CN102051584A - 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, especially refer to that a kind of copper Cu, indium In, gallium Ga and selenium Se classification are modulated into the work material powder, the work material powder is filled in the mould, melt and the pressurization program by 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
Copper-indium-galliun-selenium CIGS type thin-film solar cells known to pressing at present, its basic structure as 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 classes according to process technique, and a class is made CIGS film light absorption layer for utilizing vacuum splashing and plating processing procedure or evaporation processing procedure, and another kind of then is non-vacuum process technology (as electroplating 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 manufacture method 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 as Taiwan, wherein powder metallurgy method must prepare CIGS based material powder earlier, and the technology solvent thermal synthesis method (Solvothermal synthesis) of its CIGS based material powdered preparation, or by disclose as Taiwan No. 200932679 and No. 200932933 chemical wet synthesis method (chemical reflux synthesis 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 carried out for the ease of sputter process, target must combine with the target backboard, and the structure by 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 Resins, epoxy solid joining technique again, and target and target backboard are bonded with each other, or as the U.S. the 5th, 230, No. 459, No. 287125 disclosed technology of patent case in public gulf are to form uneven surface in the target back plate surface, after pasting target repeatedly, by 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, install an indium sheeting respectively between the target of moulding and the target backboard, 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 the manufacturing course complexity, 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 target cost costliness, if after target uses, will remain target and abandon, real is waste.And present known mode with the target recycling has the technology that reclaims at sputtered aluminium alloy target material to be developed, for example the technology of No. 483937 patent case in Taiwan.Because known target and target backboard moulding respectively, utilize joining technique again and make the two joint, desire recycling, just must earlier target be separated with the target backboard,, and the target backboard must 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 design: (i) copper is mixed mutually with indium, through vacuum-heat-melt, pressurization repeatedly, the program of cooling off and pulverizing, and prepare into copper/indium alloy powder; (ii) copper is mixed mutually with gallium,, and prepare into copper/gallium alloy powder through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize; (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 by 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 by general heat temperature raising heat again, rapid shaping includes copper Cu, indium In, gallium Ga and selenium Se phase bonded target.
Concrete steps are as follows:
A kind of manufacture method of CIGS quaternary sputtered target material includes the following step:
(a) prepare the work material powder, described work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se;
(b) described 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 described work material powder heating at least to selenium; And
(c) unloading described mould in cooling back is promptly finished the target manufacturing of strip and block, and is made described target include copper Cu, indium In, gallium Ga and selenium Se.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: the step of described preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2),, and prepare into copper/indium CuIn alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize; Be ready for selenium Se powder; And
(a3) described copper/indium CuIn powdered alloy, described copper/gallium CuGa powdered alloy and described selenium material powder are filled part and mix described work material powder.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: can repeat repeatedly the described pressurization formula of (b) step.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: the described mould of step (b) includes a frame mould and the male model that aluminum target backboard, a frame as master mold is trapped among described target backboard end face, described target backboard is fixed on the base, described male model bottom surface has a die, described die outline shape matches with the frame mouth of described frame mould, described target backboard and described frame mould surround a molding cave, insert described work material powder in described moulding die cavity.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: described aluminum target backboard end face is provided with a groove, described groove is the some of described moulding die cavity, described groove includes a wall and a bottom, described bottom is provided with one first coarse structure, and described wall is provided with one second coarse structure.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: the degree of depth of described groove is 2～3mm.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: described first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed, described second coarse structure be one along the contour loop of described groove around chase, described chase is positioned at the wall and the junction, bottom of described groove.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: the degree of depth of described slit is 2～3mm, the about 5mm of width, and the about 15mm in interval of two adjacent described slits.
The manufacture method of above-mentioned CIGS quaternary sputtered target material, wherein: in the described step (b), can place a vacuum chamber to heat on described mould and pressurize.
