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CN114464342B - Low-resistivity low-temperature solar silver paste and preparation method thereof - Google Patents

Low-resistivity low-temperature solar silver paste and preparation method thereof Download PDF

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Publication number
CN114464342B
CN114464342B CN202210065061.0A CN202210065061A CN114464342B CN 114464342 B CN114464342 B CN 114464342B CN 202210065061 A CN202210065061 A CN 202210065061A CN 114464342 B CN114464342 B CN 114464342B
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resin
curing agent
low
powder
silver
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CN114464342A (en
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金余
董飞龙
李亮
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Suzhou Beiely Polymer Materials Co ltd
Wuxi Jinrise Material Co ltd
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Suzhou Beiely Polymer Materials Co ltd
Wuxi Jinrise Material Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0036—Details
    • 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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Abstract

The invention discloses low-resistivity low-temperature solar silver paste and a preparation method thereof. The raw materials of the silver paste comprise the following components: 87-93% of silver powder, 2-5% of resin, 1-2% of diluent, 0.5-2% of curing agent, 0.01-1% of thixotropic agent, 0.01-1% of catalyst and 2-5% of organic solvent. According to the silver powder, through the combination of the silver powder with different morphologies, different dimensions and different tap densities and the matching of other auxiliary agents, the conductivity of the silver powder is optimized, and through the close packing of the space, the contact points among silver powder particles are improved, the gaps of the silver powder are reduced, and the resistivity and the intrinsic resistance of the slurry are reduced. The silver paste prepared by the invention has good stability and low volume resistivity and excellent contact resistance performance.

Description

Low-resistivity low-temperature solar silver paste and preparation method thereof
Technical Field
The invention relates to the technical field of conductive silver paste preparation, in particular to low-resistivity low-temperature solar silver paste and a preparation method thereof.
Background
With the exhaustion of non-renewable resources such as petroleum and natural gas, new energy sources such as wind energy, tidal energy and solar energy are increasingly paid attention to. Solar energy is used as an inexhaustible new energy source, and the time and cost for building the solar power station are lower than those of the traditional power station. Therefore, photovoltaic power generation is an ideal solution to the energy crisis in long-term energy strategy.
In recent years, solar cell technology has entered a rapid development stage to form various types of technical products, such as crystalline silicon solar cells, inorganic semiconductor thin film batteries, dye sensitized solar cells, perovskite solar cells, organic polymer solar cells and the like, and at present, conventional crystalline silicon is still used as a main stream, and inorganic semiconductor thin film batteries have the problems of high production cost, low conversion rate and the like, and only occupy a small part of markets, and several types of dye sensitized solar cells, perovskite solar cells and organic polymer solar cells are still in laboratories at present. The HIT cell, commonly known as a heterojunction cell, combines the advantages of a crystalline silicon cell and a thin film cell, and is a popular direction for improving the conversion rate of a silicon-based solar cell. The technology effectively prevents the recombination of carriers generated by light through passivation treatment of the front surface and the rear surface of the crystalline silicon substrate, and prolongs the service life of the carriers, thereby improving the conversion rate. Because the design of the structure leads to the production process temperature of the HIT battery below 250 ℃, the silver paste of the metalized grid formed on the surface of the HIT battery is required to be cured at a low temperature, so the silver paste is an important key raw material. The conversion rate influencing factors of the HIT silver paste generally comprise resistivity, lap joint impedance, net-drop quantity and the like, the resistivity of the HIT silver paste which is currently mainstream is 5 x 10 -6 Ω & cm, and as an important influencing part of the conversion rate, the preparation of the resistivity less than 5 x 10 -6 Ω & cm is beneficial to improving the conversion rate of the HIT silver paste. Thus, it is of great importance to prepare HIT silver pastes with low resistivity.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides low-resistivity low-temperature solar silver paste and a preparation method thereof. The silver paste prepared by the invention has good stability, fine wires are well meshed, and the silver paste has low volume resistivity and excellent contact resistance.
The technical scheme of the invention is as follows:
The low-resistivity low-temperature solar silver paste comprises the following raw materials in percentage by mass: 87-93% of silver powder, 2-5% of resin, 1-2% of diluent, 0.5-2% of curing agent, 0.01-1% of thixotropic agent, 0.01-1% of catalyst and 2-5% of organic solvent.
Further, the silver powder is flaky powder and spherical powder; the mass ratio of the flaky powder to the spherical powder is 0.01-0.3: 1, preferably 0.02 to 0.1.
Further, the D50 of the flaky powder is 2-8 mu m, and the tap density is 4-6 g/mL.
