CN101582328B - Nanometer silver paste for terminal electrode of multi-layer ceramic capacitor and method for preparing same - Google Patents
Nanometer silver paste for terminal electrode of multi-layer ceramic capacitor and method for preparing same Download PDFInfo
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- CN101582328B CN101582328B CN2009100230835A CN200910023083A CN101582328B CN 101582328 B CN101582328 B CN 101582328B CN 2009100230835 A CN2009100230835 A CN 2009100230835A CN 200910023083 A CN200910023083 A CN 200910023083A CN 101582328 B CN101582328 B CN 101582328B
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Abstract
The invention belongs to the technical field of electronic and micro-electronic materials, and particularly relates to a nanometer silver paste for a terminal electrode of a multi-layer ceramic capacitor and a method for preparing the same. The nanometer silver paste is prepared from the following components by mass percentage: 45 and 80 percent of silver powder of which the grain diameter is between 10 and 100nm, 10 to 40 percent of organic carrier, 1 to 10 percent of boron aluminum titanium silicate glass powder, 1 to 9 percent of dispersant, 0.5 to 9 percent of defoamer and 0.5 to 8 percentof surface active agent, wherein the organic carrier is an ethyl acetate or ethyl acetate system of polyacrylic resin, and the molecular weight of the polyacrylic resin is between 10,000 and 15,000. In the process of producing and processing the paste, no hazard exists, which facilitates environmental protection; the boron aluminum titanium silicate glass powder and the ceramic substrate of the corresponding multi-layer ceramic capacitor are almost the same or similar in physical property, so that the boron aluminum titanium silicate glass powder and the ceramic substrate of the correspondingmulti-layer ceramic capacitor can be formed by co-sintering for one time.
Description
Technical field
The invention belongs to electronics and technical field of microelectronic material, particularly a kind of nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor and preparation method thereof.
Background technology
Along with the develop rapidly of new material, new technology and new science and technology, microelectronic material has also obtained very fast development, more and more approaches daily life.As part indispensable in the microelectronic material, the thick-film technique technology forms integrated circuit or electronic devices and components with various assemblies (as little resistance, little electric capacity etc.) with different electrical properties with the form of thick film silk screen printing, thereby forms highly integrated, stable performance, cheap microelectronic product.
Electrode slurry in the electric slurry is the material of preparation thick film circuit or microelectronic element functional electrode, it is printing various function components and parts such as forming conductivity, resistive element, insulator, capacitance body by functional powders decentralized system in organic binder bond is become slurry on the non-conductive substrate or on the semiconductor substrate.Therefore, the electrode slurry in the electric slurry is the basic material of development microelectronic component, also is the critical material of preparation thick film high accuracy hybrid integrated circuit and other large scale integrated circuit.
Electrode slurry in the electric slurry is a kind of conductor paste that extensively is used as the electrode of electronics and microelectronic component, and being a kind of handle is dispersed in the slurry of making in the organic binder bond as the metal dust of function phase or noble metal powder and inorganic binder.Electric slurry mainly is made up of function phase, organic binder bond, inorganic binder, other additives etc.Wherein, as the function phase mainly contain metal dust or noble metal powder, as bronze, silver powder, platinum powder, copper powder, nickel powder etc.; Because silver powder belongs in the noble metal in several that price is lower, stable performance, good conductive characteristic, is difficult for oxidation in air, has been widely used in electronics industry, mainly makes low-temperature solidified silver paste and medium and high temperature sintering silver and starches.Organic bond as medium mainly contains macromolecule resin, the micromolecule resin waits and serves as, mainly play a part to make slurry to have certain shape, be easy to print or apply, removed fully along with the rising of sintering temperature, along with this part effect in electric slurry of chemical industry development of technology is more and more outstanding, especially when being applied to silk screen printing, the composition that changes organic binder bond just can change printing, drying, the sintering character of electric slurry.Play fixedly as the inorganic bond of bridging agent that electric slurry is generally served as by oxide powder and glass powder to base material, but this composition is lower at the proportion of electric slurry, have in addition do not have.
The development of multilayer ceramic capacitor develops very fast in recent years, and it is more and more towards the number of plies, the direction that bed thickness is more and more thinner develops, make the number of plies of the multilayer ceramic capacitor that unit volume is interior develop into present hundreds and thousands of layers by original tens layers, capacitor volume is also increasing.As the general sintering in neutrality or reducing atmosphere of the electrode slurry of terminal electrode of multi-layer ceramic capacitor, prevent its containing metal and internal electrode generation oxidation.