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 design: 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 as follows:
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, described work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se material;
(b1) described work material powder is inserted in the mould, described mould includes an aluminum target backboard as master mold, one frame is trapped among the frame mould and a male model of described target backboard end face, described target backboard is fixed on the base, described target backboard end face is provided with a groove, described groove includes a bottom and a wall, described bottom is provided with one first coarse structure, described wall is provided with one second coarse structure, described male model bottom surface has a die, described die outline shape matches with the frame mouth of described frame mould, the groove of described target backboard and described frame mould surround a molding cave, insert described work material powder in described moulding die cavity, described work material powder is heated to the melting temperature of selenium, and is pressurizeed, make copper, gallium, the even chemical combination of indium and selenium and engage postcooling after the one that bonds and with backboard; And
(c1) cooling back unloading described male model, described frame mould and described base promptly finished the manufacturing that target material moulding engages with described target backboard simultaneously, and the described target that includes copper Cu, indium In, gallium Ga and selenium Se element is incorporated on the described aluminum target backboard.
Above-mentioned CIGS quaternary sputtered target material moulding while and target backboard bonded method, wherein: the step of described preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2),, and prepare into copper/indium CuIn alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize; Be ready for selenium Se powder; And
(a3) described copper/indium CuIn powdered alloy, described copper/gallium CuGa powdered alloy and described selenium material powder are filled part and mix described 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 described groove is 2～3mm.
Above-mentioned CIGS quaternary sputtered target material moulding while and target backboard bonded method, wherein: described first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed, described second coarse structure be one along the contour loop of described groove around chase, described chase is positioned at the wall and the junction, bottom of described 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 described slits.
Above-mentioned CIGS quaternary sputtered target material moulding simultaneously and target backboard bonded method, wherein: in the described step (b1), can place a vacuum chamber to heat on described mould and pressurize.
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 use for continuing.
For realizing aforementioned purpose, the utility model is taked following design: utilize above-mentioned work material powder, and the principle of above-mentioned second purpose, after using and be combined with the target cleaning of 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 for use.
Concrete steps are as follows:
A kind of compensation process of CIGS quaternary sputtered target material includes the following step:
(a) prepare the work material powder, described 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 described work material powder inserted in the described mould, described mould includes an aluminum backboard as master mold, one frame is trapped among the frame mould and a male model of described target backboard end face, described target backboard is fixed on the base, described target backboard end face is provided with a groove, described bottom portion of groove is provided with coarse structure, described male model bottom surface has a die, described die outline shape matches with the frame mouth of described frame mould, the groove of described target backboard and described frame mould surround a molding cave, insert described work material powder in described moulding die cavity, to the melting temperature of described work material powder heating at least to selenium, and pressurizeed, 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 described residue target; And
(c2) the cooling back unloads described male model, described frame mould and described base, promptly finishes the processing procedure of described residue target feed supplement.
The compensation process of above-mentioned CIGS quaternary sputtered target material, wherein: the step of described preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2),, and prepare into copper/indium CuIn alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize; Be ready for selenium Se powder; And
(a3) described copper/indium CuIn powdered alloy, described copper/gallium CuGa powdered alloy and described selenium material powder are filled part and mix described 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 place a vacuum chamber to heat on described mould and pressurize.
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 put to carry out through heat, and then significantly simplify processing procedure and reduce cost with material powder.
2. the present invention is described except the 1st advantage, can be directly melt and pressurization and outside the molded and shaped CIGS quaternary sputtered target material through heat with material powder, it with the target back plate design again the some of mould, material powder in mould heat melt the moulding target in, target promptly directly combines with the target backboard, and then can significantly simplify processing procedure and reduce cost, and more known gummed mode and can improving in conjunction with stability, especially than the U.S. the 5th, 230, though No. 459 patent cases are 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 as described in 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 are 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 auditor's understood in detail and those skilled in the art, now the specific embodiment of above-mentioned three characteristics is described in detail 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 technology of the present invention has following three:
First, be to make a kind of copper Cu that includes, indium In, the method of the CIGS quaternary sputtered target material of gallium Ga and selenium Se element: it utilizes special material formulation as described below to classify allotment in advance and makes 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 by general heat temperature raising heat again, can include copper Cu by rapid shaping, indium In, the target of gallium Ga and selenium Se element, significantly simplify work program, and reduce cost.
