CN113782251A - Electrode paste, electrode thick film and preparation method thereof - Google Patents
Electrode paste, electrode thick film and preparation method thereof Download PDFInfo
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- CN113782251A CN113782251A CN202111054181.2A CN202111054181A CN113782251A CN 113782251 A CN113782251 A CN 113782251A CN 202111054181 A CN202111054181 A CN 202111054181A CN 113782251 A CN113782251 A CN 113782251A
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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
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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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The invention relates to the technical field of electrode paste materials, in particular to an electrode paste, an electrode thick film and a preparation method thereof, wherein the electrode paste comprises 70-90 wt% of metal powder, 1-8 wt% of glass composition, 5-30 wt% of organic binder and 2-30 wt% of solvent. Wherein the glass composition is Li2O‑ZnO‑Al2O3‑Na2O‑SrO‑V2O5‑B2O3‑SiO2. The electrode paste is sintered at a lower temperature, and the prepared electrode thick film has excellent electrical performance.
Description
Technical Field
The invention relates to the technical field of electrode paste materials, in particular to an electrode paste, an electrode thick film and a preparation method thereof.
Background
In current electronic products, the resistor is one of the most widely used passive components, and the application range includes high frequency chip resistors, vehicle-mounted electronic products, consumer electronic products, and household electrical appliances. The common thick film chip resistor is printed by adopting a thick film process, has various shapes and is mainly applied to power resistors and precision resistors.
In the conductive paste manufacturing technology of the thick film chip resistor, the conductive metal powder is mainly precious metal powder such as gold or silver, and particularly, the silver powder is most widely applied. However, in addition to the high cost, when silver metal is used as a material of the conductive paste and applied to a capacitor or a resistor, the silver ion mobility is high under the damp and hot conditions, so the electrical property of the device itself is easily affected.
In order to solve the above problems, there is a trend of using relatively inexpensive base metals (also referred to as base metals) instead of noble metals as conductive materials, for example, copper, nickel, or aluminum metals. Although aluminum metal has better chemical stability, the adhesion between aluminum metal and the substrate and the sulfuration resistance test result are not as expected when the aluminum metal is used as an electrode. While sintering in a low oxygen state is required due to stability problems when using copper or nickel metal as an electrode, most of the current solutions use glass powder including rare earth metal doping, which is expensive and has less than desirable high frequency conductivity characteristics.
Therefore, there is an urgent need to develop a new electrode paste, which has excellent adhesion and low dielectric loss characteristics with a substrate material, besides using base metal to replace precious metal to greatly reduce the preparation cost, and can be sintered at a relatively low temperature and compact compared with silver electrode material, especially can be co-fired at one time when applied to a ceramic substrate of a chip resistor, thereby greatly reducing the sintering cost and simplifying the preparation process.
Disclosure of Invention
The invention aims to provide an electrode paste, an electrode thick film and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
an electrode paste comprising 70 to 90 wt% of metal powder, 1 to 8 wt% of a glass composition, 5 to 30 wt% of an organic binder, and 2 to 30 wt% of a solvent;
wherein the glass composition is Li2O-ZnO-Al2O3-Na2O-SrO-V2O5-B2O3-SiO2Comprising 0.5 to 5 wt% of Li2O, 20-50 wt% of ZnO, and 1-5 wt% of Al2O31 to 10 wt% of Na2O, 0.5 to 5 wt% of SrO, and 1 to 15 wt% of V2O520 to 50 wt% of B2O3And 1 to 10 wt% of SiO2。
Further, the electrode paste is sintered under inert gas, and the sheet resistance of the prepared electrode thick film is less than 7m omega.
Further, the softening point of the glass composition is 400-900 ℃.
Further, the average particle diameter of the glass composition is 1 to 10 μm.
Further, the metal powder is copper powder, silver-coated copper powder or BaTiO3And (3) pulverizing.
Further, the average particle size of the metal powder is 0.1-10 μm.
