CN102051584B - CIGS solar photoelectric quaternary sputtering target and manufacturing method thereof, method combining CIGS solar photoelectric quaternary sputtering target and target back plate and feeding method for CIGS solar photoelectric quaternary sputtering target - Google Patents
CIGS solar photoelectric quaternary sputtering target and manufacturing method thereof, method combining CIGS solar photoelectric quaternary sputtering target and target back plate and feeding method for CIGS solar photoelectric quaternary sputtering target Download PDFInfo
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Abstract
The invention discloses a copper-indium-gallium-selenium (CIGS) solar photoelectric quaternary sputtering target and a manufacturing method thereof, a method combining the CIGS solar photoelectric quaternary sputtering target and a target back plate and a feeding method for the CIGS solar photoelectric quaternary sputtering target. The manufacturing method comprises the following steps of: mixing copper and indium, pre-forming copper/indium alloy powder by hot melting, curing and grinding, mixing copper and gallium, pre-forming copper/gallium alloy powder by hot melting, curing and grinding, and fully mixing the copper/indium alloy powder, the copper/gallium alloy powder and selenium material powder to prepare processed material powder; and filling the processed material powder into a die, and quickly forming a target comprising copper (Cu), indium (In), gallium (Ga) and selenium (Se) by common heating, hot melting and pressing programs. The target back plate is designed into one part of the die so that the target can be directly combined with the target back plate together at the same time of target forming. The used target is cleaned, placed into the die and filled with the processed material powder, and the target can be supplemented to the size of required specification for reuse after the hot melting, pressing and cooling programs. The invention fulfills the purposes of simplifying the processes of CIGS target manufacture, combination of the target and the target back plate, target supplement and the like and greatly reducing the cost.
Description
Technical field
The present invention relates to a kind of CIGS solar photoelectric quaternary sputtered target material, its method for making, itself and target backboard combining method and feed supplement method thereof, refer to that especially a kind of copper Cu, indium In, gallium Ga and selenium Se classification are modulated into the work material powder, are filled in the work material powder in the mould; Melt and the pressurization program through general heat temperature raising heat; Get final product rapid shaping CIGS target, target material moulding combines with the target backboard simultaneously, and to the target feed supplement; Significantly simplify work program and reach, and the purpose that reduces cost.
Background technology
By knowing copper-indium-galliun-selenium CIGS type thin-film solar cells at present; Its substruction is shown in figure 11; Mainly utilize the CIGS semiconductor film as light absorbing zone; To carry out the solar photoelectric conversion, it is most effective in the thin-film solar cells being proved its photoelectric transformation efficiency, thereby industry competitively actively drops into the associated fabrication techniques of copper-indium-galliun-selenium CIGS type thin-film solar cells and the research and development of equipment.Existing CIGS thin-film solar cells volume production technology can generally be divided into two types according to process technique, and one type for utilizing vacuum splashing and plating processing procedure or vapor deposition processing procedure to make CIGS film light absorption layer, and another kind of then is non-vacuum process technology (like plating or be printed as membrane technique).
Have two: 1 in the sputter process known today) carry out the metal or alloy coating thin film with sputtering equipment earlier, utilize the selenizing mode that the selenizing of metal or alloy film is formed CIGS film light absorption layer again, but its photoelectric transformation efficiency is relatively poor; 2) adopt the CIGS series target material to cooperate sputtering equipment, directly sputter is that industry actively competitively drops into research and development to form CIGS film light absorption layer because of having preferable photoelectric transformation efficiency on substrate.Wherein, the material of the common use of CIGS target has CuIn
xGa
1-xS
ySe
2-yAnd CuIn
xAl
1-xS
ySe
2-y, for example Taiwan discloses No. 200932933 and the U.S. discloses the material that is disclosed in No. 2005/0109293 patent case.Moreover; The method of manufacture of known CIGS target discloses the common sputtering method of No. 2005/0109293 patent case just like the U.S.; Or the powder metallurgy method of No. 200932933 patent case disclosed like Taiwan; Wherein powder metallurgy method must prepare CIGS based material powder earlier; And the technological solvent thermal synthesis method (Solvothermal synthesis) of its CIGS based material powdered preparation, or by disclose like Taiwan No. 200932679 and No. 200932933 chemical wet synthesis method (chemical refluxsynthesis method) obtained.Yet these above-mentioned known target manufacturing technologies are just seeming very complicated aspect the processing procedure of target material, spend man-hour, and the problem of solvent severe contamination is arranged.
Moreover owing to be able to carry out for the ease of sputter process, target must combine with the target backboard, and the structure through the target backboard makes target be able to carry among the reaction chamber of sputtering equipment.And in the known technology, all be with after target and the moulding of target backboard difference, utilize soft soldering, hard solder, diffusion bond or epoxy resin solid joining technique again; And target and target backboard are bonded with each other, or like the U.S. the 5th, 230; No. 459, the public gulf technology that No. 287125 the patent case is disclosed are to form uneven surface in the target back plate surface, after target subsides repeatedly; Through to target heating, melt through heat and to be absorbed in uneven surface, and target is combined with the target backboard.Moreover, a kind of known CIGS series target material and target backboard joining technique are also arranged, put between the target of moulding and the target backboard respectively and establish an indium sheeting, the heating make indium thin slice heat melt the back and target is engaged with the target backboard.Yet above-mentioned which kind of joining technique no matter all is target and target backboard respectively after the moulding, utilizes above-mentioned various joining techniques that the two is engaged again, causes manufacturing course complicated, increases cost.In the technology of the present invention, then can be one-body molded in the target material moulding process with the target backboard, and can effectively promote target and target backboard bonded stability.