Further, the spherical powder is spherical powder I or spherical powder II; the spherical powder I comprises the following spherical powder with the following particle size in percentage by weight: 5-15% D50 is 0.05-0.8 mu m, and tap density is 3-5 g/mL; 65-80% D50 is 2-4 mu m, and tap density is 5-8 g/mL; the D50 of 14-30 percent is 1-1.8 mu m, and the tap density is 4-6 g/mL.
Further, the particle size distribution of the spherical powder II satisfies the following conditions: d50 is 0.8-1.5 μm, tap density is 4-7 g/mL, D10 is 0.05-0.5 μm, D100 is 2-5 μm, preferably D10 is 0.1-0.5 μm, and D100 is 2.5-3.5 μm.
Further, the resin is composed of an epoxy resin and an auxiliary resin; the epoxy resin is more than two of bisphenol A epoxy resin, phenoxy resin, bisphenol F epoxy resin, aliphatic epoxy resin, organosilicon modified epoxy, polyether modified epoxy resin and epoxidized rubber; the bisphenol a epoxy resin is JER 827, JER828, JER834, JER1007, or JER1001; the phenoxy resin is PKHB, PKHH, PKHJ or PKFE; the bisphenol F epoxy resin is 4007P, 4010P, 7787, 835 or 830S; the aliphatic epoxy resin is 2021P, EHPE3150, HE200 or HE2025; the organosilicon modified epoxy is ERS-Si1700, YH600 or EPS-231; the polyether modified epoxy resin is EP4000, EP4010S or EP1307; the epoxidized rubber is JP100, JP200 or XP1740; the auxiliary resin is at least one of polyether polyol, acrylic ester polyol, polyester polyol, polyurethane resin, polyester resin and acrylic resin; the auxiliary resin is resin containing hydroxyl groups and having a hydroxyl value of more than 5 or resin containing carboxyl groups and having a carboxyl value of more than 5, and the Tg of the auxiliary resin is less than 100 ℃; the polyether polyol is CP450, 2070A, 2000ML or 3003LM; the acrylate polyol is Q850M, Q519, BM666 or BM261; the polyester polyol is 4073, 4009, 4010 or 4040; the polyurethane resin is 5836, 5778, 5715 or 5703; the polyester resin Toyobo220, 280, 296 or GK888; the acrylic AC169, AC166B or BM52.
The mass ratio of the epoxy resin to the auxiliary resin is 1-10: 1, the mass ratio of the epoxy resin to the auxiliary resin is preferably 2-5: 1.
Further, the diluent is epoxy glycidyl ether, and the diluent is one or more of ethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, 1, 4-butanediol diglycidyl ether, glycerol triglycidyl ether, pentaerythritol diglycidyl ether, resorcinol diglycidyl ether, trimethylolpropane triglycidyl ether, hexahydrobisphenol A diglycidyl ether, terephthalic acid diglycidyl ether and sorbitol diglycidyl ether; the thixotropic agent is one or more of fumed silica, organic bentonite, hydrogenated castor oil and polyamide wax.
Further, the curing agent consists of a main curing agent and an auxiliary curing agent; the main curing agent is a closed isocyanate curing agent, and the deblocking temperature is 80-150 ℃, preferably 90-120 ℃; the auxiliary curing agent is one or more of imidazole curing agent, anhydride curing agent and dicyandiamide curing agent; the imidazole curing agent is one or more of benzimidazole, DBU, dimethyl tetraethylimidazole, PN23 and PN23J, PN; the acid anhydride curing agent is one or more of methyl hexa, DDSA and methyl nadic acid anhydride; the dicyandiamide curing agent is DICY; the mass ratio of the main curing agent to the auxiliary curing agent is 1.5-5:1, preferably 2-5:1.
Further, the thixotropic agent is one or more of fumed silica, organic bentonite, modified hydrogenated castor oil and polyamide wax.
Further, the catalyst is an epoxy catalyst, and the catalyst is one or more of CXC1612, CXC1614, XC9206, XC258, CXC1756, XC2007, vicbase TC3630, vicbase TC3633 and ICAM-8409; the organic solvent is one or more of propylene carbonate, ethylene glycol diethyl ether acetate, ethylene glycol butyl ether acetate, diethylene glycol butyl ether acetate, dimethyl adipate, diethyl adipate, propylene glycol methyl ether acetate and terpineol.