Further, the organic binder is thermosetting resin, thermoplastic resin or a mixture of the thermosetting resin and the thermoplastic resin. Wherein the thermosetting resin is at least one selected from the group consisting of epoxy resin, urethane resin, vinyl ester resin, silicone resin, phenol resin, urea resin, melamine resin, unsaturated polyester resin, diallyl phthalate resin, and polyimide resin; the thermoplastic resin is at least one selected from ethyl cellulose, acrylic resin, alkyd resin, saturated polyester resin, butyral resin, polyvinyl alcohol and hydroxypropyl fiber.
Further, the solvent is at least one selected from the group consisting of organic acids, aromatic hydrocarbons, pyrrolidones, amides, ketones, and cyclic carbonates. Wherein the organic acid can be diethylene glycol ethyl ether acetate, diethylene glycol butyl ether acetate or ethyl acetate; the aromatic hydrocarbon may be toluene, or xylene; the pyrrolidones can be N-methyl-2-pyrrolidones (NMP); the amide may be N, N-Dimethylformamide (DMF); such ketones may be, for example, Methyl Ethyl Ketone (MEK); the cyclic carbonate may be Terpineol (Terpineol) or Butyl Carbitol (BC).
Further, the viscosity of the electrode paste is 20 to 100Pa · s.
Further, the electrode paste further comprises a metal oxide, wherein the metal oxide is at least one selected from copper oxide, bismuth oxide, manganese oxide, cobalt oxide, magnesium oxide, tantalum oxide, niobium oxide and tungsten oxide.
In addition, the electrode paste may further include at least one additive, such as a dispersant, a rheology modifier, a pigment, an inorganic filler, a coupling agent, a silane monomer, and an antifoaming agent. It will be apparent to those skilled in the art that at least one additive as described above may be added as desired.
The preparation method of the electrode thick film prepared from the electrode paste comprises the following steps:
(1) preparing electrode paste;
(2) and coating the electrode paste on a substrate, and sintering under inert gas to obtain the electrode thick film.
Wherein, in the step (2), the base material is a ceramic substrate.
Wherein, in the step (2), the sintering temperature is below 900 ℃.
Wherein, in the step (2), the sheet resistivity of the prepared electrode thick film is less than 7m omega.
Wherein, in the step (2), the adhesion tension between the prepared electrode thick film and the ceramic substrate is 2-3 kg.
Compared with the prior art, the invention has the beneficial effects that:
the glass composition in the electrode paste of the invention is Li2O-ZnO-Al2O3-Na2O-SrO-V2O5-B2O3-SiO2The glass composition has a low glass softening point of 400-900 ℃, so that the electrode paste has excellent sintering adhesion at a low temperature of 450-850 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
EXAMPLE 1 preparation of electrode paste
First, take Li2O、ZnO、Al2O3、Na2O、SrO、V2O5、B2O3、SiO2Powder, based on the total weight, is stirred and mixed according to the following proportions: 0.5 to 5 wt% of Li2O, 20-50 wt% of ZnO, and 1-5 wt% of Al2O31 to 10 wt% of Na2O, 0.5 to 5 wt% of SrO, and 1 to 15 wt% of V2O520 to 50 wt% of B2O3And 1 to 10 wt% of SiO2。
The powder is stirred and mixed and then put into a crucible carrier, the powder and the crucible carrier are heated to 1000 to 1500 ℃ by a resistance furnace together for melting for 2 to 4 hours, and then the powder and the crucible carrier are quickly poured into deionized water for water extraction to obtain blocky molten glass blocks. Then, the molten glass gob is ground by a rough mill, a fine mill, a bead mill or the like for about 24 hours to form a powdery glass composition having an average particle diameter of 1 to 5 μm and a glass softening point of 400 to 900 ℃. The average particle diameter referred to herein means a volume-based average particle diameter (d50) obtained by a laser diffraction scattering particle size distribution measurement method, and the softening point of the glass frit is measured by a thermogravimetric apparatus (TG-DTA instrument).