In addition, because the target cost is expensive,, be waste in fact if after target uses, will remain target and abandon.And present known mode with the target recycling has the technology that reclaims to sputtered aluminium alloy target material to be developed, for example the technology of No. 483937 patent case in Taiwan.Because the moulding respectively of known target and target backboard, utilize joining technique again and make the two joint, desire recycling; Just must earlier target be separated with the target backboard,, and must the target backboard be filled part cleaning again with the fusion double teeming of target cleaning back; Then utilize above-mentioned joining technique to engage again with the target backboard target of double teeming again; The entire treatment flow process is very complicated, spends man-hour, significantly increases cost.In the technology of the present invention, can carry out feed supplement, can go utilization again at a part of formed vacancy of target sputter post consumption position.
Summary of the invention
The present invention's first purpose is to provide a kind of method that can make the purifying CIGS quaternary sputtered target material that includes elements such as copper Cu, indium In, gallium Ga and selenium Se easy, apace.
For realizing aforementioned purpose, the present invention takes following plan: (i) copper is mixed with indium each other, through vacuum-heat-melt, pressurization repeatedly, the program of cooling off and pulverizing, and prepare into copper/indium alloy powder; (ii) copper is mixed with gallium each other, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium alloy powder; (iii) and be ready for selenium Se powder.Then; Again copper/indium alloy powder, copper/gallium alloy powder and selenium material powder are filled part mixing and prepare into the work material powder, directly the work material powder is filled in the mould, melt and the pressurization program through general heat temperature raising heat; Rapid shaping includes the target of copper Cu, indium In, gallium Ga and selenium Se element; Or mould placed vacuum cavity, and melting and the pressurization program through general heat temperature raising heat again, rapid shaping includes copper Cu, indium In, gallium Ga and selenium Se phase bonded target.
Concrete steps are following:
A kind of method of manufacture of CIGS quaternary sputtered target material includes the following step:
(a) prepare the work material powder, said work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se;
(b) said work material powder is inserted in the die cavity of a mould,, and repeatedly pressurize, make copper Cu, gallium Ga, indium In and the even chemical combination of selenium Se and cooling again after the one that bonds the melting temperature of said work material powder heating at least to selenium; And
(c) unloading said mould in cooling back is promptly accomplished the target manufacturing of strip and block, and is made said target include copper Cu, indium In, gallium Ga and selenium Se.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material, wherein: the step of said preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder; Be ready for selenium Se powder; And
(a3) said copper/indium CuIn powdered alloy, said copper/gallium CuGa powdered alloy and said selenium material powder are filled part and mix said work material powder.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material, wherein: can repeat repeatedly the described pressurization formula of (b) step.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material; Wherein: the said mould of step (b) includes a frame mould and the male model that aluminum target backboard, a frame as master mold is trapped among said target backboard end face; Said target backboard is fixed on the base, and said male model bottom surface has a die, and said die outline shape matches with the frame mouth of said frame mould; Said target backboard and said frame mould surround a molding cave, insert said work material powder in said moulding die cavity.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material; Wherein: said aluminum target backboard end face is provided with a groove; Said groove is the some of said moulding die cavity; Said groove includes a wall and a bottom, and said bottom is provided with one first coarse structure, and said wall is provided with one second coarse structure.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material, wherein: the degree of depth of said groove is 2～3mm.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material; Wherein: said first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed; Said second coarse structure be one along the contour loop of said groove around chase, said chase is positioned at the wall and the junction, bottom of said groove.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material, wherein: the degree of depth of said slit is 2～3mm, the about 5mm of width, and the about 15mm in interval of two adjacent said slits.
The method of manufacture of above-mentioned CIGS quaternary sputtered target material, wherein: in the said step (b), can said mould placed a vacuum chamber to heat and pressurizes.
The present invention's second purpose, provide a kind of can be easy, make the purifying CIGS quaternary sputtered target material that includes elements such as copper Cu, indium In, gallium Ga and selenium Se apace, and the method that in target material moulding, must be combined as a whole with the target backboard.
For realizing aforementioned purpose; The present invention takes following plan: utilize above-mentioned work material powder; The target backboard material that cooperation is selected for use especially and the structure design of target backboard; The target backboard is carried the some of the end face of target as the die cavity of mould, make the work material powder through overheatedly melt, after pressurization and the refrigerative program, can make target material moulding and directly and the target backboard be combined as a whole.
Concrete steps are following:
A kind of CIGS quaternary sputtered target material moulding while and target backboard bonded method, include the following step:
(a) prepare the work material powder, said work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se material;
(b1) said work material powder is inserted in the mould, said mould includes a frame mould and the male model that aluminum target backboard, a frame as master mold is trapped among said target backboard end face, and said target backboard is fixed on the base; Said target backboard end face is provided with a groove, and said groove includes a bottom and a wall, and said bottom is provided with one first coarse structure; Said wall is provided with one second coarse structure; Said male model bottom surface has a die, and said die outline shape matches with the frame mouth of said frame mould, and the groove of said target backboard and said frame mould surround a molding cave; Insert said work material powder in said moulding die cavity; Said work material powder is heated to the melting temperature of selenium, and pressurizes, make the even chemical combination of copper, gallium, indium and selenium and engage postcooling after the one that bonds and with backboard; And
(c1) cooling back unloading said male model, said frame mould and said base promptly accomplished the manufacturing that target material moulding engages with said target backboard simultaneously, and the said target that includes copper Cu, indium In, gallium Ga and selenium Se element is incorporated on the said aluminum target backboard.
Above-mentioned CIGS quaternary sputtered target material moulding while and target backboard bonded method, wherein: the step of said preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder; Be ready for selenium Se powder; And
(a3) said copper/indium CuIn powdered alloy, said copper/gallium CuGa powdered alloy and said selenium material powder are filled part and mix said work material powder.
Above-mentioned CIGS quaternary sputtered target material moulding while and target backboard bonded method, wherein: can repeat repeatedly the pressurization formula in (b1) step.
Above-mentioned CIGS quaternary sputtered target material moulding while and target backboard bonded method, wherein: the degree of depth of said groove is 2～3mm.
Above-mentioned CIGS quaternary sputtered target material moulding while and target backboard bonded method; Wherein: said first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed; Said second coarse structure be one along the contour loop of said groove around chase, said chase is positioned at the wall and the junction, bottom of said groove.
