CN111243779A - Preparation method for laser cutting conductive silver paste and low-temperature curing superfine spherical silver powder and preparation method for conductive silver paste and low-temperature curing superfine spherical silver powder - Google Patents
Preparation method for laser cutting conductive silver paste and low-temperature curing superfine spherical silver powder and preparation method for conductive silver paste and low-temperature curing superfine spherical silver powder Download PDFInfo
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- CN111243779A CN111243779A CN202010158249.0A CN202010158249A CN111243779A CN 111243779 A CN111243779 A CN 111243779A CN 202010158249 A CN202010158249 A CN 202010158249A CN 111243779 A CN111243779 A CN 111243779A
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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
Abstract
The invention relates to a method for preparing conductive silver paste for laser cutting and superfine spherical silver powder solidified at low temperature, which is characterized in that: the coating comprises, by weight, 10-40 parts of a resin material, 0.5-5 parts of a closed isocyanate or amino resin, 20-80 parts of a solvent, 0.1-1 part of a fluorine-containing chlorine compound conductive additive, 0-2 parts of a dispersant, and 55-60 parts of low-temperature cured superfine spherical silver powder. This a conductivity for laser cutting electrically conductive silver thick liquid is promoted greatly, and then can be applied to in the laser cutting.
Description
Technical Field
The invention relates to electronic paste, in particular to a method for preparing conductive silver paste for laser cutting and superfine spherical silver powder for low-temperature curing and a method for preparing the same.
Background
The low-temperature curing silver paste is used for various substrates which can only bear low-temperature baking, the substrates are generally plastic films (plates) or paper films (plates), and the materials of the plastic films (plates) are generally PET, PI, PC and the like; the low-temperature cured silver paste can be used in electronic products such as computer keyboards, membrane switches, touch screens and the like, and the electronic products increasingly pursue designs such as tiny, fine or bending and the like, so that strict requirements on whether the low-temperature cured silver paste can print fine lines are met; the existing low-temperature curing silver paste for screen printing can only print lines (commonly called 60/60 lines) with the width of 60 microns and the line distance of 60 microns, and the lines can not meet the requirements of the existing market on electronic products (the thin lines with the width of 20-25 microns can meet the requirements); while the screen printing technology can print lines (commonly known as 25/25 lines) with the width of 25 microns and the line distance of 25 microns, the line distance cannot reach 25 microns when the existing low-temperature curing silver paste is used for printing, and because the two lines are connected due to the diffusion of the silver paste, the two lines are conducted and short-circuited after curing, the existing low-position curing silver paste cannot be used in electronic elements with grouped wiring.
In order to solve the problems, the laser cutting method is generally adopted in the row to cut 25/25-micron or 20/20-micron ultra-fine silver wires; the method is characterized in that 1mm or even wider silver wires can be printed firstly during printing, and the ultra-fine silver wires with the width of 25/25 micrometers, 20/20 micrometers (width/line distance) or more are cut out in a laser cutting mode after solidification, so that the requirement on the fineness of the wires in a yellow light process (the yellow light process is to use an exposure mode to sun out ultra-fine wires and use a chemical etching method to manufacture the wires, and has the defects of complex process, large equipment investment, low efficiency and the like) is met; mature laser cutting can replace a yellow light manufacturing process and can be widely used in a touch screen line manufacturing process. In addition, the existing low-temperature cured silver paste has poor conductivity, because the surface of the powder is not treated (such as physical polishing, grinding and the like) after the spherical silver powder is reduced and generated, in the resin curing process, the spherical silver powder is mutually connected and overlapped and collided together to be communicated and conductive, but because the contact surfaces between the spherical silver powder are in contact between the arc surfaces of the arc surfaces, the contact area is small, the conductivity of the low-temperature cured silver paste is poor, and the quality of an electronic product is directly influenced.
Therefore, further improvements are needed.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for preparing conductive silver paste and low-temperature solidified superfine spherical silver powder by laser cutting and a method for preparing the same; the conductivity of the conductive silver paste for laser cutting is greatly improved, and the conductive silver paste can be applied to laser cutting.