The second, be must be combined as a whole with the target backboard in target material moulding: 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, mould can 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 use for continuing via supplementary material: it utilizes above-mentioned work material powder, and the principle of above-mentioned second characteristic, after using and be combined with the target cleaning of target backboard, it is added mould, again the work material powder is inserted the part of die cavity vacancy, and mould can be placed vacuum cavity, again through overheatedly melt, after pressurization and the refrigerative program, can make target be supplemented to the size of required specification, significantly simplify the program of recycling.
Two, the manufacture method of CIGS quaternary sputtered target material of the present invention
1, exploitation reason
As shown in Figures 1 to 3, the present invention particularly researches and develops at the CIGS quaternary sputtered target material that includes elements such as copper Cu, indium In, gallium Ga and selenium Se, and this quaternary sputtered target material is the usefulness for 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 make 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
Known to experiment, indium In or gallium Ga directly mix with selenium Se, when fusing, can produce vigorous reaction, measure can produce blast when big and generation is hypertoxic, and owing to the fusing point of gallium is extremely low, are difficult for being modulated into powder in general processing environment temperature.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 is mixed mutually with indium, through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize, and prepare into copper/gallium alloy powder; (ii) copper is mixed mutually with gallium,, and prepare into copper/gallium alloy powder through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize; (iii) and be ready for selenium Se powder.Then, copper/indium alloy powder, copper/gallium alloy material and selenium material powder are filled part mixing again 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
As shown in Figure 1 to Figure 3, the manufacture method 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 mutually with indium In,, and prepare into copper/indium CuIn alloy material powder 10 through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize; Copper Cu is mixed mutually with gallium Ga,, 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 pressurizeed, 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 finished 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 manufacture method 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 getting the copper/gallium CuGa powdered alloy 20 of copper/indium CuIn powdered alloy 10,100 weight parts of 100 weight parts and 157.92 weight parts fills and part mixes and prepare into work material powder 40.As shown in Figure 1 to Figure 3, this work material powder 40 is inserted in the die cavity 51 of mould 50, 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 finished 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 is not will discuss the emphasis study carefully for the present invention, the ratio value of its mole number, can be in sputter process according to the user, for solar energy generating efficiency and the corresponding needs of considering of cost, 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
As 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 is engaged 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 effectively with the target backboard.In addition, if adopt copper target backboard, when selenium Se powder is overlying on the junction surface of copper target backboard, after heat is melted and is cooled off, the selenium powder end of target backboard and target joint is fashionable with the thawing of copper target backboard heat, its bonded copper selenium alloy can be powdered, thereby the problem that target can't engage really with the target backboard takes place.So, inventor's research, melting 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, target is molded directly within on the target backboard, can directly combine by target of the present invention with the target backboard, significantly simplify the two bonded processing procedure, and because of selenium powder end meeting and copper in low temperature, indium, gallium chemical combination, and can not close with calorize, so can avoid target and target backboard joint to form the situation of powdered, so can guarantee target and target backboard mortise, and 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 known to knowledge and inventor's test, the selenium powder end is filled out and is overlayed on the copper target backboard, and it melts with copper chemical combination meeting shape powdered after cooling through heat, and causes target and target backboard joint powdered, 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, with copper/indium alloy powder, copper/gallium alloy material and selenium material powder fill part work material powder that mixing is prepared and insert mould, melt through general heat, pressurization and cooling program, it is plastic target, target directly is incorporated on the target backboard, overall process is simplified, need not to re-use indirect material, and become the technology of target at the work material powder moulding of CIGS system, target backboard of the present invention is to make with aluminium, the selenium powder end can not closed with calorize in low temperature, so can avoid target and target backboard joint to produce powdered, and can guarantee the target uniform ingredients, precision is high to be reached and target backboard mortise, and then thoroughly addresses 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 manufacture method includes the following step:
(a) prepare four kinds of element materials such as copper Cu, indium In, gallium Ga and selenium Se;
(b2),, and prepare into copper/indium CuIn alloy material powder 10 through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder 20 through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize; 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 an aluminum target backboard 52 as master mold, one frame is trapped among the frame mould 53 and a male model 54 of target backboard 52 end faces, target backboard 52 is fixed on the base 55, target backboard 52 end faces are provided with a groove 520, groove 520 bottoms are provided with coarse structure 521, 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 mould 50 can 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 pressurizeed repeatedly, make copper, gallium, indium and selenium homogenizing merge the bonding one and moulding target 60, and the while combines postcooling with target backboard 52.
