CN115910423A - Industrial low-temperature conductive paste with high conductivity and preparation method thereof - Google Patents
Industrial low-temperature conductive paste with high conductivity and preparation method thereof Download PDFInfo
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- CN115910423A CN115910423A CN202110901848.1A CN202110901848A CN115910423A CN 115910423 A CN115910423 A CN 115910423A CN 202110901848 A CN202110901848 A CN 202110901848A CN 115910423 A CN115910423 A CN 115910423A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 171
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000002184 metal Substances 0.000 claims abstract description 91
- 229910052751 metal Inorganic materials 0.000 claims abstract description 91
- 239000010949 copper Substances 0.000 claims abstract description 77
- 229910052802 copper Inorganic materials 0.000 claims abstract description 75
- 229910001128 Sn alloy Inorganic materials 0.000 claims abstract description 37
- 239000011135 tin Substances 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 32
- 239000000956 alloy Substances 0.000 claims abstract description 32
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 32
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 30
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003960 organic solvent Substances 0.000 claims abstract description 24
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 24
- 239000013543 active substance Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 229910052718 tin Inorganic materials 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 21
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 13
- 229910016331 Bi—Ag Inorganic materials 0.000 claims abstract description 11
- JWVAUCBYEDDGAD-UHFFFAOYSA-N bismuth tin Chemical compound [Sn].[Bi] JWVAUCBYEDDGAD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 25
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid group Chemical group C(CCCCC(=O)O)(=O)O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 239000011241 protective layer Substances 0.000 claims description 14
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- 239000002923 metal particle Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical group [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 10
- 238000007747 plating Methods 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 235000011037 adipic acid Nutrition 0.000 claims description 8
- 239000001361 adipic acid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 7
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical group COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 7
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 7
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- 235000019438 castor oil Nutrition 0.000 claims description 6
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 6
- 229910000570 Cupronickel Inorganic materials 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 claims description 5
- 229910021485 fumed silica Inorganic materials 0.000 claims description 5
- 229920001225 polyester resin Polymers 0.000 claims description 5
- 239000004645 polyester resin Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000012798 spherical particle Substances 0.000 claims description 2
- 229910017944 Ag—Cu Inorganic materials 0.000 claims 1
- 238000007772 electroless plating Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000005275 alloying Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 22
- 238000012360 testing method Methods 0.000 description 19
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- 238000010438 heat treatment Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
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- 239000000243 solution Substances 0.000 description 4
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical group CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- QKAJPFXKNNXMIZ-UHFFFAOYSA-N [Bi].[Ag].[Sn] Chemical compound [Bi].[Ag].[Sn] QKAJPFXKNNXMIZ-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
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- 238000000691 measurement method Methods 0.000 description 3
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- 235000012431 wafers Nutrition 0.000 description 3
- PQIJHIWFHSVPMH-UHFFFAOYSA-N [Cu].[Ag].[Sn] Chemical compound [Cu].[Ag].[Sn] PQIJHIWFHSVPMH-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910000969 tin-silver-copper Inorganic materials 0.000 description 2
- 229910017980 Ag—Sn Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 101001073212 Arabidopsis thaliana Peroxidase 33 Proteins 0.000 description 1
- 101001123325 Homo sapiens Peroxisome proliferator-activated receptor gamma coactivator 1-beta Proteins 0.000 description 1
- 102100028961 Peroxisome proliferator-activated receptor gamma coactivator 1-beta Human genes 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229910020830 Sn-Bi Inorganic materials 0.000 description 1
- 229910018728 Sn—Bi Inorganic materials 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
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- 239000012298 atmosphere Substances 0.000 description 1
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
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- 230000008023 solidification Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Conductive Materials (AREA)
Abstract
The invention relates to low-temperature conductive paste for photovoltaic industry, in particular to industrial low-temperature conductive paste with high conductivity and a preparation method thereof, aiming at solving the problems of high cost and poor conductivity of the existing low-temperature conductive paste. The composition comprises the following components in percentage by mass: 88 to 94 percent of metal powder and 6 to 12 percent of organic auxiliary agent; the metal powder comprises copper conductive metal powder and tin alloy powder; the copper conductive metal powder is copper powder containing tin, nickel and/or silver; the tin alloy powder is Sn, ag, cu, sn 0.3 Ag 0.7 Cu alloy powder, sn-Bi-Ag Sn 64.7 Bi 35 Ag 0.3 Alloy powder, sn-Bi-Ag Sn 42 Bi 57 Ag 1 Alloy powder and/or tin bismuth Sn 42 Bi 58 Alloying powder; the organic assistant comprises single-component thermosetting resin (containing a curing agent), an active agent, a thixotropic agent and an organic solvent. The invention adopts specific proportion of organic auxiliary agent and metal powderAnd the components and the microstructure of the metal powder are optimized, and the single-component thermosetting resin (containing a curing agent) is adopted, so that the slurry can be cured at the temperature of 140-150 ℃, and the average volume resistivity is about 3.9 mu omega cm.
