CN105788699A - High-temperature and high-humidity resistant electrode silver paste for ZnO piezoresistor and preparation method for electrode silver paste - Google Patents
High-temperature and high-humidity resistant electrode silver paste for ZnO piezoresistor and preparation method for electrode silver paste Download PDFInfo
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Abstract
The invention discloses high-temperature and high-humidity resistant electrode silver paste for a ZnO piezoresistor. The conductive silver paste comprises the following components in percentage by weight: 52-80% of metal silver powder, 2-5% of glass powder, 10-30% of organic carrier, 1-3% of organic additives and 1-10% of organic solvent; the preparation method for the electrode silver paste comprises the steps of uniformly mixing the organic carrier and the organic solvent to prepare a uniform colloidal solution; then adding the other components in sequence; and enabling the mixture to be mixed through a mixer, grinded through a three-roll mill, and the like to obtain the high-temperature and high-humidity resistant electrode silver paste for the ZnO piezoresistor. Compared with the prior art, the electrode silver paste for the ZnO piezoresistor prepared by the invention is high in adhesive force, high in circulation volume, high in voltage resistance, low in ohmic contact resistance, high in flatness, excellent in structural compactness, and excellent in high-temperature and high-humidity resistance.
Description
Technical field
The invention belongs to technical field of electronic materials, relate to a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm and preparation method thereof.
Background technology
Varistor ceramics materials refer at a certain temperature with a kind of semiconductor ceramic material that in a certain particular voltage range, there is nonlinear wind vibration, its resistance strongly reduces with the increase of voltage.According to this nonlinear wind vibration, it is possible to make nonlinear resistor with this semiconductor ceramic material, i.e. piezoresistor.At present, being of wide application of piezoresistor, it is possible to for spark-extinguishing, overvoltage protection, prepare discharging rod, voltage standard and voltage stabilization etc..In recent years, owing to electronic equipment develops to miniaturization, multifunction, the integrated speed of integrated circuit and density improve constantly, and in order to make electronic circuit exempt from the destruction of surge voltage, in low-pressure field, the application of piezoresistor be it is also proposed increasingly higher requirement.Since the nineties in 20th century, people are to existing ZnO system, TiO2System, SrTiO3System and BaTiO3Series pressure-sensitive ceramic material should be used as substantial amounts of research work in low pressure range, and achieves some achievements in research.
Wherein, ZnO system is the one that in varistor ceramics materials, performance is the most excellent, and ZnO varistor ceramic material is in main component ZnO, adds B2O3、Bi2O3、SiO2、Al2O3、TiO2、Co2O3、MnO2、Cr2O3、Sb2O3Forming with the oxide modifying such as PbO sintering, the effect of additive is mostly be segregated on crystal boundary formation barrier layer, and another part additive plays and reduces sintering temperature and control the effect of crystallite dimension.ZnO varistor ceramic material due to its there is cost performance height, the advantage such as non-ohmic behavior is excellent, response time is fast, leakage current is little, negotiability is strong and energy tolerance is big; therefore the fields such as industry, railway, communication, electric power and household electrical appliances it are widely used in, especially in overvoltage protection.
But, existing industrial ZnO varistor product generally uses the erosion that epoxy resin and phenolic resin carry out resisting hot and humid environment as encapsulating material, and being typically only capable to could normal operation lower than 85 DEG C when.Along with deepening continuously of application, use temperature and the use humidity of varistor are proposed higher technology requirement by various product, for instance, the varistor in automobile circuit uses temperature up to 125～150 DEG C.The electrode slurry that traditional ZnO varistor uses in preparation process is mainly leaded silver slurry, is mainly made up of argentum powder, lead bearing glass powder, organic resin and solvent.And leaded silver slurry reproduction and use procedure in all can to environment, health risk.Therefore, the research for high-temp resisting high-humidity resisting varistor lead-free silver slurry is more and more important.
