CN104478222A - Lead-free glass powder applicable to crystalline silicon solar cell back silver paste and preparation method of lead-free glass powder - Google Patents
Lead-free glass powder applicable to crystalline silicon solar cell back silver paste and preparation method of lead-free glass powder Download PDFInfo
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- CN104478222A CN104478222A CN201410839742.3A CN201410839742A CN104478222A CN 104478222 A CN104478222 A CN 104478222A CN 201410839742 A CN201410839742 A CN 201410839742A CN 104478222 A CN104478222 A CN 104478222A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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Abstract
The invention provides a lead-free glass powder applicable to crystalline silicon solar cell back silver paste and a preparation method of the lead-free glass powder. The lead-free glass powder is prepared from the following raw materials by mole percent: 10-30 percent of SiO2, 20-80 percent of Bi2O3, 1-20 percent of B2O3, 0-2 percent of Al2O3, 0-2 percent of ZnO and 0-2 percent of Sb2O3. The preparation method comprises the following steps: mixing the raw materials to obtain a mixture with the uniformity of 90% or above, adding the mixture into a corundum crucible at 900-1,000 DEG C, covering the corundum crucible, heating the corundum crucible to 1,200-1,500 DEG C at the heating rate of 10 DEG C/min, preserving heat for 1-2 h until the glass raw materials are liquefied completely, fully stirring completely liquefied glass melt, quenching the glass melt with water, ball-milling and drying dried glass material, and screening ball-milled glass powder to prepare super-fine glass powder with the particle size below 5 mm. The lead-free glass powder prepared by the invention is matched with a cell silicon wafer and an aluminum back surface field in thermal expansion coefficient and softening point, the adhesive force of the sintered lead-free glass powder to the cell silicon wafer and the aluminum back surface field is increased obviously, the welding property of the silver paste and the matchability of silver paste and aluminum are improved, and the preparation technology is simple.
Description
Technical field
The invention belongs to technical field of electronic materials, be specifically related to a kind ofly be applicable to lead-free glass powder of crystal silicon solar battery back silver paste and preparation method thereof.
Background technology
Solar cell is as the reproducible clean energy of one, and in the middle of the real life being widely used in people, wherein crystal silicon solar energy battery efficiency of conversion is the highest, and technology is also ripe.The back electrode silver paste of crystal silicon solar cell sheet is through silk screen printing then process of passing through tunnel furnace treatment reason, silver-colored back surface field is formed at the back side of silicon chip of solar cell, improve open circuit voltage, and the silicon-silver alloys formed in sintering can weaken silicon chip and interelectrode Schottky barrier, thus realize good ohmic contact, improve the efficiency of conversion of solar battery sheet.Crystal silicon solar energy battery is to its weldability of back silver paste paper examines and sticking power, and these two critical performances of cell backside welding system depend on glass powder content and the performance of glass system own in back silver slurry to a great extent.The composition of glass powder, content, size, softening temperature and thermal expansivity directly can affect contact resistance, densified sintering product and the consistency with aluminium paste, thus reduce series resistance, improve photoelectric transformation efficiency and are firmly welded to connect.
At present, in order to sintering can be adapted to and provide enough welding strengths in crystal silicon solar battery back silver paste, the low melting glass that main employing is traditional, but the glass of these low melting points is mostly containing the heavy metal element that Pb, Cd, Tl etc. are harmful, contaminate environment.Meanwhile, because crystal silicon solar back silver paste requires lower, as long as generally have good welding property, so the special research for crystal silicon solar battery back silver paste glass powder is less both at home and abroad to glass powder used.Therefore, the glass powder that the crystal silicon solar battery back silver paste of developing green environmental protection is used is next step development trend of electronics manufacturing.
