CN117238554A - Conductive silver paste and preparation method thereof - Google Patents
Conductive silver paste and preparation method thereof Download PDFInfo
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- CN117238554A CN117238554A CN202311146228.7A CN202311146228A CN117238554A CN 117238554 A CN117238554 A CN 117238554A CN 202311146228 A CN202311146228 A CN 202311146228A CN 117238554 A CN117238554 A CN 117238554A
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- silver paste
- conductive silver
- silver powder
- polyurethane resin
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 187
- 238000002360 preparation method Methods 0.000 title abstract description 12
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229920000909 polytetrahydrofuran Polymers 0.000 claims abstract description 26
- 125000005210 alkyl ammonium group Chemical group 0.000 claims abstract description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 18
- 229920005749 polyurethane resin Polymers 0.000 claims description 42
- 239000000725 suspension Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical group CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 claims description 9
- 229940073507 cocamidopropyl betaine Drugs 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 6
- 229920000570 polyether Polymers 0.000 claims description 6
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 150000003242 quaternary ammonium salts Chemical group 0.000 claims description 3
- 229920005989 resin Polymers 0.000 abstract description 9
- 239000011347 resin Substances 0.000 abstract description 9
- 238000001132 ultrasonic dispersion Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000007738 vacuum evaporation Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical class CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical class CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
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Abstract
The application discloses conductive silver paste and a preparation method thereof, which relate to the technical field of solar cells, wherein water-soluble resin is selected and compounded with silver powder, polytetrahydrofuran, alkyl ammonium salt, a silane coupling agent and silicate serving as other components in a system to prepare the conductive silver paste, and the conductive silver paste is environment-friendly and has good conductivity and mechanical property.
Description
Technical Field
The application relates to the technical field of solar cells, in particular to conductive silver paste and a preparation method thereof.
Background
Currently, the metallization of solar cells in the market mainly uses conductive silver paste to collect carriers, and as the yield of solar cells increases, the demand for conductive silver paste increases. For the existing conductive silver paste on the market, oil-soluble resin is often contained, but the oil-soluble resin can release volatile organic matters in the curing process, the volatile organic matters can pollute the environment, the environment is not polluted, and the influence of the volatile organic matters on the environment is also more and more concerned. And some conductive silver pastes which do not contain oil-soluble resin components have poor adhesion and conductivity and poor mechanical property application.
Disclosure of Invention
The application discloses conductive silver paste and a preparation method thereof, which are used for solving the problem of environmental pollution caused by the current commercial conductive silver paste.
In order to achieve the above object, the embodiment of the present specification adopts the following technical solutions:
in a first aspect, a conductive silver paste is provided, the conductive silver paste is prepared from a conductive silver paste composition, and the conductive silver paste composition comprises the following raw materials: silver powder, polytetrahydrofuran, alkyl ammonium salt, silane coupling agent, silicate and aqueous polyurethane resin, wherein the conductive silver paste composition comprises the following raw materials: 100 parts of silver powder, 1-10 parts of polytetrahydrofuran, 1-15 parts of alkyl ammonium salt, 1-10 parts of silane coupling agent, 0.1-15 parts of silicate and 1-15 parts of aqueous polyurethane resin.
Alternatively, the silver powder includes a spherical silver powder and a plate-like silver powder, and the mass ratio of the spherical silver powder to the plate-like silver powder is 3:1 to 1:2.
alternatively, the spherical silver powder has a particle diameter of 0.1 μm to 5 μm.
Alternatively, the plate-like silver powder has a thickness of 0.4 to 6 μm and a particle diameter of 5 to 20. Mu.m.
Optionally, the molecular weight of the polytetrahydrofuran is 200-5000 Da.
Optionally, the alkyl ammonium salt is a quaternary ammonium salt.
Optionally, the alkyl ammonium salt is cocamidopropyl betaine.
Optionally, the silicate is a layered silicate.
Optionally, the aqueous polyurethane resin includes, but is not limited to, one or more of polyether polyurethane resin, polyester polyurethane resin, polycarbonate polyurethane resin, and polyether, polyester hybrid polyurethane resin.
