CN115954136A - Transparent high-temperature sintered silver paste and preparation method, use method and application thereof - Google Patents
Transparent high-temperature sintered silver paste and preparation method, use method and application thereof Download PDFInfo
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- CN115954136A CN115954136A CN202310174119.XA CN202310174119A CN115954136A CN 115954136 A CN115954136 A CN 115954136A CN 202310174119 A CN202310174119 A CN 202310174119A CN 115954136 A CN115954136 A CN 115954136A
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- silver paste
- polyamide
- transparent high
- temperature sintered
- polyaniline
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 84
- 239000004332 silver Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004952 Polyamide Substances 0.000 claims abstract description 71
- 229920002647 polyamide Polymers 0.000 claims abstract description 71
- 229920000767 polyaniline Polymers 0.000 claims abstract description 69
- 239000000203 mixture Substances 0.000 claims abstract description 51
- 239000011521 glass Substances 0.000 claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 15
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 18
- 239000011812 mixed powder Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- 238000004377 microelectronic Methods 0.000 claims description 7
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 150000008064 anhydrides Chemical class 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 14
- 238000007639 printing Methods 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 238000005452 bending Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000001856 Ethyl cellulose Substances 0.000 description 4
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 4
- 229920001940 conductive polymer Polymers 0.000 description 4
- 229920001249 ethyl cellulose Polymers 0.000 description 4
- 235000019325 ethyl cellulose Nutrition 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 3
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical group CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229940116411 terpineol Drugs 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004840 adhesive resin Substances 0.000 description 1
- 229920006223 adhesive resin Polymers 0.000 description 1
- -1 butyl acetic anhydride acetate Chemical compound 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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 provides transparent high-temperature sintered silver paste and a preparation method, a use method and application thereof, and particularly relates to the technical field of conductive silver paste. The transparent high-temperature sintered silver paste comprises 15-20% of silver powder, 60-80% of polyamide/polyaniline conductive mixture, 3-15% of glass powder and 2-22% of solvent. According to the transparent high-temperature sintering silver paste, the polyamide/polyaniline conductive mixture is added into the raw materials, so that the transparency and the conductive capability of the silver paste are improved. The silver powder, the polyamide/polyaniline conductive mixture, the glass powder and the solvent in the raw materials are integrally matched with each other, so that the transparency, the conductivity, the dispersing performance and the printing performance of the silver paste are improved. The resistivity of the transparent high-temperature sintering silver paste provided by the invention is 2 multiplied by 10 ‑6 Ω·cm～4×10 ‑6 Omega cm; the adhesion test grade is 5B, and the adhesive has better bending resistanceAnd adhesion.
Description
Technical Field
The invention relates to the technical field of conductive silver paste, in particular to transparent high-temperature sintered silver paste and a preparation method, a use method and application thereof.
Background
With the development of socio-economy, the demand for energy and electronics is increasing, many high-performance core electronic materials, such as conductive silver paste, are monopolized by foreign technologies for a long time, and high-temperature conductive silver paste is a main material of high-performance electronics and is a key material for obtaining high-efficiency, low-cost and high-performance electronics.
In current high temperature conductive silver thick liquid, in order to make the silver thick liquid have good printability, add a large amount of organic carriers, the performance that the excessive use of these auxiliary materials can normally be to the silver thick liquid influences: such as the use of large amounts of organic mixtures, can reduce the conductive properties of the silver paste.
For obtaining good, efficient conductivity, a large amount of silver powder is added and makes silver thick liquid cost increase, and the use of a large amount of silver powder also can exert an influence to the dispersion properties of silver thick liquid simultaneously, is unfavorable for the later stage printing of silver thick liquid.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a transparent high-temperature sintered silver paste to relieve the technical problems of low conductivity, poor dispersibility, influence on printing and high cost of the silver paste in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a transparent high-temperature sintered silver paste, which comprises the following raw materials: silver powder, polyamide/polyaniline conductive mixture, glass powder and solvent.
Optionally, the raw materials comprise the following components in percentage by mass: 15% -20% of silver powder, 60% -80% of polyamide/polyaniline conductive mixture, 3% -15% of glass powder and 2% -22% of solvent.