In the present embodiment, the metal powder has a particle size of 0.1 to 10 μm, and it is preferable to increase the particle size of the metal powder in the electrode paste in order to exhibit the conductivity of the electrode paste. However, if the particle size of the metal powder is too large, the coating property or workability on the substrate may be affected. Or, when the external electrode of the multilayer ceramic electronic component is formed by using the electrode paste, the adhesion of the electrode paste to the ceramic body is impaired. Therefore, it is preferable to use metal powder having a large particle size as long as the electrode paste does not impair coatability or adhesion to the substrate or to the ceramic body. When considering these points, the average particle diameter of the metal powder used in the present invention is preferably in the range of 0.1 to 10 μm. The method for producing the metal powder is not particularly limited, and for example, the metal powder can be produced by a reduction method, a pulverization method, an electrolysis method, an atomization method, a heat treatment method, or a combination thereof. The flake-like metal powder can be produced, for example, by grinding spherical or granular metal particles by a ball mill or the like.
The organic binder may be a thermosetting resin, a thermoplastic resin, or a mixture thereof in the embodiment, wherein the thermosetting resin may be an epoxy resin, an amine ester resin, a vinyl ester resin, a silicone resin, a phenol resin, a urea resin, a melamine resin, an unsaturated polyester resin, a diallyl phthalate resin, or a polyimide resin; the thermoplastic resin may be ethyl cellulose, acrylic resin, alkyd resin, saturated polyester resin, butyral resin, polyvinyl alcohol, or hydroxypropyl cellulose. The use of the organic binder mainly allows the metal powders in the electrode paste to be connected to each other and removed by burning when the electrode paste is sintered.
The solvent is at least one of organic acids, aromatic hydrocarbons, pyrrolidones, amides, ketones and cyclic carbonates, wherein the organic acids can be diethylene glycol ethyl ether acetate, diethylene glycol butyl ether acetate, ethyl acetate and the like; the aromatic hydrocarbon may be toluene, xylene, or the like; the pyrrolidones can be N-methyl-2-pyrrolidones (NMP), etc.; the amide may be N, N-Dimethylformamide (DMF), etc.; the ketone may be Methyl Ethyl Ketone (MEK), etc.; the cyclic carbonate may be Terpineol (Terpineol) or Butyl Carbitol (BC). The selection of the organic binder and the composition of the solvent can be made by those skilled in the art according to actual requirements, which belong to the field of the art and are not further discussed herein.
Then, 70 to 90 wt% of metal powder (copper powder, silver-coated copper powder (Ag/Cu:20/80 wt%), or BaTiO is taken3Powder) 1 to 8The glass composition comprises the above powdered glass composition, 5-30 wt% of organic binder and 2-30 wt% of solvent. The electrode paste of the present invention is obtained by mixing thoroughly, grinding and dispersing with a three-roll mill, filtering and defoaming.
In other embodiments, the procedure of grinding and dispersing the above materials may be performed using a bead mill, a ball mill, a rotary mixer, a biaxial mixer, or the like.
In other embodiments, the electrode paste may further comprise additives, such as dispersing agents, rheology modifiers, pigments, inorganic fillers (e.g., zinc oxide, barium carbonate powder, etc.), coupling agents (e.g., silane coupling agents such as gamma-glycidoxypropyltrimethoxysilane, titanate coupling agents such as tetraoctylbis (ditridecylphosphite) titanate, etc.), silane monomers (e.g., tris (3- (trimethoxysilyl) propyl) isocyanurate), or defoamers to further modify the characteristics of the electrode paste, increase its coatability, stability, etc.
In other embodiments, metal oxides may be added to the electrode paste as needed, for example, copper oxide, bismuth oxide, manganese oxide, cobalt oxide, magnesium oxide, tantalum oxide, niobium oxide, or tungsten oxide may be added. When the electrode paste contains a metal oxide, the solder heat resistance of the electrode paste is improved. In particular, when bismuth oxide is added, sintering of the metal powder is promoted and the solder wettability of the conductive paste is improved.
