CN112750553A - Low-temperature curing wear-resistant conductive paste and preparation method thereof - Google Patents
Low-temperature curing wear-resistant conductive paste and preparation method thereof Download PDFInfo
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- CN112750553A CN112750553A CN202011498302.8A CN202011498302A CN112750553A CN 112750553 A CN112750553 A CN 112750553A CN 202011498302 A CN202011498302 A CN 202011498302A CN 112750553 A CN112750553 A CN 112750553A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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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 discloses a low-temperature curing wear-resistant conductive paste which comprises the following components in parts by weight: comprises the following components in parts by weight: 50-60 parts of micron-sized silver powder; 20-30 parts of wear-resistant metal filler; 10-15 parts of saturated polyester resin; 5-8 parts of a curing agent; 10-20 parts of a solvent; 1-2 parts of an additive; the wear-resistant metal filler is one or more of nickel powder, high-manganese alloy powder, tungsten carbide alloy powder, nickel-tungsten alloy powder and nickel-chromium alloy powder; the saturated polyester resin is oil-free alkyd resin; the micron-sized silver powder is flaky; the conductive paste comprises micron-sized silver powder and wear-resistant metal filler, and the wear-resistant metal filler has both wear resistance and conductivity, so that the wear resistance of the conductive paste is improved; oil-free alkyd resin is used as a bonding phase, and the structure of the oil-free alkyd resin contains a large number of polar structures, so that the oil-free alkyd resin has good wettability on silver powder and is beneficial to uniform dispersion of the silver powder; meanwhile, the molecular chain of the oil-free alkyd resin has excellent flexibility, and the conductive paste prepared by using the resin as a bonding phase has better bending resistance.
Description
Technical Field
The invention relates to the field of conductive silver paste, in particular to low-temperature curing wear-resistant conductive paste and a manufacturing method thereof.
Background
Silver conductive pastes fall into two categories: 1. polymer silver conductive paste (dried or solidified to form a film, and organic polymer is used as a bonding phase); 2. sintering type silver conductive paste (sintering film forming, sintering temperature >500 ℃, glass powder or oxide as bonding phase).
The existing low-temperature normal-temperature curing conductive paste has the characteristics of low curing temperature, extremely high bonding strength, stable electrical property, suitability for screen printing and the like. The adhesive is suitable for electric conduction and heat conduction adhesion in normal temperature curing welding occasions, such as quartz crystals, infrared pyroelectric detectors, piezoelectric ceramics, potentiometers, flash lamps, shielding, circuit repair and the like, and can also be used for electric conduction adhesion in the radio instrument industry; conductive bonding can also be achieved instead of solder paste.
With the development of conductive slurry, a plurality of types of slurry are available at present, but most of the slurry has insufficient wear resistance and is difficult to adapt to certain special application scenes; when the conductive paste is subjected to screen printing, the common conductive paste has relatively high curing temperature, and the cured paste has insufficient flexibility and insufficient bending resistance.
Therefore, how to solve the defects of the prior art is a subject of the present invention.
Disclosure of Invention
In order to solve the problems, the invention discloses low-temperature curing wear-resistant conductive paste and a manufacturing method thereof.
In order to achieve the above purpose, the invention provides the following technical scheme: the low-temperature curing wear-resistant conductive paste comprises the following components in parts by weight:
50-60 parts of micron-sized silver powder;
20-30 parts of wear-resistant metal filler;
10-15 parts of saturated polyester resin;
5-8 parts of a curing agent;
10-20 parts of a solvent;
1-2 parts of an additive;
the wear-resistant metal filler is one or more of nickel powder, high-manganese alloy powder, tungsten carbide alloy powder, nickel-tungsten alloy powder and nickel-chromium alloy powder;
the saturated polyester resin is oil-free alkyd resin, is high molecular weight linear saturated polyester resin, contains a large amount of polar groups, and has better flexibility;
the micron silver powder is flaky, the D50 of the micron silver powder is 1-3 mu m, and the tap density of the micron silver powder is 5.5-7.5g/cm 3;
the micron-sized silver powder is used as a main conductive phase and is flaky, linear contact or surface contact is formed among the flaky silver powders in the cured conductive paste, and the contact area of the flaky silver powders is larger than that of point contact formed among the conventional spherical silver powders, so that the conductivity of the prepared conductive paste is relatively better;
as an improvement of the invention, the additive comprises a dispersant, a defoaming agent and an adhesion promoter, wherein the dispersant can adopt a BYK 154 wetting dispersant for improving wettability, the defoaming agent is used for preventing foam formation, and specifically, a polyether modified polysiloxane defoaming agent can be adopted.