Optionally, the solvent comprises at least one of isophorone, butyl anhydrouse acetate, diethylene glycol butyl ether acetate, and diethylene glycol ethyl ether acetate.
Optionally, in the polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is (1-4): 5.
The second aspect of the invention provides a preparation method of the transparent high-temperature sintered silver paste, which comprises the following steps:
step A: uniformly mixing the polyamide/polyaniline conductive mixture with a solvent to obtain a polyamide/polyaniline conductive mixture solution;
and B: uniformly mixing silver powder and glass powder and then grinding to obtain mixed powder;
step C: and D, adding the mixed powder obtained in the step B into the polyamide/polyaniline conductive mixture solution obtained in the step A, and uniformly mixing to obtain the transparent high-temperature sintered silver paste.
Optionally, in step B, the particle size of the mixed powder is less than or equal to 4.5 μm.
Optionally, in the step C, the viscosity of the transparent high-temperature sintered silver paste is 10000mPa · s to 12000mPa · s.
The third aspect of the invention provides a use method of the transparent high-temperature sintered silver paste, wherein the transparent high-temperature sintered silver paste is printed on a device and then sintered to obtain a silver conductive layer.
Optionally, the sintering temperature is 700-950 ℃;
preferably, the sintering time is 5min to 10min.
The fourth aspect of the invention provides the application of the transparent high-temperature sintered silver paste in a PCB (printed circuit board), a microelectronic or solar panel.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the transparent high-temperature sintered silver paste provided by the invention, a polyamide/polyaniline conductive mixture is added into a raw material, wherein a polyamide molecular chain contains a certain number of amide groups, and the chemical structure determines that the polyamide/polyaniline conductive mixture can form a hydrogen bond with polyaniline and mutually adsorb to form a mixture; the main chain of polyaniline contains alternate benzene rings and nitrogen atoms, and is a special conductive polymer. Polyaniline and polyamide are both conductive polymers, and after the polyaniline is compounded with polyamide polymer materials, the polyaniline can partially replace adhesive resin when applied to silver paste, so that the conductive composite material which has good processability and mechanical properties and controllable conductivity can be obtained, and the transparency and the conductivity of the silver paste are improved. The glass powder improves the sintering performance of the silver paste and the glass substrate and improves the bonding force. The silver powder, the polyamide/polyaniline conductive mixture, the glass powder and the solvent are integrally matched with one another, so that the transparency, the conductivity, the dispersibility and the printing performance of the silver paste are improved. The resistivity of the transparent high-temperature sintering silver paste provided by the invention is 2 multiplied by 10 -6 Ω·cm～4×10 -6 Omega cm, the adhesion test grade is 5B, and the paint has excellent bending resistance and adhesion.
The preparation method provided by the invention is simple, large in treatment capacity, low in cost, high in method repeatability and beneficial to large-scale production.
The application method provided by the invention is simple, the mechanical operation is convenient, the treatment capacity is large, and the large-scale operation is facilitated.
The application provided by the invention provides conductive silver paste with better performance and lower cost for a PCB, a microelectronic and a solar cell panel, and improves the communication of circuits in the PCB, the microelectronic and the solar cell panel and the photoelectric conversion efficiency.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The components of embodiments of the present invention may be arranged and designed in a wide variety of different configurations.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
In the invention, the temperature is not particularly indicated, namely the temperature is normal temperature or room temperature, namely the temperature influence is not particularly considered in related operation, and heating or refrigerating treatment is not required.
According to the first aspect of the invention, the transparent high-temperature sintered silver paste comprises the following raw materials: silver powder, polyamide/polyaniline conductive mixture, glass powder and solvent.