When the spherical powder is spherical powder II, the preparation method comprises the following steps in percentage by mass:
(1) Adding 2-5% of organic solvent into a reaction kettle for mixing, adding 2-5% of resin, heating and stirring, cooling to room temperature, and filtering to obtain a resin solution;
(2) Adding 0.01-1% of catalyst, 0.01-1% of thixotropic agent, 0.5-2% of curing agent and 1-2% of diluent into the resin solution prepared in the step (1) in sequence, and centrifugally dispersing to obtain an organic carrier;
(3) Adding 87-93% silver powder into the organic carrier prepared in the step (2), centrifugally dispersing, shearing and dispersing by a three-roller machine until the fineness of the slurry is less than 5 mu m, and filtering to obtain finished silver slurry;
in the step (1), the heating temperature is 70-95 ℃; the stirring speed is 200-300 r/min, and the stirring time is 1-2 h;
In the step (2), the centrifugal dispersion speed is 800-850 rpm, and the time is 2-4 min;
in the step (3), the specific process of centrifugal dispersion is as follows: dispersing at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1-3 min.
When the spherical powder is spherical powder I, the preparation method of the low-resistivity low-temperature solar silver paste comprises the following steps in percentage by mass:
(1) Adding 2-5% of organic solvent into a reaction kettle for mixing, adding 2-5% of resin, heating and stirring, cooling to room temperature, and filtering to obtain a resin solution;
(2) Adding 0.01-1% of catalyst, 0.01-1% of thixotropic agent, 0.5-2% of curing agent and 1-2% of diluent into the resin solution prepared in the step (1) in sequence, and centrifugally dispersing to obtain an organic carrier;
(3) Adding spherical powder accounting for 5-15% of the spherical powder I and having D50 of 0.05-0.8 mu m into the organic carrier prepared in the step (2), centrifugally dispersing, adding residual silver powder, centrifugally dispersing, shearing and dispersing by a three-roller machine until the fineness of the slurry is less than 5 mu m, and filtering to obtain finished silver slurry;
in the step (1), the heating temperature is 70-95 ℃; the stirring speed is 200-300 r/min, and the stirring time is 1-2 h;
In the step (2), the centrifugal dispersion speed is 800-850 rpm, and the time is 2-4 min;
in the step (3), the specific process of centrifugal dispersion is as follows: dispersing at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1-3 min.
The beneficial technical effects of the invention are as follows:
(1) According to the silver powder compact stacking method, through the combination of the silver powder with different morphologies, different dimensions and different tap densities, the silver powder compact stacking is realized, the contact points among the silver powder particles are improved, the gaps of the silver powder are reduced, the resistivity and the intrinsic resistance of the slurry are reduced, and the conductivity of the silver powder is optimized. The silver paste prepared by the invention has good stability, fine wires are well meshed, and the silver paste has low volume resistivity and excellent contact resistance.
(2) The resin used in the invention is composed of main resin and auxiliary resin, wherein the main resin is epoxy resin and mainly bears the cohesiveness, heat resistance and stability of slurry; the addition of the auxiliary resin improves the flexibility of the paste resin and promotes the improvement of the electrical property of the paste.
(3) The invention uses the dual curing agent, and the curing degree of the slurry is deepened together by introducing the dual curing agent and the catalyst, so that the performance of the slurry is improved.
Drawings
Fig. 1 is an SEM image of low resistivity low temperature solar silver paste prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
Example 1
The low-resistivity low-temperature solar silver paste comprises the following raw materials in percentage by mass: 93% of silver powder, 1.5% of resin, 1% of diluent, 1.2% of curing agent, 0.2% of thixotropic agent, 0.1% of catalyst and 3% of organic solvent.
Wherein, the silver powder is composed of flaky powder with the density of 4.5g/mL, the density of 3.0 μm and the tap density of 5% of the slurry, spherical powder with the density of 4.8g/mL, the density of 0.6 μm and the tap density of 4.8% of the 10% D50, spherical powder with the density of 55% D50 of 2 μm and spherical powder with the density of 6g/mL, the density of 23% D50 of 1 μm and the tap density of 5.8g/mL, and the spherical powder is spherical powder and spheroidal powder.
Epoxy resin is the main resin: 0.5% phenoxy resin PKHH and 0.7% bisphenol a epoxy resin JER 8237, auxiliary resins: 2000ML at 0.3%.
A diluent: 1% resorcinol diglycidyl ether.
Curing agent: the adhesive comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1% of G282 isocyanate curing agent, wherein the deblocking temperature is 80 ℃, and the auxiliary curing agent: 0.2% benzimidazole.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: 0.1% xc2007.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the low-resistivity low-temperature solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% resin, heating to 85 ℃, stirring at a speed of 260r/min for 1h until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.1% of an XC2007 catalyst, 0.2% of a polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether, 1% of a G282 isocyanate curing agent and 0.2% of a benzimidazole auxiliary curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier was taken, 10% of spherical powder having D50 of 0.6 μm was added and stirred, and then centrifuged and dispersed at 800rpm, 1000rpm, 1200rpm, 1600rpm, respectively, for 1min.
