CN114512263A - High-impedance anti-heterochromatic conductive silver paste and preparation method thereof - Google Patents
High-impedance anti-heterochromatic conductive silver paste and preparation method thereof Download PDFInfo
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
The invention discloses a high-impedance heterochromatic conductive silver paste and a preparation method thereof, wherein the conductive silver paste comprises the following raw materials: resin, a coupling agent, a flow assistant, conductive powder and a resistance assistant for resisting heterochromous rise. The invention has the beneficial effects that: the conductive silver paste disclosed by the invention has excellent anti-heterochrosis and resistance-raising effects by using the anti-heterochrosis resistance-raising auxiliary agent, and can avoid carbon-based conductive substances used by conventional high-resistance paste, so that the color is kept to be attractive silvery white, and fillers such as silicon dioxide, calcium carbonate, bentonite, hydrotalcite and other hard non-conductive substances are avoided, so that the silver paste has good flexibility. The addition of the discoloration-resistant and discoloration-resistant resistance-increasing assistant in the high-impedance discoloration-resistant conductive silver paste can greatly improve the discoloration behavior of silver, so that the obtained silver paste has excellent corrosion-resistant and discoloration-resistant effects, and the conductivity of the silver paste can be adjusted by adjusting the addition amount of the discoloration-resistant and discoloration-resistant resistance-increasing assistant.
Description
Technical Field
The invention belongs to the technical field of conductor materials, and particularly relates to high-impedance heterochromatic conductive silver paste and a preparation method thereof.
Background
Since the 50 s of the 20 th century, with the progress and development of semiconductor technology, the rise of silicon-based semiconductor technology has greatly pushed the development of information technology industry, resulting in great changes in people's lives. However, with the acceleration of the world informatization process and the development of the internet of things, flexible and wearable electronic products have attracted more and more interest and become popular products pursued by the industry, such as: the device comprises a flexible wearable heating device, a flexible wearable massage device, a flexible wearable health information monitoring device and the like.
Compared with rigid silicon-based electronic devices, flexible electronic devices have many unique and superior properties, such as high flexibility, ultra-light weight, and conformality, which make flexible and wearable electronic devices more widely used. At the same time, the industry's pursuit of the aesthetics of flexible electronics is also increasing, and in particular, people are inventing new devices to consistently provide functional output as aesthetically as possible and comfortable for heating, massaging, monitoring functional flexibility and wearable medical devices that are used to provide beneficial help to human health on a regular and continuous basis.
Especially, in wearable heating devices using a large amount of high-resistance conductive paste printing devices as core functions, carbon-based high-resistance paste such as: graphite type high resistance thick liquids, carbon black type high resistance thick liquids, graphite alkene type high resistance thick liquids, carbon nanotube type high resistance thick liquids, carbon system composite high resistance thick liquids, in product design and use, product development company and customer all put forward higher requirement to the outward appearance is pleasing to the eye, comparatively exclude carbon series's black thick liquids, require to use silver thick liquids to beautify the outward appearance as far as, if: conductive silver paste, but two types of outstanding problems are found in the use process of the existing conductive silver paste: firstly, conductive silver paste is easy to discolor: in the subsequent testing process of the noble metal silver paste device, the silver paste is found to have yellow, brown, gray and black color changes in the testing process of 85-85% RH, salt fog, sweat, cold and hot impact and room temperature air atmosphere placement, so that the aesthetic degree of the device is seriously influenced, and meanwhile, the doubtful worry and complaint of customers on the reliability of the product are easily caused; secondly, the conductive silver paste is not easy to be made into high impedance: the conductivity of the conventional conductive silver paste on the market is most common between 5m omega/sq/mil and 50m omega/sq/mil, and is 1 multiplied by 104mΩ/sq/mil-2×106Ultra-high impedance silver paste of m omega/sq/mil is extremely rare.