Above-mentioned CIGS quaternary sputtered target material moulding simultaneously and target backboard bonded method, wherein: the degree of depth of slit is 2～3mm, the about 5mm of width, and the about 15mm in interval of two adjacent said slits.
Above-mentioned CIGS quaternary sputtered target material moulding simultaneously and target backboard bonded method, wherein: in the said step (b1), can said mould placed a vacuum chamber to heat and pressurizes.
The present invention's the 3rd purpose; Provide a kind of can be easy, make the purifying CIGS quaternary sputtered target material that includes elements such as copper Cu, indium In, gallium Ga and selenium Se apace; And make used target via simple program, get final product supplementary material to original required specification shape, and can supply to continue to use.
For realizing aforementioned purpose, the utility model is taked following plan: utilize above-mentioned work material powder, and the principle of above-mentioned second purpose; After the target cleaning of using and be combined with the target backboard, it is added mould, again the work material powder is inserted the part of die cavity vacancy; Through overheatedly melt, pressurization and refrigerative program; Or mould placed in the vacuum cavity through heat melt, after pressurization and the refrigerative program, can make target be supplemented to the size of required specification, continue to supply to use.
Concrete steps are following:
A kind of compensation process of CIGS quaternary sputtered target material includes the following step:
(a) prepare the work material powder, said work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se;
(b2) the residue target that used and still be combined with a target backboard with is cleaned; And insert in the mould, and said work material powder to be inserted in the said mould, said mould includes a frame mould and the male model that an aluminum backboard as master mold, a frame are trapped among said target backboard end face; Said target backboard is fixed on the base; Said target backboard end face is provided with a groove, and said bottom portion of groove is provided with coarse structure, and said male model bottom surface has a die; Said die outline shape matches with the frame mouth of said frame mould; The groove of said target backboard and said frame mould surround a molding cave, insert said work material powder in said moulding die cavity, to the melting temperature of said work material powder heating at least to selenium; And pressurize, make copper Cu, gallium Ga, indium In and the even chemical combination of selenium Se and merge postcooling after the one that bonds and with said residue target; And
(c2) the cooling back unloads said male model, said frame mould and said base, promptly accomplishes the processing procedure of said residue target feed supplement.
The compensation process of above-mentioned CIGS quaternary sputtered target material, wherein: the step of said preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder; Be ready for selenium Se powder; And
(a3) said copper/indium CuIn powdered alloy, said copper/gallium CuGa powdered alloy and said selenium material powder are filled part and mix said work material powder.
The compensation process of above-mentioned CIGS quaternary sputtered target material, wherein: can repeat repeatedly the pressurization formula in (b2) step.
The compensation process of above-mentioned CIGS quaternary sputtered target material, wherein: in the step (b2), can said mould placed a vacuum chamber to heat and pressurizes.
Advantage of the present invention and beneficial effect:
1. the present invention goes ahead of the rest to classify and is deployed into copper/indium alloy powder, copper/gallium alloy powder; Again they and selenium powder end are modulated into the processing powder; Can solve the direct blended of selenium and gallium or indium difficulty and institute and produce problem hypertoxic or that explode; Make directly and to melt and pressurization and molded and shaped CIGS quaternary sputtered target material is able to put into carry out through heat, and then significantly simplify processing procedure and reduce cost with material powder.
2. the present invention is said except the 1st advantage, can be directly melts and pressurization and outside the molded and shaped CIGS quaternary sputtered target material, be again the some of mould with the target back plate design through heat with material powder; When heat was melted the moulding target in mould, target promptly directly combined with the target backboard, and then can significantly simplify processing procedure and reduce cost at material powder; Reach more known gummed mode and can improve the combination stability, especially than the U.S. the 5th, 230; Though No. 459 the patent case is provided with coarse structure; But still after being difference moulding target and target backboard, again target and target backboard heat are fused the technology of closing, more can improve target and target backboard bonded stability.
3. the present invention is of the 2nd advantage, can be directly melt and pressurization and molded and shaped CIGS quaternary sputtered target material through heat with material powder, and design target and target backboard is the some of mould; As long as will remain target combines with male model, frame mould together with the target backboard; Insert the work material powder in die cavity, through general heat melt, pressurization and cooling program, can make the target polishing; And still keep combining, significantly simplify the processing procedure of recycling with the target backboard.
Can implement according to this for ease of inspector's understood in detail and those skilled in the art, now the specific embodiment of above-mentioned three characteristics is detailed as after.
Description of drawings
Fig. 1 is the preparation flow synoptic diagram of work material powder of the present invention;
Fig. 2 is first kind of processing procedure embodiment synoptic diagram of target of the present invention;
Fig. 3 is the prepared target synoptic diagram of first kind of processing procedure embodiment of the present invention;
The target backboard synoptic diagram that Fig. 4 is adopted for second kind of processing procedure embodiment of the present invention;
The mould synoptic diagram that Fig. 5 is adopted for second kind of processing procedure embodiment of the present invention;
Fig. 6 is the enlarged diagram of A-A circle among Fig. 5;
Fig. 7 is the schematic flow sheet of second kind of processing procedure embodiment of the present invention;
Fig. 8 is the prepared target synoptic diagram of second kind of processing procedure embodiment of the present invention;
Fig. 9 is the schematic flow sheet of the third processing procedure of the present invention embodiment;
Figure 10 is the prepared target synoptic diagram of the third processing procedure of the present invention embodiment;
Figure 11 is known CIGS type film solar battery structure synoptic diagram; And
Figure 12 is combined with the actual finished product photo of target of target backboard for the present invention.