(4) Slowly adding the rest silver powder, manually stirring, and centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min until the fineness of the paste is below 2 μm, and stopping three rollers.
(5) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the low-resistivity low-temperature solar silver slurry.
Example 2
The low-resistivity low-temperature solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of resin, 1% of diluent, 1.2% of curing agent, 0.2% of thixotropic agent, 0.1% of catalyst and 3% of organic solvent.
Wherein the silver powder consists of flaky powder with the density of 4.5g/mL, the density of 10% D50 of 0.6 μm, the density of 4.8g/mL, spherical powder with the density of 55% D50 of 2 μm, the density of 6g/mL and spherical powder with the density of 23% D50 of 1 μm and the density of 5.8g/mL, wherein the flaky powder is 5% of the slurry, the density of the flaky powder is 4.5g/mL, and the spherical powder comprises spherical powder and spheroidal powder.
Epoxy resin is the main resin: 0.4% phenoxy resin PKFE and 0.7% bisphenol a epoxy resin JER S, auxiliary resin: 220 at 0.4%.
A diluent: 1% resorcinol diglycidyl ether.
Curing agent: the adhesive comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1% of G282 isocyanate curing agent, wherein the deblocking temperature is 80 ℃, and the auxiliary curing agent: 0.2% dimethyltetraethylimidazole.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: 0.1% xc2007.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the low-resistivity low-temperature solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min for 2 hours until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.1% of an XC2007 catalyst, 0.2% of a polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether, 1% of a G282 isocyanate curing agent and 0.2% of an auxiliary curing agent of dimethyl tetraethyl imidazole, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier was stirred with 10% of spherical powder having a D50 of 0.6. Mu.m, and then was subjected to centrifugal dispersion at speeds of 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, respectively.
(4) Slowly adding silver powder, manually stirring, and centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min until the fineness of the slurry is below 2 μm, and stopping three rollers.
(4) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the low-resistivity low-temperature solar silver slurry.
Example 3
The low-resistivity low-temperature solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of resin, 1% of diluent, 1.2% of curing agent, 0.2% of thixotropic agent, 0.1% of catalyst and 3% of organic solvent.
Wherein the silver powder is flake powder with the density of 4.5g/mL and the D50 accounting for 5 percent of the slurry and 3.0 mu m; 88% D50 is 1 μm, tap density is 5.8g/mL, D10 is 0.1 μm, D100 is 3 μm, and particle size distribution is wide.
Epoxy resin is the main resin: 0.5% phenoxy resin PKHH and 0.7% bisphenol a epoxy resin JER 8237, auxiliary resins: 2000ML at 0.3%.
A diluent: 1% resorcinol diglycidyl ether.
Curing agent: the adhesive comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1% of G282 isocyanate curing agent, wherein the deblocking temperature is 80 ℃, and the auxiliary curing agent: 0.2% benzimidazole.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: 0.1% xc2007.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the low-resistivity low-temperature solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.1% of XC2007, 0.2% of polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether, 1% of G282 isocyanate curing agent and 0.2% of benzimidazole auxiliary curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) Taking the prepared organic carrier, adding 93% silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, shearing and dispersing the slurry by using a three-roller machine after the slurry is uniformly centrifuged until the fineness of the slurry is less than 2 mu m, and stopping three rollers.
(4) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the low-resistivity low-temperature solar silver slurry.
Example 4
The low-resistivity low-temperature solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 0.5% of resin, 2% of diluent, 1.2% of curing agent, 0.2% of thixotropic agent, 0.1% of catalyst and 3% of organic solvent.
Wherein the silver powder consists of flaky powder with the density of 4.5g/mL, the density of 10% D50 of 0.6 μm, the density of 4.8g/mL, spherical powder with the density of 55% D50 of 2 μm, spherical powder with the density of 6g/mL and 23% D50 of 1 μm, and the density of 5.8g/mL, wherein the flaky powder is a spherical powder.
Epoxy resin is the main resin: 0.4% phenoxy resin PKHH, auxiliary resin: GK888 at 0.1%.
A diluent: 2% of hexahydrobisphenol A diglycidyl ether.