The purpose of the invention is realized as follows:
the utility model provides a be used for laser cutting electrically conductive silver thick liquid which characterized in that: the coating comprises, by weight, 10-40 parts of a resin material, 0.5-5 parts of a closed isocyanate or amino resin, 20-80 parts of a solvent, 0.1-1 part of a fluorine-containing chlorine compound conductive additive, 0-2 parts of a dispersant, and 55-60 parts of low-temperature cured superfine spherical silver powder.
The resin material is one or a mixture of more than two of polyester resin, polyurethane resin or hydroxyl acrylic resin.
The fluorine-containing chlorine compound conductive additive comprises a fluorine compound and/or a chlorine compound, wherein the fluorine compound is one or a mixture of more than two of sodium fluoride, potassium fluoride, copper fluoride, magnesium fluoride, calcium fluoride, zinc fluoride, boron fluoride and silver fluoride, and the chlorine compound is one or a mixture of more than two of magnesium chloride, copper chloride, silver chloride, sodium chloride, potassium chloride, calcium chloride, aluminum chloride, zinc chloride and lithium chloride.
The solvent is one or a mixture of more than two of isophorone, butyl carbitol acetate and dibasic ester.
The dispersant is one or a mixture of BYK333 and BYK 163.
The preparation method for laser cutting of the conductive silver paste is characterized by comprising the following steps: the method comprises the following steps:
step a, dissolving a resin material into a resin solution by using a solvent for later use;
and b, mixing the resin solution, the closed isocyanate or amino resin, the fluorine-containing chlorine compound conductive additive, the dispersing agent and the low-temperature cured superfine spherical silver powder to obtain the conductive silver paste for laser cutting.
The low-temperature solidified superfine spherical silver powder is characterized in that: comprises 10 to 50 portions of silver nitrate, 10 to 40 portions of ascorbic acid, 40 to 300 portions of deionized water, 0.5 to 2 portions of PVP polyvinylpyrrolidone and 0.1 to 2 portions of gelatin according to the weight portion.
The preparation method of the low-temperature solidified superfine spherical silver powder is characterized by comprising the following steps: the method comprises the following steps:
dissolving silver nitrate in a part of deionized water for standby, dissolving PVP polyvinylpyrrolidone in another part of deionized water for standby, dissolving gelatin in another part of deionized water for standby, and dissolving ascorbic acid in another part of deionized water for standby;
putting an ultrasonic oscillator into a reaction kettle, adding an ascorbic acid solution into the reaction kettle, starting the ultrasonic oscillator to uniformly oscillate and disperse the ascorbic acid solution, gradually adding a PVP polyvinylpyrrolidone solution and a gelatin solution in the midway, stirring and mixing, gradually dripping the mixed solution obtained by ultrasonic into a silver nitrate solution while uniformly oscillating and stirring, and then completing a reduction reaction, wherein at the moment, a precipitate is formed at the bottom of the reaction kettle under the vibration and stirring of the ultrasonic oscillator;
and step three, washing the precipitate with the balance of deionized water, centrifuging and filtering water, and finally drying and dispersing by an air flow mill to obtain the low-temperature cured superfine spherical silver powder.
In the second step, the ratio of the silver nitrate solution to the ascorbic acid solution is 1:1, and the dropping speed of the silver nitrate solution is one percent of the total amount of the silver nitrate solution dropped per second.
In the third step, the drying temperature is 80-100 ℃, and the drying time is 24 h.