Embodiment
One, characteristic of the present invention and principle:
The principal feature of the present invention's technology has following three:
The first, be to make a kind of method that includes the CIGS quaternary sputtered target material of copper Cu, indium In, gallium Ga and selenium Se element: the special material formulation that its utilization is described below is classified allotment in advance and is processed powder; Again each classification powder is filled part and be mixed into the forming process material powder; It directly is filled in the mould with the work material powder; Or can again mould be placed in the vacuum cavity, melt and the pressurization program through general heat temperature raising heat again, get final product the target that rapid shaping includes copper Cu, indium In, gallium Ga and selenium Se element; Significantly simplify work program, and reduce cost.
The second, be in target material moulding, must be combined as a whole with the target backboard: it utilizes above-mentioned work material powder; The target backboard material that cooperation is selected for use especially and the structure design of target backboard; The target backboard is carried the some of the end face of target as the die cavity of mould, the work material powder is inserted the die cavity of mould, can mould be placed vacuum chamber; Through overheatedly melt, after pressurization and the refrigerative program; Can make the work material powder target that in die cavity, is shaped, can make simultaneously target directly and the target backboard be combined as a whole, significantly simplify work program.
Three, the target that then was to use can supply via supplementary material to continue to use: it utilizes above-mentioned work material powder; And the principle of above-mentioned second characteristic; After the target cleaning of using and be combined with the target backboard, it is added mould, again the work material powder is inserted the part of die cavity vacancy; And can mould be placed vacuum cavity; Through overheatedly melting, after pressurization and the refrigerative program, can making target be supplemented to the size of required specification, significantly simplify the program of recycling again.
Two, the method for manufacture of CIGS quaternary sputtered target material of the present invention
1, exploitation reason
Shown in Fig. 1 to 3, the present invention particularly researches and develops to including the CIGS quaternary sputtered target material of elements such as copper Cu, indium In, gallium Ga and selenium Se, and this quaternary sputtered target material is the usefulness that supplies sputter moulding solar energy photoelectric thin-film.Because general known CIGS series target material is shown in the preceding case that the background in this specification sheets is put down in writing, all is the compound that adopts aforementioned elements mainly, utilize the mode of complicated chemical reaction and process the CIGS series target material, cause its manufacturing cost significantly to promote.So the inventor studies directly with material powder melts and pressurization and molded and shaped through heat, in order to significantly to simplify processing procedure, reduces cost.And open through studying for a long time, test and sending out, research and development achievement of the present invention is arranged eventually.
2. the solution of problem
Knows that according to experiment institute indium In or gallium Ga directly mix with selenium Se, when fusing, can produce vigorous reaction, measure can produce when big explode and generation hypertoxic, and, in general processing environment temperature, be difficult for being modulated into powder owing to the fusing point of gallium is extremely low.In order to overcome, to solve the above problems, these elements can be put into effect with powder mode machine-shaping composite target material.The inventor is design: (i) copper mixed with indium each other, and repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium alloy powder; (ii) copper is mixed with gallium each other, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium alloy powder; (iii) and be ready for selenium Se powder.Then, again copper/indium alloy powder, copper/gallium alloy material and selenium material powder are filled part mixing and prepare into the work material powder, this work material powder after experiment, neither can produce the problem of severe toxicity and blast, but the extrusion forming target is melted in heat supply again.
3. specific embodiment
Extremely shown in Figure 3 like Fig. 1, the method for manufacture of CIGS quaternary sputtered target material of the present invention, specific embodiment includes the following step:
(a) prepare four kinds of element materials such as copper Cu, indium In, gallium Ga and selenium Se.
(b1) copper Cu is mixed with indium In each other, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder 10; Copper Cu is mixed with gallium Ga each other,, and prepare into copper/gallium CuGa alloy material powder 20 through repeatedly vacuum-heat-melt, pressurization, cooling and grinding; If the selenium of being prepared is solid, then with selenium Se solid 30 grind into powders 31.
(c1) copper/indium CuIn powdered alloy 10, copper/gallium CuGa powdered alloy 20 and selenium Se material powder 31 are filled part mixing and prepare into work material powder 40.
(d1) this work material powder 40 is inserted in the die cavity 51 of mould 50; This work material powder 40 is heated to the melting temperature of selenium; And pressurize, make in the work material powder 40 the even chemical combination of copper, indium, gallium and selenium and after being bonded to one again the cooling, wherein; Can repeat repeatedly the compression motion in (d1) step, so that mix more even and closely knit.
(e1) cooling back this mould 50 of removal is promptly accomplished the target 60 of strip and block and is made, and makes this target 60 include copper Cu, indium In, gallium Ga and selenium Se.
4. experimental example
The experimental example of the method for manufacture of CIGS quaternary sputtered target material of the present invention; Get copper Cu 44.48 weight parts and the mutual uniform mixing of indium In80.37 weight part; Through the program of vacuum-heat-melt repeatedly-pressurize-cool off-pulverize, and prepare into copper/indium CuIn alloy material powder 10 that particle diameter is about 74 μ m.With the mutual uniform mixing of gallium Ga of copper Cu19.06 weight part and 20.92 weight parts,, and prepare into copper/gallium CuGa alloy material powder 20 that particle diameter is about 74 μ m through the program of vacuum-heat-melt repeatedly-pressurize-cool off-pulverize.The selenium Se material powder 31 of copper/gallium CuGa powdered alloy 20 and 157.92 weight parts of getting copper/indium CuIn powdered alloy 10,100 weight parts of 100 weight parts fills and part mixes and prepare into work material powder 40., this work material powder 40 is inserted in the die cavity 51 of mould 50 to shown in Figure 3 like Fig. 1, this work material powder 40 is heated to 217 ℃ of the melting temperatures of about selenium; The male model 54 feedings pressurization of mould 50 three times; After cooling, the removal mould is promptly accomplished the target manufacturing of the strip and block of 1400 * 120 * 7mm; And target includes copper Cu, indium In, gallium Ga and selenium Se element, and the mole ratio of the copper of target, gallium, indium and selenium is about 1: 0.7: 0.3: 2.At this lay special stress on; Above-mentioned mole ratio be not for the present invention to discuss the emphasis of studying carefully, the ratio value of its mole number can be according to the user in sputter process; For solar energy generating efficiency and cost needs to considered; Adjust the part by weight of each material in the allotment powder, and can see through thermal treatment again, to promote the solar photoelectric efficiency of conversion with selenizing function.