Curing agent: the adhesive comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1% of B-897N isocyanate curing agent, wherein the deblocking temperature is 120 ℃, and the auxiliary curing agent is as follows: 0.2% benzimidazole.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: 0.1% xc2007.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the low-resistivity low-temperature solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 0.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.1% of XC2007, 0.2% of polyamide wax thixotropic agent, 2% of hexahydrobisphenol A diglycidyl ether, 1% of B-897N isocyanate curing agent and 0.2% of benzimidazole auxiliary curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier, spherical powder with D50 of 0.6 μm, was added and stirred, and then put into a centrifugal disperser, and centrifugally stirred at speeds of 800rpm, 1000rpm and 1200rpm, respectively, for 1min.
(4) Slowly adding the rest silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, shearing and dispersing the slurry by using a three-roller machine after the silver powder is uniformly centrifuged until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(5) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the low-resistivity low-temperature solar silver slurry.
Example 5
The low-resistivity low-temperature solar silver paste comprises the following components in percentage by mass: 87% of silver powder, 5% of resin, 1% of diluent, 2% of curing agent, 0.2% of thixotropic agent, 0.2% of catalyst and 4.6% of organic solvent.
Wherein the silver powder is flaky powder with the D50 accounting for 10 percent of the slurry and 3.0 mu m and the tap density of 4.5 g/mL; 77% D50 is 1 μm, tap density is 5.8g/mL, D10 is 0.1 μm, D100 is 3 μm, and particle size distribution is wide, wherein the spherical powder is spherical powder.
Epoxy resin is the main resin: 3% phenoxy resin PKFE and 1.5% bisphenol a epoxy resin JER 828, auxiliary resins: 0.5% AC166B.
A diluent: 1% of hexahydrobisphenol A diglycidyl ether.
Curing agent: the adhesive comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1.5% of G282 isocyanate curing agent, wherein the deblocking temperature is 80 ℃, and the auxiliary curing agent: 0.5% benzimidazole.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: 0.1% xc2007.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the low-resistivity low-temperature solar silver paste comprises the following steps:
(1) Mixing 4.6% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 5% polymer resin, heating to 90 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.1% of XC2007, 0.2% of polyamide wax thixotropic agent, 1% of hexahydrobisphenol A diglycidyl ether, 1.5% of G282 isocyanate curing agent and 0.5% of benzimidazole auxiliary curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) Slowly adding silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring for 1min at 800rpm, 1000rpm, 1200rpm and 1600rpm, shearing and dispersing the slurry by using a three-roller machine after the silver powder is uniformly centrifuged until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(4) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the low-resistivity low-temperature solar silver slurry.
Comparative example 1
The solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of resin, 1% of epoxy diluent, 1.3% of curing agent, 0.2% of thixotropic agent, 0% of catalyst and 3% of organic solvent.
Wherein the silver powder consists of flaky powder with the D50 of 3.0 mu m and the tap density of 4.5g/mL accounting for 5% of the slurry and spherical powder with the D50 of 2 mu m and the tap density of 6g/mL accounting for 85% of the slurry.
Epoxy resin is the main resin: 0.5% phenoxy resin PKHH and 1.3% bisphenol a epoxy resin JER 8237, auxiliary resins: and no.
Epoxy diluent: 1% resorcinol diglycidyl ether.
Curing agent: the adhesive comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1% of a G282 isocyanate curing agent, wherein the auxiliary curing agent comprises the following components: and no.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: and no.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.2% of polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether and 1% of G282 isocyanate curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) Taking the prepared organic carrier, adding 93% silver powder, manually stirring, and after all silver powder is uniformly stirred, sequentially and respectively centrifugally dispersing for 1min at 800rpm, 1000rpm, 1200rpm and 1600rpm, shearing and dispersing the slurry by using a three-roller machine after the centrifugal is uniform until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(4) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the finished silver slurry.
Comparative example 2
The solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of high polymer resin, 1% of diluent, 1.3% of curing agent, 0.2% of thixotropic agent, 0% of catalyst and 3% of organic solvent.
Wherein, the silver powder is composed of 5% of tablet powder with D50 of 3.0 μm, tap density of 4.5g/mL, 10% of spherical powder with D50 of 0.6 μm, tap density of 4.8g/mL, 78% of spherical powder with D50 of 2 μm and tap density of 6 g/mL.
The polymer resin is used as main resin: 0.5% phenoxy resin PKHH and 0.7% bisphenol a epoxy resin JER 8237, auxiliary resins: and no.
A diluent: 1% resorcinol diglycidyl ether.
