details.
Claims (6)
1. a kind of preparation method of CIGS target material metal layer, it is characterised in that step includes：
1) it is 8~10 by ratio of weight and the number of copies：23~26：7~9 choose copper, indium, gallium material, are broken into coarse powder, are well mixed；
2) coarse powder after will be broken carries out air-flow and ground, and powder is made, and the powder size is 4.5~5.5 μm；
3) mixed-powder after air-flow is ground is fitted into reactor, vacuumizes and argon gas is filled with backward reactor, the argon gas
Pressure be 0.3~0.5MPa, flow be 30~40cc/min；
4) reactor is warming up to 300~400 DEG C, is incubated 1~3h；
5) reactor is warming up to 600~800 DEG C, is incubated 2~4h；
6) reactor is warming up to 900~1100 DEG C, is incubated 3~5h；
7) reactor is cooled down to 80~100 DEG C, obtains copper and indium gallium alloy；
8) the copper and indium gallium alloy and selenium powder are respectively charged into the two ends of quartz ampoule, and vacuum pumping is carried out to quartz ampoule, very
Reciprocal of duty cycle reaches 1 × 10-1~1 × 10-4Rear enclosed quartz ampoule；
9) using tube furnace to equipped with copper and indium gallium alloy heating one end to 1050~1100 DEG C, and keeping temperature；
10) heating is equipped with selenium powder one end while diamond heating is equipped with copper and indium gallium alloy one end, and described selenium powder one end is warming up to
400~450 DEG C, 20~30min is incubated, 500~550 DEG C are then heated to, 6~9h is incubated, is then heated to 800 DEG C, and protect
Hold temperature；
11) it will be equipped with copper and indium gallium alloy one end and be cooled to 800 DEG C, copper and indium gallium is reacted 20~30h at 800 DEG C with selenium；
12) tube furnace is closed, stops heating, is cooled to room temperature, obtains copper-indium-gallium-selenium alloy ingot；
13) the copper-indium-gallium-selenium alloy ingot is broken into a diameter of 1~3mm alloy block, be placed in ball mill with 300~
500r/min rotating speed 0.5~1h of ball milling, is sieved more than 100 mesh, obtains CIGS powder；
14) thickness is placed on the push-down head of hot pressing furnace mould for 8~13mm graphite bolster plate, is then 18~23mm by thickness
Copper sheet be placed on graphite bolster plate, process the groove that depth is 12~15mm in the one side of the copper sheet, the groove is located at
The central part of the copper sheet, the area of the groove is not less than the 2/3 of copper sheet area；
15) CIGS powder made from step 13 is put into groove, places into seaming chuck；
16) hot pressing furnace mould is put into hot pressing furnace and carries out hot pressed sintering, the hot pressing furnace is warming up to 300~400 DEG C, insulation
1~3h, 500~600 DEG C are warming up to by the hot pressing furnace, are incubated 2~5h, and the hot pressing furnace is warming up into 650~700 DEG C, guarantor
Defend 0.5~1.2h；
17) target is taken out from hot pressing furnace.
2. the preparation method of CIGS target material metal layer according to claim 1, it is characterised in that use hydrogen explosion
Broken copper, indium, gallium material.
3. the preparation method of CIGS target material metal layer according to claim 1, it is characterised in that elemental copper, indium,
5N copper, 5N indiums, 5N galliums and 5N selenium that it is purity 99.999% that gallium, selenium, which are,.
4. the preparation method of CIGS target material metal layer according to claim 1, it is characterised in that the heating speed
Rate is 90~100 DEG C/h.
5. the preparation method of CIGS target material metal layer according to claim 1, it is characterised in that the reactor
Structure is completely enclosed for integral type.
6. the preparation method of CIGS target material metal layer according to claim 1, it is characterised in that the reactor
With the degrees second oscillating motion of angular speed 0.8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109877335A (en) * | 2019-03-12 | 2019-06-14 | 先导薄膜材料（广东）有限公司 | Copper indium gallium selenide raw powder's production technology |
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| CN103572089A (en) * | 2013-11-12 | 2014-02-12 | 中国科学院金属研究所 | Preparation method of Cu-Im-Ga-Se quaternary semiconductor alloy |
| 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 |
| CN106180721A (en) * | 2015-05-08 | 2016-12-07 | 北京有色金属研究总院 | CIGS target material metal layer preparation method |
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| CN103215541A (en) * | 2013-03-26 | 2013-07-24 | 无锡舒玛天科新能源技术有限公司 | Preparation method of planar copper-indium-gallium-selenium sputtering target material |
| CN103255367A (en) * | 2013-04-28 | 2013-08-21 | 柳州百韧特先进材料有限公司 | Preparation method of target material of solar cell CIGS (Copper Indium Gallium Selenide) absorbing layer |
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| CN109877335A (en) * | 2019-03-12 | 2019-06-14 | 先导薄膜材料（广东）有限公司 | Copper indium gallium selenide raw powder's production technology |
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