Three, CIGS quaternary sputtered target material of the present invention and target backboard bonded method
1. exploitation reason
Like the target that above-mentioned the present invention researched and developed, for including the CIGS quaternary sputtered target material of elements such as copper Cu, indium In, gallium Ga and selenium Se.Press CIS system or CIGS series target material or other targets in the known technology, all must engage, could supply the usefulness of sputter with the target backboard.And known moulding target earlier respectively and target backboard engage target again with the target backboard, for example the preceding case of patent carried of aforementioned background.In the known technology, all must utilize indirect material, target engaged after utilizing indirect material heat to melt with the target backboard; For example CIS is or the CIGS series target material; Be between target and target backboard, to be situated between to put indium In sheeting, indium heat is melted the back and target is engaged with the target backboard, yet; The indium of putting that is situated between can cause skewness, so that target can't firmly engage with the target backboard effectively.In addition; If adopt copper target backboard; When selenium Se powder was overlying on the junction surface of copper target backboard, after heat was melted and cooled off, the selenium powder of target backboard and target joint end was fashionable with the thawing of copper target backboard heat; Its bonded copper selenium alloy can be powderised, thereby the problem that target can't engage with the target backboard really takes place.So inventor research is being melted and pressurization and in molded and shaped through heat with the work material powder; The special aluminum target backboard that adopts with the some of aluminum target backboard as mould, is molded directly within on the target backboard target; Can directly combine by target of the present invention, significantly simplify the two bonded processing procedure with the target backboard, and because of the only meeting and copper, indium, gallium chemical combination in low temperature of selenium powder end; And can not close with calorize; So can avoid the situation of target and target backboard joint formation powderised, thus can guarantee target and target backboard mortise, and also the two bonded tolerance range and stability all can be guaranteed.
2. the solution of problem
Known technology, respectively moulding target and target backboard utilize welding, diffusion bond again or make the two joint with indirect material, and processing procedure is comparatively complicated, and still has the unstable disappearance of joint, and can cause the uneven phenomenon of whole target material.Moreover, according to knowledge and the inventor test know that the selenium powder end is filled out and overlayed on the copper target backboard, it melts with copper chemical combination after cooling through heat can the shape powderised, and causes target and target backboard joint powderised, and can't effectively engage.In order to overcome, to solve the above problems.The inventor is the some of mould with the target back plate design, copper/indium alloy powder, copper/gallium alloy material and selenium material powder are filled part mix a work material powder that is prepared and insert mould, through general heat melt, pressurization and cooling program; It is plastic target; Target directly is incorporated on the target backboard, and overall process is simplified, and need not to re-use indirect material; And the work material powder moulding that is directed against CIGS system becomes the technology of target; The target backboard that the present invention adopted is to process with aluminium, and the selenium powder end can not closed with calorize in low temperature, so can avoid target and target backboard joint to produce powderised; And can guarantee that target uniform ingredients, precision height reach and target backboard mortise, and then thoroughly address the above problem.
3. specific embodiment
Shown in Fig. 1 and 4 to 8, the specific embodiment of CIGS quaternary sputtered target material of the present invention and target backboard bonded method of manufacture includes the following step:
(a) prepare four kinds of element materials such as copper Cu, indium In, gallium Ga and selenium Se;
(b2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder 10; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder 20; If the selenium of being prepared is solid, then with selenium Se solid 30 grind into powders 31.
(c2) copper/indium CuIn powdered alloy 10, copper/gallium CuGa powdered alloy 20 and selenium Se material powder 31 are filled part mixing and prepare into work material powder 40.
(d2) this work material powder 40 is inserted in the mould 50, this mould 50 includes a frame mould 53 and the male model 54 that aluminum target backboard 52, a frame as master mold is trapped among target backboard 52 end faces, and target backboard 52 is fixed on the base 55; Target backboard 52 end faces are provided with a groove 520, and groove 520 bottoms are provided with coarse structure 521, and these male model 54 bottom surfaces have a die 540; Die 540 outline shapes match with the frame mouth 530 of frame mould 53; The groove 520 and the frame mould 53 of target backboard 52 surround a molding cave 51, insert work material powder 40 in moulding die cavity 51, maybe can mould 50 be placed vacuum cavity; Again to the melting temperature of 40 heating of the work material powder in the die cavity 51 at least to selenium; And pressurize repeatedly, make copper, gallium, indium and selenium homogenizing merge the bonding one and moulding target 60, the while combines postcooling with target backboard 52.
(e2) cooling back removal male model 54, frame mould 53 and base 55 are promptly accomplished target material moulding simultaneously and target backboard 52 bonded processing procedures, and this target 60 is made up of copper Cu, indium In, gallium Ga and selenium Se and is incorporated on the aluminum target backboard 52.
4. experimental example
Shown in Fig. 1 and 4 to 8; The experimental example of CIGS quaternary sputtered target material of the present invention and target backboard bonded method of manufacture; Get copper Cu 44.48 weight parts and the mutual uniform mixing of indium In powder 80.37 weight parts; Through repeatedly vacuum-heat-melt, pressurization, cooling and grinding, and prepare into copper/indium CuIn alloy material powder 10 that particle diameter is about 74 μ m.With the mutual uniform mixing of gallium Ga of copper Cu19.06 weight part and 20.92 weight parts, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder 20 that particle diameter is about 74 μ m.The selenium Se material powder 31 of copper/gallium CuGa powdered alloy 20 and 157.92 weight parts of getting copper/indium CuIn powdered alloy 10,100 weight parts of 100 weight parts fills and part mixes and prepare into work material powder 40.