In view of the above two problems of high-impedance silver paste, a great deal of research has been made by the majority of practitioners, such as: an anti-oxidation low-temperature conductive silver paste and a preparation method thereof, application No. 202011183957.6, an anti-heterochrosis low-temperature conductive silver paste and a preparation method thereof, wherein the silver paste disclosed by application No. 202011240204.4 has excellent anti-heterochrosis effect, but the resistance of the silver paste is low, and the silver paste cannot be used as a high-resistance silver paste generating heat, and meanwhile, if the resistance is improved by reducing the silver content, the silver content is low, the continuity of the silver powder in the paste is poor, and the paste performance stability is poor; if the resistance of the silver paste is improved by adding the non-conductive powder, the continuity of the conductive phase in the paste is also deteriorated after a large amount of hard insulating powder is added, so that the batch stability of the silver paste printing device is poor, and the overall flexibility and stretchability of the device are poor; if the resistance of the silver paste is regulated and controlled by adding the carbon conductive filler, the color of the silver paste is grayed, blacked and not beautiful, and the development of the high-silver flexible and stretchable silver paste which does not use the carbon conductive filler, does not use hard non-conductive powder and has high resistance and heterochrosis resistance and silvery white is urgent.
Disclosure of Invention
The invention aims to provide the high-impedance heterochromatic-resistant conductive silver paste which is high in resistance after being cured and good in flexibility and tensile property.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-impedance heterochromatic conductive silver paste comprises the following raw materials in parts by weight: 5-10 parts of resin, 0.5-1 part of coupling agent, 10-30 parts of flow assistant, 50-80 parts of conductive powder and 2-10 parts of resistance-change-rise resistance assistant.
The silver paste is a bonding composition taking resin bonded silver powder as a final product in an expression form, and the resin and the auxiliary agent with excellent comprehensive flexibility enable a high-molecular phase of the silver paste to have excellent flexibility, so that a foundation is provided for development of the silver paste with high flexibility.
As a preferred embodiment, the resin is at least one of polyurethane resin, vinyl chloride-vinyl acetate resin, polyacrylate, EVA resin, PVB resin, polybutadiene, polyester, hydrogen-containing silicone oil, vinyl silicone resin and liquid silicone rubber. Of the resins we prefer the resin with the greater elongation at break, which has excellent elasticity and requires lower force under the same tension, thus providing flexibility.
As a preferred embodiment, the coupling agent is at least one of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent and a fluorosilane coupling agent. The coupling agent can generate stronger interaction with resin even generates chemical reactions such as ester exchange and the like, and different final effects can be generated due to different mechanisms, for example, the titanium-containing coupling agent can improve the flexibility of the silver paste and the like. The interaction between the powder and the polymer can be regulated and controlled according to different elements and group compositions of the coupling agent, for example, the fluorine-containing coupling agent has the characteristics of reducing the interaction between the powder and the polymer, reducing the friction force and the like.
As a preferred embodiment, the flow aid is at least one of white gasoline, kerosene, heptane, octane, undecane, dodecane, cyclohexanone, isophorone, ethylene glycol methyl ether, dipropylene glycol methyl ether, diethylene glycol dimethyl ether, diethylene glycol butyl ether, propylene glycol methyl ether acetate, diethylene glycol ethyl ether acetate, ethylene glycol butyl ether acetate, dimethyl adipate, diethyl adipate, DBE, dibasic ester, N-methylpyrrolidone or terpineol.
As a preferred embodiment, the conductive powder comprises flake conductive powder and spherical conductive powder, wherein the flake conductive powder is silver powder, and the spherical conductive powder is at least one of pure silver powder, silver-coated nickel powder, silver-coated copper powder, silver-coated aluminum powder and silver-plated glass powder; the weight ratio of the flaky conductive powder to the spherical conductive powder is 7: 3-9: 1.
the silver powder with smooth surface is selected, so that the friction force between the silver powder and the silver powder quality inspection can be reduced, and meanwhile, the small-particle-size spherical conductive particles are added among the flaky conductive powder, so that the contact efficiency of the conductive filler can be improved, and the conductive powder can keep a good conductive path when moving relatively.