Application number be 201110202073.5 Chinese invention patent disclose a kind of environment-friendly type piezoresistor electrode silver plasm and preparation method thereof, the piezoresistor electrode silver plasm of this patent disclosure, in mass fraction, including the argentum powder of 60～80 parts, the nikel powder of 2～4 parts, the glass dust of 1～3 part, the organic bond of 11～25 parts and 3～11 parts diluent；Described glass dust is by Bi2O3、SiO2、SrO、ZnO、B2O3And Li2At 900～1200 DEG C of sintering after the mixing of O powder；Described organic bond is with organic solvent for solvent, in mass fraction, and ethyl cellulose including 10～20% and the phenolic resin of 5～10%；Described organic solvent is one or more in butyl carbitol, propylene glycol methyl ether acetate, ethylene glycol, ethylene glycol monomethyl ether acetate, petroleum ether, Oleum Terebinthinae, terpineol；Described diluent is one or more in butyl carbitol, propylene glycol methyl ether acetate, ethylene glycol, ethylene glycol monomethyl ether acetate, petroleum ether, Oleum Terebinthinae, terpineol, Oleum Ricini, Ketohexamethylene.In the technical scheme of above-mentioned patent disclosure, the argentum powder of employing and the particle diameter of glass dust are relatively big, and this can affect the performance of high-temp resisting high-humidity resisting of final electrode silver plasm, the selection in glass dust kind and argentum powder kind, is further improved.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide one to can be used in high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 52～80%, glass dust 2～5%, organic carrier 10～30%, organic additive 1～3% and organic solvent 1～10%.
The component of described electrode silver plasm and weight percent content are preferably: silver powder 56～78%, glass dust 2～3%, organic carrier 14～28%, organic additive 1～3% and organic solvent 5～10%.
Described silver powder is spherical argentum powder, and particle diameter is 0.5～2.0 μm, and tap density is 2.0～3.0g/ml.
Described glass dust is lead-free glass powder, and thermal coefficient of expansion is 110～120 × 10-7/ DEG C, sintering temperature is 550～750 DEG C, and described glass dust includes following components and weight percent content: Bi2O375～85%, ZnO5～15%, B2O33～10%, SiO21～5%, Na2O1～3%, TiO20～3% and Al2O30～2%.
Described organic carrier is mixed by macromolecule resin and organic solvent, concrete preparation method is: be 1:4 by the mass ratio of macromolecule resin Yu organic solvent, macromolecule resin is joined in organic solvent, it is heated to 70～80 DEG C, constant temperature, until macromolecule resin is completely dissolved, it is filtered remove impurity with the screen cloth of 300～400 orders, namely prepares organic carrier.
Described macromolecule resin includes one or more in ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, wood rosin, and described organic solvent is one or more in terpinol, Oleum Terebinthinae, butyl, dibutyl ethylene glycol ether, butyl carbitol acetate, dipropylene glycol monomethyl ether, Tripropylene glycol monomethyl Ether.
One in described macromolecule resin preferred, ethyl, NC Nitroncellulose or both mixture, the mixture of the preferred terpinol of described organic solvent, Tripropylene glycol monomethyl Ether or butyl and dipropylene glycol monomethyl ether.
Described organic additive includes plasticizer, levelling agent and coupling agent, in described organic additive, the mass ratio between plasticizer, levelling agent and coupling agent three is (1～2): 1:1, and described plasticizer includes one or more in dibutyl phthalate, tributyl citrate, dioctyl phthalate, trioctyl lemon acid；Described levelling agent includes one or more in organic siliconresin, castor oil hydrogenated, polyvinyl butyral resin, polyacrylate；Described coupling agent includes one or more in Silane coupling agent KH550, KH560, KH570.
One in the preferred dibutyl phthalate of described plasticizer or tributyl citrate, the one in the preferred organic siliconresin of described levelling agent, polyvinyl butyral resin or castor oil hydrogenated.