Research development abroad for the electrode multilayered ceramic capacitors slurry is also very fast, and the electrode slurry that uses on many multilayer ceramic capacitor production lines that China introduces is dependence on import basically also.The company of foreign study silver slurry technology of preparing is also many, the report patent also some, this wherein more representational agglutinating property silver slurry patent is that JP05009623A proposes silver powder as electric conducting material, adopt softening point at 350～620 ℃ flint glass, the interpolation mass content is 0.01～10% transition metal such as iron, cobalt, vanadium, oxides such as manganese, the silver slurry sintering preference temperature of its preparation is 580～680 ℃, but the used glass powder of this silver slurry is high flint glass powder, unfavorable to environment and human beings'health, do not meet the environmental requirement of modern people's growing interest.The glass dust that in Chinese patents CN1903764A, proposes of Samsung motor and for example as the low-temperature sintering agent, melt temperature is about 1100 ℃, though its use is leadless glass powder, but the melt temperature of its glass dust is higher, does not meet the requirement of the energy-saving and emission-reduction of present conservation-minded society.
Along with the multilayer ceramic capacitor Development of Preparation Technology, for the requirement of electrode slurry of preparation electrode multilayered ceramic capacitors be: low more good more and once sintered the finishing of sintering temperature; The reduction of cost of sizing agent; Do not contain harmful elements such as lead, compliance with environmental protection requirements.Along with the fast development of China's electronics industry, multilayer ceramic capacitor also is exponential increase with the demand of electrode slurry.At present, reached a certain scale with producing with the research of metal dust such as gold, silver, copper, nickel etc. for electric slurry, each main company all have oneself independently tandem product sell.But, the multilayer ceramic capacitor of China still depends on import with the electrode slurry major part, domestic multilayer ceramic capacitor still achieves no breakthrough with the electrode silver plasm technology of preparing of electrode slurry, the performance of slurry and the product of foreign vendor still have a certain distance, mainly be owing to can not solve under the not leaded condition that waits harmful element of in sintering temperature low and inorganic binder, multilayer ceramic capacitor is stable with once burning altogether of silver electrode paste and multilayer ceramic capacitor, the yields deficiency of finished product.
Summary of the invention
The problem that the present invention solves is to provide a kind of nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor; make by the nano-silver powder that is dispersed in the organic carrier; intermediate sintering temperature in neutrality or reducing atmosphere; there is not harmfulness in its process of manufacture, can large-scale production, meet existing environmental regulation, can instead of part import silver electrode paste.
The present invention is achieved through the following technical solutions:
A kind of nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor comprises by mass fraction: 45～80% particle diameter is the silver powder of 10～100nm, 10～40% organic carrier, 1～10% boron manosil AS titanium glass powder, 1～9% dispersant, 0.5～9% defoamer and 0.5～8% surfactant;
Described organic carrier is the ethyl acetate or the ethyl acetate system of polyacrylic resin, polyacrylic resin: the mass ratio of ethyl acetate or ethyl acetate is 40～70: 30～60, and polyacrylic resin is one or more of the polymethyl acrylate of molecular weight between 10000～15000, polyethyl acrylate, polymethyl methacrylate.
Described dispersant is one or more of dodecyl sodium sulfate, DP270, glycerine tristearate.
Described defoamer is one or more of calcium carbonate, tricalcium phosphate, polysiloxanes.
Described surfactant is one or more of di-tert-butyl hydroxy toluene, polyvinylpyrrolidone, Si Ban-60.
The preparation method of the above-mentioned nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor is as follows:
1) powder: the silver powder that with load weighted particle diameter is 10～100nm is in the same place with boron manosil AS titanium glass powder, makes carrier with absolute ethyl alcohol, mixes 3～10 hours with ball mill or ball grinder;
2) powder for drying: silver powder that mixes and boron manosil AS titanium glass powder were dried 1～2 hour under 40～80 ℃ of conditions, naturally cool to room temperature then;
3) organic carrier preparation: polyacrylic resin is joined in ethyl acetate or the ethyl acetate, in water-bath under 60～80 ℃ of conditions, constant temperature dissolves polyacrylic resin fully, be cooled to room temperature then, wherein, polyacrylic resin: the mass ratio of ethyl acetate or ethyl acetate is 40～70: 30～60; Polyacrylic resin is one or more of the polymethyl acrylate of molecular weight between 10000～15000, polyethyl acrylate, polymethyl methacrylate;
4) add organic carrier: load weighted organic carrier, dispersant, defoamer and surfactant are joined in the mixture of dried silver powder and boron manosil AS titanium glass powder, fully stir, till mixing, filter and obtain preliminary nanometer silver paste;
5) slurry grinds: preliminary nanometer silver paste is fully ground with three-high mill, check that fineness reaches till 0～2 μ m, cross the nanometer silver paste that 800 purpose screen filtrations obtain being used for terminal electrode of multi-layer ceramic capacitor then.