Description
Technical Field
The invention relates to low-temperature conductive paste for photovoltaic industry, in particular to industrial low-temperature conductive paste with high conductive performance and a preparation method thereof.
Background
In recent years, the heterojunction solar cell is popular in the industry due to low temperature coefficient and low attenuation effect, and the newly built capacity of a heterojunction solar cell production line is increased explosively along with the continuous improvement of conversion efficiency. However, the manufacturing cost of the heterojunction solar cell is always high, and mainly reflects the cost of silicon wafers and metallization. The cost of the silicon wafer can be reduced by reducing the thickness of the silicon wafer, but the cost of metallization rises sharply along with the rise of the metal price, and the price of low-temperature silver paste adopted by the current collection of the heterojunction solar cell is increased by nearly 100% in comparison with the price of the low-temperature silver paste adopted in the previous year. Meanwhile, the conductive silver paste of the M6 heterojunction solar cell is reduced to about 220mg, the consumption of low-temperature silver paste is reduced to the limit by part of enterprises, and the cost gain caused by metallization cannot be kept equal to the cost of the PERC cell, so that the metallization cost of the heterojunction solar cell can be lowered revolutionarily by replacing the low-temperature silver paste, and the industrial application of the heterojunction solar cell is accelerated.
At present, the electrolytic copper plating grid line and the silver-coated copper slurry expose the rudiment in the metallization direction of the heterojunction battery. The scheme of etching the electroplated grid line by adopting dry film exposure for the electroplated grid line of the heterojunction battery has the problems of expensive dry film, complex process, high additional cost, environment friendliness and the like; the cost of the prior silver-clad copper paste is reduced by 30% in the process verification process, the metallization cost cannot be reduced fundamentally, and the conductivity of the prior silver-clad copper paste is not ideal.
In order to realize the revolutionary reduction of the metallization cost of the heterojunction solar cell and simultaneously improve the conductivity, the development of a low-temperature and low-cost conductive paste with high conductivity is urgently needed.
Disclosure of Invention
The invention aims to provide industrial low-temperature conductive paste with high conductive performance so as to solve the problems of high cost and poor conductive performance of the conventional low-temperature conductive paste.
The technical scheme of the invention is to provide industrial low-temperature conductive slurry with high conductive performance, which is characterized by comprising the following components in percentage by mass:
88 to 94 percent of metal powder and 6 to 12 percent of organic auxiliary agent;
the metal powder comprises copper conductive metal powder and tin alloy powder;
the copper conductive metal powder is copper powder containing tin, nickel and/or silver; the tin alloy powder is Sn, ag, cu, sn 0.3 Ag 0.7 Cu alloy powder, sn-Bi-Ag Sn 64.7 Bi 35 Ag 0.3 Alloy powder, sn-Bi-Ag Sn 42 Bi 57 Ag 1 Alloy powder and/or tin bismuth Sn 42 Bi 58 Alloying powder;
the organic assistant comprises single-component thermosetting resin (containing a curing agent), an active agent, a thixotropic agent and an organic solvent.
Further, the copper powder containing tin, nickel and/or silver is metal particle powder in which a tin, nickel and/or silver elemental metal protective layer is plated on the surface of pure copper particles.
In order to further improve the conductivity of the conductive paste, the pure copper particles are spherical, and the copper content is more than 99%.
Further, in order to realize fine line printing, the particle diameter of the metal particles in the above copper conductive metal powder is less than 25 μm; in order to ensure uniform thickness of the coating, the surface coating is generated by chemical plating, and the copper powder can be protected from being oxidized and the electrical property of the copper powder can be ensured when the thickness of the coating is less than 2 microns.
Further, the copper conductive metal powder may be copper-tin alloy powder and/or copper-nickel alloy powder, wherein the copper content is greater than 90%.
In order to further improve the conductivity of the sintered grid line, sn, ag, cu and Sn 0.3 Ag 0.7 Cu alloy powder, sn-Bi-Ag Sn 64.7 Bi 35 Ag 0.3 Alloy powder, sn-Bi-Ag-Sn 42 Bi 57 Ag 1 Alloy powder and tin bismuth Sn 42 Bi 58 Alloy powder is uniformIs spherical particle alloy powder, and the particle size is less than 35 microns.
Further, the mass ratio of the copper conductive metal powder to the tin alloy powder is 4:1-1:1, the high proportion of copper powder can improve the conductivity and reduce the fluidity of the molten tin powder, and is beneficial to forming lines after solidification without aggregating into balls or breaking lines.
Further, the one-component thermosetting resin is one or more of an epoxy resin, a silicone resin, an acrylic resin or a polyester resin having no benzene ring structure.
Further, the active agent is adipic acid and/or glutaric acid. The thixotropic agent is one or more of fumed silica, organic bentonite, graphene and hydrogenated castor oil. The organic solvent is ethylene glycol monomethyl ether and/or ethylene glycol ethyl ether.