A kind of preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, the method comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, make the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
In the present invention, the preparation process of electrode silver plasm is first by organic carrier and organic solvent mix homogeneously, makes uniform colloid solution, is then sequentially added into other components, through techniques such as batch mixer mixing, three-roll grinder grindings, namely prepare high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Compared with prior art, the invention have the characteristics that:
1) the ultrafine spherical argentum powder owing to adopting particle diameter to be 0.5～2.0 μm, particle diameter is little, the electrode silver plasm of narrowly distributing is after high temperature sintering, the surface of silver layer is finer and close, it is susceptible to the infiltration of dampness, ohmic contact resistance is less, it is possible to be effectively improved the electric conductivity of electrode silver plasm, scolding tin performance and compactness；
2) owing to adopting glass dust, it is possible to effectively solve the pulling force between electrode silver plasm and ZnO pottery, bonding die problem；
3) owing to adopting the organic additive collectively constituted by plasticizer, levelling agent and coupling agent, it is possible to the process industrial art performance of modified electrode silver slurry, and be conducive to improving the performance of the high-temp resisting high-humidity resisting of electrode silver plasm；
4) preparation process is simple, and process conditions are gentle, and the ZnO varistor electrode silver plasm adhesive force preparing gained is strong, high throughput, high proof voltage, and ohmic contact resistance is little, and flatness is good, and compact structure is superior.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 55%, glass dust 3%, organic carrier 29%, organic additive 3% and organic solvent 10%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 0.95 μm, and tap density is 2.2g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 115 × 10-7/ DEG C, sintering temperature is 650 DEG C, and this glass dust includes following components and weight percent content: Bi2O379%, ZnO8%, B2O37%, SiO23%, Na2O2%, TiO20.5% and Al2O30.5%.
Organic carrier is mixed by ethyl cellulose and terpinol, concrete preparation method is: be 1:4 by the mass ratio of ethyl cellulose Yu terpinol, ethyl cellulose is joined in terpinol, it is heated to 80 DEG C, constant temperature, until ethyl cellulose is completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is terpinol.
Organic additive is that dibutyl phthalate, organic siliconresin and Silane coupling agent KH550 are mixed with for 1:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, make the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 2:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 80%, glass dust 2%, organic carrier 16%, organic additive 1% and organic solvent 1%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 1.2 μm, and tap density is 2.5g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 110 × 10-7/ DEG C, sintering temperature is 550 DEG C, and this glass dust includes following components and weight percent content: Bi2O381%, ZnO6.5%, B2O36.5%, SiO22%, Na2O3%, TiO20.5% and Al2O30.5%.
Organic carrier is mixed by NC Nitroncellulose and Tripropylene glycol monomethyl Ether, concrete preparation method is: be 1:4 by the mass ratio of NC Nitroncellulose Yu Tripropylene glycol monomethyl Ether, NC Nitroncellulose is joined in Tripropylene glycol monomethyl Ether, it is heated to 80 DEG C, constant temperature, until NC Nitroncellulose is completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is Tripropylene glycol monomethyl Ether.
Organic additive is that dibutyl phthalate, polyvinyl butyral resin and silane coupler KH560 are mixed with for 2:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 6 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 3:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 70%, glass dust 5%, organic carrier 18%, organic additive 2% and organic solvent 5%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 1.5 μm, and tap density is 3.0g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 120 × 10-7/ DEG C, sintering temperature is 750 DEG C, and this glass dust includes following components and weight percent content: Bi2O379%, ZnO8%, B2O37%, SiO23%, Na2O2%, TiO20.5% and Al2O30.5%.
Organic carrier is mixed by ethyl cellulose, NC Nitroncellulose, butyl and dipropylene glycol monomethyl ether, concrete preparation method is: be 1:1:4:4 by the mass ratio of ethyl cellulose, NC Nitroncellulose, butyl and dipropylene glycol monomethyl ether, NC Nitroncellulose is joined in Tripropylene glycol monomethyl Ether, it is heated to 80 DEG C, constant temperature, until NC Nitroncellulose is completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is butyl is the mixed solvent of 1:1 in mass ratio with dipropylene glycol monomethyl ether.
Organic additive is that dibutyl phthalate, polyvinyl butyral resin and silane coupler KH560 are mixed with for 2:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 7 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 4:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 56%, glass dust 3%, organic carrier 28%, organic additive 3% and organic solvent 10%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 0.5 μm, and tap density is 2.0g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 115 × 10-7/ DEG C, sintering temperature is 700 DEG C, and this glass dust includes following components and weight percent content: Bi2O385%, ZnO5%, B2O33%, SiO21%, Na2O1%, TiO23% and Al2O32%.
Organic carrier is mixed by ethylhydroxyethylcellulose and butyl carbitol acetate, concrete preparation method is: be 1:4 by the mass ratio of ethylhydroxyethylcellulose Yu butyl carbitol acetate, ethylhydroxyethylcellulose is joined in butyl carbitol acetate, it is heated to 70 DEG C, constant temperature, until ethylhydroxyethylcellulose is completely dissolved, it is filtered remove impurity with the screen cloth of 300 orders, namely prepares organic carrier.