Curing agent: comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1.3 percent of G282 isocyanate curing agent, and the auxiliary curing agent: and no.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: and no.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.2% of polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether and 1.3% of G282 isocyanate curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier, 10% of spherical powder with D50 of 0.6 μm, is added and stirred, and then put into a centrifugal dispersing machine to be respectively centrifugally stirred for 1min at the speeds of 800rpm, 1000rpm and 1200 rpm.
(4) Slowly adding the rest silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, shearing and dispersing the slurry by using a three-roller machine after the silver powder is uniformly centrifuged until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(5) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the finished silver slurry.
Comparative example 3
The solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of high polymer resin, 1% of diluent, 1.3% of curing agent, 0.2% of thixotropic agent, 0% of catalyst and 3% of organic solvent.
Wherein the silver powder consists of flaky powder with the density of 4.5g/mL, the density of 0.6 μm, the density of 4.8g/mL, the density of 55% D50 of 2 μm, the density of 6g/mL, the density of 23% D50 of 1 μm and the density of 5.8g/mL, which are 5% of the slurry.
The polymer resin is used as main resin: 0.5% phenoxy resin PKHH and 0.7% bisphenol a epoxy resin jER827, auxiliary resins: and no.
A diluent: 1% resorcinol diglycidyl ether.
Curing agent: comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1.3 percent of G282 isocyanate curing agent, and the auxiliary curing agent: and no.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: and no.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.2% of polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether and 1.3% of G282 isocyanate curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier, 10% of spherical powder with D50 of 0.6 μm, is added and stirred, and then put into a centrifugal dispersing machine to be respectively centrifugally stirred for 2min at the speeds of 800rpm, 1200rpm and 1600 rpm.
(4) Slowly adding the rest silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, shearing and dispersing the slurry by using a three-roller machine after the silver powder is uniformly centrifuged until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(5) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the finished silver slurry.
Comparative example 4
The solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of high polymer resin, 1% of epoxy diluent, 1.3% of curing agent, 0.2% of thixotropic agent, 0% of catalyst and 3% of organic solvent.
Wherein the silver powder consists of flaky powder with the density of 4.5g/mL, the density of 10% D50 of 0.6 μm, the density of 5.3g/mL, spherical powder with the density of 55% D50 of 2 μm, spherical powder with the density of 6g/mL, 23% D50 of 1 μm and the density of 5.8g/mL, which account for 5% of the slurry.
The polymer resin is used as main resin: 0.5% phenoxy resin PKHH and 0.7% bisphenol a epoxy resin jER827, auxiliary resins: 2000ML at 0.3%.
Epoxy diluent: 1% resorcinol diglycidyl ether.
Curing agent: comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1.1 percent of G282 isocyanate curing agent, and the auxiliary curing agent: and no.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: and no.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 2.3% polymer resin, heating to 70-95 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.2% of polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether and 1.1% of G282 isocyanate curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier, 10% of spherical powder with D50 of 0.6 μm, is added and stirred, and then put into a centrifugal dispersing machine to be respectively centrifugally stirred for 1min at the speeds of 800rpm, 1000rpm and 1200 rpm.
(4) Slowly adding the rest silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, shearing and dispersing the slurry by using a three-roller machine after the silver powder is uniformly centrifuged until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(5) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the finished silver slurry.
Comparative example 5
The solar silver paste comprises the following components in percentage by mass: 93% of silver powder, 1.5% of high polymer resin, 1% of epoxy diluent, 1.3% of curing agent, 0.2% of thixotropic agent, 0% of catalyst and 3% of organic solvent.
Wherein, the silver powder is tablet powder with the D50 of 3.0 mu m accounting for 5 percent of the slurry and the tap density of 4.5 g/mL; 10% of D50 is 0.6 μm, the tap density is 4.8g/mL, 55% of D50 is 2 μm, the tap density is 6g/mL, and 23% of D50 is 1 μm, the tap density is 5.8 g/mL.
The polymer resin is used as main resin: 0.5% phenoxy resin PKHH and 0.7% bisphenol a epoxy resin JER 8237, auxiliary resins: 2000ML at 0.3%.
Epoxy diluent: 1% resorcinol diglycidyl ether.
Curing agent: comprises an isocyanate curing agent and an auxiliary curing agent, specifically 1.1 percent of G282 isocyanate curing agent, and the auxiliary curing agent: 0.2% benzimidazole.
Thixotropic agent: 0.2% polyamide wax.
Catalyst: and no.
Organic solvent: 3% diethylene glycol butyl ether acetate.