Compared with prior art, in the present invention, conducting function is mutually for being used for the nanometer silver paste of terminal electrode of multi-layer ceramic capacitor, nano-silver powder is the last word of a kind of silver powder of getting up of development in recent years, obtain industrialization in part company, because its particle diameter reaches nanoscale, is more prone to be uniformly dispersed in slurry, has than the better electric conductivity of super fine silver powder;
Organic carrier has been selected polyacrylic resin ethyl acetate or polyacrylic resin ethyl acetate system, polyacrylic resin is one or more of polymethyl acrylate, polyethyl acrylate, polymethyl methacrylate, molecular weight is between 10000～15000, the physical property that the composition of change organic carrier can be regulated the silver electrode paste of finally making, as viscosity etc., and this resin system thermal decomposition performance in neutrality or reducing atmosphere is good, helps removing behind sintering the resin in the slurry;
Boron manosil AS titanium glass powder is a leadless glass powder, can be according to the physical property of the ceramic matrix of the multilayer ceramic capacitor of selected preparation such as the composition that the coefficient of expansion, transition temperature etc. are selected leadless glass powders, make both physical property such as the coefficient of expansion, transition temperature etc. basic identical or approaching, so just can obtain stronger adhesive force and identical softening point;
The adding proportion that changes dispersant, defoamer and surfactant can be regulated apparent and printing performances such as the trickling of the nanometer silver paste of finally making, thixotropy.
Use the nanometer silver paste printing that this method obtains or be coated on the corresponding substrate, drying is 5～30 minutes under 100～150 ℃ of temperature conditions, under 600～750 ℃ of temperature conditions, once burn altogether, the multilayer ceramic capacitor silver electrode surface that obtains is smooth, electrical property is good, is applicable to the large-scale mass production of multilayer ceramic capacitor product.
Because there is not harmfulness in the harmful substance of European environmental protection ban regulations such as the nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor of the present invention is not leaded, halogen, benzene in the process of manufacture of slurry, help environmental protection simultaneously; The leadless glass powder of the nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor of the present invention in addition is basic identical or approaching with physical property such as the coefficient of expansion, the transition temperature etc. of the ceramic matrix of corresponding multilayer ceramic capacitor, can once burn till shape altogether, solved in the past multilayer ceramic capacitor produces the factor that distortion waits influences the product yields before and after sintering, help reducing production costs, meet the trend of current social development.
Embodiment
The nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor provided by the invention, comprise following component, and the mass fraction of each component is: 45～80% particle diameter is the silver powder of 10～100nm, 10～40% organic carrier, 1～10% boron manosil AS titanium glass powder, 1～9% dispersant, 0.5～9% defoamer and 0.5～8% surfactant; Described organic carrier is the ethyl acetate or the ethyl acetate system of polyacrylic resin, polyacrylic resin: the mass ratio of ethyl acetate or ethyl acetate is 40～70: 30～60, and polyacrylic resin is one or more of the polymethyl acrylate of molecular weight between 10000～15000, polyethyl acrylate, polymethyl methacrylate;
Preparation method according to the nanometer silver paste of said components proportioning is as follows:
1) powder: the silver powder that with load weighted particle diameter is 10～100nm is in the same place with boron manosil AS titanium glass powder, makes carrier with absolute ethyl alcohol, mixes 3～10 hours with ball mill or ball grinder;
2) powder for drying: silver powder that mixes and boron manosil AS titanium glass powder were dried 1～2 hour under 40～80 ℃ of conditions, naturally cool to room temperature then;
3) organic carrier preparation: polyacrylic resin is joined in ethyl acetate or the ethyl acetate, in water-bath under 60～80 ℃ of conditions, constant temperature dissolves polyacrylic resin fully, be cooled to room temperature then, wherein, polyacrylic resin: the mass ratio of ethyl acetate or ethyl acetate is 40～70: 30～60; Polyacrylic resin is one or more of the polymethyl acrylate of molecular weight between 10000～15000, polyethyl acrylate, polymethyl methacrylate;
4) add organic carrier: load weighted organic carrier, dispersant, defoamer and surfactant are joined in the mixture of dried silver powder and boron manosil AS titanium glass powder, fully stir, till mixing, filter and obtain preliminary nanometer silver paste;
5) slurry grinds: preliminary nanometer silver paste is fully ground with three-high mill, check that fineness reaches till 0～2 μ m, cross the nanometer silver paste that 800 purpose screen filtrations obtain being used for terminal electrode of multi-layer ceramic capacitor then.
