CN114420342A - Low-VOCs touch screen silver paste and preparation method thereof - Google Patents
Low-VOCs touch screen silver paste and preparation method thereof Download PDFInfo
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- CN114420342A CN114420342A CN202110893261.0A CN202110893261A CN114420342A CN 114420342 A CN114420342 A CN 114420342A CN 202110893261 A CN202110893261 A CN 202110893261A CN 114420342 A CN114420342 A CN 114420342A
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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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- 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
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Abstract
The invention relates to a low-VOCs touch screen silver paste and a preparation method thereof, wherein the low-VOCs touch screen silver paste comprises the following raw material components in parts by weight: 7-15 parts of epoxy resin, 2-5 parts of hyperbranched epoxy resin, 5-15 parts of reactive diluent, 1-3 parts of curing agent, 1-3 parts of assistant and 60-80 parts of silver powder. The low-VOCs touch screen silver paste provided by the invention is small in curing and volatilization, has excellent printing property, conductivity and adhesive force on various film materials, and is particularly suitable for glass touch screens.
Description
Technical Field
The silver paste has excellent printing property, conductivity and adhesive force on various base materials, is suitable for a glass base material process, and has good fluidity and leveling property.
Background
The touch screen has a very wide application range in China, and is mainly used for inquiring mobile phones, computers, vehicle-mounted central control and public information; such as business inquiry of departments of telecommunication bureau, tax bureau, bank, electric power and the like; inquiring information of city streets; in addition, the system is applied to leadership office work, industrial control, military command, electronic games, song and dish ordering, multimedia teaching, real estate pre-sale and the like. In the future, touch screens are also required to be walked into the home. The touch screen conductive silver paste is specially designed for the loop wires of the resistance type and the capacitance type touch screens, and the working principle is as follows: a circuit pattern is formed through screen printing, and then organic solvent in silver paste is volatilized and resin is shrunk through heating and curing, so that gaps among silver powder are reduced, and conductivity is formed. Currently, organic solvents such as DBE, butyl carbitol, diethyl acetate oxalate, dimethyl adipate and the like are commonly adopted in printing silver paste on the market. The solvent can volatilize into the air in the production process, so that the silver content of the silver paste after solidification is greatly improved, and further the silver paste circuit with good electric conduction is obtained. However, the volatilization of the organic solvent causes serious environmental pollution. With the implementation of the national environmental protection policy, the popularization and implementation of concepts such as green manufacturing, clean production, ecological design and the like are realized. The situation that the content of VOCs in the touch screen silver paste is too high is eliminated gradually.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the touch screen silver paste which takes the low-viscosity epoxy resin as the main body resin, is modified by the hyperbranched epoxy resin and has the viscosity adjusted by a small amount of reactive diluent to replace the traditional touch screen silver paste containing a large amount of high-boiling-point solvent. And a small amount of active diluent is used as a solvent to reduce the release of VOCs gas in the using process. The hyperbranched epoxy resin and the low-viscosity epoxy resin are used as main resin, are more easily dissolved in a diluent, and the curing system has higher crosslinking density, can effectively resist the corrosion of severe cold and hot environments, salt mist and sweat, and achieves the aim of weather resistance. Meanwhile, the toughness of hyperbranched polymer molecules and the use of flaky silver powder with small particle size can improve the conductivity of the silver paste
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
7-15 parts of epoxy resin, 2-5 parts of hyperbranched epoxy resin, 5-15 parts of reactive diluent, 1-3 parts of curing agent, 1-3 parts of assistant and 60-80 parts of silver powder.
Preferably, the epoxy resin comprises one or a mixture of a plurality of alicyclic epoxy resin, hydrogenated epoxy resin and novolac epoxy resin, wherein the mixture has a viscosity of less than 4000 mpas;
preferably, the hyperbranched epoxy resin comprises but is not limited to one or a mixture of polyester type hyperbranched epoxy resin, aromatic polyester polyether hyperbranched epoxy resin and aliphatic hyperbranched epoxy resin.