The viscosity of the electrode paste prepared in this example is 20 to 100Pa · s, and the electrode paste has good coating properties and handling properties, and can be uniformly coated on a substrate.
EXAMPLE 2 preparation of thick electrode films
First, a ceramic substrate is provided, which is obtained by pressing the laminated dielectric sheet and then sintering the dielectric sheet.
Coating the electrode paste on the end face of the ceramic substrate, then putting the ceramic substrate coated with the electrode paste into an electric furnace, and carrying out a sintering process at a temperature of 850-900 ℃ in an inert gas environment, wherein metal powder in the electrode paste is mutually sintered and organic binder, solvent and other components in the electrode paste are burnt off by the sintering process, so that an electrode thick film with a conductive pattern is obtained, and the formed electrode thick film has extremely high conductivity and excellent electromigration resistance, solder heat resistance and adhesiveness to the ceramic substrate.
In order to show more clearly that the specific glass composition and the base metal copper or silver-coated copper powder (Ag/Cu:20/80 wt%) are used as metal powder, which do contribute to the excellent electrical property of the electrode paste and the prepared electrode thick film and the excellent adhesion between the electrode paste and the ceramic substrate, the following test examples are that the electrode thick film is prepared on the ceramic substrate by using the commercially available silver electrode paste and the electrode paste provided by the invention, and the electrode thick film is used for a vulcanization resistance test using type ASTMB809-95 vulcanization tester, wherein water, potassium nitrate and vulcanization powder are used as media, a thick film chip sample is heated to 60-90 ℃ for 800 & lt 1000 & gt lifetime test, and the electrode adhesion pull test (model AMETEK-LS1, the wire diameter of a tinned copper wire is 3.5mm, and the wire length is 15mm is used for welding two ends of the test piece, and then a tensile test is performed at a speed of 30 mm/min).
Wherein, comparative example 1 is silver-palladium electrode paste (PP-8020) of Taiwan corporation, China, comparative example 2 is silver electrode paste (PE-7015) of Taiwan corporation, China, and examples 1 to 5 to 9 are electrode pastes provided by the present invention, wherein the metal powder is copper powder, and the test results are as the following table 2; in addition, examples 6 to 10-9 used the electrode paste according to the present invention, in which the metal powder was silver-coated copper (Ag/Cu:20/80 wt%) powder, and the test results were as shown in Table 2 below. Table 1 shows the glass composition ratios.
TABLE 1 glass composition proportions and numbering
| Firm of the type | Li2O | ZnO | Al2O3 | Na2O | SrO | V2O5 | B2O3 | SiO2 | Hei |
| 1 | 2.20 | 28.49 | 0.20 | 7.90 | 1.52 | 14.48 | 35.57 | 9.63 | 100.0 |
| 2 | 4.75 | 18.47 | 2.54 | 3.28 | 0.71 | 12.07 | 48.15 | 10.00 | 100.0 |
| 3 | 1.41 | 49.00 | 0.05 | 5.07 | 3.97 | 13.77 | 22.40 | 4.38 | 100.0 |
| 4 | 1.13 | 43.82 | 1.64 | 4.05 | 0.78 | 10.55 | 30.06 | 8.00 | 100.0 |
| 5 | 1.07 | 40.68 | 1.56 | 3.85 | 3.74 | 7.46 | 34.51 | 7.13 | 100.0 |
| 6 | 0.96 | 36.39 | 1.39 | 3.44 | 0.66 | 9.36 | 41.40 | 6.38 | 100.0 |
| 7 | 0.85 | 32.11 | 3.23 | 1.04 | 0.58 | 8.26 | 48.30 | 5.63 | 100.0 |
| 8 | 0.73 | 27.83 | 4.06 | 2.63 | 0.51 | 9.16 | 50.19 | 4.88 | 100.0 |
| 9 | 1.62 | 26.65 | 4.90 | 2.23 | 5.30 | 6.06 | 49.08 | 4.13 | 100.0 |
| 10 | 3.75 | 27.37 | 2.54 | 9.28 | 4.71 | 5.07 | 38.15 | 9.10 | 100.0 |
TABLE 2
As can be seen from the test results in table 2, the thick electrode film prepared from the electrode paste of the present invention has a relatively high adhesion to the ceramic substrate under the high temperature 300 cycles (corresponding to 2 years) of the anti-vulcanization test, has a superior adhesion property, and shows that the resistance changes less than 1% after the anti-vulcanization test, which indicates that the thick electrode film can maintain excellent electrical characteristics for a long time.