Prepare a mould, it includes one 1450 * 180 * 10mm's and is trapped among the frame mould 53 and a male model 54 of target backboard 52 end faces as aluminum target backboard 52, a frame of master mold; Target backboard 52 is fixed on the base 55; Its end face is provided with the groove 520 that a degree of depth is 2mm, and (the general depth range of implementing can be 2～3mm); The bottom 520a of groove 520 is provided with first coarse structure, 521, the first coarse structures 521 and includes a plurality of vertical slit 522 and a plurality of transverse slot 523 that are interspersed, and the degree of depth of slit 522/523 is that (the general depth range of implementing can be 2～3mm) to 3mm; The about 5mm of width; And the about 15mm in interval of two adjacent slits 522/523 (the general depth range of implementing can be 15～20mm), and the wall 520b of groove 520 is provided with second coarse structure 524, its second coarse structure 524 be one along groove 520 contour loops around chase 525; Chase 525 is positioned at the wall 520b and the 520a junction, bottom of groove 520, is in the shape of the letter V like the transverse section of the chase in the illustrated example of Fig. 6 525; Male model 54 bottom surfaces have a die 540, and die 540 outline shapes match with the frame mouth 530 of frame mould 53, and the groove 520 and the frame mould 53 of target backboard 52 surround a molding cave 51.Work material powder 40 is inserted in the die cavity 51 of mould 50; Work material powder 40 is heated to the melting temperature of selenium; The male model 54 feedings pressurization of mould 50 three times, after cooling, removal male model 54 and frame mould 53; Promptly accomplish 1400 * 120 * 7mm strip and block target 60 moulding simultaneously with aluminum target backboard 52 bonded processing procedures as master mold; Its finished product is shown in Fig. 8 and annex one, and target 60 includes copper Cu, indium In, gallium Ga and selenium Se element, and the mole ratio of the copper of target 60, indium, gallium and selenium is 1: 0.7: 0.3: 2.Stress once more at this; Above-mentioned mole ratio be not for the present invention to discuss the emphasis of studying carefully, the ratio value of its mole number can be according to the user in sputter process; For solar energy generating efficiency and cost needs, adjust the part by weight of each material in the above-mentioned allotment powder to considered.Moreover because in this experimental example, the bottom and the sidewall of target backboard groove respectively are provided with coarse structure, the work material powder is not only effectively inserted in the coarse structure, after hardening by cooling, can effectively combine with these coarse structures, so can improve the bonded stability significantly.
Four, CIGS quaternary sputtered target material of the present invention reclaims the method that feed supplement utilizes again
1. exploitation reason
Like the target that above-mentioned the present invention researched and developed, for including element bonded CIGS quaternary sputtered target materials such as copper Cu, indium In, gallium Ga and selenium Se.CIS is or CIGS series target material or other targets in the known technology and press; All must target be engaged with the target backboard; Just can attach in the reaction chamber that is hung on sputtering equipment usefulness for sputter; Then must the residue target be pulled down on the target backboard after using, on former target backboard, connect new target again, the technology that for example case is disclosed before the patent carried of above-mentioned background.In the known technology, dismounting residue target on the target backboard is removed the bonding material in centre on the target backboard, rejoins and adorns new target, and global procedures is complicated, increases man-hour, and the residue target is handled and utilized also very difficultly again, and still can produce above-mentioned problem when engaging.So inventor's research must not separated target and target backboard; And with after it cleaning, directly insert in the mould, insert the work material powder; As the invention described above procedure for processing; Melt, pressurize and cool off through heat, can make the residue target fill material and form complete target plate, and can reach the effect that quick recovery utilizes again.
2. the solution of problem
Known technology is that the residue target is separated on the target backboard, utilizes indirect material on original target backboard, to connect target again, causes processing procedure complicated, engages insecurely, and target material is inhomogeneous, and the cleaning of target backboard and residue target are handled and defective such as be difficult for.In order to solve the above problems, the work material powder of the special allotment of the inventor makes the CIGS quaternary sputtered target material can be directly molded and shaped; And be the some of mould with the target back plate design, so add mould together with the target backboard, insert the work material powder in die cavity as long as will remain target; Heat through general is melted, pressurization and cooling program, can make the target polishing, and still keeps combining with the target backboard; Significantly simplify processing procedure, and can thoroughly address the above problem.
3. specific embodiment
Like Fig. 1, shown in 9 and 10, CIGS quaternary sputtered target material of the present invention reclaims the method that feed supplement utilizes again, mainly includes the following step:
(a) prepare four kinds of element materials such as copper Cu, indium In, gallium Ga and selenium Se;
(b3) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder 10; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder 20; If the selenium of being prepared is solid, then with selenium Se solid 30 grind into powders 31.
(c3) copper/indium CuIn powdered alloy 10, copper/gallium CuGa powdered alloy 20 and selenium Se material powder 31 are filled part mixing and prepare into work material powder 40.
(d3) CIGS target 61 used with one and that be combined on the target backboard 52 cleans, and inserts in the mould 50, and work material powder 40 is inserted in the mould 50; This mould 50 includes this backboard 52 as master mold, a frame mould 53 and the male model 54 that a frame is trapped among target backboard 52 end faces, and target backboard 52 is fixed on the base 55, and target backboard 52 end faces are provided with a groove 520; Groove 520 bottoms are provided with coarse structure 521; Male model 54 bottom surfaces have a die 540, and die 540 outline shapes match with the frame mouth 530 of frame mould 53, and the groove 520 and the frame mould 53 of target backboard 52 surround a molding cave 51; Insert work material powder 40 in this moulding die cavity 51; Work material powder 40 is heated to the melting temperature of selenium, and repeatedly pressurizes, make after the even chemical combination bonding of copper, indium, gallium and the selenium one and and merge postcooling with remaining target.
(e3) cooling back removal male model, frame mould and base are promptly accomplished the work program that the target feed supplement becomes required specification, and can continue to supply to use.