Further, the single-component thermosetting resin (containing a curing agent), the active agent, the thixotropic agent and the organic solvent in the organic auxiliary agent respectively comprise the following components in percentage by mass:
10-30% of thermosetting resin (containing curing agent);
10-20% of active agent;
10-15% of thixotropic agent;
35-70% of organic solvent;
the thermosetting resin is used for bonding the metal on the transparent conductive film after curing and realizing the electrical contact and communication between the metal and the transparent conductive film. After the tin alloy powder is solidified, the tin alloy powder can form metal bond contact with the copper conductive metal powder, so that organic matters are extruded out, and the conductivity is improved.
Furthermore, the transparency of the single-component thermosetting resin (containing the curing agent), the activator, the thixotropic agent and the organic solvent in the organic auxiliary agent is higher than 80%, and the high transparency is favorable for reducing shading loss caused by cured organic matters.
The invention also provides a preparation method of the industrial low-temperature conductive paste with high conductive performance, which is characterized by comprising the following steps:
if the metal particle powder is adopted, the surface of the pure copper particle is plated with a tin, nickel or silver protective layer, the chemical tin, nickel or silver protective layer is plated on the surface of the pure copper particle by adopting a chemical metal plating method under the protection of inert gas;
if copper-tin alloy powder and copper-nickel alloy powder are adopted, weighing corresponding alloy powder according to the required content;
weighing the components according to the proportion, sequentially adding the active agent, the thixotropic agent and the thermosetting resin into the organic solvent, and uniformly stirring and mixing;
weighing the copper conductive metal powder, the tin alloy powder and the organic auxiliary agent according to the proportion, after weighing, uniformly mixing the copper conductive metal powder and the tin alloy powder, adding the organic auxiliary agent, mixing and stirring in a planetary mixer, rolling after stirring, and then uniformly mixing in a three-roll mill.
The beneficial effects of the invention are:
1. according to the invention, the organic auxiliary agent and the metal powder are specifically proportioned, the components and the microstructure of the metal powder are optimized, and the single-component thermosetting resin (containing the curing agent) is adopted, so that the slurry can be cured at the temperature of 140-150 ℃, and meanwhile, the average volume resistivity is about 3.9 mu omega cm, which is superior to the volume resistivity of the existing low-temperature conductive silver slurry and is lower than the volume resistivity of the existing silver-coated copper slurry of the most mature Japanese precision electronic KE.
2. The tin alloy powder in the invention is melted after the slurry is sintered and wraps the copper conductive metal powder, so that on one hand, the connection between metal and intermetallic metal is realized, the conductive performance and the mechanical performance are good, meanwhile, the volume of the tin alloy powder is reduced, the shading area is reduced, organic resin is extruded to the edge (organic matter is transparent), the solidified metal wire is fixedly bonded on the substrate by the resin, and the adhesive force of the grid line on the ITO film is further improved.
3. According to the invention, by adjusting the mass ratio of the copper conductive metal powder to the tin alloy powder, grid lines with a certain distance are formed on the ITO thin film of the heterojunction solar cell by screen printing, and are not aggregated into balls or broken lines. Sintering in a hot oven at 140-150 deg.C to form grid lines with width of 80-90 μm and height of 15-25 μm.
4. The copper content in the copper conductive metal powder is at least more than 90%, and the solidified tin alloy powder can form metal bond contact with the copper conductive metal powder to extrude out organic matters, so that the requirement of resin is reduced, and the cost is lower.
Drawings
Fig. 1 is a schematic diagram showing the effect of the low-temperature paste of the present invention after curing, wherein 1 is a substrate, 2 is a cured metal wire, and 3 is a one-component thermosetting resin (containing a curing agent).
FIG. 2 is a photograph of the sintered product of example 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with figures are described in detail below, and it is apparent that the described embodiments are a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention, shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein, and it will be appreciated by those skilled in the art that the present invention may be practiced without departing from the spirit and scope of the present invention and that the present invention is not limited by the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the present invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
The industrial low-temperature conductive slurry with high conductivity in the embodiment comprises the following components in percentage by mass:
10% of organic auxiliary agent and 90% of metal powder;
the metal powder comprises copper conductive metal powder and tin alloy powder;
the copper conductive metal powder is metal particle powder with a silver protective layer plated on the surface of pure copper particles; the average particle size of the copper conductive metal powder is 5.5 microns, the thickness of the silver protective layer is about 1 micron, and the copper content is more than 90 percent; the proportion of the copper conductive metal powder in the total mass of the metal powder is 68 percent.
The tin alloy powder is No. 6 tin bismuth silver (Sn) 42 Bi 57 Ag 1 ) Alloy powder with the grain diameter of 10-20 microns; the ratio of the tin alloy powder to the total mass of the metal powder is 32%.