In a second aspect, a method for preparing conductive silver paste is provided, comprising the following steps:
(1) Adding silver powder, polytetrahydrofuran, alkyl ammonium salt, a silane coupling agent and silicate into water to dissolve and disperse to form suspension;
(2) And adding aqueous polyurethane resin into the suspension, stirring and dispersing to obtain the conductive silver paste.
The above at least one technical scheme adopted by the embodiment of the application can achieve the following beneficial effects:
the application provides a conductive silver paste and a preparation method thereof, wherein water-soluble resin is selected and compounded with other components of silver powder, polytetrahydrofuran, alkyl ammonium salt, a silane coupling agent and silicate in a system to prepare the conductive silver paste, and the conductive silver paste is environment-friendly and has good conductivity and mechanical property.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be clearly and completely described below in connection with specific embodiments of the present application. It will be apparent that the described embodiments are only some, but not all, embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
According to an embodiment of the present application, there is provided a conductive silver paste prepared from a conductive silver paste composition including the following raw materials: silver powder, polytetrahydrofuran, alkyl ammonium salt, silane coupling agent, silicate and aqueous polyurethane resin, wherein the conductive silver paste composition comprises the following raw materials: 100 parts of silver powder, 1-10 parts of polytetrahydrofuran, 1-15 parts of alkyl ammonium salt, 1-10 parts of silane coupling agent, 0.1-15 parts of silicate and 1-15 parts of aqueous polyurethane resin.
In the embodiment of the present application, the silver powder may be any silver powder, which is not limited in the present application. Preferably, the silver powder comprises spherical silver powder and plate-like silver powder, and the mass ratio of the spherical silver powder to the plate-like silver powder is 3:1 to 1:2. alternatively, the mass ratio of the spherical silver powder to the plate-like silver powder may be 3: 1. 2: 1. 1: 1. 1:2 or any value therebetween.
The particle diameter of the spherical silver powder may be arbitrarily selected, and the present application is not limited thereto. Preferably, the spherical silver powder has a particle diameter of 0.1 μm to 5 μm. Alternatively, the particle size of the spherical silver powder may be 0.1 μm, 0.3 μm, 0.5 μm, 0.7 μm, 0.9 μm, 1.1 μm, 1.3 μm, 1.5 μm, 1.7 μm, 1.9 μm, 2.1 μm, 2.3 μm, 2.5 μm, 2.7 μm, 2.9 μm, 3.1 μm, 3.3 μm, 3.5 μm, 3.7 μm, 3.9 μm, 4.1 μm, 4.3 μm, 4.5 μm, 4.7 μm, 4.9 μm, 5 μm or any value therebetween.
The thickness and particle diameter of the plate-like silver powder can be arbitrarily selected, and the present application is not limited thereto. Preferably, the plate-like silver powder has a thickness of 0.4 to 6 μm and a particle diameter of 5 to 20 μm. Alternatively, the plate-like silver powder may have a thickness of 0.4 μm, 0.6 μm, 0.8 μm, 1 μm, 1.2 μm, 1.4 μm, 1.6 μm, 1.8 μm, 2 μm, 2.2 μm, 2.4 μm, 2.6 μm, 2.8 μm, 3 μm, 3.2 μm, 3.4 μm, 3.6 μm, 3.8 μm, 4 μm, 4.2 μm, 4.4 μm, 4.6 μm, 4.8 μm, 5 μm, 5.2 μm, 5.4 μm, 5.6 μm, 5.8 μm, 6 μm or any value therebetween. Alternatively, the particle diameter of the plate-like silver powder may be 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm, 20 μm or any value therebetween.