The glass powder of some sun power back of the body ag paste electrode is provided in the Patent Application Publication such as China Patent Publication No. CN103951264A, CN102992633A, but the composition of these glass powder is relatively complicated, reach more than tens kinds of composition raw materials, cause difficulty to production control, be also unfavorable for controlling follow-up welding and the consistency with aluminium.In patent CN103951264A, sun power back of the body silver slurry glass powder disclosed in it, its softening temperature, within the scope of 550 ~ 630 DEG C, though lower than the softening temperature of traditional glass, but still belongs to comparatively high temps.
Summary of the invention
The present invention overcomes the deficiency that prior art exists, and in order to provide, a kind of softening temperature is low, glass composition is simple, particle diameter is little, sticking power is high for technical problem to be solved, with the good lead-free glass powder of aluminium consistency and preparation method thereof.In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of lead-free glass powder being applicable to crystal silicon solar battery back silver paste, is prepared from by the raw material of following molar percentage: SiO
210 ~ 30%, Bi
2o
320 ~ 80%, B
2o
31 ~ 20%, Al
2o
30 ~ 2%, ZnO0 ~ 2%, Sb
2o
30 ~ 2%.
Be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, comprise the following steps:
(1) above-mentioned raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 900 ~ 1000 DEG C, and add a cover; Then 1200 ~ 1500 DEG C of insulation 1 ~ 2h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
The described preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
Described glass powder is the palladium powder of median size 0.8 ~ 3.5mm, and its softening temperature point is 460 ~ 520 DEG C, and thermal expansivity is 70 ~ 90 ' 10
-7/ DEG C.
The silver paste of described lead-free glass powder preparation, the weight percent of component contained by preferred silver paste is that described lead-free glass powder accounts for 3 ~ 5% of silver paste gross weight, silver powder accounts for silver paste gross weight 50 ~ 60%, organic carrier accounts for 30 ~ 40% of silver paste gross weight, additive accounts for 1 ~ 2% of silver paste gross weight, use the silver paste of this proportioning to sinter at 630 DEG C, during insulation 5min, the silverskin of gained and the sticking power of silicon chip are 6 ~ 9N.Improve the welding property of silver slurry, and better with aluminium consistency, meet the requirement of sun power crystal sun power back of the body silver slurry to glass powder used.
Described glass powder uses Bi
2o
3, B
2o
3, SiO
2for the crown glass of the Bi-B-Si system of principal constituent, by adding Al
2o
3, ZnO, Sb
2o
3regulate the softening temperature of glass powder, thermal expansivity, increase its density and chemical stability simultaneously, thus improve the conductivity of silver slurry.
The present invention compared with prior art has following beneficial effect: thermal expansivity, the softening temperature of lead-free glass powder of the present invention and cell silicon chip and aluminium back surface field match, can be significantly improved it and sinter rear and silicon chip and aluminium back surface field sticking power, improve the welding property of silver slurry and the matching with aluminium, and preparation technology is simple, after being pulverized by planetary ball mill, this glass powder particle diameter little (0.8 ~ 3.5mm) is unleaded palladium powder.Simultaneously, the silver slurry using this glass powder to prepare, sinter at 630 DEG C, during insulation 5min, the silverskin of gained, the sticking power comparatively large (being not less than 6 N) with silicon chip, improves the welding property of silver slurry, and better with aluminium consistency, meet the requirement of sun power crystal sun power back of the body silver slurry to glass powder used.
Embodiment
The technique means realized for making the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with embodiment, setting forth the present invention further.
The proportioning components of table 1 glass powder embodiment and performance test
Embodiment 1:
(1) first, by molar fraction will be: the SiO of 25 mol%
2, the B of 20 mol %
2o
3, the Bi of 51 mol %
2o
3, the Al of 2 mol %
2o
3, and the ZnO of 2 mol % is mixed into the compound that uniformity coefficient is greater than 98%.
(2) then, admixtion is added in the crucible of 950 DEG C, and add a cover; Then, 1300 DEG C of insulation 2h are risen to the temperature rise rate of 10 DEG C/min.
