CN110942842A - Conductor paste and conductor material - Google Patents
Conductor paste and conductor material Download PDFInfo
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- CN110942842A CN110942842A CN201911302883.0A CN201911302883A CN110942842A CN 110942842 A CN110942842 A CN 110942842A CN 201911302883 A CN201911302883 A CN 201911302883A CN 110942842 A CN110942842 A CN 110942842A
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- conductor
- silver powder
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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
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- 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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/18—Conductive material dispersed in non-conductive inorganic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/003—Thick film resistors
Abstract
The invention relates to a conductor paste and a conductor material. The conductor paste comprises the following components in percentage by weight: 20-40% of silver powder, 0.01-20% of graphene, 1-8% of glass powder and 45-70% of organic carrier. The silver content in the conductor paste is extremely low, and is only 20-40%, so that the thought constraint of high silver conductivity in the traditional method is broken through, the conductor paste is a new breakthrough in the limit field of domestic electronic materials, the production cost can be effectively reduced for downstream enterprises, and the living space is improved; meanwhile, graphene is added into the conductor slurry, and the defects caused by silver reduction are made up by using the excellent electrical properties of the graphene.
Description
Technical Field
The invention relates to a paste and application thereof, in particular to a conductor paste and a conductor material.
Background
Since the chip resistor was produced, the back electrode paste has been available, the first manufacturing enterprises have been the mine residence in japan, the continent in korea, and the like, and with the advance of the cost of chip resistor enterprises, we have developed back electrode paste with a metal content of 50%, replacing importation at a time. However, high metal content back electrode pastes increase production costs. The field of conductor materials requires continuous exploration and challenge, and continuous excavation of technical potential and limits.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the conductor paste with low production cost and good conductivity and the conductor material prepared from the conductor paste.
In order to achieve the purpose, the invention adopts the technical scheme that: a conductor paste comprises the following components in percentage by weight: 20-40% of silver powder, 0.01-20% of graphene, 1-8% of glass powder and 45-70% of organic carrier.
The silver content in the conductor paste is extremely low, and is only 20-40%, so that the thought constraint of high silver conductivity in the traditional method is broken, the conductor paste is a new breakthrough in the limit field of domestic electronic materials, the production cost can be effectively reduced for downstream enterprises, and the living space is improved. The silver powder can be prepared by dissolving and reducing silver nitrate through chemical reactions.
Meanwhile, graphene is added into the conductor slurry, and the defects caused by silver reduction are made up by using the excellent electrical properties of the graphene. The peculiar hexagonal honeycomb lattice of graphene can effectively control the shrinkage of a silver layer in the sintering process, and the hexagonal honeycomb lattice serves as a bridge in a new crystal phase, so that the sintering continuity of the silver layer is ensured, and the conductive effect of the silver layer is greatly improved. Along with the increase of the addition amount of graphene, the resistance of the conductor paste is obviously reduced, and the conductivity is better and better, but the excessive addition of graphene causes the mobility of the paste to be poor, so that the printing requirement cannot be met. Through a great deal of research, the inventor finds that when the weight percentage of graphene in the conductor material is 0.01-20%, the conductor paste has good conductivity and can meet the printing requirement.
The preparation method of the conductor paste comprises the following steps: and mixing, grinding and modulating the components in the conductor slurry according to a ratio to obtain the conductor slurry. The conductor paste is black brown paste in appearance, has proper thixotropy and fluidity, is printed on the surface of a substrate (such as an alumina substrate) by screen printing, and forms a conductor material with excellent performance after sintering. The micron-sized conductor layer has the advantages of smoothness, compactness, low direct-current resistance, strong bonding property with a ceramic substrate and the like. The function of connection, electric conduction, welding resistance and the like is realized in the element.
As a preferred embodiment of the conductor paste of the present invention, the silver powder includes spherical silver powder. As a more preferable embodiment of the conductor paste of the present invention, the silver powder is composed of spherical silver powder and plate-like silver powder, and a weight ratio of the spherical silver powder to the plate-like silver powder is 9: 1-2: 3. the conductive paste prepared from the powder formed by matching the spherical silver powder and the flake silver powder has the characteristics of good dispersion performance, good sintering compactness, low sintering shrinkage and the like, and is the most ideal matching of the conductive paste with low silver content. In addition, the research also shows that the weight ratio of the spherical silver powder to the flake silver powder is 9: 1-2: 3, the conductive paste has good appearance and moderate viscosity, can be further debugged, and is not suitable for screen printing because the viscosity of the paste is increased and the fluidity of the paste is poor along with the increase of the flaky silver powder.