The invention has the following beneficial effects:
the conductive silver paste for laser cutting is at least prepared from a resin material, closed isocyanate or amino resin, a solvent, a fluorine-chlorine-containing compound conductive auxiliary agent, a dispersing agent and low-temperature cured superfine spherical silver powder; in the preparation process, the conductivity of the conductive silver paste can be promoted by adding the fluorine-containing chlorine compound conductive additive. The chlorine and the fluorine can promote the resin material to be tightly jointed with the low-temperature cured superfine spherical silver powder in a formula system, so that the molecular or molecular chain crosslinking density of the resin is higher, and the capacity of jointing the silver powder is stronger, so that the spherical silver powder can also exert good conductivity, and further can replace flaky silver powder in the formula of the traditional low-temperature cured silver paste, and the conductive silver paste can be selected whether needing laser cutting or not; and through to this application that is used for laser cutting conductive silver thick liquid, can guarantee that the superfine globular silver powder of low temperature solidification that laser arrived in the laser cutting technology place all is globular, the superfine globular silver powder of low temperature solidification is cut the well or probability greatly reduced who cuts off (in traditional conductive silver thick liquid, flake silver powder and flake silver powder joint, flake silver powder is easily cut the well or is cut off during laser cutting, wherein can be cracked by the silver powder of cutting the well, lead to lines deckle edge or direct short circuit, short circuit probability is just bigger when especially meetting the silver powder that the particle diameter reaches 10 microns). Specifically, since the spherical silver powder has uniform particle size and narrow particle size distribution, and is uniformly distributed on the silver wire, the probability of cutting the spherical silver powder during laser cutting is low, and even if the spherical silver powder is cut, the spherical silver powder is not cracked to form burrs due to stress or is not slipped through gaps among the spherical silver powders to cause short circuit.
The low-temperature solidified superfine spherical silver powder is at least prepared from silver nitrate, ascorbic acid, deionized water, PVP polyvinylpyrrolidone and gelatin material; in the preparation process, the round spherical silver powder can be reduced under the vibration and stirring of the ultrasonic oscillator, the silver powder reduced by using the ascorbic acid as a reducing agent has high crystallinity and uniform particle size and distribution, the conductivity of the low-temperature cured superfine spherical silver powder is effectively improved, and the conductivity of the conductive silver paste is further improved.
Detailed Description
The present invention will be further described with reference to the following examples.
The conductive silver paste for laser cutting in the embodiment is a manufacturing process for various products such as computer keyboards, membrane switches, touch screens and the like, and comprises, by weight, 10-40 parts of a resin material, 0.5-5 parts of closed isocyanate or amino resin, 20-80 parts of a solvent, 0.1-1 part of a fluorine-containing chlorine compound conductive additive, 0-2 parts of a dispersing agent and 55-60 parts of low-temperature curing superfine spherical silver powder. In the formula, the conductivity of the spherical silver powder can be enhanced by adding the fluorine-containing chlorine compound conductive additive, the problem of poor conductivity of the spherical silver powder is solved, the conductivity of the spherical silver powder is good, and the laser cutting effect can be improved (the traditional flaky silver powder has good conductivity, but the laser cutting effect is not good). The conductive silver paste for laser cutting has excellent conductivity and strong adhesive force, and can be used for laser cutting to obtain compact and fine conductive circuits.
Further, the resin material is one or a mixture of more than two of polyester resin, polyurethane resin, hydroxy acrylic resin and the like.
Further, the fluorine-containing chlorine compound conductive aid comprises a fluorine compound and/or a chlorine compound; the fluorine compound is one or a mixture of more than two of sodium fluoride, potassium fluoride, copper fluoride, magnesium fluoride, calcium fluoride, zinc fluoride, boron fluoride, silver fluoride and the like, preferably sodium fluoride and silver fluoride, and the selection of the fluorine compound is to take the solubility and the compatibility of a resin system into consideration; the chlorine compound is one or a mixture of more than two of the same substances such as magnesium chloride, copper chloride, silver chloride, sodium chloride, potassium chloride, calcium chloride, aluminum chloride, zinc chloride, lithium chloride and the like, preferably magnesium chloride, copper chloride and silver chloride, and the selection of the chlorine compound also needs to be compatible with the solubility and the compatibility of a resin system.
Furthermore, the solvent is one or a mixture of more than two of similar substances such as isophorone, butyl carbitol acetate, dibasic ester and the like.