The organic assistant comprises single-component thermosetting resin (containing a curing agent), an active agent, a thixotropic agent and an organic solvent. In the embodiment, the single-component thermosetting resin (containing a curing agent) is hydrogenated bisphenol A epoxy resin (containing a curing agent), the active agent is adipic acid, the thixotropic agent is hydrogenated castor oil, and the organic solvent is ethylene glycol diethyl ether; the proportion of the hydrogenated bisphenol A epoxy resin (containing a curing agent), the adipic acid, the hydrogenated castor oil and the ethylene glycol ethyl ether in the organic auxiliary agent is respectively 20%, 10% and 50%.
The conductive paste may be prepared by the following method:
first, copper conductive metal powder is prepared: weighing a certain amount of pure copper powder, adding the pure copper powder into a certain amount of chemical plating solution, wherein the chemical plating solution selected in the embodiment is a mixed solution of silver nitrate, sodium hydroxide and ammonia water, continuously stirring the mixed solution under the protection of an inert atmosphere to ensure that pure copper powder particles are fully separated and uniformly distributed in the plating solution, and after the stirring is continued for 5 minutes, separating and drying the plating solution and the copper powder on which the plating layer is finished.
Secondly, preparing an organic auxiliary agent, weighing the components according to the proportion, sequentially adding the active agent, the thixotropic agent and the thermosetting resin into the organic solvent, and uniformly stirring and mixing.
And finally, weighing the metal powder and the organic auxiliary agent according to the mass ratio, uniformly mixing the copper conductive metal powder and the tin alloy powder, adding the organic auxiliary agent, mixing and stirring in a planetary stirrer, rolling after stirring, and uniformly mixing in a three-roll mill. Then storing at low temperature, wherein the storage temperature is 2-10 ℃.
And (3) performing roller rotation and temperature return on the slurry stored at low temperature at room temperature, performing screen printing to form grid lines with a certain distance on the ITO thin film of the heterojunction solar cell, and performing sintering treatment in a heat oven at 140-150 ℃ to form the grid lines with the width of 80-90 micrometers and the height of 15-20 micrometers. As shown in fig. 1 and fig. 2, the tin alloy powder in the paste begins to melt, the tin alloy powder is melted to connect copper conductive metal powder particles, the grid lines shrink and become thin, organic matters in the grid lines are extruded out, the solvent is volatilized, the hydrogenated bisphenol a epoxy resin is cured, copper powder which is densely connected with tin liquid is fixed on the surface of the ITO film, and the contact reliability between the grid lines and the ITO film is ensured. Fig. 2 is a photograph after sintering, and it can be seen that a thin gate line is formed on the ITO thin film.
The volume resistivity is one of the important indexes for evaluating the electrical property of the conductive paste, in the embodiment, test samples of the conductive paste with different film thicknesses or different widths are prepared by screen printing and are subjected to heat treatment at 140-150 ℃ for 2min. And measuring the thickness and the width of the slurry sample by using a microscope, and finally measuring the resistance of the slurry sample by using a direct current resistance measurement method, thereby calculating the volume resistivity of the conductive slurry. Test samples were printed, 5 strips each having a length of about 50mm, a width of about 0.5mm and a thickness of about 22 μm, with the following detailed test data:
| numbering | H thickness(μm) | W width (mm) | L Length (mm) | R resistance (omega) | Rho bulk resistivity (Ω. Cm) |
| 1 | 22.673 | 0.52 | 50.238 | 0.184 | 4.31815E-06 |
| 2 | 21.982 | 0.51 | 50.163 | 0.176 | 3.93339E-06 |
| 3 | 21.795 | 0.5 | 49.897 | 0.182 | 3.97488E-06 |
| 4 | 22.054 | 0.49 | 50.065 | 0.178 | 3.84211E-06 |
| 5 | 22.289 | 0.51 | 50.133 | 0.155 | 3.51454E-06 |
According to the calculation of test data, the average volume resistivity of the conductive paste is about 3.9 mu omega cm, and compared with the volume resistivity of low-temperature conductive silver paste manufactured by international and domestic enterprises of 4-8 mu omega cm, the conductive paste has the advantages that the conductive performance is obviously improved, the power loss of a battery on a metal grid line can be reduced, and the filling factor of the battery is improved. Compared with the existing silver-coated copper paste, the silver-coated copper paste has the bulk resistivity of 6-11 mu omega cm and the conductivity is also obviously improved.