The invention provides a transparent high temperatureSintering silver paste, adding a polyamide/polyaniline conductive mixture into raw materials, wherein the polyamide molecular chain contains a certain number of amide groups, and the chemical structure determines that the polyamide/polyaniline conductive mixture can form hydrogen bonds with polyaniline to be mutually adsorbed to form a mixture; the main chain of polyaniline contains alternate benzene rings and nitrogen atoms, and is a special conductive polymer. When the polyaniline is compounded with the polyamide high polymer material, the conductive composite material which has good processability and mechanical property and controllable conductivity can be obtained, and the transparency and the conductive capability of the silver paste are improved. The glass powder improves the sintering performance of the silver paste and the glass substrate and improves the bonding force. The silver powder, the polyamide/polyaniline conductive mixture, the glass powder and the solvent are integrally matched with each other, so that the transparency, the conductivity, the dispersibility and the printing performance of the silver paste are improved. The resistivity of the transparent high-temperature sintering silver paste provided by the invention is 2 multiplied by 10 -6 Ω·cm～4×10 -6 Omega cm; the adhesion test grade is 5B, and the adhesive has better bending resistance and adhesion.
The polyamide/polyaniline conductive mixture, the glass frit and the solvent form a carrier, and the components shrink by a self-curing process such that the silver powder dispersed therein contacts each other to form a conductive network.
The solvent dissolves the polyamide/polyaniline conductive mixture, and the dispersibility, viscosity and printability of the conductive silver paste and the wettability of the conductive silver paste and the substrate are adjusted.
Optionally, the raw materials comprise the following components in percentage by mass: 15% -20% of silver powder, 60% -80% of polyamide/polyaniline conductive mixture, 3% -15% of glass powder and 2% -22% of solvent.
When the mass fraction of the silver powder is less than 15%, the silver particles cannot be effectively connected in a molecular network structure of the polymer to form a conductive network body, so that the resistivity is too high; when the mass fraction of the silver powder is more than 20%, the silver particles are easily agglomerated in the organic solvent matrix, and the dispersibility is deteriorated. When the mass fraction of the polyamide/polyaniline conductive mixture is less than 60%, silver particles cannot be effectively connected into a conductive network, so that the resistivity is too high, and the sintering curing time is prolonged; when the mass fraction of the polyamide/polyaniline conductive mixture is higher than 80%, the viscosity of the transparent high-temperature sintered silver paste becomes high, and the dispersibility becomes poor. When the mass fraction of the glass powder is less than 3%, the sintering performance of the glass powder and a glass substrate is influenced, and the adhesion is poor; when the mass fraction of the glass frit is higher than 15%, the conductivity becomes small.
In some embodiments of the present invention, the mass fraction of silver powder in the transparent high temperature sintered silver paste is typically but not limited to 15%, 16%, 17%, 18%, 19%, or 20%; the mass fraction of the polyamide/polyaniline conductive mixture is typically, but not limited to, 60%, 65%, 70%, 75%, or 80%; the mass fraction of glass frit is typically but not limited to 3%, 6%, 9%, 12% or 15%; the mass fraction of solvent is typically but not limited to 2%, 7%, 12%, 17% or 22%.
Optionally, the solvent comprises at least one of isophorone, butyl anhydrouse acetate, diethylene glycol butyl ether acetate, and diethylene glycol ethyl ether acetate.
Optionally, in the polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is 1-4.
When the mass ratio of the polyamide to the polyaniline is lower than 1; when the mass ratio of the polyamide to the polyaniline is higher than 4.
In some embodiments of the invention, the mass ratio of polyamide to polyaniline in the polyamide/polyaniline conductive mixture is typically, but not limited to, 1.
The second aspect of the invention provides a preparation method of the transparent high-temperature sintered silver paste, which comprises the following steps:
step A: uniformly mixing the polyamide/polyaniline conductive mixture with a solvent to obtain a polyamide/polyaniline conductive mixture solution;
and B: uniformly mixing silver powder and glass powder and then grinding to obtain mixed powder;
step C: and D, adding the mixed powder obtained in the step B into the polyamide/polyaniline conductive mixture solution obtained in the step A, and uniformly mixing to obtain the transparent high-temperature sintered silver paste.
The preparation method provided by the invention is simple, large in treatment capacity, low in cost, high in method repeatability and beneficial to large-scale production.
Optionally, in step B, the particle size of the mixed powder is less than or equal to 4.5 μm.