Further, the dispersant is one or two mixtures of BYK333, BYK163 and the like.
The preparation method for laser cutting of the conductive silver paste comprises the following steps:
step a, dissolving a resin material into a resin solution with the solid content of 10-20% by using a solvent for later use; specifically, one or more than two of polyester resin, polyurethane resin and hydroxy acrylic resin in the resin material are dissolved in a solvent, and the solvent is a mixture formed by mixing isophorone, butyl carbitol acetate and dibasic ester according to a formula of 1:1: 1.
And b, mixing the resin solution, the closed isocyanate or amino resin, the fluorine-containing chlorine compound conductive additive, the dispersing agent and the low-temperature cured superfine spherical silver powder to obtain the conductive silver paste for laser cutting.
Further, the solvent is a mixture of isophorone, butyl carbitol acetate and dibasic ester mixed according to the proportion of 1:1:1, and the mixture is used as a solvent three-in-one mixture R-H1.
The following is a table of various specific formulations:
| material scheme | ① | ② | ③ | ④ | ⑤ |
| Polyester resin solution | 20 | — | — | 15 | 20 |
| Polyurethane resin solution | — | 20 | — | — | — |
| Acrylic resin solution | — | — | 20 | — | — |
| Low-temperature solidified superfine spherical silver powder | 55 | 55 | 55 | 60 | 55 |
| Fluorine-containing chlorine compound conductive additive | 0.2 | 0.2 | 0.2 | 0.4 | 0.5 |
| Dispersing agent | 1.0 | 1.0 | 1.0 | — | — |
| Solvent three-in-one mixture R-H1 | 24 | 24 | 24 | 25 | 25 |
| Blocked isocyanates or amino resins | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
In the scheme, the schemes ④ and ⑤ are better schemes, namely the conductive silver paste prepared in the schemes ④ and ⑤ are better in whole, wherein the conductive silver paste prepared in the scheme ④ is relatively lower in resistance but not better than the scheme ⑤ in laser cutting effect, the conductive silver paste prepared in the scheme ⑤ is relatively higher in resistance but better than the scheme ④ in laser cutting effect, and a large number of experiments prove that the addition of the silver powder can influence the laser cutting effect, for example, the silver powder is coarse in lines and large in burrs due to large addition of the silver powder, and the cut lines are fine and have no burrs due to small addition of the silver powder.
The low-temperature solidified superfine spherical silver powder comprises, by weight, 10-50 parts of silver nitrate (industrial grade), 10-40 parts of ascorbic acid (industrial grade), 40-300 parts of deionized water, 0.5-2 parts of PVP polyvinylpyrrolidone and 0.1-2 parts of gelatin (industrial grade). In the low-temperature curing superfine spherical silver powder, ascorbic acid is used for reduction, and gelatin and PVP polyvinylpyrrolidone are used as dispersing agents in a reduction process system, so that the core grows into spherical low-temperature curing superfine spherical silver powder with small particle size in the reduction process.
The preparation method of the low-temperature solidified superfine spherical silver powder comprises the following steps:
step one, stirring and dissolving 20 parts of silver nitrate in 20 parts of deionized water to prepare a silver nitrate solution for later use; stirring and dissolving 2 parts of PVP polyvinylpyrrolidone in 98 parts of deionized water to prepare a PVP polyvinylpyrrolidone solution for later use, wherein the content of the PVP polyvinylpyrrolidone is about 2%; stirring and dissolving 2 parts of gelatin in 98 parts of deionized water to prepare a gelatin solution for later use, wherein the content of the gelatin is about 2%; stirring and dissolving 20 parts of ascorbic acid in 20 parts of deionized water to prepare an ascorbic acid solution for later use;
putting an ultrasonic oscillator into a reaction kettle, adding an ascorbic acid solution into the reaction kettle, starting the ultrasonic oscillator to uniformly oscillate and disperse the ascorbic acid solution, gradually adding a PVP polyvinylpyrrolidone solution and a gelatin solution in the midway, stirring and mixing (at this time, no chemical reaction exists, only physical mixing exists), gradually dripping the mixed solution obtained by ultrasonic waves into a silver nitrate solution during uniform oscillation and stirring, then completing a reduction reaction, and forming a gray yellow precipitate at the bottom of the reaction kettle under the vibration and stirring of the ultrasonic oscillator;
and step three, washing the precipitate for 5-10 times by using the balance of deionized water, centrifuging and filtering water, and finally drying and dispersing by using an air flow mill to obtain the low-temperature cured superfine spherical silver powder.