The welding tension of the conductive silver paste can be effectively improved by selecting the flake silver powder, so that the contact resistance between the conductive silver paste and the silicon wafer is low, but excessive flake silver powder can cause poor fluidity of the conductive silver paste, the phenomenon of gate breakage is easy to occur, and the printed gate line is uneven. The spherical silver powder is selected to ensure that the conductive silver paste has good fluidity and better printing performance, but the acquisition cost is high. The sheet silver powder and the spherical silver powder are selected for mixed use, so that the welding tension of the conductive silver paste can be improved, and the fluidity of the conductive silver paste can be ensured. Controlling the mass ratio of the spherical silver powder to the plate-like silver powder to be 3:1 to 1: within the range of 2, the effect of soldering tension and fluidity is most suitable, and the cost of the conductive silver paste is not excessively increased. Spherical silver powder with the particle size of 0.1-5 mu m, flake silver powder with the thickness of 0.4-6 mu m and/or flake silver powder with the particle size of 5-20 mu m are selected and mixed, so that the welding tension and the fluidity of the conductive silver paste are the best.
In the embodiment of the present application, the polytetrahydrofuran may be polytetrahydrofuran with any molecular weight, which is not limited in the present application. Preferably, the molecular weight of the polytetrahydrofuran is 200-5000 Da. Alternatively, the molecular weight of the polytetrahydrofuran may be 200Da, 500Da, 800Da, 1100Da, 1400Da, 1700Da, 2000Da, 2300Da, 2600Da, 2900Da, 3200Da, 3500Da, 3800Da, 4100Da, 4400Da, 4700Da, 5000Da or any value therebetween. The polytetrahydrofuran has a large number of ether bonds, can promote the dispersion of silver powder and silicate in water and the uniform dispersion of the silver powder and silicate with aqueous polyurethane resin, prevent the settlement of the silver powder and silicate, has plasticity, and can lead the fluidity of the conductive silver paste to be better and the conductive silver paste to be easier to print.
In the embodiment of the present application, the alkylammonium salt may be any kind of alkylammonium salt, which is not limited in the present application. Preferably, the alkyl ammonium salt is a quaternary ammonium salt, more preferably, the alkyl ammonium salt is one or more of cetyl ammonium salt, stearyl ammonium salt and cocamidopropyl betaine, and most preferably, the alkyl ammonium salt is cocamidopropyl betaine. The cocoamidopropyl betaine is an excellent surfactant, is extracted from natural coconuts, is low in cost, is natural and green, is pollution-free, and can effectively promote uniform dispersion of silver powder and silicate in water and aqueous polyurethane resin when being added into conductive silver paste.
In the embodiment of the present application, the silane coupling agent may be any kind or form of silane coupling agent, which is not limited in the present application. The silane coupling agent can set up a molecular bridge between inorganic matters such as silver powder, silicate and the like and the aqueous polyurethane resin, can effectively improve the uniformity of the conductive silver paste and increase the adhesion strength of the conductive silver paste.
In the embodiment of the present application, the silicate may be any kind of silicate, and the present application is not limited thereto. Preferably, the silicate is a layered silicate. When the layered silicate is undissolved, the layered silicate is formed by stacking layers, and the layered silicate is dissolved in water, and the layered silicate sheets are peeled and separated. The alkyl ammonium salt in the raw material of the conductive silver paste composition can promote dissolution and peeling of the layered silicate, so that silicate sheets are not overlapped on a microscopic level. The even distribution of the layered silicate can effectively reduce the contact resistance between silver powder and the surface of the silicon wafer, and promote the adhesion of the conductive silver paste on the silicon wafer after high-temperature sintering.
In the embodiment of the present application, the aqueous polyurethane resin may be any kind of aqueous polyurethane resin, and the present application is not limited thereto. The aqueous polyurethane resin includes, but is not limited to, one or more of polyether polyurethane resin, polyester polyurethane resin, polycarbonate polyurethane resin, polyether and polyester mixed polyurethane resin. The conductive silver paste adopts the water-based resin, namely the water-based polyurethane resin, as the raw material, so that the influence on the environment can be reduced, and the national concept of green development is met.
According to another embodiment of the present application, there is provided a method for preparing conductive silver paste, comprising the steps of:
(1) Adding silver powder, polytetrahydrofuran, alkyl ammonium salt, a silane coupling agent and silicate into water, stirring and dissolving, and performing ultrasonic dispersion to form a suspension;
(2) And adding the aqueous polyurethane resin into the suspension in batches, stirring and performing ultrasonic dispersion to obtain the conductive silver paste.