In order to verify the contact reliability of the grid line and the ITO thin film, the contact resistance and the adhesive force between the ITO thin film and the grid line are tested through experiments. Firstly, a contact resistance sample of an ITO film and a grid line is manufactured, a screen printing plate with a plurality of hollow patterns with the space of 500 micrometers and the length of 5 millimeters is arranged, and the grid line is conducted through silk screen printing and heat treatment at 140-150 ℃. And selecting 11 continuous grid lines, respectively testing the resistance R1 between the first grid line and the second grid line, the resistance R2 between the second grid line and the fourth grid line, the resistance R3 between the fourth grid line and the seventh grid line, and the resistance R4 between the seventh grid line and the eleventh grid line, and calculating the contact resistivity through linear fitting. The data are as follows
| Group of | R1(Ω) | R2(Ω) | R3(Ω) | R4(Ω) | ρ(mΩ·cm 2 ) |
| 1 | 7.32 | 14.08 | 20.92 | 27.68 | 0.2488 |
| 2 | 6.98 | 13.47 | 19.84 | 26.18 | 0.3816 |
| 3 | 7.54 | 14.13 | 20.02 | 28.02 | 1.1247 |
The average contact resistivity value calculated by linear fitting according to the test data is 0.585m omega cm 2 Compared with the contact resistivity between the low-temperature silver paste grid line and the ITO film in the current industry, the effect is better.
In general, the conductive performance of the paste is better than that of low-temperature silver paste, the paste can be applied to printing of thin grid lines of solar cells, the silver paste can be replaced, the series resistance is reduced, the conversion efficiency is improved, and the cost is reduced.
Example 2
The industrial low-temperature conductive paste with high conductive performance comprises the following components in percentage by mass:
6% of organic auxiliary agent and 94% of metal powder; in other embodiments, the organic auxiliary agent is 6-12%, and the metal powder is 88-94%.
The metal powder comprises copper conductive metal powder and tin alloy powder;
the copper conductive metal powder is metal particle powder with a tin protective layer plated on the surface of pure copper particles; the average particle size of the copper conductive metal powder is 8.5 microns, the thickness of the tin protective layer is about 1.5 microns, and the copper content is greater than 90%; the ratio of the copper conductive metal powder to the total mass of the metal powder was 80%. In other embodiments, the copper conductive metal powder may be metal particle powder with a nickel protective layer plated on the surface of pure copper particles; or a mixture of metal particle powder with a nickel protective layer plated on the surface of the pure copper particle, metal particle powder with a silver protective layer plated on the surface of the pure copper particle, and metal particle powder with a tin protective layer plated on the surface of the pure copper particle. Tin-plated copper powder is preferred for cost sensitive applications and silver-plated copper powder is preferred for performance demanding applications. The ratio of the copper conductive metal powder in the total mass of the metal powder is not less than 50% and not more than 80%.
The tin alloy powder is Sn-Bi (Sn) 42 Bi 58 ) Alloy powder with a particle size of 15-25 microns, in other embodiments less than 35 microns; the ratio of the tin alloy powder to the total mass of the metal powder is 20%. High temperature tin silver copper (Sn) may also be used in other embodiments 0.3 Ag 0.7 Cu) alloy powder, medium-temperature Sn-Bi-Ag (Sn) 64.7 Bi 35 Ag 0.3 ) Alloy powder, low-temperature tin bismuth silver (Sn) 42 Bi 57 Ag 1 ) Alloy powder, tin bismuth (Sn) 42 Bi 58 ) One or more of alloy powder; the ratio of the tin alloy powder to the total mass of the metal powder corresponds to the ratio of the copper conductive metal powder to the total mass of the metal powder, and the ratio is greater than 20% and less than or equal to 50%.
The organic assistant comprises single-component thermosetting resin (containing a curing agent), an active agent, a thixotropic agent and an organic solvent. In the present embodiment, the one-component thermosetting resin (containing the curing agent) is a silicone resin, and in other embodiments, at least two of an epoxy resin, a silicone resin, an acrylic resin and a polyester resin without a benzene ring structure may be hydrogenated or hydrogenated. Glutaric acid is selected as the active agent in the embodiment, and a mixed reagent of adipic acid and glutaric acid can be selected in other embodiments. Fumed silica is used as the thixotropic agent in the embodiment, and one or more of organic bentonite and graphene can be used in other embodiments. Ethylene glycol monomethyl ether is used as the organic solvent in this embodiment, and a mixed solvent of ethylene glycol diethyl ether and ethylene glycol monomethyl ether may be used in other embodiments. The organic silicon resin, glutaric acid, fumed silica and ethylene glycol monomethyl ether account for 30%, 10%, 15% and 45% of the organic auxiliary agent respectively. In other embodiments, the percentages of the single-component thermosetting resin (containing the curing agent), the active agent, the thixotropic agent and the organic solvent are 10-30%, 10-20%, 10-15% and 35-70%.
The above conductive paste can be prepared by the same method as example 1.
And (3) rotating the slurry stored at low temperature to return the temperature at room temperature, screen-printing grid lines with a certain interval on the ITO thin film of the heterojunction solar cell, and sintering in a hot oven at 140-150 ℃ to form the grid lines with the width of 80-90 microns and the height of 15-25 microns. As shown in fig. 1, the tin alloy powder in the paste starts to melt, the tin alloy powder melts and then connects the copper conductive metal powder particles, the grid lines shrink and become thin, the organic matter in the grid lines is extruded out, the solvent is volatilized, the hydrogenated bisphenol a epoxy resin is cured, the copper powder densely connected with the tin liquid is fixed on the surface of the ITO film, and the contact reliability between the grid lines and the ITO film is ensured. After photographing, a photograph similar to fig. 2 is obtained, and a thin gate line is formed on the ITO thin film.