The preparation method of the solar silver paste comprises the following steps:
(1) Mixing 3% diethylene glycol butyl ether acetate organic solvent in a reaction kettle, gradually adding 1.5% high polymer resin, heating to 85 ℃, stirring at a speed of 260r/min until the resin is completely dissolved, standing, cooling to room temperature, and filtering with 300-400 mesh fabrics to obtain a resin solution;
(2) Taking the prepared resin solution, gradually adding 0.2% of polyamide wax thixotropic agent, 1% of resorcinol diglycidyl ether, 1.1% of G282 isocyanate curing agent and 0.2% of benzimidazole auxiliary curing agent, centrifugally dispersing for 2min at 800rpm, and fully and uniformly stirring to obtain an organic carrier;
(3) The prepared organic carrier, 10% of spherical powder with D50 of 0.6 μm, is added and stirred, and then put into a centrifugal dispersing machine to be respectively centrifugally stirred for 1min at the speeds of 800rpm, 1000rpm and 1200 rpm.
(4) Slowly adding the rest silver powder, manually stirring, putting into a centrifugal dispersing machine after all silver powder is uniformly stirred, sequentially and respectively centrifugally stirring at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1min, shearing and dispersing the slurry by using a three-roller machine after the silver powder is uniformly centrifuged until the fineness of the slurry is below 2 mu m, and stopping three rollers.
(5) And filtering to remove impurities and uneven large particles in the slurry by using a 500-mesh screen to obtain the finished silver slurry.
Test example:
Using examples 1 to 5, the silver pastes prepared in comparative examples 1 to 5 were prepared into patterns, and the patterns were put into an oven at 200 ℃ to be cured for 30 minutes, the resistance after curing was measured, and the resistivity was calculated by a resistivity formula; the overlap resistance was calculated by the intercept method, the viscosity was measured by a plate viscometer, and the ratio of the viscosity at the cut-off rate of 4.62rpm to the viscosity at 46.6rpm was recorded as a thixotropic index, and the measurement results are shown in Table 1.
TABLE 1
As can be seen from table 1 above, comparative example 3 improved the silver powder particle size distribution and silver powder combination, and the apparent decrease in the resistivity and lap resistance of the paste, probably because these particle size powders entered the gaps between the filled raw silver powders, improved the effective contact points of the silver powders, and improved the resistivity, as well as the lap resistance, as compared to comparative examples 1-2. Comparative example 4 has reduced viscosity, increased thixotropic index, reduced resistivity and overlap resistance, possibly small molecular polyester addition, improved viscosity of the paste, and it has a small amount of hydroxyl groups, increases hydrogen bonds of the resin of the paste, and forms a gel-like state which is advantageous for increasing its thixotropic properties, such resin itself having flexibility and multi-functionality, improving rigidity of the original epoxy system of the paste, thereby promoting reduction of resistivity thereof, increasing adhesion, and improving overlap resistance, as compared with comparative example 3. The viscosity of comparative example 5 is not significantly different from that of comparative example 4, and the resistivity and the overlap resistance of comparative example 5 are reduced, possibly because of the use of imidazole curing agent, dual curing effect is formed, the curing speed and the curing degree of the slurry are improved, the resistance is reduced, and the adhesion effect is increased, thereby improving the overlap effect.
Example 1 has a slight decrease in resistivity and overlap resistance compared to comparative example 5, and it is possible that the catalyst would increase this dual cure effect, promoting a decrease in resistivity and overlap resistance, but less strongly affecting overall performance than the latter, and example 1 has an increase in thixotropic index and a decrease in viscosity while decreasing resistivity and overlap resistance compared to comparative example 5. Example 2 compared with the raw material of example 1, the multi-powder combination scheme is replaced by single silver powder with wide distribution, but the mechanism of improving the particle size distribution of the powder with different particle sizes is consistent with that of the powder introduced in the embodiment 1, the space effective accumulation of the silver powder is improved, the resistivity and the lap resistance are also smaller than those of the powder with 1-5, the single silver powder with wide distribution can have good space accumulation effect, but the lap resistance is bigger than that of the powder with small particle size, possibly related to less powder with small particle size. Example 3 compared to example 1, the resin and its proportions were varied and it was found that the resistivity and overlap resistance could also be less than those of comparative examples 1-5, indicating that the resin combination is beneficial for improving the conductive properties of the paste. In example 4 and example 5, both the viscosity and the resistivity were lowered compared to example 1, and example 4 increased the content of the diluent to lower the viscosity, but an excessive amount of the diluent may cause insufficient curing, resulting in lowered resistivity. Example 5 increases the proportion of the resin, causing the viscosity of the entire paste to decrease, but the decrease in silver content still causes the problem of deterioration in resistivity, so that example increases the proportion of the flake, and improves the resistivity of the paste by increasing the content of the flake.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (6)