The conventional preparation method of the silver powder comprises the following steps: dissolving silver nitrate in a medium, adding a reducing agent (hydrazine hydrate and the like) and adding a morphology inducing aid (components such as PVP and the like), reducing silver particles with different diameters and morphologies, adding different grinding aids (auxiliaries such as stearic acid and the like) through different ball milling processes, and shaping the silver powder to obtain commonly used silver particles with different diameters and different morphologies, such as: flake, spherical silver powder particles.
As a preferred embodiment, the resistance-change-increasing resistance assistant is at least one of benzotriazole, methylbenzotriazole, aminotriazole, aminotetrazole, lauryl mercaptan, hexadecylmercaptan, mercaptobenzene, 2-mercaptobenzothiazole, stearic acid, and ethylene glycol monostearate.
The second aspect of the invention provides a preparation method of high-impedance heterochromatic conductive silver paste, which comprises the following steps:
(1) mixing and stirring the raw materials uniformly to obtain a mixture;
(2) and grinding the mixture, and filtering to obtain the high-impedance heterochromatic conductive silver paste.
As a preferred embodiment, in the step (1), the mixing and stirring speed is 100-1500r/min, and the mixing and stirring time is 5-100 min; in the step (2), the fineness of the high-impedance heterochromatic conductive silver paste is 3-25 μm.
When silver reacts, the silver ions are generated by corrosion and electrochemical reaction preferentially from active reaction sites on the surface of the silver powder, if a corresponding measure is adopted to react with the silver ions in preference to oxygen, sulfur and chlorine, the color change behavior of the silver can be greatly improved, for example, benzotriazole can interact with the silver ions to form an insoluble complex film which is deposited on the surface of the silver layer, so that the silver has excellent corrosion resistance and heterochrosis resistance effects, and meanwhile, because the compounds can react with a large amount of silver, the obtained silver complex has poor conductivity, so that the use amount is optimized, silver paste products with different conductivities under the same silver content, especially high-resistance silver paste under the high silver content can be obtained by regulating and controlling.
The invention has the beneficial effects that: the high-impedance heterochromatic-color-resistant conductive silver paste disclosed by the invention has heterochromatic-color-resistant and resistance-increasing effects by using the heterochromatic-color-resistant resistance-increasing auxiliary agent, and can avoid carbon-based conductive substances used by conventional resistance-increasing resistance paste, so that the color is kept to be beautiful silvery white, and fillers such as hard non-conductive substances such as silicon oxide, calcium carbonate, bentonite, hydrotalcite and the like are avoided from being used, so that the silver paste has good flexibility.
The addition of the resistance-change and resistance-increase assistant for the high-impedance heterochromatic conductive silver paste can greatly improve the color-change behavior of silver, so that the obtained silver paste has excellent corrosion-resistant and heterochromatic-resistant effects, the conductivity of the silver paste can be adjusted by adjusting the addition amount of the resistance-change and resistance-increase assistant, and thus the high-impedance conductive silver paste with high silver content is obtained, and meanwhile, the use of carbon materials can be avoided, so that attractive silvery white is obtained, and the addition of hard non-conductive fillers can also be avoided, so that the flexibility of the silver paste is greatly improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The types of polyurethane resin are as follows: luobu Pearlstick 5703; the EVA resin has the following types: chemical Tri-well 40W; the types of the vinyl chloride-vinyl acetate copolymer resin are as follows: threca VAGH 003; the polyacrylate type is: mitsubishi yang LR 65S.
Example 1
The high-impedance heterochromatic conductive silver paste comprises the following raw materials in parts by weight: 5 parts of polyurethane resin, 0.5 part of silane coupling agent, 10 parts of DBE, 50 parts of conductive powder and 2 parts of benzotriazole;
the conductive powder comprises the following components in percentage by weight: 3, the flake conductive powder is silver powder, and the spherical conductive powder is pure silver powder.