The volume resistivity is one of the important indexes for evaluating the electrical properties of the conductive paste, and in the same manner as in example 1, the test samples of the conductive paste with different film thicknesses or different widths are prepared by screen printing and are subjected to heat treatment at 140-150 ℃ for 2min. And measuring the thickness and the width of the slurry sample by using a microscope, and finally measuring the resistance of the slurry sample by using a direct current resistance measurement method, thereby calculating the volume resistivity of the conductive slurry. Test samples were printed as 5 strips of conductive film each having a length of about 50mm, a width of about 0.5mm and a thickness of about 20 μm, with the following detailed test data:
according to the calculation of test data, the average volume resistivity of the conductive paste is about 3.288 mu omega cm, and compared with the volume resistivity of 4-8 mu omega cm of low-temperature conductive silver paste manufactured by international and domestic enterprises, the conductive paste has the advantages that the conductive performance is obviously improved, the power loss of a battery on a metal grid line can be reduced, and the filling factor of the battery is improved. Compared with the existing silver-coated copper paste, the silver-coated copper paste has the bulk resistivity of 6-11 mu omega cm and the conductivity is also obviously improved.
In order to verify the contact reliability of the gate line and the ITO thin film, the present embodiment adopts the same experiment as that of embodiment 1 to test the contact resistance and the adhesion between the ITO thin film and the gate line. Firstly, a contact resistance sample of an ITO film and a grid line is manufactured, a screen printing plate with a plurality of hollow patterns with the spacing of 500 micrometers and the length of 5 millimeters is arranged, and the grid line is conducted through screen printing and heat treatment at 140-150 ℃. And selecting 11 continuous grid lines, respectively testing the resistance R1 between the first grid line and the second grid line, the resistance R2 between the second grid line and the fourth grid line, the resistance R3 between the fourth grid line and the seventh grid line, and the resistance R4 between the seventh grid line and the eleventh grid line, and calculating the contact resistivity through linear fitting. The data are as follows:
| group of | R1(Ω) | R2(Ω) | R3(Ω) | R4(Ω) | ρ(mΩ·cm 2 ) |
| 1 | 6.54 | 13.38 | 19.76 | 26.22 | 0.1238 |
| 2 | 6.26 | 13.22 | 18.94 | 24.78 | 0.5278 |
| 3 | 7.03 | 13.95 | 19.84 | 27.85 | 0.079 |
The average contact resistivity value is 0.24m omega cm calculated by linear fitting according to the test data 2 Compared with the contact resistivity between the low-temperature silver paste grid line and the ITO film in the current industry, the effect is better.
Generally, the conductive performance of the paste is better than that of low-temperature silver paste, the paste can be applied to printing of thin grid lines of solar cells, the silver paste can be replaced, the series resistance is reduced, the conversion efficiency is improved, and the cost is reduced.
Example 3
The industrial low-temperature conductive paste with high conductive performance comprises the following components in percentage by mass:
12% of organic auxiliary agent and 88% of metal powder; in other embodiments, the organic auxiliary agent is 6-12%, and the metal powder is 88-94%.
The metal powder comprises copper conductive metal powder and tin alloy powder;
the copper conductive metal powder is copper-tin alloy powder, wherein the copper content is more than 90%. The ratio of the copper-tin alloy powder in the total mass of the metal powder is 50%. In other embodiments, the copper-nickel alloy powder or the mixture of the copper-tin alloy powder and the copper-tin alloy powder may be used, and the ratio of the copper conductive metal powder in the total mass of the metal powder is greater than or equal to 50% and less than 80%.
The tin alloy powder is medium temperature tin bismuth silver (Sn) 64.7 Bi 35 Ag 0.3 ) Alloy powder; the ratio of the tin alloy powder to the total mass of the metal powder was 50%. High temperature tin silver copper (Sn) may also be used in other embodiments 0.3 Ag 0.7 Cu) alloy powder, low-temperature Sn-Bi-Ag (Sn) 42 Bi 57 Ag 1 ) Alloy powder, tin bismuth (Sn) 42 Bi 58 ) One or more of alloy powders; the ratio of tin alloy powder in the total mass of the metal powder is more than 20% and not more than 50% corresponding to the ratio of copper conductive metal powder in the total mass of the metal powder.