(3) glass metal of complete post liquefaction is fully stirred rear shrend.
(4) frit after oven dry is carried out ball milling, drying.
(5) last, sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of 0.8 ~ 3.5 mm.
Embodiment 2:
(1) first, by molar fraction will be: the SiO of 25 mol%
2, the B of 18 mol %
2o
3, the Bi of 52.75 mol %
2o
3, the Al of 2 mol %
2o
3, the ZnO of 2 mol % and the Sb of 0.25 mol %
2o
3be mixed into the compound that uniformity coefficient is greater than 98%.
(2) then, admixtion is added in the crucible of 950 DEG C, and add a cover; Then, 1250 DEG C of insulation 2h are risen to the temperature rise rate of 10 DEG C/min.
(3) glass metal of complete post liquefaction is fully stirred rear shrend.
(4) frit after oven dry is carried out ball milling, drying.
(5) last, sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of 0.8 ~ 3.5 mm.
Embodiment 3:
(1) first, by molar fraction will be: the SiO of 25 mol%
2, the B of 15 mol %
2o
3, the Bi of 55.5 mol %
2o
3, the Al of 2 mol %
2o
3, the Sb of ZnO and the 0.5mol % of 2 mol %
2o
3be mixed into the compound that uniformity coefficient is greater than 98%.
(2) then, admixtion is added in the crucible of 950 DEG C, and add a cover; Then, 1250 DEG C of insulation 2h are risen to the temperature rise rate of 10 DEG C/min.
(3) glass metal of complete post liquefaction is fully stirred rear shrend.
(4) frit after oven dry is carried out ball milling, drying.
(5) last, sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of 0.8 ~ 3.5 mm.
Embodiment 4:
(1) first, by molar fraction will be: the SiO of 25 mol%
2, the B of 12 mol %
2o
3, the Bi of 58 mol %
2o
3, the Al of 2 mol %
2o
3, the ZnO of 2 mol % and the Sb of 1 mol %
2o
3be mixed into the compound that uniformity coefficient is greater than 98%.
(2) then, admixtion is added in the crucible of 950 DEG C, and add a cover; Then, 1250 DEG C of insulation 2h are risen to the temperature rise rate of 10 DEG C/min.
(3) glass metal of complete post liquefaction is fully stirred rear shrend.
(4) frit after oven dry is carried out ball milling, drying.
(5) last, sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of 0.8 ~ 3.5 mm.
Embodiment 5:
(1) first, by molar fraction will be: the SiO of 25 mol%
2, the B of 10 mol %
2o
3, the Bi of 59.5 mol %
2o
3, the Al of 2 mol %
2o
3, the ZnO of 2 mol % and the Sb of 1.5 mol %
2o
3be mixed into the compound that uniformity coefficient is greater than 98%.
(2) then, admixtion is added in the crucible of 950 DEG C, and add a cover; Then, 1250 DEG C of insulation 2h are risen to the temperature rise rate of 10 DEG C/min.
(3) glass metal of complete post liquefaction is fully stirred rear shrend.
(4) frit after oven dry is carried out ball milling, drying.
(5) last, sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of 0.8 ~ 3.5 mm.
Embodiment 6:
(1) first, by molar fraction will be: the SiO of 25 mol%
2, the B of 5 mol %
2o
3, the Bi of 64 mol %
2o
3, the Al of 2 mol %
2o
3, the ZnO of 2 mol % and the Sb of 2 mol %
2o
3be mixed into the compound that uniformity coefficient is greater than 98%.
(2) then, admixtion is added in the crucible of 950 DEG C, and add a cover; Then, 1250 DEG C of insulation 2h are risen to the temperature rise rate of 10 DEG C/min.
(3) glass metal of complete post liquefaction is fully stirred rear shrend.
(4) frit after oven dry is carried out ball milling, drying.
(5) last, sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of 0.8 ~ 3.5 mm.