In the embodiment of the application, the duration of stirring and dissolving in the step (1) is 10-60 min. Alternatively, the duration of the stirring dissolution in step (1) may be 10min, 20min, 30min, 40min, 50min, 60min or any value therebetween. When the time is too short, the silver powder cannot be uniformly dispersed in the suspension, and when the time is too long, the time is time-consuming, but the dispersibility of the silver powder in the suspension cannot be further improved, so that the stirring and dissolution duration is 10-60 min, which is determined to ensure that the silver powder is uniformly dispersed in the suspension and no time is wasted. The stirring speed in the stirring and dissolving step (1) is 100-500 r/min. Alternatively, the stirring speed in the stirring and dissolving in the step (1) may be 100r/min, 200r/min, 300r/min, 400r/min, or 500r/min. The lower rotating speed can not uniformly mix the raw materials, and the excessively high rotating speed can cause excessively high heat generation due to friction between the liquids, so that the preparation of the conductive silver paste is affected. The stirring speed is 100 r/min-500 r/min, which is determined according to the viscosity of the suspension and the raw material amount.
In the embodiment of the present application, the duration of the ultrasonic dispersion in the step (1) is 10 to 30 minutes. Alternatively, the duration of the ultrasonic dispersion in step (1) may be 10min, 15min, 20min, 25min, 30min or any value therebetween. The time is too short, the silver powder cannot be uniformly dispersed in the suspension, and the time is too long, but the dispersibility of the silver powder in the suspension cannot be further improved, so the duration of the ultrasonic dispersion is 10-30 min, which is determined to ensure that the silver powder is uniformly dispersed in the suspension and the time is not wasted.
In the embodiment of the present application, the duration of stirring in the step (2) is 10 to 60 minutes. Alternatively, the duration of the stirring in step (2) may be 10min, 20min, 30min, 40min, 50min, 60min or any value therebetween. The time is too short, the suspension after the aqueous polyurethane resin is added cannot be uniformly dispersed, and the time is too long, but the dispersibility cannot be further improved, so the duration of stirring and dissolution is 10-60 min, which is determined to ensure that the aqueous polyurethane resin is uniformly dispersed in the suspension and the time is not wasted. The rotating speed during stirring in the step (2) is 100 r/min-500 r/min. Alternatively, the rotation speed during stirring in the step (2) may be 100r/min, 200r/min, 300r/min, 400r/min, or 500r/min. The suspension and the aqueous polyurethane resin cannot be uniformly mixed at a lower rotating speed, and the excessive high rotating speed can cause excessive heat generation due to friction between the liquids, so that the preparation of the conductive silver paste is affected. The rotation speed during stirring is 100 r/min-500 r/min, which is determined according to the viscosity of the conductive silver paste and the raw material amount.
In the embodiment of the present application, the duration of the ultrasonic dispersion in the step (2) is 10 to 30 minutes. Alternatively, the duration of the ultrasonic dispersion in step (2) may be 10min, 15min, 20min, 25min, 30min or any value therebetween. The time is too short, the suspension after the aqueous polyurethane resin is added cannot be uniformly dispersed, and the time is too long, but the dispersibility cannot be further improved, so the duration of the ultrasonic dispersion is 10-30 min, which is determined to ensure that the aqueous polyurethane resin is uniformly dispersed in the suspension and the time is not wasted.
In the step (2), a vacuum evaporation mode is adopted, so that redundant solvent in the obtained conductive silver paste can be evaporated, and the conductive silver paste with required viscosity is obtained. In the embodiment of the present application, any method may be used as long as the excess solvent can be removed and the performance of the conductive silver paste is not affected. The viscosity of the conductive silver paste is also determined according to the viscosity actually required.
In the embodiment of the present application, the number of batches of the aqueous polyurethane resin added to the suspension in step (2) is not limited thereto. Preferably, the addition is divided into three portions, which allows the suspension to be more uniformly dispersed with the aqueous polyurethane resin. Specifically, the stirring is carried out while the materials are added in batches, and ultrasonic dispersion is carried out after the stirring is carried out.