4. experimental example
Like Fig. 1, shown in 9 and 10; CIGS quaternary sputtered target material of the present invention reclaims the experimental example that feed supplement utilizes again; Get copper Cu 44.48 weight parts and the mutual uniform mixing of indium In 80.37 weight parts; Repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder 10 that particle diameter is about 74 μ m.With the mutual uniform mixing of gallium Ga of copper Cu 19.06 weight parts and 20.92 weight parts, repeatedly vacuum-heat-melt, pressurization of warp, the program of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder 20 that particle diameter is about 74 μ m.The selenium Se material powder 31 of copper/gallium CuGa powdered alloy 20 and 157.92 weight parts of getting copper/indium CuIn powdered alloy 10,100 weight parts of 100 weight parts fills and part mixes and prepare into work material powder 40.
Prepare a mould 50, it includes a frame mould 53 and a male model 54; And with one be combined with remaining target 61 target backboard 52 as master mold, target backboard 52 is fixed on the base 55; Male model 54 bottom surfaces have a die 540, and die 540 outline shapes match with the frame mouth 530 of frame mould 53, and target 61, target backboard 52 and frame mould 53 surround a molding cave 51.Work material powder 40 is inserted in the moulding die cavity 51, work material powder 40 is heated to the melting temperature of selenium, the male model 54 feedings pressurization of mould 50 once; After the cooling, be heated to the melting temperature of selenium again, and control male model 54 feeding pressurization is once again; After cooling; Removal male model 54 and frame mould 53 are promptly accomplished the processing procedure that makes target 61 polishings to the strip and block that is required specification, and its target includes copper Cu, indium In, gallium Ga and selenium Se element; And the mole ratio of the copper of target, indium, gallium and selenium is 1: 0.7: 0.3: 2; So may command is identical with the composition and the mole number of original residue target, and target 61 and target backboard 52 mortise still, and can continue use.
Five, conclusion
Through the detailed description of above-mentioned specific embodiment and experimental example, can conclude the present invention and have following several major advantage:
1. the present invention goes ahead of the rest to classify and is deployed into copper/indium alloy powder, copper/gallium alloy powder; Again they and selenium powder end are modulated into the processing powder; Can solve the direct blended of selenium and gallium or indium difficulty and institute and produce problem hypertoxic or that explode; Make directly and to melt and pressurization and molded and shaped CIGS quaternary sputtered target material is able to put into carry out through heat, and then significantly simplify processing procedure and reduce cost with material powder.
2. the present invention is said except the 1st advantage, can be directly melts and pressurization and outside the molded and shaped CIGS quaternary sputtered target material, be again the some of mould with the target back plate design through heat with material powder; When heat was melted the moulding target in mould, target promptly directly combined with the target backboard, and then can significantly simplify processing procedure and reduce cost at material powder; Reach more known gummed mode and can improve the combination stability, especially than the U.S. the 5th, 230; Though No. 459 the patent case is provided with coarse structure; But still after being difference moulding target and target backboard, again target and target backboard heat are fused the technology of closing, more can improve target and target backboard bonded stability.
3. the present invention is of the 2nd advantage, can be directly melt and pressurization and molded and shaped CIGS quaternary sputtered target material through heat with material powder, and design target and target backboard is the some of mould; As long as will remain target combines with male model, frame mould together with the target backboard; Insert the work material powder in die cavity, through general heat melt, pressurization and cooling program, can make the target polishing; And still keep combining, significantly simplify the processing procedure of recycling with the target backboard.
The above is merely the feasible specific embodiment of the present invention, is not in order to limit claim of the present invention.
Claims (17)
1. the method for manufacture of a CIGS quaternary sputtered target material is characterized in that, includes the following step:
(a) prepare the work material powder, said work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se;
(b) said work material powder is inserted in the die cavity of a mould,, and repeatedly pressurize, make copper Cu, gallium Ga, indium In and the even chemical combination of selenium Se and cooling again after the one that bonds the melting temperature of said work material powder heating at least to selenium; And
(c) unloading said mould in cooling back is promptly accomplished the target manufacturing of strip and block, and is made said target include copper Cu, indium In, gallium Ga and selenium Se;
The step of said preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder; Be ready for selenium Se powder; And
(a3) said copper/indium CuIn powdered alloy, said copper/gallium CuGa powdered alloy and said selenium material powder thorough mixing are formed said work material powder.
2. the method for manufacture of CIGS quaternary sputtered target material according to claim 1 is characterized in that: repeat repeatedly the described pressurization formula of (b) step.
3. the method for manufacture of CIGS quaternary sputtered target material according to claim 1; It is characterized in that: the said mould of step (b) includes a frame mould and the male model that aluminum target backboard, a frame as master mold is trapped among said target backboard end face; Said target backboard is fixed on the base; Said male model bottom surface has a die; Said die outline shape matches with the frame mouth of said frame mould, and said target backboard and said frame mould surround a molding cave, insert said work material powder in said moulding die cavity.
4. the method for manufacture of CIGS quaternary sputtered target material according to claim 3; It is characterized in that: said aluminum target backboard end face is provided with a groove; Said groove is the some of said moulding die cavity; Said groove includes a wall and a bottom, and said bottom is provided with one first coarse structure, and said wall is provided with one second coarse structure.
5. the method for manufacture of CIGS quaternary sputtered target material according to claim 4 is characterized in that: the degree of depth of said groove is 2～3mm.
6. the method for manufacture of CIGS quaternary sputtered target material according to claim 4; It is characterized in that: said first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed; Said second coarse structure be one along the contour loop of said groove around chase, said chase is positioned at the wall and the junction, bottom of said groove.
7. the method for manufacture of CIGS quaternary sputtered target material according to claim 6 is characterized in that: the degree of depth of said slit is 2～3mm, the about 5mm of width, and the about 15mm in interval of two adjacent said slits.
8. the method for manufacture of CIGS quaternary sputtered target material according to claim 1 is characterized in that: in the said step (b), said mould is placed a vacuum chamber to heat and pressurizes.