As an improvement of the present invention, in order to further improve the adhesion of the conductive paste, the adhesion promoter is tetraethyl titanate.
As a modification of the present invention, the solvent is a ketone solvent for dissolving the resin.
As an improvement of the invention, the ketone solvent is one or more of acetone, methyl butanone and methyl isobutyl ketone.
As an improvement of the invention, the curing agent is an amine curing agent, and the amine curing agent is one or more of ethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine and diethylaminopropylamine.
A manufacturing method of low-temperature cured wear-resistant conductive paste comprises the following steps:
the method comprises the following steps: preparing a carrier: mixing the saturated polyester resin, the curing agent, the solvent and the additive, and then centrifugally dispersing for 10-20min under the conditions of 2000-2500rpm to obtain a material A;
step two: slurry premixing: uniformly mixing the micron-sized silver powder and the wear-resistant metal filler, uniformly dividing into 2-3 parts, sequentially adding the mixture into the material A, and stirring in an ultrasonic stirrer for 10-20min after each time of adding to obtain a material B;
step three: and (3) performing high-speed shearing, grinding and dispersing on the premixed material B in a three-roller machine, and filtering by using a 300-mesh and 500-mesh screen to remove impurities and uneven particles in the material B to obtain the conductive slurry.
The nanometer silver powder has small particle size, and the particles attract each other spontaneously, so that the problems of agglomeration and low-temperature non-intensive diffusion exist, and the force can be dispersed again through external energy and ultrasonic oscillation to inhibit the occurrence of agglomeration.
As an improvement of the invention, the micron-sized silver powder is prepared by reducing and depositing silver powder by a reducing agent by a wet reduction method, and is dried in a vacuum environment, the drying temperature is set below 80 ℃, and the granularity of the silver powder prepared by the method is uniform.
Compared with the prior art, the invention has the following advantages: the conductive paste comprises micron-sized silver powder and a wear-resistant metal filler, and the wear-resistant metal filler has both wear resistance and conductivity, so that the wear resistance of the conductive paste is improved; oil-free alkyd resin is used as a bonding phase, and the structure of the oil-free alkyd resin contains a large number of polar structures, so that the oil-free alkyd resin has good wettability on silver powder and is beneficial to uniform dispersion of the silver powder; meanwhile, the molecular chain of the oil-free alkyd resin has excellent flexibility, so that the conductive paste prepared by using the resin as a bonding phase has better bending resistance.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used merely to facilitate describing the invention and to simplify the description, and do not indicate or imply that the referenced devices or components must be in a particular orientation, constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the 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.
The preparation method of the conductive paste in the following examples and comparative examples is as follows:
the method comprises the following steps: preparing a carrier: mixing the saturated polyester resin, the curing agent, the solvent and the additive, and then centrifugally dispersing for 10-20min under the conditions of 2000-2500rpm to obtain a material A;
step two: slurry premixing: uniformly mixing the micron-sized silver powder and the wear-resistant metal filler, uniformly dividing into 2-3 parts, sequentially adding the mixture into the material A, and stirring in an ultrasonic stirrer for 10-20min after each time of adding to obtain a material B;
step three: and (3) performing high-speed shearing, grinding and dispersing on the premixed material B in a three-roller machine, and filtering by using a 300-mesh and 500-mesh screen to remove impurities and uneven particles in the material B to obtain the conductive slurry.
And preparing the micron-sized silver powder by reducing and depositing the silver powder by using a reducing agent by adopting a wet reduction method, and drying the micron-sized silver powder in a vacuum environment, wherein the drying temperature is set to be below 80 ℃.