(e2) cooling back removal male model 54, frame mould 53 and base 55 are promptly finished target material moulding simultaneously and target backboard 52 bonded processing procedures, and this target 60 is made 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 manufacture method, 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,, and prepare into copper/gallium CuGa alloy material powder 20 that particle diameter is about 74 μ m through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize.The selenium Se material powder 31 of getting the copper/gallium CuGa powdered alloy 20 of copper/indium CuIn powdered alloy 10,100 weight parts of 100 weight parts and 157.92 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, first coarse structure 521 includes a plurality of vertical slit 522 and a plurality of transverse slot 523 that are interspersed, 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 general depth range of implementing can be 15～20mm) to the about 15mm in interval of two adjacent slits 522/523, 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 as 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 finish 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, 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.Emphasize once more at this, above-mentioned mole ratio is not that the ratio value of its mole number can be according to the user in sputter process for the present invention will discuss the emphasis of studying carefully, for solar energy generating efficiency and the corresponding needs of considering of cost, adjust the part by weight of each material in the above-mentioned allotment powder.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, can combine with these coarse structures are effective after hardening by cooling, 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
As 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 target must be engaged with the target backboard, could be attached be hung in the reaction chamber of sputtering equipment usefulness for sputter, then the residue target must be pulled down on the target backboard after using, on former target backboard, connect new target again, for example the disclosed technology of case before the patent put forward 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, target and target backboard must not separated, 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 to connect target again on original target backboard, 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, make the CIGS quaternary sputtered target material can be directly molded and shaped, and be the some of mould, so add mould together with the target backboard as long as will remain target with the target back plate design, 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 with the target backboard, significantly simplify processing procedure, and can thoroughly address the above problem.
3. specific embodiment
Shown in Fig. 1,9 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),, and prepare into copper/indium CuIn alloy material powder 10 through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder 20 through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize; 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 insert in the mould 50, and work material powder 40 inserted in the mould 50, this mould 50 includes this backboard 52 as master mold, one frame is trapped among the frame mould 53 and a male model 54 of target backboard 52 end faces, target backboard 52 is fixed on the base 55, 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, 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 this moulding die cavity 51, work material powder 40 is heated to the melting temperature of selenium, and repeatedly pressurizes, make copper, indium, merge postcooling after the even chemical combination bonding of gallium and the selenium one and with remaining target.
(e3) cooling back removal male model, frame mould and base are promptly finished the work program that the target feed supplement becomes required specification, and can continue for using.