1. The low-resistivity low-temperature solar silver paste is characterized by comprising the following raw materials in percentage by mass: 87-93% of silver powder, 2-5% of resin, 1-2% of diluent, 0.5-2% of curing agent, 0.01-1% of thixotropic agent, 0.01-1% of catalyst and 2-5% of organic solvent;
The silver powder consists of flaky powder and spherical powder; the mass ratio of the flaky powder to the spherical powder is 0.01-0.3: 1, a step of; the spherical powder is one or two of spherical powder and ball-like powder;
The spherical powder is spherical powder I or spherical powder II; the spherical powder I comprises the following spherical powder with the following particle size in percentage by weight: 5-15% D50 is 0.05-0.8 mu m, and tap density is 3-5 g/mL; 65-80% D50 is 2-4 mu m, and tap density is 5-8 g/mL; 14-30% D50 is 1-1.8 mu m, and tap density is 4-6 g/mL; the particle size distribution of the spherical powder II meets the following conditions: d50 is 0.8-1.5 mu m, D10 is 0.05-0.5 mu m, and D100 is 2-5 mu m;
The resin is composed of a main resin and an auxiliary resin; the main resin is more than two of bisphenol A epoxy resin, phenoxy resin, bisphenol F epoxy resin, aliphatic epoxy resin, organosilicon modified epoxy, polyether modified epoxy resin and epoxidized rubber; the auxiliary resin is at least one of polyether polyol, acrylic ester polyol, polyester polyol, polyurethane resin, polyester resin and acrylic resin; the mass ratio of the main resin to the auxiliary resin is 1-10: 1, a step of;
the curing agent consists of a main curing agent and an auxiliary curing agent; the main curing agent is a closed isocyanate curing agent, and the deblocking temperature is 80-150 ℃; the auxiliary curing agent is one or more of imidazole curing agent, anhydride curing agent and dicyandiamide curing agent; the mass ratio of the main curing agent to the auxiliary curing agent is 1.5-5: 1.
2. The low resistivity, low temperature solar silver paste of claim 1, wherein the flake has a D50 of 2 to 8 μm and a tap density of 4 to 6g/mL.
3. The low resistivity, low temperature solar silver paste of claim 1, wherein the diluent is an epoxy glycidyl ether and the diluent is one or more of ethylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, 1, 4-butanediol diglycidyl ether, glycerol triglycidyl ether, pentaerythritol glycidyl ether, resorcinol diglycidyl ether, trimethylolpropane triglycidyl ether, hexahydrobisphenol a diglycidyl ether, terephthalic acid diglycidyl ether, sorbitol diglycidyl ether.
4. The low resistivity, low temperature solar silver paste of claim 1, wherein the thixotropic agent is one or more of fumed silica, organobentonite, modified hydrogenated castor oil, polyamide wax.
5. The low resistivity, low temperature solar silver paste of claim 1, wherein the catalyst is one or more of CXC1612, CXC1614, XC9206, XC258, CXC1756, XC2007, vicbase TC3630, vicbaseTC3633, ICAM-8409; the organic solvent is one or more of propylene carbonate, ethylene glycol diethyl ether acetate, ethylene glycol butyl ether acetate, diethylene glycol butyl ether acetate, dimethyl adipate, diethyl adipate, propylene glycol methyl ether acetate and terpineol.
6. A method for preparing the low-resistivity and low-temperature solar silver paste according to any one of claims 1 to 5, which is characterized by comprising the following steps in percentage by mass:
(1) Adding 2-5% of organic solvent into a reaction kettle for mixing, adding 2-5% of resin, heating and stirring, cooling to room temperature, and filtering to obtain a resin solution;
(2) Adding 0.01-1% of catalyst, 0.01-1% of thixotropic agent, 0.5-2% of curing agent and 1-2% of diluent into the resin solution prepared in the step (1) in sequence, and centrifugally dispersing to obtain an organic carrier;
(3) Adding 87-93% silver powder into the organic carrier prepared in the step (2), centrifugally dispersing, shearing and dispersing by a three-roller machine until the fineness of the slurry is less than 5 mu m, and filtering to obtain low-temperature solar silver slurry with low resistivity;
in the step (1), the heating temperature is 70-95 ℃; the stirring speed is 200-300 r/min, and the stirring time is 1-2 h;
In the step (2), the centrifugal dispersion speed is 800-850 rpm, and the time is 2-4 min;
in the step (3), the specific process of centrifugal dispersion is as follows: dispersing at 800rpm, 1000rpm, 1200rpm and 1600rpm for 1-3 min.
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