Organic solvent is butyl carbitol acetate.
Organic additive is that tributyl citrate, castor oil hydrogenated and silane coupler KH570 are mixed with for 1.6:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 3 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 5:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 78%, glass dust 2%, organic carrier 14%, organic additive 1% and organic solvent 5%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 1.5 μm, and tap density is 2.8g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 115 × 10-7/ DEG C, sintering temperature is 750 DEG C, and this glass dust includes following components and weight percent content: Bi2O375%, ZnO15%, B2O33%, SiO25%, Na2O2%.
Organic carrier is mixed by wood rosin and Oleum Terebinthinae, concrete preparation method is: be 1:4 by wood rosin and terebinthine mass ratio, wood rosin is joined in Oleum Terebinthinae, it is heated to 76 DEG C, constant temperature, until wood rosin is completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is Oleum Terebinthinae.
Organic additive is that dioctyl phthalate, polyacrylate and Silane coupling agent KH550 are mixed with for 1.2:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 5 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 6:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 55%, glass dust 5%, organic carrier 30%, organic additive 2% and organic solvent 8%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 0.8 μm, and tap density is 2.4g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 110 × 10-7/ DEG C, sintering temperature is 550 DEG C, and this glass dust includes following components and weight percent content: Bi2O375%, ZnO6%, B2O310%, SiO25%, Na2O3%, TiO20.5% and Al2O30.5%.
Organic carrier is mixed by ethyl cellulose, NC Nitroncellulose and dibutyl ethylene glycol ether, concrete preparation method is: be 1:1:8 by the mass ratio of ethyl cellulose, NC Nitroncellulose and dibutyl ethylene glycol ether, ethyl cellulose, NC Nitroncellulose are joined in dibutyl ethylene glycol ether, it is heated to 78 DEG C, constant temperature, until ethyl cellulose, NC Nitroncellulose are completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is dibutyl ethylene glycol ether.
Organic additive is that trioctyl lemon acid, polyvinyl butyral resin and silane coupler KH560 are mixed with for 1:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 8 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 7:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 52%, glass dust 5%, organic carrier 30%, organic additive 3% and organic solvent 10%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 0.8 μm, and tap density is 2.4g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 110 × 10-7/ DEG C, sintering temperature is 550 DEG C, and this glass dust includes following components and weight percent content: Bi2O379%, ZnO6%, B2O35%, SiO25%, Na2O3%, TiO21% and Al2O31%.
Organic carrier is mixed by ethyl cellulose, ethylhydroxyethylcellulose and terpinol, concrete preparation method is: be 1:1:8 by the mass ratio of ethyl cellulose, ethylhydroxyethylcellulose and terpinol, ethyl cellulose, ethylhydroxyethylcellulose are joined in terpinol, it is heated to 75 DEG C, constant temperature, until ethyl cellulose, ethylhydroxyethylcellulose are completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is terpinol.
Organic additive is that tributyl citrate, castor oil hydrogenated and silane coupler KH570 are mixed with for 1.7:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 6 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Embodiment 8:
In the present embodiment, a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, this electrode silver plasm includes following components and weight percent content: silver powder 75%, glass dust 5%, organic carrier 10%, organic additive 2% and organic solvent 8%.
Wherein, silver powder is spherical argentum powder, and particle diameter is 2.0 μm, and tap density is 3.0g/ml.Glass dust is lead-free glass powder, and thermal coefficient of expansion is 120 × 10-7/ DEG C, sintering temperature is 700 DEG C, and this glass dust includes following components and weight percent content: Bi2O382%, ZnO10%, B2O33%, SiO21%, Na2O2%, TiO21% and Al2O31%.
Organic carrier is mixed by NC Nitroncellulose, ethylhydroxyethylcellulose and Tripropylene glycol monomethyl Ether, concrete preparation method is: be 1:1:8 by the mass ratio of NC Nitroncellulose, ethylhydroxyethylcellulose and Tripropylene glycol monomethyl Ether, NC Nitroncellulose, ethylhydroxyethylcellulose are joined in Tripropylene glycol monomethyl Ether, it is heated to 80 DEG C, constant temperature, until NC Nitroncellulose, ethylhydroxyethylcellulose are completely dissolved, it is filtered remove impurity with the screen cloth of 400 orders, namely prepares organic carrier.