The glass powder that Example 1-6 obtains is mixed with silver slurry, according to solar cell size industry standard YS/T612-2006, slurry is stirred, after silk screen printing, sinter at 630 DEG C, insulation 5min, obtain silverskin, by Shimadzu S-J type tensile testing machine, the sticking power of test silverskin, as shown in table 1.
Embodiment 7:
Be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, be prepared from by the raw material of following molar percentage: SiO
210%, Bi
2o
350%, B
2o
320%, Al
2o
32%, ZnO2%.
Be applicable to a preparation method for the lead-free glass powder of crystal silicon solar battery back silver paste, comprise the following steps:
(1) above-mentioned raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 900 DEG C, and add a cover; Then 1500 DEG C of insulation 1h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
The described preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste, is characterized in that: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
Embodiment 8:
Be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, be prepared from by the raw material of following molar percentage: SiO
225%, Bi
2o
320%, B
2o
315%, ZnO2%, Sb
2o
30.5%.
Be applicable to a preparation method for the lead-free glass powder of crystal silicon solar battery back silver paste, comprise the following steps:
(1) above-mentioned raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 1000 DEG C, and add a cover; Then 1400 DEG C of insulation 2h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
The described preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste, is characterized in that: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
Embodiment 9:
Be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, be prepared from by the raw material of following molar percentage: SiO
225%, Bi
2o
340%, B
2o
312%, Al
2o
32%, ZnO1%, Sb
2o
31%.
Be applicable to a preparation method for the lead-free glass powder of crystal silicon solar battery back silver paste, comprise the following steps:
(1) above-mentioned raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 1000 DEG C, and add a cover; Then 1300 DEG C of insulation 1h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
The described preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste, is characterized in that: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
Embodiment 10:
Be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, be prepared from by the raw material of following molar percentage: SiO
225%, Bi
2o
360%, B
2o
310%, Al
2o
31%, Sb
2o
31.5%.
Be applicable to a preparation method for the lead-free glass powder of crystal silicon solar battery back silver paste, comprise the following steps:
(1) above-mentioned raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 950 DEG C, and add a cover; Then 1400 DEG C of insulation 1.5h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
The described preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste, is characterized in that: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
Embodiment 11:
Be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, be prepared from by the raw material of following molar percentage: SiO
230%, Bi
2o
380%, B
2o
31%, Al
2o
32%, ZnO2%, Sb
2o
32%.
Be applicable to a preparation method for the lead-free glass powder of crystal silicon solar battery back silver paste, comprise the following steps:
(1) above-mentioned raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 1000 DEG C, and add a cover; Then 1400 DEG C of insulation 2h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
The described preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste, is characterized in that: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, above-mentioned embodiment of the present invention all can only be thought explanation of the present invention and can not limit invention, claims indicate scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any change in the implication suitable with claims of the present invention and scope, all should think to be included in the scope of claims.
Claims (5)
1. be applicable to a lead-free glass powder for crystal silicon solar battery back silver paste, it is characterized in that being prepared from by the raw material of following molar percentage: SiO
210 ~ 30%, Bi
2o
320 ~ 80%, B
2o
31 ~ 20%, Al
2o
30 ~ 2%, ZnO0 ~ 2%, Sb
2o
30 ~ 2%.
2. a kind of preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste as claimed in claim 1, is characterized in that comprising the following steps:
(1) described raw material is mixed into the compound that uniformity coefficient is greater than 98%;
(2) compound is added in the corundum crucible of 900 ~ 1000 DEG C, and add a cover; Then 1200 ~ 1500 DEG C of insulation 1 ~ 2h are risen to, until frit liquefies completely with the temperature rise rate of 10 DEG C/min;
(3) glass metal of complete post liquefaction is fully stirred rear Water Quenching;
(4) frit after oven dry is carried out ball milling, drying;
(5) sieved by the glass powder after ball milling, obtained particle diameter is the palladium powder of below 5mm.