4. experimental example
Shown in Fig. 1,9 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, through repeatedly vacuum-heat-melt, pressurization, the program cooling off and 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 Cu 19.06 weight parts and 20.92 weight parts,, and prepare into copper/gallium CuGa alloy material powder 20 that particle diameter is about 74 μ m through repeatedly vacuum-heat-melt, pressurization, the program cooling off and pulverize.The selenium Se material powder 31 of getting the copper/gallium CuGa powdered alloy 20 of copper/indium CuIn powdered alloy 10,100 weight parts of 100 weight parts and 157.92 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 a target backboard 52 that is combined with remaining target 61 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, promptly finish and make the processing procedure of target 61 polishings to the strip and block that is required specification, its target includes copper Cu, indium In, gallium Ga and selenium Se element, and the copper of target, indium, the mole ratio of 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
By 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 put to carry out through heat, and then significantly simplify processing procedure and reduce cost with material powder.
2. the present invention is described except the 1st advantage, can be directly melt and pressurization and outside the molded and shaped CIGS quaternary sputtered target material through heat with material powder, it with the target back plate design again the some of mould, material powder in mould heat melt the moulding target in, target promptly directly combines with the target backboard, and then can significantly simplify processing procedure and reduce cost, and more known gummed mode and can improving in conjunction with stability, especially than the U.S. the 5th, 230, though No. 459 patent cases are 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 as described in 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 are 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 only is the feasible specific embodiment of the present invention, is not in order to limit claim of the present invention.
Claims (20)
1. the manufacture method of a CIGS quaternary sputtered target material is characterized in that, includes the following step:
(a) prepare the work material powder, described work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se;
(b) described 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 described work material powder heating at least to selenium; And
(c) unloading described mould in cooling back is promptly finished the target manufacturing of strip and block, and is made described target include copper Cu, indium In, gallium Ga and selenium Se.
2. the manufacture method of CIGS quaternary sputtered target material according to claim 1 is characterized in that: the step of described preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2),, and prepare into copper/indium CuIn alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize; Be ready for selenium Se powder; And
(a3) described copper/indium CuIn powdered alloy, described copper/gallium CuGa powdered alloy and described selenium material powder are filled part and mix described work material powder.
3. the manufacture method of CIGS quaternary sputtered target material according to claim 1 is characterized in that: can repeat repeatedly the described pressurization formula of (b) step.
4. the manufacture method of CIGS quaternary sputtered target material according to claim 1, it is characterized in that: the described mould of step (b) includes a frame mould and the male model that aluminum target backboard, a frame as master mold is trapped among described target backboard end face, described target backboard is fixed on the base, described male model bottom surface has a die, described die outline shape matches with the frame mouth of described frame mould, described target backboard and described frame mould surround a molding cave, insert described work material powder in described moulding die cavity.
5. the manufacture method of CIGS quaternary sputtered target material according to claim 4, it is characterized in that: described aluminum target backboard end face is provided with a groove, described groove is the some of described moulding die cavity, described groove includes a wall and a bottom, described bottom is provided with one first coarse structure, and described wall is provided with one second coarse structure.
6. the manufacture method of CIGS quaternary sputtered target material according to claim 5 is characterized in that: the degree of depth of described groove is 2～3mm.
7. the manufacture method of CIGS quaternary sputtered target material according to claim 5, it is characterized in that: described first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed, described second coarse structure be one along the contour loop of described groove around chase, described chase is positioned at the wall and the junction, bottom of described groove.
8. the manufacture method of CIGS quaternary sputtered target material according to claim 7 is characterized in that: the degree of depth of described slit is 2～3mm, the about 5mm of width, and the about 15mm in interval of two adjacent described slits.
9. the manufacture method of CIGS quaternary sputtered target material according to claim 1 is characterized in that: in the described step (b), can place a vacuum chamber to heat on described mould and pressurize.