The following describes in detail the technical solutions provided by the embodiments of the present application.
The relevant information of the raw materials used in the specific embodiment of the application is as follows:
aqueous polyurethane resins were purchased from: the specification of Shenzhen Jitian chemical industry Co., ltd is: model 1526, appearance: transparent, viscosity: 350mpa.s, solid 35, characteristic: after the adhesive is dried, the adhesive is hard.
Example 1:
the preparation method of the conductive silver paste comprises the following steps:
(1) Adding 100g of silver powder, 3g of polytetrahydrofuran, 7g of cocamidopropyl betaine, 5gKH-560 silane coupling agent and 5g of layered borosilicate into water, stirring and dissolving for 30min at a rotation speed of 400r/min, and performing ultrasonic dispersion for 20min to form silver-layered silicate suspension;
wherein the silver powder is a mixture of spherical silver powder and flake silver powder, the weight ratio of the spherical silver powder to the flake silver powder is 2:1, the particle size of the spherical silver powder is 1 mu m, the thickness of the flake silver powder is 2 mu m, and the particle size of the flake silver powder is 7 mu m. The molecular weight of the polytetrahydrofuran is 800Da.
(2) 7g F1526 aqueous polyurethane resin is added to the silver-layered silicate suspension in batches, stirred for 30min at the rotation speed of 400r/min, dispersed for 20min by ultrasonic, and the redundant solvent is evaporated by vacuum evaporation to obtain the conductive silver paste.
Example 2:
the preparation method of the conductive silver paste comprises the following steps:
(1) Adding 100g of silver powder, 3g of polytetrahydrofuran, 5g of cocamidopropyl betaine, 5gKH-560 silane coupling agent and 3g of layered borosilicate into water, stirring and dissolving for 30min at the rotation speed of 400r/min, and performing ultrasonic dispersion for 20min to form silver-layered silicate suspension;
wherein the silver powder is a mixture of spherical silver powder and flake silver powder, the weight ratio of the spherical silver powder to the flake silver powder is 1:1, the particle size of the spherical silver powder is 3 mu m, the thickness of the flake silver powder is 4 mu m, and the particle size of the flake silver powder is 12 mu m. The molecular weight of the polytetrahydrofuran is 800Da.
(2) Adding 6g F1526 aqueous polyurethane resin into the silver-layered silicate suspension in batches, stirring for 30min at a rotation speed of 400r/min, performing ultrasonic dispersion for 20min, and evaporating the redundant solvent by adopting vacuum evaporation to obtain the conductive silver paste.
Example 3:
the preparation method of the conductive silver paste comprises the following steps:
(1) Adding 100g of silver powder, 1g of polytetrahydrofuran, 1g of cocamidopropyl betaine, 1gKH-560 silane coupling agent and 0.1g of layered borosilicate into water, stirring and dissolving for 60min at a rotating speed of 100r/min, and performing ultrasonic dispersion for 30min to form silver-layered silicate suspension;
wherein the silver powder is a mixture of spherical silver powder and flake silver powder, the weight ratio of the spherical silver powder to the flake silver powder is 3:1, the particle size of the spherical silver powder is 0.1 mu m, the thickness of the flake silver powder is 0.4 mu m, and the particle size of the flake silver powder is 5 mu m. The molecular weight of the polytetrahydrofuran is 200Da.
(2) 1g F1526 aqueous polyurethane resin is added to the suspension in batches, stirred for 10min at a rotation speed of 500r/min, dispersed for 10min by ultrasonic, and the redundant solvent is evaporated by vacuum evaporation to obtain the conductive silver paste.