Preferably, the reactive diluent comprises but is not limited to one or a mixture of more of 1, 4-butanediol diglycidyl ether and polypropylene glycol diglycidyl ether.
Preferably, the curing agent includes but is not limited to one or a mixture of several of cationic epoxy curing agent, diethylenetriamine-acrylonitrile adduct, organic acid hydrazide, boron trifluoride-ammonia complex, and diaminomaleonitrile derivative.
Preferably, the auxiliary agent includes but is not limited to one or more of a coupling agent, a thixotropic agent, a leveling agent, a conductive agent and an antifoaming agent.
Preferably, the silver powder is plate-like silver powder, the average particle diameter is 0.7-1.25 μm, the tap density is 3.5-4.5g/ml, and the specific surface area is 1.6-2.2 square meters/g.
The invention also provides a preparation method of the touch screen silver paste, which comprises the following steps:
s1: adding epoxy resin and hyperbranched epoxy resin into an active diluent, heating and stirring until the resin is completely dissolved, then filtering, and cooling the collected filtrate to room temperature to obtain a resin dispersion;
s2: adding auxiliary agents such as curing agents, coupling agents and the like into the resin dispersion liquid, and uniformly stirring; then uniformly dispersing by three-roller grinding to obtain a silver paste precursor;
s3: adding silver powder into the precursor, uniformly stirring, grinding by using a three-roll grinder, performing rotary defoaming, and filtering to obtain the conductive silver paste.
Preferably, in S1, the heating temperature is 80 ℃, the stirring time is 6 hours, the filter screen used for filtering is a 400-mesh filter screen, and the filter screen is a polyester screen. In S2, the rotating speed of the dispersion is 50-300 r/min, and the dispersion time is 10 min; in S3, the rotating speed of dispersion is 50-300 r/min, the dispersion time is 5min, three-roller grinding is adopted for grinding, the fineness of the ground mixture is not more than 5 microns, the rotary defoaming parameter is 3min800-1600r/min, the rotary defoaming vacuum degree is less than-0.08 MPa, the filter screen adopted for filtering is a 400-mesh filter screen, and the filter screen is a stainless steel screen.
The invention also protects silver paste on a touch screen, and particularly relates to low-VOCs touch screen silver paste and preparation thereof.
The technical scheme provided by the invention has the following beneficial effects:
aiming at the defects in the prior art, the invention aims to provide the touch screen silver paste which takes the low-viscosity epoxy resin as the main body resin, is modified by the hyperbranched epoxy resin and has the viscosity adjusted by a small amount of reactive diluent to replace the traditional touch screen silver paste containing a large amount of high-boiling-point solvent. And a small amount of active diluent is used as a solvent to reduce the release of VOCs gas in the using process. The polyester hyperbranched epoxy resin and the low-viscosity epoxy resin are used as main resin, are more easily dissolved in a diluent, and the curing system has higher crosslinking density, can effectively resist the corrosion of severe cold and hot environments, salt mist and sweat, and achieves the aim of weather resistance. Meanwhile, the toughness of hyperbranched polymer molecules and the use of flaky silver powder with small particle size can improve the conductivity of the silver paste
(1) According to the touch screen silver paste provided by the invention, low-viscosity epoxy resin is used as main resin, the hyperbranched epoxy resin is modified, a small amount of reactive diluent is used for adjusting the viscosity, the traditional touch screen silver paste containing a large amount of high-boiling-point solvent is replaced, the release of VOCs in the production process is less than 10%, and the harm to production personnel and environment is small;
(2) according to the touch screen silver paste provided by the invention, the hyperbranched epoxy resin and the low-viscosity epoxy resin are used as main resins, and the curing system has higher crosslinking density, can effectively resist the corrosion of severe cold and hot environments, salt mist and sweat, and achieves the purpose of weather resistance;
(3) according to the touch screen silver paste provided by the invention, the electric conductivity of the silver paste is improved through the toughness of the hyperbranched polymer molecules and the flaky silver powder with small particle size.