As a preferable embodiment of the conductor paste of the present invention, the spherical silver powder has a shake-out ratio of 3.5 to 5.0g/cm3The specific surface area is 0.2-8.0m2(ii)/g, particle size distribution D50 is 3.0-5.0 μm; the shaking-out ratio of the flake silver powder is 1.5-3.6g/cm3The specific surface area is 0.5-1.3m2(iv)/g, particle size distribution D50 is 5.0-9.0. mu.m. More preferably, the purity of the spherical silver powder and/or the plate-like silver powder is not less than 99.5%. The basic performance of the silver layer after sintering is influenced to a greater or lesser extent by the shape, size and purity of the silver powder, and the specific silver powder meets the technical characteristics and technical requirements of chip resistor chip production.
The graphene used in the invention can be prepared by a graphite oxide reduction method, for example, strong oxidants such as concentrated sulfuric acid, concentrated nitric acid, potassium permanganate and the like are used for oxidizing graphite into graphite oxide, in the oxidation process, oxygen-containing functional groups are inserted between graphite layers, so that the distance between graphite layers is increased, and then the graphene can be formed after ultrasonic treatment for a period of timeAnd (3) single-layer or multi-layer graphene oxide, and then reducing the graphene oxide into graphene by using a strong reducing agent hydrazine hydrate, sodium borohydride and the like. The graphene prepared by the method is a hexagonal two-dimensional carbon nano material in a honeycomb lattice form by using sp2 hybridized orbits of carbon atoms, belongs to single-layer graphene, has high purity, large specific surface area and good dispersion performance, can be better combined with silver ions in a sintering process to form a new phase, makes up the cavity of the shrinkage parameter of the silver ions, plays a role of a bridge, and improves the conductivity of a sintered coating while controlling the shrinkage of a silver layer. Preferably, the tap density of the graphene is 0.7-6.2g/mL, and the specific surface area is 3.0-12.0m2(ii)/g, the particle size distribution D50 is 3.0 to 5.0. mu.m.
As a preferred embodiment of the conductive paste of the present invention, the weight percentage of the glass frit in the conductive paste is 3% to 8%. The adhesion of the lead-free electronic paste is always a difficult problem, and the adhesion after acid resistance is an insurmountable gap in the past ten years. The content of the glass of the electronic paste not only solves the problem of adhesive force, but also influences the conductivity, so that a proper matching must be found out. Research shows that when the content of the glass powder is 3% -8%, the conductivity, the corrosion resistance and the adhesive force of the conductor paste are all good.
In a preferred embodiment of the conductive paste of the present invention, the glass frit has a softening point of 700 to 900 ℃. The softening point of the glass frit is selected in relation to the sintering temperature at the application end, and the softening point of the glass frit is selected to be lower than the sintering temperature in order to help the silver powder to melt, drive the silver layer powder to realign, lower the sintering temperature (the melting point of silver is 950 ℃ if no glass frit is present), and penetrate the alumina substrate. The glass with the softening point of 700-900 ℃ is selected, has good wettability and permeability with an alumina matrix, can drive metal powder to flow in the sintering process, can form a new phase with an alumina material, firmly attaches a silver layer on the surface of the chip resistor, has strong acid corrosion resistance, and avoids being influenced by environmental factors. Preferably, the glass powder is Si-Zr-B-Mg system glass. More preferably, the preparation method of the Si-Zr-B-Mg system glass comprises the following steps: the material is prepared by burdening, mixing, sintering at 1600 ℃, quenching, coarse grinding, fine grinding and drying. The glass transition temperature of the obtained glass is 800 ℃, particularly, after the prepared conductor slurry is tested and soaked for one hour by 5 percent hydrochloric acid, the adhesive force of the silver layer and the alumina substrate is more than or equal to 3 kg.
As a preferred embodiment of the conductive paste of the present invention, the glass frit has a tap density of 1.0 to 4.8g/ml and a specific surface area of 1.0 to 12.0m2(ii)/g, particle size distribution D50 is 1.5-5.0. mu.m.
As a preferred embodiment of the conductive paste of the present invention, the organic vehicle comprises the following components in percentage by weight: 80-92% of organic solvent and 8-20% of polymer resin. The preparation method of the organic carrier comprises the following steps: uniformly mixing an organic solvent in a water bath at the temperature of 80-90 ℃, slowly adding high molecular resin under the stirring state, and fully dissolving to obtain the organic carrier. The viscosity of the slurry is regulated and controlled by the content of the high molecular resin in the organic carrier, the fluidity of the slurry is determined, and the quality of screen printing is ensured, so that the performance of a chip resistor product is ensured.