The organic assistant comprises single-component thermosetting resin (containing a curing agent), an active agent, a thixotropic agent and an organic solvent. In the present embodiment, the one-component thermosetting resin (containing the curing agent) is selected from polyester resin, and in other embodiments, one or more of epoxy resin, silicone resin or acrylic resin without a benzene ring structure may be selected. The active agent is adipic acid, and in other embodiments, glutaric acid or a mixed reagent of adipic acid and glutaric acid may be used. The thixotropic agent is hydrogenated castor oil, and in other embodiments, one or more of fumed silica, organic bentonite, and graphene may be used. The organic solvent is ethylene glycol ether; in other embodiments, a mixed solvent of ethylene glycol diethyl ether and ethylene glycol monomethyl ether or pure ethylene glycol monomethyl ether may be used.
The proportion of the polyester resin, the adipic acid, the hydrogenated castor oil and the ethylene glycol ethyl ether in the organic auxiliary agent is 20%, 15% and 50% respectively. In other embodiments, the percentages of the single-component thermosetting resin (containing the curing agent), the active agent, the thixotropic agent and the organic solvent are 10-30%, 10-20%, 10-15% and 35-70%.
The conductive paste may be prepared by the following method:
first, copper conductive metal powder is prepared: a certain amount of copper-tin alloy powder was weighed.
Secondly, preparing an organic auxiliary agent, weighing the components according to the proportion, sequentially adding the active agent, the thixotropic agent and the thermosetting resin into the organic solvent, and uniformly stirring and mixing.
And finally, weighing the metal powder and the organic auxiliary agent according to the mass ratio, uniformly mixing the copper-tin alloy powder and the tin alloy powder, adding the organic auxiliary agent, mixing and stirring in a planetary stirrer, rolling after stirring, and uniformly mixing in a three-roll mill. Then storing at low temperature, wherein the storage temperature is 2-10 ℃.
And (3) rotating the slurry stored at a low temperature to return the temperature at room temperature, screen-printing grid lines with a certain interval on the ITO thin film of the heterojunction solar cell, and sintering in a 170-180 ℃ hot oven to form the grid lines with the width of 80-90 micrometers and the height of 15-25 micrometers. As shown in fig. 1, the tin alloy powder in the paste begins to melt, the tin alloy powder is melted to connect copper conductive metal powder particles, the grid lines shrink and become thin, organic matters in the grid lines are extruded out, the solvent is volatilized, the hydrogenated bisphenol a epoxy resin is cured, copper powder densely connected with tin liquid is fixed on the surface of the ITO film, and the contact reliability between the grid lines and the ITO film is ensured. After sintering, a picture similar to fig. 2 can be formed by photographing, and fine lines are realized on the ITO thin film.
The volume resistivity is one of the important indexes for evaluating the electrical properties of the conductive paste, and in the same manner as in the above examples, test samples of conductive pastes with different film thicknesses or different widths are prepared by screen printing and subjected to heat treatment at 170-180 ℃ for 2min. And measuring the thickness and the width of the slurry sample by using a microscope, and finally measuring the resistance of the slurry sample by using a direct current resistance measurement method, thereby calculating the volume resistivity of the conductive slurry. Test samples were printed as 5 strips of conductive film each having a length of about 50mm, a width of about 0.5mm and a thickness of about 22 μm, and the detailed test data were as follows:
according to the calculation of test data, the average volume resistivity of the conductive paste is about 4.273 mu omega cm, and compared with the volume resistivity of 4-8 mu omega cm of low-temperature conductive silver paste manufactured by international and domestic enterprises, the conductive paste has the advantages that the conductive performance is improved, the power loss of a battery on a metal grid line can be reduced, and the filling factor of the battery is improved.
In order to verify the contact reliability of the grid line and the ITO thin film, the contact resistance and the adhesive force between the ITO thin film and the grid line are tested through experiments. Firstly, a contact resistance sample of an ITO film and a grid line is manufactured, a screen printing plate with a plurality of hollow patterns with the spacing of 500 micrometers and the length of 5 millimeters is arranged, and the grid line is conducted through screen printing and heat treatment at 140-150 ℃. And selecting 11 continuous grid lines, testing the resistance R1 between the first grid line and the second grid line, the resistance R2 between the second grid line and the fourth grid line, the resistance R3 between the fourth grid line and the seventh grid line, and the resistance R4 between the seventh grid line and the eleventh grid line respectively, and calculating the contact resistivity through linear fitting. The data are as follows:
| group of | R1(Ω) | R2(Ω) | R3(Ω) | R4(Ω) | ρ(mΩ·cm 2 ) |
| 1 | 8.32 | 15.24 | 21.32 | 28.67 | 1.659 |
| 2 | 7.85 | 14.89 | 21.82 | 28.83 | 0.8849 |
| 3 | 8.72 | 15.98 | 23.03 | 29.98 | 1.7295 |
The average contact resistivity value calculated from the linear fit of the test data was 1.424m Ω cm 2 Compared with the contact resistivity between the low-temperature silver paste grid line and the ITO film in the current industry, the low-temperature silver paste grid line has the same effect.
In general, the conductive performance of the paste of the embodiment is better than that of low-temperature silver paste, is slightly weaker than that of the pastes of the embodiments 1 and 2, can be applied to printing of thin grid lines of solar cells, can replace silver paste, reduces series resistance, improves conversion efficiency and reduces cost.