Example 4:
the preparation method of the conductive silver paste comprises the following steps:
(1) Adding 100g of silver powder, 10g of polytetrahydrofuran, 15g of cocamidopropyl betaine, 10gKH-560 silane coupling agent and 15g of layered borosilicate into water, stirring and dissolving for 10min at a rotating speed of 500r/min, and performing ultrasonic dispersion for 10min to form silver-layered silicate suspension;
wherein the silver powder is a mixture of spherical silver powder and flake silver powder, the weight ratio of the spherical silver powder to the flake silver powder is 1:2, the particle size of the spherical silver powder is 5 mu m, the thickness of the flake silver powder is 6 mu m, and the particle size of the flake silver powder is 20 mu m. The molecular weight of the polytetrahydrofuran is 5000Da.
(2) 15g of F1526 aqueous polyurethane resin is added to the suspension in batches, stirred for 60min at a rotating speed of 100r/min, dispersed for 30min by ultrasonic, and the redundant solvent is evaporated by vacuum evaporation, so as to obtain the conductive silver paste.
Comparative example 1:
commercial oil-soluble resin-based conductive silver paste is selected.
Performance test:
the testing method comprises the steps of printing the conductive silver paste prepared in the embodiment 1, the conductive silver paste prepared in the embodiment 2 and the commercially available oil-soluble resin-based conductive silver paste selected in the comparative embodiment 1 on a solar cell silicon wafer plate in a screen printing mode, and then curing the solar cell silicon wafer plates corresponding to the embodiment 1, the embodiment 2 and the comparative embodiment 3 at the temperature of 300-850 ℃ for 2-5 min to form corresponding silver paste dry films, wherein the resistivity, the adhesive force and the pencil hardness of the dry films are measured respectively.
Resistivity testing method: and (3) screen printing conductive silver paste into a silver paste dry film with the length of 25mm, the width of 10mm and the thickness of about 50 mu m, and measuring the cured silver paste dry film by adopting an RTS-9 type double-electric-measurement four-probe tester.
The adhesive force testing method comprises the following steps: and (3) dividing longitudinal lines and transverse lines on the surface of the silver paste dry film at intervals of 1mm, wherein the dividing depth is not less than the thickness of the dry film, and more than 10 square grids with the side length of 1mm are formed. The surface dust of the scribing line is removed, the surface is stuck by a 3M adhesive tape and is rubbed and pressed by an eraser, one end of the adhesive tape is grasped, the adhesive tape is rapidly torn off perpendicular to the test surface, and no silver paste is removed, so that the method is defined as excellent.
The pencil hardness test is carried out for national standard GB/T6739-2006 paint and varnish pencil method to measure paint film hardness. The test results are shown in Table 1 below.
TABLE 1
| Performance of | Resistivity (Ω. Cm) | Adhesion force | Hardness grade of pencil |
| Example 1 | 1.5×10 -4 | Excellent quality | H |
| Example 2 | 1.4×10 -4 | Excellent quality | H |
| Example 3 | 1.8×10 -4 | Excellent quality | H |
| Example 4 | 2.1×10 -4 | Excellent quality | H |
| Comparative example 1 | 2.6×10 -4 | Excellent quality | H |
As can be seen from the data in Table 1 above, examples 1-4 all have a more excellent resistivity than the commercially available oil-soluble resin-based conductive silver pastes. The adhesion test results demonstrate that: examples 1-4 meet the adhesion requirements of commercial applications. The pencil hardness grade test results show that: examples 1 and 2 meet the hardness requirements of commercial applications.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.
Claims (10)
1. The conductive silver paste is characterized by being prepared from a conductive silver paste composition, wherein the conductive silver paste composition comprises the following raw materials: silver powder, polytetrahydrofuran, alkyl ammonium salt, silane coupling agent, silicate and aqueous polyurethane resin, wherein the conductive silver paste composition comprises the following raw materials: 100 parts of silver powder, 1-10 parts of polytetrahydrofuran, 1-15 parts of alkyl ammonium salt, 1-10 parts of silane coupling agent, 0.1-15 parts of silicate and 1-15 parts of aqueous polyurethane resin.
2. The conductive silver paste according to claim 1, wherein the silver powder comprises a spherical silver powder and a plate-like silver powder, and the mass ratio of the spherical silver powder to the plate-like silver powder is 3:1 to 1:2.