3. the preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste according to right 2, is characterized in that: wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Bi
2o
3, Al
2o
3, ZnO and Sb
2o
3introduced by bismuthous oxide bismuth trioxide, aluminum oxide, zinc oxide and antimonous oxide respectively.
4. lead-free glass powder prepared by the preparation method being applicable to the lead-free glass powder of crystal silicon solar battery back silver paste according to right 2, it is characterized in that: the median size of described glass powder is 0.8 ~ 3.5mm, its softening temperature point is 460 ~ 520 DEG C, and thermal expansivity is 70 ~ 90 ' 10
-7/ DEG C.
5. the silver paste of the lead-free glass powder preparation according to right 4, it is characterized in that: contained by preferred silver paste, the weight percent of component is that described lead-free glass powder accounts for 3 ~ 5% of silver paste gross weight, silver powder accounts for silver paste gross weight 50 ~ 60%, organic carrier accounts for 30 ~ 40% of silver paste gross weight, additive accounts for 1 ~ 2% of silver paste gross weight, use the silver paste of this proportioning to sinter at 630 DEG C, during insulation 5min, the silverskin of gained and the sticking power of silicon chip are 6 ~ 9N.
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Cited By (7)
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CN105000806A (en) * | 2015-08-14 | 2015-10-28 | 海宁市瑞银科技有限公司 | Lead-free glass powder for back silver paste of silicon-based solar battery and preparation method of lead-free glass powder |
CN107032623A (en) * | 2017-02-20 | 2017-08-11 | 江苏瑞德新能源科技有限公司 | A kind of lead-free glass powder used for solar batteries and positive silver paste |
CN107117824A (en) * | 2017-05-18 | 2017-09-01 | 江苏东昇光伏科技有限公司 | A kind of lead-free glass powder used for solar batteries and preparation method thereof |
CN107500549A (en) * | 2017-08-14 | 2017-12-22 | 广东工业大学 | A kind of microcrystalline glass powder, its preparation method and silver paste |
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CN105000806A (en) * | 2015-08-14 | 2015-10-28 | 海宁市瑞银科技有限公司 | Lead-free glass powder for back silver paste of silicon-based solar battery and preparation method of lead-free glass powder |
CN105000806B (en) * | 2015-08-14 | 2017-07-04 | 海宁市瑞银科技有限公司 | A kind of silica-based solar cell back side silver paste lead-free glass powder and preparation method thereof |
CN107032623A (en) * | 2017-02-20 | 2017-08-11 | 江苏瑞德新能源科技有限公司 | A kind of lead-free glass powder used for solar batteries and positive silver paste |
CN107117824A (en) * | 2017-05-18 | 2017-09-01 | 江苏东昇光伏科技有限公司 | A kind of lead-free glass powder used for solar batteries and preparation method thereof |
CN107500549A (en) * | 2017-08-14 | 2017-12-22 | 广东工业大学 | A kind of microcrystalline glass powder, its preparation method and silver paste |
CN108147672A (en) * | 2017-12-29 | 2018-06-12 | 北京市合众创能光电技术有限公司 | A kind of PERC crystal silicon solars positive silver paste glass dust |
CN109384393A (en) * | 2018-10-15 | 2019-02-26 | 海宁市瑞银科技有限公司 | PERC crystal silicon solar battery back silver paste lead-free glass powder and preparation method thereof |
CN110498603A (en) * | 2019-09-25 | 2019-11-26 | 山东国瓷功能材料股份有限公司 | Glass powder and preparation method thereof, piezoelectric ceramics and preparation method thereof, piezoelectric ceramic devices |
CN110498603B (en) * | 2019-09-25 | 2021-11-23 | 山东国瓷功能材料股份有限公司 | Glass powder and preparation method thereof, piezoelectric ceramic and preparation method thereof, and piezoelectric ceramic device |
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