Claims (12)
1. The industrial low-temperature conductive paste with high conductive performance is characterized by comprising the following components in percentage by mass:
88 to 94 percent of metal powder and 6 to 12 percent of organic auxiliary agent;
the metal powder comprises copper conductive metal powder and tin alloy powder;
the copper conductive metal powder is copper powder containing tin, nickel and/or silver;
the tin alloy powder is Sn, ag, cu and Sn 0.3 Ag 0.7 Cu alloy powder, sn-Bi-Ag Sn 64.7 Bi 35 Ag 0.3 Alloy powder, sn-Bi-Ag Sn 42 Bi 57 Ag 1 Alloy powder and/or tin bismuth Sn 42 Bi 58 Alloy powder;
the organic auxiliary agent comprises single-component thermosetting resin containing a curing agent, an active agent, a thixotropic agent and an organic solvent.
2. The industrial low-temperature conductive paste with high conductive performance according to claim 1, wherein: the copper powder containing tin, nickel and/or silver is metal particle powder with pure copper particles plated with tin, nickel and/or silver metal simple substance protective layers.
3. The industrial low-temperature conductive paste with high conductive performance according to claim 2, wherein: the pure copper particles are spherical, and the copper content is more than 99%.
4. The industrial low-temperature conductive paste with high conductive performance according to claim 3, wherein: the particle size of the metal particles in the copper conductive metal powder is less than 25 microns; the surface coating is produced by electroless plating, the coating thickness being less than 2 microns.
5. The industrial low-temperature conductive paste with high conductive performance according to claim 1, wherein: the copper conductive metal powder is copper-tin alloy powder and/or copper-nickel alloy powder, wherein the copper content is more than 90%.
6. The industrial low-temperature conductive paste with high conductive performance according to any one of claims 1 to 5, wherein: sn-Ag-Cu Sn 0.3 Ag 0.7 Cu alloy powder, sn-Bi-Ag Sn 64.7 Bi 35 Ag 0.3 Alloy powder, sn-Bi-Ag Sn 42 Bi 57 Ag 1 Alloy powder and tin bismuth Sn 42 Bi 58 The alloy powder is spherical particle alloy powder, and the particle size is less than 35 microns.
7. The industrial low-temperature conductive paste with high conductive property according to any one of claims 1 to 5, wherein: the mass ratio of the copper conductive metal powder to the tin alloy powder is 4:1-1:1.
8. the industrial low-temperature conductive paste with high conductive performance according to claim 7, wherein: the single-component thermosetting resin is one or more of epoxy resin, organic silicon resin, acrylic resin or polyester resin without a benzene ring structure.
9. The industrial low-temperature conductive paste with high conductive performance according to claim 8, wherein: the active agent is adipic acid and/or glutaric acid; the thixotropic agent is one or more of fumed silica, organic bentonite, graphene and hydrogenated castor oil; the organic solvent is ethylene glycol monomethyl ether and/or ethylene glycol ethyl ether.
10. The industrial low-temperature conductive paste with high conductive performance according to claim 9, wherein: the organic auxiliary agent contains single-component thermosetting resin containing a curing agent, an active agent, a thixotropic agent and an organic solvent, and the mass percentages of the single-component thermosetting resin, the active agent, the thixotropic agent and the organic solvent are respectively as follows:
10-30% of thermosetting resin containing a curing agent;
10-20% of an active agent;
10-15% of thixotropic agent;
35-70% of organic solvent.
11. The industrial low-temperature conductive paste with high conductive performance according to claim 10, wherein: the transparency of the single-component thermosetting resin containing the curing agent in the organic auxiliary agent, the active agent, the thixotropic agent and the organic solvent is higher than 80 percent.
12. The preparation method of the industrial low-temperature conductive paste with high conductive performance is characterized by comprising the following steps of:
step 1, preparing copper conductive metal powder;
if the metal particle powder is adopted, the surface of the pure copper particle is plated with a tin, nickel and/or silver simple substance protective layer, the chemical tin, nickel and/or silver protective layer is carried out on the surface of the pure copper particle by adopting a chemical metal plating method under the protection of inert gas;
if copper-tin alloy powder and copper-nickel alloy powder are adopted, the corresponding alloy powder is weighed according to the required content;
step 2, preparing an organic auxiliary agent;
weighing the components according to the proportion, sequentially adding the active agent, the thixotropic agent and the thermosetting resin into the organic solvent, and uniformly stirring and mixing;
step 3, preparing industrial low-temperature conductive slurry with high conductive performance;
weighing the copper conductive metal powder, the tin alloy powder and the organic auxiliary agent according to the proportion, after weighing, uniformly mixing the copper conductive metal powder and the tin alloy powder, adding the organic auxiliary agent, mixing and stirring in a planetary mixer, rolling after stirring, and then uniformly mixing in a three-roll mill.
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