According to the preparation method, the spherical silver powder with high roundness can be produced by stirring with the ultrasonic oscillator, and the silver powder produced by using the ascorbic acid as the reducing agent has high crystallinity and uniform particle size and distribution, so that the conductivity of the silver powder is better, and the conductive silver paste with low resistance and good conductivity is prepared.
Further, in the second step, the power of the ultrasonic oscillator is provided with proper power according to the amount of the silver powder reduced at one time; the dropping amount of the silver nitrate solution depends on the capacity of the reaction kettle, the ratio of the silver nitrate solution to the ascorbic acid solution is 1:1, and the dropping speed of the silver nitrate solution is one percent of the total amount of the silver nitrate solution dropped per second (namely, for example, 100 liters of the silver nitrate solution is dropped at a flow rate of 1 liter per second, and all the amount addition is completed within 100 seconds).
Further, in the third step, the drying temperature is 80-100 ℃, and the drying time is 24 hours.
Further, low-temperature curing means baking at normal temperature-below 200 ℃ to generate chemical reaction or evaporating and drying the solution to naturally cure and form a film, so that the conductive silver coating with adhesive force and electrical property is formed, and the conductive silver coating is prepared by using resin (or) and a curing agent to perform a crosslinking reaction as a bonding material; the superfine spherical silver powder is spherical (spherical or sphere-like) silver powder, and has an average particle diameter of 0.5-1 micrometer and a particle diameter range of 0.1-2 micrometers. The traditional spherical silver powder is generally only suitable for being used as a high-temperature sintered (600-950 ℃) silver paste conductive carrier, because the conductivity of the traditional spherical silver powder can be half-fused and overlapped to form a conductive connector only through high-temperature sintering, and the low-temperature sintering is carried outCured, connected with resin, has poor conductivity and even non-conductivity (the resistivity is 10 after high-temperature sintering)-6Omega.cm, and the resistance after low-temperature curing is only about 10-1000 omega.cm); the conductivity of the flake silver powder for low-temperature curing reaches 10-5About omega.cm, the flake silver powder is not suitable for being cut into thin lines by some printed thin lines or laser, and the flake silver powder can be broken during laser cutting, so that the lines can be bounced or loosened, and the adhesive force is influenced; the flaky silver powder has poor reticulation property when printing fine lines, so that spherical silver powder is generally required; the low-temperature curing superfine spherical silver powder provided by the invention can be better suitable for laser cutting and fine line printing.
Further, laser cutting means that thick lines are printed by laser cutting silk screen, for example, lines with a width of 1mm, lines with a width of 20 micrometers can be cut, lines with a spacing of 20 micrometers can also be cut, 20 groups of superfine lines with a width of 20 micrometers can be cut, and the requirements of electronic circuits which are increasingly miniaturized and refined can be met.
The foregoing is a preferred embodiment of the present invention, and the basic principles, principal features and advantages of the invention are shown and described. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are intended to illustrate the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and the invention is intended to be protected by the following claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The utility model provides a be used for laser cutting electrically conductive silver thick liquid which characterized in that: the coating comprises, by weight, 10-40 parts of a resin material, 0.5-5 parts of a closed isocyanate or amino resin, 20-80 parts of a solvent, 0.1-1 part of a fluorine-containing chlorine compound conductive additive, 0-2 parts of a dispersant, and 55-60 parts of low-temperature cured superfine spherical silver powder.