In summary, the electrode paste provided by the invention can be used for preparing electronic components with excellent electrical characteristics, and is particularly suitable for co-firing with a ceramic substrate to form external electrodes on the end face of the ceramic substrate so as to prepare a laminated ceramic electronic component.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (16)
1. An electrode paste characterized in that: comprises 70-90 wt% of metal powder, 1-8 wt% of glass composition, 5-30 wt% of organic binder and 2-30 wt% of solvent;
wherein the glass composition is Li2O-ZnO-Al2O3-Na2O-SrO-V2O5-B2O3-SiO2Comprising 0.5 to 5 wt% of Li2O, 20-50 wt% of ZnO, and 1-5 wt% of Al2O31 to 10 wt% of Na2O, 0.5 to 5 wt% of SrO, and 1 to 15 wt% of V2O520 to 50 wt% of B2O3And 1 to 10 wt% of SiO2。
2. The electrode paste according to claim 1, wherein: and sintering the electrode paste in inert gas, wherein the sheet resistance of the prepared electrode thick film is less than 7m omega.
3. The electrode paste according to claim 1, wherein: the softening point of the glass composition is 400-900 ℃.
4. The electrode paste according to claim 1, wherein: the average particle diameter of the glass composition is 1 to 10 μm.
5. The electrode paste according to claim 1, wherein: the metal powder is copper powder, silver-coated copper powder or BaTiO3And (3) pulverizing.
6. The electrode paste according to claim 1, wherein: the average particle size of the metal powder is 0.1-10 μm.
7. The electrode paste according to claim 1, wherein: the organic binder is thermosetting resin, thermoplastic resin or a mixture of the thermosetting resin and the thermoplastic resin.
8. The electrode paste according to claim 1, wherein: the solvent is at least one selected from organic acids, aromatic hydrocarbons, pyrrolidones, amides, ketones and cyclic carbonates.
9. The electrode paste according to claim 1, wherein: the viscosity of the electrode paste is 20 to 100 pas.
10. The electrode paste according to claim 1, wherein: the metal oxide is at least one selected from copper oxide, bismuth oxide, manganese oxide, cobalt oxide, magnesium oxide, tantalum oxide, niobium oxide and tungsten oxide.
11. An electrode thick film obtained by using the electrode paste according to any one of claims 1 to 10.
12. The method for preparing an electrode thick film according to claim 11, comprising the steps of:
(1) preparing an electrode paste according to any one of claims 1 to 10;
(2) and coating the electrode paste on a substrate, and sintering under inert gas to obtain the electrode thick film.
13. The method for preparing an electrode thick film according to claim 12, wherein: in the step (2), the base material is a ceramic substrate.
14. The method for preparing an electrode thick film according to claim 12, wherein: in the step (2), the sintering temperature is below 900 ℃.
15. The method for preparing an electrode thick film according to claim 12, wherein: in the step (2), the sheet resistivity of the prepared electrode thick film is less than 7m omega.
16. The method for preparing an electrode thick film according to claim 12, wherein: in the step (2), the adhesion tension between the prepared electrode thick film and the ceramic substrate is 2-3 kg.
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| CN102426871A (en) * | 2010-08-18 | 2012-04-25 | 住友金属矿山株式会社 | Composition for forming a thick film conductor, the thick film conductor obtained by using the same and the chip resistor using the same |
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