Further specify nanometer silver paste and the preparation process thereof that is used for terminal electrode of multi-layer ceramic capacitor of the present invention below in conjunction with specific embodiment:
Embodiment 1
At first the particle diameter of weighing 60g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 4g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 4 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and boron manosil AS titanium glass powder were dried 1.5 hours room temperature cooling then under 60 ℃ of conditions;
Weighing 65g molecular weight is that 12000 polyacrylic acid formicester joins in the ethyl acetate of 35g, under 65 ℃ of conditions of constant temperature polyacrylic resin is dissolved fully in water-bath, is cooled to room temperature then.
The defoamer polysiloxanes of dispersant DP270, the 2.5g of aforementioned above-mentioned organic carrier of weighing 30g and 1g, the surfactant Si Ban-60 (Span-60) of 3.5g join in the mixture of silver powder and boron manosil AS titanium glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 5 times with three-high mill, check to reach till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Embodiment 2
At first the particle diameter of weighing 45g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 10g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 4.5 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and leadless glass powder were dried 1～3 hour room temperature cooling then under 70 ℃ of conditions;
Weighing 70g molecular weight is that 13000 polyacrylic acid second fat joins in the ethyl acetate of 60g, under 65 ℃ of conditions of constant temperature polyacrylic resin is dissolved fully in water-bath, is cooled to room temperature then.
The aforementioned above-mentioned organic carrier of weighing 40g and the dispersant dodecyl sodium sulfate of 1g, the defoamer calcium carbonate of 2g, the surfactant di-tert-butyl hydroxy toluene of 2g join in the mixture of aforesaid nano-silver powder and leadless glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Embodiment 3
At first the particle diameter of weighing 160g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 2g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 6 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and boron manosil AS titanium glass powder were dried 2 hours room temperature cooling then under 70 ℃ of conditions;
Weighing 40g molecular weight is that 13000 polyacrylic acid second fat joins in the ethyl acetate of 30g, under 65 ℃ of conditions of constant temperature resin is dissolved fully in water-bath, is cooled to room temperature then.
The aforementioned above-mentioned organic carrier of weighing 20g and the dispersant glycerine tristearate of 10g, the defoamer tricalcium phosphate of 1g, the surfactant polyvinylpyrrolidone of 1g join in the mixture of aforesaid nano-silver powder and boron manosil AS titanium glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Embodiment 4
At first the particle diameter of weighing 65.5g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 1.75g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 5.5 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and boron manosil AS titanium glass powder were dried 1.5 hours room temperature cooling then under 70 ℃ of conditions;
Weighing 52g molecular weight is that 13000 polymethyl methacrylate joins in the ethyl acetate of 48g, under 65 ℃ of conditions of constant temperature resin is dissolved fully in water-bath, is cooled to room temperature then.
The defoamer polysiloxanes of dispersant DP270, the 1.2g of aforementioned above-mentioned organic carrier of weighing 21.25g and 1.5g, the surfactant Span-60 of 1.8g join in the mixture of aforesaid nano-silver powder and boron manosil AS titanium glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Embodiment 5
At first the particle diameter of weighing 69g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 3.5g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 4.5 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and leadless glass powder were dried 1 hour room temperature cooling then under 80 ℃ of conditions;
Weighing 30g molecular weight is that 13000 polyacrylic acid second fat, 35g molecular weight are that 12000 polyacrylic acid formicester joins in the ethyl acetate of 32g, under 65 ℃ of conditions of constant temperature polyacrylic resin is dissolved fully in water-bath, is cooled to room temperature then.
The aforementioned above-mentioned organic carrier of weighing 22g and the dispersant dodecyl sodium sulfate of 1.5g, the defoamer calcium carbonate of 10g, the surfactant di-tert-butyl hydroxy toluene of 2g join in the mixture of aforesaid nano-silver powder and leadless glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Embodiment 6
At first the particle diameter of weighing 75g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 1.5g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 6 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and boron manosil AS titanium glass powder were dried 2 hours room temperature cooling then under 40 ℃ of conditions;
Weighing 59g molecular weight is that 13000 polyacrylic acid second fat joins in the ethyl acetate of 41g, under 65 ℃ of conditions of constant temperature resin is dissolved fully in water-bath, is cooled to room temperature then.