A CIGS quaternary sputtered target material moulding simultaneously with target backboard bonded method, it is characterized in that, include the following step:
(a) prepare the work material powder, said work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se material;
(b1) said work material powder is inserted in the mould, said mould includes a frame mould and the male model that aluminum target backboard, a frame as master mold is trapped among said target backboard end face, and said target backboard is fixed on the base; Said target backboard end face is provided with a groove, and said groove includes a bottom and a wall, and said bottom is provided with one first coarse structure; Said wall is provided with one second coarse structure; Said male model bottom surface has a die, and said die outline shape matches with the frame mouth of said frame mould, and the groove of said target backboard and said frame mould surround a molding cave; Insert said work material powder in said moulding die cavity; Said work material powder is heated to the melting temperature of selenium, and pressurizes, make the even chemical combination of copper, gallium, indium and selenium and engage postcooling after the one that bonds and with backboard; And
(c1) cooling back unloading said male model, said frame mould and said base promptly accomplished the manufacturing that target material moulding engages with said target backboard simultaneously, and the said target that includes copper Cu, indium In, gallium Ga and selenium Se element is incorporated on the said aluminum target backboard;
The step of said preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder; Be ready for selenium Se powder; And
(a3) said copper/indium CuIn powdered alloy, said copper/gallium CuGa powdered alloy and said selenium material powder thorough mixing are formed said work material powder.
10. CIGS quaternary sputtered target material moulding while according to claim 9 and target backboard bonded method, it is characterized in that: repeat repeatedly the pressurization formula in (b1) step.
11. CIGS quaternary sputtered target material moulding while according to claim 9 and target backboard bonded method, it is characterized in that: the degree of depth of said groove is 2～3mm.
12. CIGS quaternary sputtered target material moulding while according to claim 9 and target backboard bonded method; It is characterized in that: said first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed; Said second coarse structure be one along the contour loop of said groove around chase, said chase is positioned at the wall and the junction, bottom of said groove.
13. CIGS quaternary sputtered target material moulding according to claim 12 simultaneously and target backboard bonded method, it is characterized in that: the degree of depth of slit is 2～3mm, the about 5mm of width, and the about 15mm in interval of two adjacent said slits.
14. CIGS quaternary sputtered target material moulding according to claim 9 simultaneously and target backboard bonded method, is characterized in that: in the said step (b1), said mould is placed a vacuum chamber to heat and pressurizes.
15. the compensation process of a CIGS quaternary sputtered target material is characterized in that, includes the following step:
(a) prepare the work material powder, said work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se;
(b2) the residue target that used and still be combined with a target backboard with is cleaned; And insert in the mould, and said work material powder to be inserted in the said mould, said mould includes a frame mould and the male model that an aluminum backboard as master mold, a frame are trapped among said target backboard end face; Said target backboard is fixed on the base; Said target backboard end face is provided with a groove, and said bottom portion of groove is provided with coarse structure, and said male model bottom surface has a die; Said die outline shape matches with the frame mouth of said frame mould; The groove of said target backboard and said frame mould surround a molding cave, insert said work material powder in said moulding die cavity, to the melting temperature of said work material powder heating at least to selenium; And pressurize, make copper Cu, gallium Ga, indium In and the even chemical combination of selenium Se and merge postcooling after the one that bonds and with said residue target; And
(c2) the cooling back unloads said male model, said frame mould and said base, promptly accomplishes the processing procedure of said residue target feed supplement;
The step of said preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2) with copper Cu and the mutual uniform mixing of indium In, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/indium CuIn alloy material powder; With copper Cu and the mutual uniform mixing of gallium Ga, repeatedly vacuum-heat-melt, pressurization of warp, the formula of cooling off and pulverizing, and prepare into copper/gallium CuGa alloy material powder; Be ready for selenium Se powder; And
(a3) said copper/indium CuIn powdered alloy, said copper/gallium CuGa powdered alloy and said selenium material powder thorough mixing are formed said work material powder.
16. the compensation process of CIGS quaternary sputtered target material according to claim 15 is characterized in that: repeat repeatedly the pressurization formula in (b2) step.
17. the compensation process of CIGS quaternary sputtered target material according to claim 15 is characterized in that: in the step (b2), said mould is placed a vacuum chamber to heat and pressurizes.
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| WO2012145895A1 (en) * | 2011-04-26 | 2012-11-01 | Chang Sheng-Chang | Method of manufacturing cigs solar energy photoelectric quaternary sputtering target, method of bonding the same with target backing plate, and method of supplementing material thereof |
| CN103343321A (en) * | 2012-03-12 | 2013-10-09 | 有研亿金新材料股份有限公司 | Method of manufacturing sputtering target |
| CN102677013A (en) * | 2012-05-25 | 2012-09-19 | 大连交通大学 | Cu (In1-xGax) Se2 film, and preparation method and application thereof |
| WO2014002127A1 (en) * | 2012-06-25 | 2014-01-03 | 株式会社栗本鐵工所 | Long light metal billet and manufacturing method therefor |
| CN103014623A (en) * | 2012-12-11 | 2013-04-03 | 中国科学院电工研究所 | Ceramic target material preparation method for CIGS (copper indium gallium selenide) based solar film battery light absorption layer |
| CN103695850B (en) * | 2013-12-27 | 2016-01-20 | 柳州百韧特先进材料有限公司 | The preparation method of solar cell CIGS target |
| CN103706799A (en) * | 2013-12-27 | 2014-04-09 | 柳州百韧特先进材料有限公司 | Method for preparing CIGS powder through dry 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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| CN101245443A (en) * | 2007-02-17 | 2008-08-20 | 光洋应用材料科技股份有限公司 | Target material and thin membrane manufactured with the target material |
| CN101260513A (en) * | 2008-04-23 | 2008-09-10 | 王东生 | Solar energy battery copper-indium-gallium-selenium film key target material and preparation method thereof |
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| CN101260513A (en) * | 2008-04-23 | 2008-09-10 | 王东生 | Solar energy battery copper-indium-gallium-selenium film key target material and preparation method thereof |
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