When the particle size of the mixed powder is not more than 4.5 μm, the smaller its particle size in the transparent high temperature sintered silver paste, the more dense the filling of the silver powder and the lower the required curing temperature will be. When the size of the silver powder particles is larger than 4.5 micrometers, gaps among the silver powder particles are easily filled by the carrier, so that a conductive path is formed among conductive particles, and the performance of the transparent high-temperature sintered silver paste is influenced.
Optionally, in the step C, the viscosity of the transparent high-temperature sintered silver paste is 10000mPa · s to 12000mPa · s.
In some embodiments of the invention, the viscosity of the transparent high temperature sintering silver paste is typically, but not limited to, 10000mPa · s, 11000mPa · s, or 12000mPa · s.
The third aspect of the invention provides a use method of the transparent high-temperature sintered silver paste, wherein the transparent high-temperature sintered silver paste is printed on a device and then sintered to obtain a silver conductive layer.
The application method provided by the invention is simple, the mechanical operation is convenient, the treatment capacity is large, and the large-scale operation is facilitated.
Optionally, the temperature of sintering is 700 ℃ to 950 ℃.
In some embodiments of the invention, the temperature of sintering is typically, but not limited to, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃ or 950 ℃.
Preferably, the sintering time is 5min to 10min.
In some embodiments of the invention, the sintering time is typically, but not limited to, 5min, 6min, 7min, 8min, 9min, or 10min.
The fourth aspect of the invention provides the application of the transparent high-temperature sintered silver paste in PCB boards, microelectronics and solar panels.
The application provided by the invention provides conductive silver paste with better performance and lower cost for a PCB, a microelectronic and a solar cell panel, and improves the communication of circuits in the PCB, the microelectronic and the solar cell panel and the photoelectric conversion efficiency.
Some embodiments of the present invention will be described in detail below with reference to examples. The embodiments described below and the features of the embodiments can be combined with each other without conflict.
The raw materials used in the examples and comparative examples of the present invention, for which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer.
Example 1
The embodiment provides a transparent high-temperature sintered silver paste, which comprises 17kg of silver powder, 70kg of polyamide/polyaniline conductive mixture, 9kg of glass powder and 4kg of isophorone; wherein in the polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is 1. The glass powder is Bi 2 0 3 -CuO-SiO 2 The system is glass powder.
The preparation process of the transparent high-temperature sintered silver paste comprises the following steps:
1. and (2) uniformly mixing polyamide and polyaniline according to a mass ratio, adding part of isophorone for mixing, stirring at the room temperature at the rotating speed of 1000 revolutions per minute until the system is completely and uniformly mixed to be transparent, and stopping stirring to obtain the polyamide/polyaniline conductive mixture solution.
2. The silver powder and the glass frit were completely mixed at room temperature, a little isophorone was added to wet the mixed powder, and the mixed powder was ground with a grinder, and the particle size of the mixed powder was measured to be 4um.
3. And stirring and mixing the mixed powder and the polyamide/polyaniline conductive mixture solution at the room temperature at the rotating speed of 1000 revolutions per minute, adding the rest isophorone until uniform silver paste is formed, and measuring the viscosity of the silver paste to be 11000mP.S.
Example 2
The embodiment provides a transparent high-temperature sintered silver paste, which comprises 15kg of silver powder, 60kg of polyamide/polyaniline conductive mixture, 15kg of glass powder and 10kg of isophorone; in the polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is 1.
The preparation method of the transparent high-temperature sintered silver paste is the same as that in the embodiment 1, and is not described herein again.
Example 3
The embodiment provides a transparent high-temperature sintered silver paste, which comprises 20kg of silver powder, 70kg of polyamide/polyaniline conductive mixture, 3kg of glass powder and 7kg of isophorone; wherein in the polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is 1.
The preparation method of the transparent high-temperature sintered silver paste is the same as that in the embodiment 1, and the details are not repeated herein.
Example 4
The embodiment provides a transparent high-temperature sintered silver paste, which comprises 15kg of silver powder, 80kg of polyamide/polyaniline conductive mixture, 3kg of glass powder and 2kg of butyl acetic anhydride acetate; wherein in the polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is 1.
The preparation method of the transparent high-temperature sintered silver paste is the same as that in the embodiment 1, and the details are not repeated herein.