3. the conductive silver paste according to claim 2, wherein the spherical silver powder has a particle diameter of 0.1 μm to 5 μm.
4. The conductive silver paste according to claim 2, wherein the plate-like silver powder has a thickness of 0.4 to 6 μm and a particle diameter of 5 to 20 μm.
5. The conductive silver paste of claim 1, wherein the molecular weight of the polytetrahydrofuran is 200-5000 Da.
6. The conductive silver paste of claim 1, wherein the alkyl ammonium salt is a quaternary ammonium salt.
7. The conductive silver paste of claim 6, wherein the alkyl ammonium salt is cocamidopropyl betaine.
8. The conductive silver paste of claim 1, wherein the silicate is a layered silicate.
9. The conductive silver paste of claim 1, wherein the aqueous polyurethane resin comprises one or more of a polyether polyurethane resin, a polyester polyurethane resin, a polycarbonate polyurethane resin, and a combination of polyether and polyester hybrid polyurethane resins.
10. A method for preparing the conductive silver paste according to any one of claims 1 to 9, comprising the steps of:
(1) Adding silver powder, polytetrahydrofuran, alkyl ammonium salt, a silane coupling agent and silicate into water to dissolve and disperse to form suspension;
(2) And adding aqueous polyurethane resin into the suspension, stirring and dispersing to obtain the conductive silver paste.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311146228.7A CN117238554A (en) | 2023-09-06 | 2023-09-06 | Conductive silver paste and preparation method thereof |
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| CN202311146228.7A CN117238554A (en) | 2023-09-06 | 2023-09-06 | Conductive silver paste and preparation method thereof |
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| CN117238554A true CN117238554A (en) | 2023-12-15 |
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| CN202311146228.7A Pending CN117238554A (en) | 2023-09-06 | 2023-09-06 | Conductive silver paste and preparation method thereof |
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| CN112175567A (en) * | 2020-10-29 | 2021-01-05 | 烟台德邦科技有限公司 | Hydrolysis-resistant anti-settling conductive adhesive and preparation method thereof |
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| CN114479574A (en) * | 2022-01-19 | 2022-05-13 | 得嘉工业(北京)有限公司 | Water-based conductive coating and preparation method thereof |
| CN115762848A (en) * | 2022-11-09 | 2023-03-07 | 宁夏中色新材料有限公司 | Heterojunction low-temperature silver paste and preparation method thereof |
| CN116072328A (en) * | 2022-10-26 | 2023-05-05 | 南通大学 | Water-based environment-friendly solar cell welding silver paste and preparation method thereof |
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| CN1134962A (en) * | 1994-11-07 | 1996-11-06 | W·C·赫罗伊斯有限公司 | Aqueous silver composition |
| CN104036844A (en) * | 2014-02-28 | 2014-09-10 | 深圳市银和新材料科技有限公司 | Environment-friendly water-soluble solar cell anode silver paste and preparation method thereof |
| CN105244076A (en) * | 2015-11-02 | 2016-01-13 | 云南师范大学 | Environment-friendly and low-filling conductive silver paste and preparation method thereof |
| CN106398227A (en) * | 2016-07-28 | 2017-02-15 | 天津凯华绝缘材料股份有限公司 | A silicone composition, a preparing method thereof and uses of the composition |
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| CN112480858A (en) * | 2020-11-20 | 2021-03-12 | 山东北方现代化学工业有限公司 | High-strength conductive single-component silane modified polyurethane sealant with electromagnetic shielding performance and preparation method thereof |
| CN114479574A (en) * | 2022-01-19 | 2022-05-13 | 得嘉工业(北京)有限公司 | Water-based conductive coating and preparation method thereof |
| CN116072328A (en) * | 2022-10-26 | 2023-05-05 | 南通大学 | Water-based environment-friendly solar cell welding silver paste and preparation method thereof |
| CN115762848A (en) * | 2022-11-09 | 2023-03-07 | 宁夏中色新材料有限公司 | Heterojunction low-temperature silver paste and preparation method thereof |
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