The preparation method of the high-impedance anti-heterochrosis conductive silver paste in the embodiment 1 comprises the following steps:
(1) putting resin, a coupling agent, a flow assistant, conductive powder and an anti-discoloration resistance-increasing assistant into a double-planet stirring device, and mixing and stirring for 100min at a stirring speed of 100r/min to obtain a mixture;
(2) and (3) grinding the mixture on a three-roller machine, and filtering to obtain the high-impedance heterochromatic-resistant conductive silver paste with the fineness of 20 mu m.
Example 2
The difference between the high-resistance anti-discoloration conductive silver paste of example 2 and the high-resistance anti-discoloration conductive silver paste of example 1 is: the high-impedance anti-heterochrosis conductive silver paste in the embodiment 2 contains 10 parts by weight of benzotriazole.
Example 3
The high-impedance heterochromatic conductive silver paste comprises the following raw materials in parts by weight: 8 parts of polyacrylate, 2 parts of titanate coupling agent, 4 parts of isophorone, 16 parts of DBE, 65 parts of conductive powder and 6 parts of methylbenzotriazole;
the conductive powder comprises the following components in percentage by weight: 3, the flaky conductive powder is silver powder, and the spherical conductive powder is silver-coated copper powder.
The preparation method of the high-impedance anti-heterochrosis conductive silver paste in the embodiment 3 comprises the following steps:
(1) putting resin, a coupling agent, a flow assistant, conductive powder and an anti-discoloration resistance-increasing assistant into a double-planet stirring device, and mixing and stirring for 50min at a stirring speed of 1000r/min to obtain a mixture;
(2) and (3) grinding the mixture on a three-roller machine, and filtering to obtain the high-impedance heterochromatic-resistant conductive silver paste with the fineness of 10 mu m.
Example 4
A high-impedance heterochromatic conductive silver paste comprises the following raw materials in parts by weight: 5 parts of EVA resin, 2 parts of fluorosilane coupling agent, 16 parts of isophorone, 65 parts of conductive powder and 7 parts of 2-mercaptobenzothiazole;
the conductive powder is 9: 1, the flaky conductive powder is silver powder, and the spherical conductive powder is silver-coated aluminum powder.
The preparation method of the high-resistance anti-heterochrosis conductive silver paste described in the embodiment 4 is the same as that of the high-resistance anti-heterochrosis conductive silver paste described in the embodiment 3.
Example 5
The high-impedance heterochromatic conductive silver paste comprises the following raw materials in parts by weight: 7 parts of hydrogen-containing silicone oil, 3 parts of vinyl silicone resin, 2 parts of platinum water, 1 part of aluminate coupling agent, 30 parts of octane, 80 parts of conductive powder and 10 parts of aminotriazole;
the conductive powder comprises the following components in percentage by weight: 1, the flake conductive powder is silver powder, and the spherical conductive powder is pure silver powder.
The preparation method of the high-impedance anti-heterochrosis conductive silver paste in the embodiment 5 comprises the following steps:
(1) putting the resin, the coupling agent, the flow assistant, the conductive powder and the resistance-change-increasing resistance assistant into a double-planet stirring device, and mixing and stirring for 5min at a stirring speed of 1500r/min to obtain a mixture;
(2) and grinding the mixture on a three-roller machine, and filtering to obtain the high-impedance heterochromatic conductive silver paste with the fineness of 25 micrometers.
Comparative example 1
The high-impedance anti-heterochromatic conductive silver paste of comparative example 1 is different from the conductive silver paste of example 1 in that: the conductive silver paste described in comparative example 1 does not contain a resistance-increasing aid for discoloration of the raw material.
Comparative example 2
The high-impedance anti-heterochromatic conductive silver paste of comparative example 2 is different from the conductive silver paste of example 3 in that: the conductive silver paste of comparative example 2 uses carbon black instead of the resistance-to-discoloration and resistance-increasing assistant.
Comparative example 3
The high-impedance anti-heterochromatic conductive silver paste of comparative example 3 is different from the conductive silver paste of example 4 in that: the conductive silver paste in comparative example 3 adopts silicon oxide to replace the resistance-change and resistance-increase assistant.