Organic solvent is Tripropylene glycol monomethyl Ether.
Organic additive is that dioctyl phthalate, organic siliconresin and Silane coupling agent KH550 are mixed with for 1.3:1:1 in mass ratio and form.
In the present embodiment, the preparation method of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm specifically includes following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, grind 9 times, making the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
Claims (10)
1. a high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm, it is characterized in that, this electrode silver plasm includes following components and weight percent content: silver powder 52～80%, glass dust 2～5%, organic carrier 10～30%, organic additive 1～3% and organic solvent 1～10%.
2. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 1, it is characterized in that, the component of described electrode silver plasm and weight percent content are preferably: silver powder 56～78%, glass dust 2～3%, organic carrier 14～28%, organic additive 1～3% and organic solvent 5～10%.
3. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 1, it is characterised in that described silver powder is spherical argentum powder, and particle diameter is 0.5～2.0 μm, and tap density is 2.0～3.0g/ml.
4. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 1, it is characterised in that described glass dust is lead-free glass powder, and thermal coefficient of expansion is 110 × 10-7～120 × 10-7/ DEG C, sintering temperature is 550～750 DEG C, and described glass dust includes following components and weight percent content: Bi2O375～85%, ZnO5～15%, B2O33～10%, SiO21～5%, Na2O1～3%, TiO20～3% and Al2O30～2%.
5. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 1, it is characterized in that, described organic carrier is mixed by macromolecule resin and organic solvent, concrete preparation method is: be 1:4 by the mass ratio of macromolecule resin Yu organic solvent, is joined by macromolecule resin in organic solvent, is heated to 70～80 DEG C, constant temperature, until macromolecule resin is completely dissolved, it is filtered remove impurity with the screen cloth of 300～400 orders, namely prepares organic carrier.
6. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 5, it is characterized in that, described macromolecule resin includes one or more in ethyl cellulose, NC Nitroncellulose, ethylhydroxyethylcellulose, wood rosin, and described organic solvent is one or more in terpinol, Oleum Terebinthinae, butyl, dibutyl ethylene glycol ether, butyl carbitol acetate, dipropylene glycol monomethyl ether, Tripropylene glycol monomethyl Ether.
7. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 6, it is characterized in that, one in described macromolecule resin preferred, ethyl, NC Nitroncellulose or both mixture, the mixture of the preferred terpinol of described organic solvent, Tripropylene glycol monomethyl Ether or butyl and dipropylene glycol monomethyl ether.
8. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 1, it is characterized in that, described organic additive includes plasticizer, levelling agent and coupling agent, in described organic additive, the mass ratio between plasticizer, levelling agent and coupling agent three is (1～2): 1:1, and described plasticizer includes one or more in dibutyl phthalate, tributyl citrate, dioctyl phthalate, trioctyl lemon acid；Described levelling agent includes one or more in organic siliconresin, castor oil hydrogenated, polyvinyl butyral resin, polyacrylate；Described coupling agent includes one or more in Silane coupling agent KH550, KH560, KH570.
9. a kind of high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm according to claim 8, it is characterized in that, one in the preferred dibutyl phthalate of described plasticizer or tributyl citrate, the one in the preferred organic siliconresin of described levelling agent, polyvinyl butyral resin or castor oil hydrogenated.
10. the preparation method of a high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm as claimed in claim 1, it is characterised in that the method comprises the following steps:
(1) get the raw materials ready according to following components and percentage by weight:
(2) preparation of electrode silver plasm: first organic carrier, organic solvent are joined in batch mixer according to percentage by weight in step (1), add silver powder, glass dust and organic additive, after being sufficiently mixed, transfer in high speed dispersor, high speed dispersion is uniform, namely prepares electrode silver plasm；
(3) production of electrode silver plasm: the electrode silver plasm that step (2) prepares is ground in three-high mill, make the fineness of electrode silver plasm less than 10 μm by finely tuning roller, viscosity is 30～50Pa S, namely prepares high-temp resisting high-humidity resisting ZnO varistor electrode silver plasm.
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