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, described work material powder is that hybrid packet contains copper Cu, indium In, gallium Ga and selenium Se material;
(b1) described work material powder is inserted in the mould, described mould includes an aluminum target backboard as master mold, one frame is trapped among the frame mould and a male model of described target backboard end face, described target backboard is fixed on the base, described target backboard end face is provided with a groove, described groove includes a bottom and a wall, described bottom is provided with one first coarse structure, described wall is provided with one second coarse structure, described male model bottom surface has a die, described die outline shape matches with the frame mouth of described frame mould, the groove of described target backboard and described frame mould surround a molding cave, insert described work material powder in described moulding die cavity, described work material powder is heated to the melting temperature of selenium, and is pressurizeed, make copper, gallium, the even chemical combination of indium and selenium and engage postcooling after the one that bonds and with backboard; And
(c1) cooling back unloading described male model, described frame mould and described base promptly finished the manufacturing that target material moulding engages with described target backboard simultaneously, and the described target that includes copper Cu, indium In, gallium Ga and selenium Se element is incorporated on the described aluminum target backboard.
11. CIGS quaternary sputtered target material moulding while according to claim 10 and target backboard bonded method, it is characterized in that: the step of described preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2),, and prepare into copper/indium CuIn alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize; Be ready for selenium Se powder; And
(a3) described copper/indium CuIn powdered alloy, described copper/gallium CuGa powdered alloy and described selenium material powder are filled part and mix described work material powder.
12. CIGS quaternary sputtered target material moulding while according to claim 10 and target backboard bonded method, it is characterized in that: can repeat repeatedly the pressurization formula in (b1) step.
13. CIGS quaternary sputtered target material moulding while according to claim 10 and target backboard bonded method, it is characterized in that: the degree of depth of described groove is 2～3mm.
14. CIGS quaternary sputtered target material moulding while according to claim 10 and target backboard bonded method, it is characterized in that: described first coarse structure includes a plurality of vertical slits and a plurality of transverse slot that is interspersed, described second coarse structure be one along the contour loop of described groove around chase, described chase is positioned at the wall and the junction, bottom of described groove.
15. CIGS quaternary sputtered target material moulding according to claim 14 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 described slits.
16. CIGS quaternary sputtered target material moulding according to claim 10 simultaneously and target backboard bonded method, is characterized in that: in the described step (b1), can place a vacuum chamber to heat on described mould and pressurize.
17. the compensation process of a CIGS quaternary sputtered target material is characterized in that, includes the following step:
(a) prepare the work material powder, described 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 described work material powder inserted in the described mould, described mould includes an aluminum backboard as master mold, one frame is trapped among the frame mould and a male model of described target backboard end face, described target backboard is fixed on the base, described target backboard end face is provided with a groove, described bottom portion of groove is provided with coarse structure, described male model bottom surface has a die, described die outline shape matches with the frame mouth of described frame mould, the groove of described target backboard and described frame mould surround a molding cave, insert described work material powder in described moulding die cavity, to the melting temperature of described work material powder heating at least to selenium, and pressurizeed, 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 described residue target; And
(c2) the cooling back unloads described male model, described frame mould and described base, promptly finishes the processing procedure of described residue target feed supplement.
18. the compensation process of CIGS quaternary sputtered target material according to claim 17 is characterized in that: the step of described preparation work material powder comprises:
(a1) prepare copper Cu, indium In, gallium Ga and selenium Se;
(a2),, and prepare into copper/indium CuIn alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize with copper Cu and the mutual uniform mixing of indium In; With copper Cu and the mutual uniform mixing of gallium Ga,, and prepare into copper/gallium CuGa alloy material powder through repeatedly vacuum-heat-melt, pressurization, the formula cooling off and pulverize; Be ready for selenium Se powder; And
(a3) described copper/indium CuIn powdered alloy, described copper/gallium CuGa powdered alloy and described selenium material powder are filled part and mix described work material powder.
19. the compensation process of CIGS quaternary sputtered target material according to claim 17 is characterized in that: can repeat repeatedly the pressurization formula in (b2) step.
20. the compensation process of CIGS quaternary sputtered target material according to claim 17 is characterized in that: in the step (b2), can place a vacuum chamber to heat on described mould and pressurize.
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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 |
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