Comparative example 4
The high-resistance anti-heterochrosis conductive silver paste in the comparative example 4 is different from the high-resistance anti-heterochrosis conductive silver paste in the example 1 in that: the weight part of benzotriazole in the high-impedance anti-heterochromatic conductive silver paste in comparative example 4 is 0.5 part.
Comparative example 5
The difference between the high resistance anti-heterochromatic conductive silver paste of comparative example 5 and the high resistance anti-heterochromatic conductive silver paste of example 1 is that: the high-impedance anti-heterochrosis conductive silver paste in the comparative example 5 contains 15 parts by weight of benzotriazole.
The invention discloses a performance research of a high-impedance heterochromatic-resistant conductive silver paste, which comprises the following steps:
1. study of discoloration resistance
1.1. Examples 1, 2, 3 and comparative examples 1, 2, 4, 5 were printed on a PET substrate, example 4 and comparative example 3 were printed on a TPU substrate, example 5 was printed on a silica gel substrate, baked at 130 ℃ for 30min, placed in a constant temperature and humidity chamber, treated at 85-85% RH for 72h at high temperature and high humidity, and the color change was observed.
1.2. Examples 1, 2, 3 and comparative examples 1, 2, 4, 5 were printed on a PET substrate, example 4 and comparative example 3 were printed on a TPU substrate, example 5 was printed on a silica gel substrate, baked at 130 ℃ for 30min, placed in a cold and hot impact box, and subjected to cold and hot impact for 72h at-40 ℃ to 80 ℃ to observe color change.
1.3. Examples 1, 2, 3 and comparative examples 1, 2, 4, 5 were printed on a PET substrate, example 4 and comparative example 3 were printed on a TPU substrate, example 5 was printed on a silica gel substrate, baked at 130 ℃ for 30min, placed in a salt spray laboratory box, subjected to salt spray corrosion for 72h under the conditions of neutral salt spray, 5% sodium chloride, 95% RH, and 35 ℃, and observed for color change. The results are shown in Table 1.
Table 1 research on discoloration resistance of high-impedance, discoloration-resistant conductive silver paste according to the present application
2. Conductivity testing method
Examples 1, 2 and 3 and comparative examples 1, 2, 4 and 5 were printed on a PET substrate, example 4 and comparative example 3 were printed on a TPU substrate, example 5 was printed on a silica gel substrate, and the resistance of a silver paste was obtained by calculation after measuring the line resistance, the thickness of a line silver paste and the width of the line silver paste according to the method a of appendix in GB/T17473.3-2008 "test method of a noble metal paste for microelectronics-determination of the square resistance", and the results are shown in table 2.
Table 2 study of conductivity of high-impedance anti-heterochromatic conductive silver paste of the present invention
3. Study on conductivity flexibility
3.1. The conductive silver pastes of examples 1 to 3 and comparative examples 1, 2, 4 and 5 were respectively coated on 7 PET sample strips of 5mm x 100mm by screen printing, the posts of 5mm diameter were wound, the positive and negative winding of the posts was performed once and 50 times, and the rate of change of resistance was measured after winding the posts, and the results are shown in table 3.
3.2. The conductive silver paste described in example 4 and comparative example 3 was coated on 2 TPU samples of 5mm by 100mm by screen printing, and example 5 was coated on a silica gel substrate of 10mm by 100mm by screen printing, and a column of 5mm in diameter was wound, and the resistance change rate was measured after winding the column for 50 times, and the results are shown in table 3.
3.3. The conductive silver paste of example 4 and comparative examples 1, 3 and 5 was coated on 4 TPU substrates of 10mm by 100mm by screen printing, and example 5 was coated on a silicone substrate of 10mm by 100mm by screen printing, and the length was set to 10% by stretching, and the resistance change rate after stretching by 10% and the resistance change rate after recovery were measured, and the results are shown in table 3.
TABLE 3
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (8)
1. The high-impedance heterochromatic conductive silver paste is characterized by comprising the following raw materials in parts by weight: 5-10 parts of resin, 0.5-1 part of coupling agent, 10-30 parts of flow assistant, 50-80 parts of conductive powder and 2-10 parts of resistance-change-rise resistance assistant.