(4) The touch screen silver paste provided by the invention is cured at low temperature, has excellent printing property, conductivity and adhesive force on various base materials, is suitable for a glass base material process, and has good fluidity and leveling property.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following will clearly and completely describe the embodiments of the present invention. The following examples are merely for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
The experimental procedures in the following examples are conventional unless otherwise specified. The test materials used in the following examples were purchased from conventional companies or stores unless otherwise specified. In the quantitative tests in the following examples, three replicates were set up, and the data are the mean or mean ± standard deviation of the three replicates.
7-15 parts of epoxy resin, 2-5 parts of hyperbranched epoxy resin, 5-15 parts of reactive diluent, 1-3 parts of curing agent, 1-3 parts of assistant and 60-80 parts of silver powder.
Wherein, the epoxy resin comprises but is not limited to one or a mixture of more of alicyclic epoxy resin, hydrogenated epoxy resin and novolac epoxy, and the viscosity of the mixture is lower than 4000 mpas;
the hyperbranched epoxy resin comprises but is not limited to one or a mixture of polyester hyperbranched epoxy resin, aromatic polyester polyether hyperbranched epoxy resin and aliphatic hyperbranched epoxy resin. The polyester type hyperbranched epoxy resin can be prepared by taking trimethylolpropane and dimethylolpropionic acid as reaction monomers, synthesizing hydroxyl-terminated hyperbranched polyester through self-polycondensation, and then performing epoxidation modification on the hydroxyl-terminated group with epichlorohydrin.
The reactive diluent comprises but is not limited to one or a mixture of more of 1, 4-butanediol diglycidyl ether and polypropylene glycol diglycidyl ether;
the curing agent comprises but is not limited to one or a mixture of more of cationic epoxy curing agent, diethylenetriamine-acrylonitrile adduct, organic acid hydrazide, boron trifluoride-ammonia complex and diamino maleonitrile derivative;
the auxiliary agent comprises one or more of but not limited to a coupling agent, a thixotropic agent, a leveling agent, a conductive agent and an antifoaming agent;
the silver powder is flake silver powder, the average particle diameter is 0.5-5 mu m, the tap density is 1-5g/ml, the specific surface area is 0.2-2.5 square meters/g, the preferred average particle diameter is 0.7-1.25 mu m, the tap density is 3.5-4.5g/ml, and the specific surface area is 1.6-2.2 square meters/g.
In addition, the invention also provides a preparation method of the conductive silver paste, which comprises the following steps:
s1: adding low-viscosity epoxy resin and polyester type hyperbranched epoxy resin into an active diluent, heating and stirring for 6 hours at 80 ℃, then filtering by adopting a 400-mesh polyester net, and cooling the collected filtrate to room temperature to obtain a resin dispersion;
s2: adding auxiliary agents such as curing agents, coupling agents and the like into the resin dispersoid, and dispersing at a high speed of 50-300 r/min for 10 min; then uniformly dispersing by three-roller grinding to obtain a silver paste precursor; (ii) a
S3: adding silver powder into the precursor, dispersing for 5min at a high speed, grinding the obtained mixture for 5-7 times by using three rollers to ensure that the fineness of the ground mixture is not more than 5 microns, then using a revolution and rotation rotary defoaming machine for 3min1600r/min to perform rotary defoaming, wherein the rotary defoaming vacuum degree is less than-0.08 MPa, and filtering by using a 400-mesh stainless steel net to obtain the touch screen silver paste.
The touch screen silver paste and the preparation method thereof provided by the invention are further explained by combining specific embodiments.