As a preferred embodiment of the conductor paste of the present invention, the organic solvent is at least one of terpineol, turpentine, diethylene glycol ethyl ether acetate, butyl carbitol, perchloroethylene, trichloroethylene, ethylene glycol ether aromatic hydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, and oleic acid; the polymer resin is at least one of ethyl cellulose, polyvinyl butyral resin, hydroxyethyl cellulose, acrylic resin, hydrogenated rosin, hydrogenated castor oil, aldehyde ketone resin and cellulose acetate butyrate.
In addition, the invention provides a conductor material, and the preparation method of the conductor material comprises the following steps: and coating the conductor slurry on the surface of a base material through screen printing, and then sintering to obtain the conductor material.
As a preferred embodiment of the conductor material of the present invention, the substrate is an alumina substrate.
As a preferred embodiment of the conductor material of the present invention, the conductor material is a resistor; more preferably, the conductor material is a ceramic resistor; further, the conductor material is a chip ceramic resistor.
Compared with the prior art, the invention has the beneficial effects that:
(1) the silver content in the conductor paste is reduced, the production cost of chip resistor production enterprises is reduced, the market share and profit margin of domestic components are improved, and the competitive advantage with imported components is improved.
(2) The conductive slurry of the invention introduces graphene, which is a novel conductive material, and can further improve the conductive performance of the slurry coating.
(3) Due to the special formula of the conductor paste, the problem of production cost is solved, and new problems caused by reduction of silver content, such as poor conductivity, poor compactness of a silver layer and the like, are solved.
Drawings
FIG. 1 is a flow chart of the preparation of an organic vehicle and conductor paste according to the present invention;
FIG. 2 is a photographic image of a conductive paste according to the present invention;
FIG. 3 is a photographic image of the conductive material of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Examples 1 to 4
The compositions of the conductive pastes of examples 1 to 4 of the present invention are shown in table 1 below.
TABLE 1
In the above embodiments, the preparation/treatment methods of the graphene, the glass frit, the organic carrier, and the conductor paste of embodiments 1 to 5 are as follows:
coating the surface of graphene: adding a surfactant into graphene, soaking and wetting the graphene for 6 hours by using the surfactant, and then drying at 60 ℃ for later use. A layer of substance is coated on the surface of the graphene, so that the protection effect is achieved, the subsequent air environment operation process is facilitated, and the graphene can be uniformly dispersed into a carrier system by the coated substance.
The preparation method of the glass powder comprises the following steps: and (3) ball-milling the glass (such as microcrystalline glass) for 3 hours by using a planetary ball mill, and detecting for later use.
The preparation method of the organic carrier comprises the following steps: firstly drying the polymer resin, then uniformly mixing the organic solvent in a water bath at the temperature of 80-90 ℃, then slowly adding the polymer resin in a high-speed stirring state, fully dissolving, filtering, and standing to obtain the organic carrier. The preparation process of the organic vehicle is shown in FIG. 1.
The preparation method of the conductor paste in the embodiment 1-5 comprises the following steps: after the surface of graphene is coated, firstly, mixing the graphene, glass powder and an organic carrier, performing ball milling, then adding silver powder, rolling slurry, filtering, stirring to obtain a semi-finished product, and further adjusting to obtain a finished product of the conductor slurry. The preparation process of the conductive paste of examples 1 to 5 is shown in FIG. 1, and the appearance is shown in FIG. 2.
The conductive paste of examples 1 to 5 was coated on the surface of the base material by screen printing, and then sintered to obtain a conductive material, the appearance of which is shown in fig. 3.
Effect example 1
In order to investigate the influence of the proportion of spherical silver powder and flake silver powder and the content of glass powder and graphene in the conductor paste on the performance of the conductor material, the invention uniformly mixes the components according to the formula in the following table 2 to prepare the conductor paste, and then the conductor paste is coated on the surface of a base material by screen printing and sintered to obtain the conductor material (the chip resistor). After that, the resulting chip resistors were examined for the thickness of the printed film, the resistivity, the corrosion resistance and the average adhesion, and the results are shown in table 3. The specific detection method comprises the following steps: 1. the thickness of the printed film is as follows: detecting with a film thickness tester, wherein the standard of the film thickness is 5-8 μm; 2. resistivity: a resistivity tester is used, and the standard is less than or equal to 25m omega; 3. corrosion resistance: soaking the fired printing pattern in 5% HCl for 1 hour, and sticking and tearing the printing pattern by using a high-temperature adhesive tape without falling off to obtain a qualified printing pattern; 4. adhesion force: adhesion tester: welding a lead on the sintered silver layer, and judging the combination effect of the silver layer and the alumina substrate by drawing the lead by using a tester, wherein the standard is as follows: not less than 3 kg.