Example 5
The embodiment provides a transparent high-temperature sintered silver paste, which is different from embodiment 1 in that in a polyamide/polyaniline conductive mixture, the mass ratio of polyamide to polyaniline is 1.
Example 6
The present embodiment provides a transparent high-temperature sintered silver paste, which is different from embodiment 1 in that, in a polyamide/polyaniline conductive mixture, a mass ratio of polyamide to polyaniline is 4.
Example 7
The embodiment provides a transparent high-temperature sintered silver paste, which is different from embodiment 1 in that the particle size of mixed powder is controlled to be 3um in the preparation process, and other raw materials and steps are the same as those in embodiment 1, and are not described again.
Comparative example 1
The comparative example provides a conductive silver paste, and the raw materials comprise 75kg of silver powder, 2.5kg of glass powder, 4.5kg of resin and 18kg of organic solvent.
The glass powder is Bi 2 0 3 -CuO-SiO 2 The system is glass powder.
The resin comprises ethyl cellulose and polyamide wax, and the mass ratio of the ethyl cellulose to the polyamide wax is 3.5.
The organic solvent is terpineol, isooctanol and diethylene glycol butyl ether acetate, and the mass ratio of the terpineol, the isooctanol and the diethylene glycol butyl ether acetate is (6).
The preparation process of the conductive silver paste is as follows:
1. dissolving ethyl cellulose and polyamide wax in a mixed solvent of part of terpineol and isooctanol, and uniformly stirring to form the organic carrier, wherein in the organic solvent, the mass ratio of the sum of the mass of the ethyl cellulose and the mass of the polyamide wax to the mixed solvent is 35.
2. And dissolving silver powder, glass powder and the balance of organic solvent in the organic carrier, and uniformly dispersing the mixture by sequentially adopting mechanical stirring and grinding dispersion to obtain the conductive silver paste.
Comparative example 2
The comparative example provides a conductive silver paste, which is different from the conductive silver paste in example 1 in that polyamide is used for replacing a polyamide/polyaniline conductive mixture, and other raw materials and preparation steps are the same as those in example 1 and are not described again.
Comparative example 3
The comparative example provides a conductive silver paste, which is different from the conductive silver paste in example 1 in that polyaniline is used for replacing a polyamide/polyaniline conductive mixture, and other raw materials and preparation steps are the same as those in example 1 and are not repeated.
Test example 1
The conductive silver pastes obtained in examples 1 to 7 and comparative examples 1 to 3 were printed on a glass substrate using a screen printing technique. The printed silver paste is placed in an oven to be cured for 8min at 850 ℃.
Test example 2
The silver conductive layer obtained in test example 1 was subjected to a resistivity test and an adhesion test.
The specific test process is as follows:
and (3) resistivity testing: and (5) carrying out meter resistance test by adopting a resistance meter.
And (3) testing the adhesive force: adhesion test was performed using a 3M 600 tape, and peeling was used as a criterion for passing or failing.
The above test data are recorded in table 1.
Table 1 table of performance data of silver conductive layers
As can be seen from Table 1, the higher the silver powder content, the higher the conductivity of the silver paste, and the lower the resistivity; on the premise that the organic-conductive polymer is definite, the higher the content of the polyamide is, the higher the conductivity of the silver paste is. The higher the glass frit content, the worse the conductivity.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The transparent high-temperature sintered silver paste is characterized by comprising the following raw materials: silver powder, polyamide/polyaniline conductive mixture, glass powder and solvent.
2. The transparent high-temperature sintered silver paste according to claim 1, comprising the following raw materials in parts by mass: 15-20% of silver powder, 60-80% of polyamide/polyaniline conductive mixture, 3-15% of glass powder and 2-22% of solvent.
3. The transparent high temperature sintering silver paste of claim 1 or 2, wherein the solvent comprises at least one of isophorone, butyl anhydride acetate, diethylene glycol butyl ether acetate, and diethylene glycol ethyl ether acetate.
4. The transparent high-temperature sintered silver paste according to claim 1 or 2, wherein the mass ratio of polyamide to polyaniline in the polyamide/polyaniline conductive mixture is (1-4): 5.