Example one
The embodiment provides a touch screen silver paste, and the raw material components include by weight: 10 parts of bisphenol F type epoxy ED-509S epoxy resin, 2 parts of polyester type hyperbranched epoxy resin, 11 parts of 1, 4-butanediol glycidyl ether, 1 part of hexafluoroantimonate, 0.8 part of fumed silica, 0.2 part of silane coupling agent and 75 parts of flake silver powder with the average particle size of 2 microns.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the conductive silver paste:
s1: adding low-viscosity epoxy resin and polyester type hyperbranched epoxy resin into an active diluent, heating and stirring for 6 hours at 80 ℃, then filtering by adopting a 400-mesh polyester net, and cooling the collected filtrate to room temperature to obtain a resin dispersion; s2: adding auxiliary agents such as curing agents, coupling agents and the like into the resin dispersion liquid, and dispersing at a high speed of 50-300 r/min for 10 min; then uniformly dispersing by three-roller grinding to obtain a silver paste precursor; s3: adding silver powder into the precursor, dispersing for 5min at a high speed, grinding the obtained mixture for 5-7 times by using three rollers to ensure that the fineness of the ground mixture is not more than 5 microns, then using a revolution, rotation and rotation defoaming machine for 3min1600r/min to perform rotary defoaming, wherein the rotary defoaming vacuum degree is less than-0.08 MPa, and filtering by using a 400-mesh stainless steel net to obtain the touch screen silver paste.
Example two
The embodiment provides a touch screen silver paste, and the raw material components include by weight: 12 parts of NPEF-170 phenolic epoxy resin, 2 parts of polyester hyperbranched epoxy resin, 11 parts of 1, 4-butanediol glycidyl ether, 1 part of hexafluoroantimonate, 0.8 part of fumed silica, 0.2 part of silane coupling agent and 73 parts of flake silver powder with the average particle size of 2 microns.
According to the raw materials, the preparation method provided by the invention is adopted to prepare the conductive silver paste:
s1: adding low-viscosity epoxy resin and polyester type hyperbranched epoxy resin into an active diluent, heating and stirring for 6 hours at 80 ℃, then filtering by adopting a 400-mesh polyester net, and cooling the collected filtrate to room temperature to obtain a resin dispersion; s2: adding auxiliary agents such as curing agents, coupling agents and the like into the resin dispersion liquid, and dispersing at a high speed of 50-300 r/min for 10 min; then uniformly dispersing by three-roller grinding to obtain a silver paste precursor; s3: adding silver powder into the precursor, dispersing for 5min at a high speed, grinding the obtained mixture for 5-7 times by using three rollers to ensure that the fineness of the ground mixture is not more than 5 microns, then using a revolution, rotation and rotation defoaming machine for 3min1600r/min to perform rotary defoaming, wherein the rotary defoaming vacuum degree is less than-0.08 MPa, and filtering by using a 400-mesh stainless steel net to obtain the touch screen silver paste.
After being cured, the conductive silver paste prepared in the first embodiment to the second embodiment of the invention is subjected to conductivity test and weather resistance test.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains. Unless specifically stated otherwise, the relative steps, numerical expressions, and values of the components and steps set forth in these embodiments do not limit the scope of the present invention. In all examples shown and described herein, unless otherwise specified, any particular value should be construed as merely illustrative, and not restrictive, and thus other examples of example embodiments may have different values.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
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; 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, and all of the technical solutions are covered in the protective scope of the present invention.
Claims (9)
1. The low-VOCs touch screen silver paste is characterized by comprising the following raw material components in parts by weight: 7-15 parts of epoxy resin, 2-5 parts of hyperbranched epoxy resin, 5-15 parts of reactive diluent, 1-3 parts of curing agent, 1-3 parts of assistant and 60-80 parts of silver powder.
2. The silver paste for a touch screen with low VOCs according to claim 1, wherein the epoxy resin includes but is not limited to one or more of alicyclic epoxy resin, hydrogenated epoxy resin and novolac epoxy, and the mixture of the alicyclic epoxy resin, the hydrogenated epoxy resin and the novolac epoxy resin has a viscosity of less than 4000 mpas.
3. The low-VOCs touch screen silver paste of claim 1, wherein the hyperbranched epoxy resin includes but is not limited to one or a mixture of polyester type hyperbranched epoxy resin, aromatic polyester polyether hyperbranched epoxy resin, and aliphatic hyperbranched epoxy resin.