Examples 1 to 3 and comparative example 1
In table 1, examples 1, 2 and 3 show the resistivity and wear resistance of conductive pastes prepared by using different weight parts of raw materials; the difference between the comparative example 1 and the example 3 is that the resin in the raw material of the conductive paste prepared in the comparative example 1 is polyurethane resin;
the resistivity and wear resistance of the conductive pastes prepared in examples 1-3 and comparative example 1 are shown in table 1; wherein, the wear resistance detection adopts a rotating friction rubber wheel method, namely, under the specified test conditions that the rotating speed of a rotating disc is 60r/min and a certain load is borne by a pressurizing arm, a hard rubber friction wheel embedded with carborundum abrasive is adopted to abrade the surface of the solidified conductive slurry;
TABLE 1
Comparison of the abrasion resistance of comparative example 1 with that of examples 1 to 3 further proves that the electroconductive paste of the present invention is relatively excellent in abrasion resistance.
The conductive pastes prepared in the above examples 1 to 3 and comparative example 1 were tested for electrical resistance and mechanical properties, and the test results are shown in the following table 2:
TABLE 2
The technical means disclosed in the invention scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (8)
1. The low-temperature curing wear-resistant conductive paste is characterized in that: comprises the following components in parts by weight:
50-60 parts of micron-sized silver powder;
20-30 parts of wear-resistant metal filler;
10-15 parts of saturated polyester resin;
5-8 parts of a curing agent;
10-20 parts of a solvent;
1-2 parts of an additive;
the wear-resistant metal filler is one or more of nickel powder, high-manganese alloy powder, tungsten carbide alloy powder, nickel-tungsten alloy powder and nickel-chromium alloy powder;
the saturated polyester resin is oil-free alkyd resin;
the micron silver powder is flaky, the D50 of the micron silver powder is 1-3 mu m, and the tap density of the micron silver powder is 5.5-7.5g/cm 3.
2. The low-temperature-curing wear-resistant conductive paste as claimed in claim 1, wherein: the additive comprises a dispersing agent, a defoaming agent and an adhesion promoter.
3. The low-temperature-curing wear-resistant conductive paste as claimed in claim 2, wherein: the adhesion promoter is tetraethyl titanate.
4. The low-temperature-curing wear-resistant conductive paste as claimed in claim 1, wherein: the solvent is a ketone solvent.
5. The low-temperature-curing wear-resistant conductive paste as claimed in claim 4, wherein: the ketone solvent is one or more of acetone, methyl butanone and methyl isobutyl ketone.
6. The low-temperature-curing wear-resistant conductive paste as claimed in claim 1, wherein: the curing agent is an amine curing agent, and the amine curing agent is one or more of ethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine and diethylaminopropylamine.
7. The manufacturing method of the low-temperature cured wear-resistant conductive paste is characterized by comprising the following steps of: the method comprises the following steps:
the method comprises the following steps: preparing a carrier: mixing the saturated polyester resin, the curing agent, the solvent and the additive, and then centrifugally dispersing for 10-20min under the conditions of 2000-2500rpm to obtain a material A;
step two: slurry premixing: uniformly mixing the micron-sized silver powder and the wear-resistant metal filler, uniformly dividing into 2-3 parts, sequentially adding the mixture into the material A, and stirring in an ultrasonic stirrer for 10-20min after each time of adding to obtain a material B;
step three: and (3) performing high-speed shearing, grinding and dispersing on the premixed material B in a three-roller machine, and filtering by using a 300-mesh and 500-mesh screen to remove impurities and uneven particles in the material B to obtain the conductive slurry.
8. The method for preparing the low-temperature curing wear-resistant conductive paste as claimed in claim 7, wherein the method comprises the following steps: and reducing and depositing the silver powder by using a reducing agent by adopting a wet reduction method to prepare the micron-sized silver powder, and drying the micron-sized silver powder in a vacuum environment, wherein the drying temperature is set to be below 80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011498302.8A CN112750553A (en) | 2020-12-17 | 2020-12-17 | Low-temperature curing wear-resistant conductive paste and preparation method thereof |
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| CN202011498302.8A CN112750553A (en) | 2020-12-17 | 2020-12-17 | Low-temperature curing wear-resistant conductive paste and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114709004A (en) * | 2022-03-15 | 2022-07-05 | 福建省乔杨科技有限公司 | Conductive silver paste and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114709004A (en) * | 2022-03-15 | 2022-07-05 | 福建省乔杨科技有限公司 | Conductive silver paste and preparation method thereof |
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