2. The conductive silver paste for laser cutting according to claim 1, wherein: the resin material is one or a mixture of more than two of polyester resin, polyurethane resin or hydroxyl acrylic resin.
3. The conductive silver paste for laser cutting according to claim 1, wherein: the fluorine-containing chlorine compound conductive additive comprises a fluorine compound and/or a chlorine compound, wherein the fluorine compound is one or a mixture of more than two of sodium fluoride, potassium fluoride, copper fluoride, magnesium fluoride, calcium fluoride, zinc fluoride, boron fluoride and silver fluoride, and the chlorine compound is one or a mixture of more than two of magnesium chloride, copper chloride, silver chloride, sodium chloride, potassium chloride, calcium chloride, aluminum chloride, zinc chloride and lithium chloride.
4. The conductive silver paste for laser cutting according to claim 1, wherein: the solvent is one or a mixture of more than two of isophorone, butyl carbitol acetate and dibasic ester.
5. The conductive silver paste for laser cutting according to claim 1, wherein: the dispersant is one or a mixture of BYK333 and BYK 163.
6. The method for preparing conductive silver paste for laser cutting according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
step a, dissolving a resin material into a resin solution by using a solvent for later use;
and b, mixing the resin solution, the closed isocyanate or amino resin, the fluorine-containing chlorine compound conductive additive, the dispersing agent and the low-temperature cured superfine spherical silver powder to obtain the conductive silver paste for laser cutting.
7. The low-temperature-curable ultrafine spherical silver powder according to claim 1, wherein: comprises 10 to 50 portions of silver nitrate, 10 to 40 portions of ascorbic acid, 40 to 300 portions of deionized water, 0.5 to 2 portions of PVP polyvinylpyrrolidone and 0.1 to 2 portions of gelatin according to the weight portion.
8. The method for preparing the low-temperature curable ultrafine spherical silver powder according to claim 7, wherein: the method comprises the following steps:
dissolving silver nitrate in a part of deionized water for standby, dissolving PVP polyvinylpyrrolidone in another part of deionized water for standby, dissolving gelatin in another part of deionized water for standby, and dissolving ascorbic acid in another part of deionized water for standby;
putting an ultrasonic oscillator into a reaction kettle, adding an ascorbic acid solution into the reaction kettle, starting the ultrasonic oscillator to uniformly oscillate and disperse the ascorbic acid solution, gradually adding a PVP polyvinylpyrrolidone solution and a gelatin solution in the midway, stirring and mixing, gradually dripping the mixed solution obtained by ultrasonic into a silver nitrate solution while uniformly oscillating and stirring, and then completing a reduction reaction, wherein at the moment, a precipitate is formed at the bottom of the reaction kettle under the vibration and stirring of the ultrasonic oscillator;
and step three, washing the precipitate with the balance of deionized water, centrifuging and filtering water, and finally drying and dispersing by an air flow mill to obtain the low-temperature cured superfine spherical silver powder.
9. The method for preparing the low-temperature curable ultrafine spherical silver powder according to claim 8, wherein: in the second step, the ratio of the silver nitrate solution to the ascorbic acid solution is 1:1, and the dropping speed of the silver nitrate solution is one percent of the total amount of the silver nitrate solution dropped per second.
10. The method for preparing the low-temperature curable ultrafine spherical silver powder according to claim 8, wherein: in the third step, the drying temperature is 80-100 ℃, and the drying time is 24 h.
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| CN202010158249.0A CN111243779A (en) | 2020-03-09 | 2020-03-09 | Preparation method for laser cutting conductive silver paste and low-temperature curing superfine spherical silver powder and preparation method for conductive silver paste and low-temperature curing superfine spherical silver powder |
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| CN202010158249.0A CN111243779A (en) | 2020-03-09 | 2020-03-09 | Preparation method for laser cutting conductive silver paste and low-temperature curing superfine spherical silver powder and preparation method for conductive silver paste and low-temperature curing superfine spherical silver powder |
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Application publication date: 20200605 |