4. The low-VOCs touch screen silver paste of claim 1, wherein the reactive diluent includes, but is not limited to, one or a mixture of 1, 4-butanediol diglycidyl ether and polypropylene glycol diglycidyl ether.
5. The low-VOCs touch screen silver paste of claim 1, wherein the curing agent includes, but is not limited to, one or more of a cationic epoxy curing agent, diethylenetriamine-acrylonitrile adduct, organic acid hydrazide, boron trifluoride-ammonia complex, and diaminomaleonitrile derivative.
6. The low-VOCs touch screen silver paste of claim 1, wherein the additives include, but are not limited to, one or more of coupling agents, thixotropic agents, leveling agents, conductive agents, and defoaming agents.
7. The touch screen silver paste with low VOCs (volatile organic compounds) according to claim 1, wherein the silver powder is a flake silver powder, the average particle size is 0.5-5 μm, the tap density is 1-5g/ml, the specific surface area is 0.2-2.5 square meters per gram, the preferred average particle size is 0.7-1.25 μm, the tap density is 3.5-4.5g/ml, and the specific surface area is 1.6-2.2 square meters per gram.
8. The preparation method of the low-VOCs touch screen silver paste is characterized by comprising the following steps:
s1: adding low-viscosity epoxy resin and hyperbranched epoxy resin into an active diluent, heating and stirring until the resin is completely dissolved, then filtering, and cooling the collected filtrate to room temperature to obtain a resin dispersion;
s2: adding auxiliary agents such as curing agents, coupling agents and the like into the resin dispersoid, and uniformly stirring; then uniformly dispersing by three-roller grinding to obtain a silver paste precursor;
s3: adding silver powder into the precursor, uniformly stirring, grinding by using a three-roll grinder, performing rotary defoaming, and filtering to obtain the conductive silver paste.
9. The method for preparing conductive silver paste according to claim 8, wherein the method comprises the following steps:
in S1, the heating temperature is 80 ℃, the stirring time is 6 hours, the filter screen used for filtering is a 400-mesh filter screen, and the filter screen is a polyester screen;
in S2, the rotating speed of the dispersion is 50-300 r/min, and the dispersion time is 10 min;
in S3, the rotating speed of dispersion is 50-300 r/min, the dispersion time is 5min, three-roller grinding is adopted for grinding, the fineness of the ground mixture is not more than 5 microns, the rotary defoaming parameter is 3min800-1600r/min, the rotary defoaming vacuum degree is less than-0.08 MPa, the filter screen adopted for filtering is a 400-mesh filter screen, and the filter screen is a stainless steel mesh.
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| CN202110893261.0A CN114420342A (en) | 2021-08-04 | 2021-08-04 | Low-VOCs touch screen silver paste and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016179769A1 (en) * | 2015-05-11 | 2016-11-17 | 深圳华力兴新材料股份有限公司 | Hyperbranched resin-toughened pbt engineering plastic composition |
| CN108133767A (en) * | 2017-12-18 | 2018-06-08 | 深圳市思迈科新材料有限公司 | Weatherability glass touch screen conductive silver paste and preparation method thereof |
| CN111446020A (en) * | 2019-01-16 | 2020-07-24 | 北京氦舶科技有限责任公司 | Conductive silver paste, preparation method thereof and metal grid conductive film |
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- 2021-08-04 CN CN202110893261.0A patent/CN114420342A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016179769A1 (en) * | 2015-05-11 | 2016-11-17 | 深圳华力兴新材料股份有限公司 | Hyperbranched resin-toughened pbt engineering plastic composition |
| CN108133767A (en) * | 2017-12-18 | 2018-06-08 | 深圳市思迈科新材料有限公司 | Weatherability glass touch screen conductive silver paste and preparation method thereof |
| CN111446020A (en) * | 2019-01-16 | 2020-07-24 | 北京氦舶科技有限责任公司 | Conductive silver paste, preparation method thereof and metal grid conductive film |
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