TABLE 2
TABLE 3
As can be seen from Table 3, the weight ratio of the spherical silver powder to the plate-like silver powder was 9: 1-2: 3, the conductive paste has good appearance and moderate viscosity, can be further debugged, and is not suitable for screen printing because the viscosity of the paste is increased and the fluidity of the paste is poor along with the increase of the flaky silver powder. The content of the glass powder in the conductor paste is 3% -8% or the content of the graphene is 0.01% -20%, and the conductor material prepared from the conductor paste has better performance.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The conductor paste is characterized by comprising the following components in percentage by weight: 20-40% of silver powder, 0.01-20% of graphene, 1-8% of glass powder and 45-70% of organic carrier.
2. The conductor paste according to claim 1, wherein the silver powder comprises spherical silver powder.
3. The conductor paste according to claim 2, wherein the silver powder is composed of spherical silver powder and plate-like silver powder, and a weight ratio of the spherical silver powder to the plate-like silver powder is 9: 1-2: 3.
4. the conductor paste according to claim 2 or 3, wherein the spherical silver powder has a shake ratio of 3.5 to 5.0g/cm3The specific surface area is 0.2-8.0m2(ii)/g, particle size distribution D50 is 3.0-5.0 μm; the shaking-out ratio of the flake silver powder is 1.5-3.6g/cm3The specific surface area is 0.5-1.3m2(iv)/g, particle size distribution D50 is 5.0-9.0. mu.m.
5. The conductive paste according to claim 1, wherein the graphene has a tap density of 0.7 to 6.2g/mL and a specific surface area of 3.0 to 12.0m2(ii)/g, the particle size distribution D50 is 3.0 to 5.0. mu.m.
6. The conductive paste according to claim 1, wherein the glass frit is present in the conductive paste in an amount of 3 to 8% by weight.
7. The conductive paste according to claim 1, wherein the glass frit has a softening point of 700 to 900 ℃.
8. The conductive paste according to claim 1, 6 or 7, wherein the glass frit has a tap density of 1.0 to 4.8g/ml and a specific surface area of 1.0 to 12.0m2(ii)/g, particle size distribution D50 is 1.5-5.0. mu.m.
9. The conductive paste of claim 1, wherein the organic vehicle comprises the following components in weight percent: 80-92% of organic solvent and 8-20% of polymer resin.
10. The conductor material is characterized in that the preparation method of the conductor material comprises the following steps: the conductive material is obtained by applying the conductive paste according to any one of claims 1 to 9 to the surface of a base material by screen printing and then sintering.
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| CN201911302883.0A CN110942842A (en) | 2019-12-17 | 2019-12-17 | Conductor paste and conductor material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592785A (en) * | 2020-05-26 | 2020-08-28 | 南京精进材料科技有限公司 | Application of graphene, spraying slurry for filter, preparation method of spraying slurry and filter |
| CN112791801A (en) * | 2020-12-18 | 2021-05-14 | 中国振华集团云科电子有限公司 | Method for improving quality consistency of glass powder |
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| CN109785994A (en) * | 2018-12-29 | 2019-05-21 | 广州市儒兴科技开发有限公司 | A kind of PERC battery backplane slurry and preparation method thereof |
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2019
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| JP2000331535A (en) * | 1999-05-20 | 2000-11-30 | Toray Ind Inc | Conductor paste |
| CN104464883A (en) * | 2014-12-26 | 2015-03-25 | 苏州格瑞丰纳米科技有限公司 | Graphene electrocondution slurry with dispersants adsorbed on surface and manufacturing method and application thereof |
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| CN111592785A (en) * | 2020-05-26 | 2020-08-28 | 南京精进材料科技有限公司 | Application of graphene, spraying slurry for filter, preparation method of spraying slurry and filter |
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| CN112791801A (en) * | 2020-12-18 | 2021-05-14 | 中国振华集团云科电子有限公司 | Method for improving quality consistency of glass powder |
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