2. The high-impedance anti-heterochromatic conductive silver paste of claim 1, wherein the resin is at least one of polyurethane resin, vinyl chloride-vinyl acetate resin, polyacrylate, EVA resin, PVB resin, polybutadiene, polyester, hydrogen-containing silicone oil, vinyl silicone resin and liquid silicone rubber.
3. The high-impedance anti-heterochromatic conductive silver paste as recited in claim 1, wherein the coupling agent is at least one of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent, a rare earth coupling agent and a fluorosilane coupling agent.
4. The high-impedance anti-heterochromatic conductive silver paste of claim 1, wherein the flow aid is at least one of white gasoline, kerosene, heptane, octane, undecane, dodecane, cyclohexanone, isophorone, ethylene glycol methyl ether, dipropylene glycol methyl ether, diethylene glycol dimethyl ether, diethylene glycol butyl ether, propylene glycol methyl ether acetate, diethylene glycol ethyl ether acetate, ethylene glycol butyl ether acetate, dimethyl adipate, diethyl adipate, DBE, dibasic esters, N-methylpyrrolidone, or terpineol.
5. The high-impedance heterochromatic-color-resistant conductive silver paste according to claim 1, wherein the conductive powder comprises flake conductive powder and spherical conductive powder, the flake conductive powder is silver powder, and the spherical conductive powder is at least one of pure silver powder, silver-coated nickel powder, silver-coated copper powder, silver-coated aluminum powder and silver-plated glass powder; the weight ratio of the flaky conductive powder to the spherical conductive powder is 7: 3-9: 1.
6. the high-impedance anti-heterochromatic conductive silver paste as recited in claim 1, wherein the resistance-discoloration and resistance-increase assistant is at least one of benzotriazole, methylbenzotriazole, aminotriazole, aminotetrazole, lauryl mercaptan, cetyl mercaptan, mercaptobenzene, 2-mercaptobenzothiazole, stearic acid, and ethylene glycol monostearate.
7. The method for preparing the high-impedance anti-heterochrosis conductive silver paste as recited in any one of claims 1-6, comprising the following steps:
(1) mixing and stirring the raw materials uniformly to obtain a mixture;
(2) and grinding the mixture, and filtering to obtain the high-impedance heterochromatic conductive silver paste.
8. The method for preparing the high-impedance anti-heterochromatic conductive silver paste as recited in claim 7, wherein in the step (1), the mixing and stirring speed is 100-1500r/min, and the mixing and stirring time is 5-100 min; in the step (2), the fineness of the high-impedance heterochromatic conductive silver paste obtained by grinding is 3-25 μm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102610296A (en) * | 2012-03-13 | 2012-07-25 | 江苏金陵特种涂料有限公司 | Thermosetting carbon/silver composite nano conductive silver paste and preparation method thereof |
| CN103258584A (en) * | 2013-01-09 | 2013-08-21 | 深圳市创智材料科技有限公司 | Electric conductive silver paste and manufacturing method thereof |
| CN112309608A (en) * | 2020-11-09 | 2021-02-02 | 无锡晶睿光电新材料有限公司 | Heterochrosis-resistant low-temperature conductive silver paste and preparation method thereof |
-
2022
- 2022-02-24 CN CN202210173412.XA patent/CN114512263A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102610296A (en) * | 2012-03-13 | 2012-07-25 | 江苏金陵特种涂料有限公司 | Thermosetting carbon/silver composite nano conductive silver paste and preparation method thereof |
| CN103258584A (en) * | 2013-01-09 | 2013-08-21 | 深圳市创智材料科技有限公司 | Electric conductive silver paste and manufacturing method thereof |
| CN112309608A (en) * | 2020-11-09 | 2021-02-02 | 无锡晶睿光电新材料有限公司 | Heterochrosis-resistant low-temperature conductive silver paste and preparation method thereof |
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