5. The preparation method of the transparent high-temperature sintered silver paste according to any one of claims 1 to 4, characterized by comprising the following steps:
step A: uniformly mixing the polyamide/polyaniline conductive mixture with a solvent to obtain a polyamide/polyaniline conductive mixture solution;
and B: uniformly mixing silver powder and glass powder and then grinding to obtain mixed powder;
and C: and D, adding the mixed powder obtained in the step B into the polyamide/polyaniline conductive mixture solution obtained in the step A, and uniformly mixing to obtain the transparent high-temperature sintered silver paste.
6. The method according to claim 5, wherein in step B, the particle size of the mixed powder is not more than 4.5 μm.
7. The preparation method according to claim 5, wherein in step C, the viscosity of the transparent high-temperature sintered silver paste is 10000 mPa-s to 12000 mPa-s.
8. The use method of the transparent high-temperature sintered silver paste according to any one of claims 1 to 4, wherein the transparent high-temperature sintered silver paste is printed on a device and then sintered to obtain a silver conductive layer.
9. The use according to claim 8, wherein the sintering temperature is 700 ℃ -950 ℃;
preferably, the sintering time is 5min to 10min.
10. Use of the transparent high temperature sintered silver paste according to any one of claims 1-4 or the transparent high temperature sintered silver paste prepared by the preparation method according to any one of claims 5-7 in a PCB (printed circuit board), a microelectronic or a solar panel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310174119.XA CN115954136A (en) | 2023-02-28 | 2023-02-28 | Transparent high-temperature sintered silver paste and preparation method, use method and application thereof |
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| CN202310174119.XA CN115954136A (en) | 2023-02-28 | 2023-02-28 | Transparent high-temperature sintered silver paste and preparation method, use method and application thereof |
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| CN115954136A true CN115954136A (en) | 2023-04-11 |
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| CN202310174119.XA Pending CN115954136A (en) | 2023-02-28 | 2023-02-28 | Transparent high-temperature sintered silver paste and preparation method, use method and application thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05105828A (en) * | 1991-10-16 | 1993-04-27 | Matsushita Electric Works Ltd | Conductive paste |
| KR20110079173A (en) * | 2009-12-31 | 2011-07-07 | 조규진 | Conductivity polymer hybrid ink composition of low temperature plasticity and ultra low cost for roll to roll printing |
| CN102163471A (en) * | 2010-11-29 | 2011-08-24 | 马洋 | Compound electrode paste for solar battery and preparation method of compound electrode paste |
| CN104505151A (en) * | 2014-12-16 | 2015-04-08 | 安徽凤阳德诚科技有限公司 | Chromium-containing high-dispersity conductive silver paste |
| CN104650653A (en) * | 2013-11-22 | 2015-05-27 | 苏州冷石纳米材料科技有限公司 | Nano-conductive silver paste and preparation method thereof |
| CN105741904A (en) * | 2014-12-09 | 2016-07-06 | 湖南利德电子浆料股份有限公司 | Touch screen silver paste doped with polyaniline |
-
2023
- 2023-02-28 CN CN202310174119.XA patent/CN115954136A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05105828A (en) * | 1991-10-16 | 1993-04-27 | Matsushita Electric Works Ltd | Conductive paste |
| KR20110079173A (en) * | 2009-12-31 | 2011-07-07 | 조규진 | Conductivity polymer hybrid ink composition of low temperature plasticity and ultra low cost for roll to roll printing |
| CN102163471A (en) * | 2010-11-29 | 2011-08-24 | 马洋 | Compound electrode paste for solar battery and preparation method of compound electrode paste |
| CN104650653A (en) * | 2013-11-22 | 2015-05-27 | 苏州冷石纳米材料科技有限公司 | Nano-conductive silver paste and preparation method thereof |
| CN105741904A (en) * | 2014-12-09 | 2016-07-06 | 湖南利德电子浆料股份有限公司 | Touch screen silver paste doped with polyaniline |
| CN104505151A (en) * | 2014-12-16 | 2015-04-08 | 安徽凤阳德诚科技有限公司 | Chromium-containing high-dispersity conductive silver paste |
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