The aforementioned above-mentioned organic carrier of weighing 19.5g and the dispersant glycerine tristearate of 1g, the defoamer tricalcium phosphate of 1g, the surfactant polyvinylpyrrolidone of 2g join in the mixture of aforesaid nano-silver powder and boron manosil AS titanium glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Embodiment 7
At first the particle diameter of weighing 75g is at the nano-silver powder of 10～100nm, the boron manosil AS titanium glass powder of weighing 3g then, again load weighted nano-silver powder and boron manosil AS titanium glass powder are in the same place, make carrier, mixed 5.5 hours with ball mill or ball grinder with absolute ethyl alcohol; Nano-silver powder that mixes and boron manosil AS titanium glass powder were dried 1～3 hour room temperature cooling then under 70 ℃ of conditions;
Weighing 50g molecular weight is that 13000 polymethyl methacrylate, 25g molecular weight are that 13000 polymethyl methacrylate joins in the ethyl acetate of 45g, under 65 ℃ of conditions of constant temperature resin is dissolved fully in water-bath, is cooled to room temperature then.
The defoamer polysiloxanes of dispersant DP270, the 1.2g of aforementioned above-mentioned organic carrier of weighing 21.25g and 1.5g, the surfactant Span-60 of 1.8g join in the mixture of aforesaid nano-silver powder and boron manosil AS titanium glass powder, fully stir with planetary stirring machine, till mixing, obtain preliminary slurry then after filtration;
The preliminary slurry that obtains is carried out rolling 8 times with three-high mill, be checked through till the fineness of 0～2 μ m, obtain the slurry finished product through 800 purpose screen filtrations then.
Claims (5)
1. nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor, it is characterized in that, comprise by mass fraction: 45～80% particle diameter is the silver powder of 10～100nm, 10～40% organic carrier, 1～10% boron manosil AS titanium glass powder, 1～9% dispersant, 0.5～9% defoamer and 0.5～8% surfactant;
Described organic carrier is the ethyl acetate system of polyacrylic resin, polyacrylic resin: the mass ratio of ethyl acetate is 40～70: 30～60, and polyacrylic resin is one or more of the polymethyl acrylate of molecular weight between 10000～15000, polyethyl acrylate, polymethyl methacrylate.
2. a kind of nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor as claimed in claim 1 is characterized in that, described dispersant is one or more of dodecyl sodium sulfate, DP270, glycerine tristearate.
3. a kind of nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor as claimed in claim 1 is characterized in that, described defoamer is one or more of calcium carbonate, tricalcium phosphate, polysiloxanes.
4. a kind of nanometer silver paste that is used for terminal electrode of multi-layer ceramic capacitor as claimed in claim 1 is characterized in that, described surfactant is one or more of di-tert-butyl hydroxy toluene, polyvinylpyrrolidone, Si Ban-60.
5. the preparation method who is used for the nanometer silver paste of terminal electrode of multi-layer ceramic capacitor as claimed in claim 1 is characterized in that, may further comprise the steps:
1) powder: the silver powder that with load weighted particle diameter is 10～100nm is in the same place with boron manosil AS titanium glass powder, makes carrier with absolute ethyl alcohol, mixes 3～10 hours with ball mill or ball grinder;
2) powder for drying: silver powder that mixes and boron manosil AS titanium glass powder were dried 1～2 hour under 40～80 ℃ of conditions, naturally cool to room temperature then;
3) organic carrier preparation: polyacrylic resin is joined in the ethyl acetate, under 60～80 ℃ of conditions, constant temperature dissolves polyacrylic resin fully, is cooled to room temperature then in water-bath, wherein, polyacrylic resin: the mass ratio of ethyl acetate is 40～70: 30～60; Polyacrylic resin is one or more of the polymethyl acrylate of molecular weight between 10000～15000, polyethyl acrylate, polymethyl methacrylate;
4) add organic carrier: load weighted organic carrier, dispersant, defoamer and surfactant are joined in the mixture of dried silver powder and boron manosil AS titanium glass powder, fully stir, till mixing, filter and obtain preliminary nanometer silver paste;
5) slurry grinds: preliminary nanometer silver paste is fully ground with three-high mill, check that fineness reaches till 0～2 μ m, cross the nanometer silver paste that 800 purpose screen filtrations obtain being used for terminal electrode of multi-layer ceramic capacitor then.
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| CN101777423B (en) * | 2010-03-16 | 2011-07-20 | 彩虹集团公司 | Preparation method of electrode paste for environment protective ceramic capacitor |
| CN101872653A (en) * | 2010-06-28 | 2010-10-27 | 彩虹集团公司 | Nano silver conductive paste and preparation method thereof |
| CN101877251B (en) * | 2010-06-30 | 2011-12-21 | 彩虹集团公司 | Method for preparing nickel-containing silver electrode slurry |
| CN102222536B (en) * | 2011-03-28 | 2012-10-24 | 彩虹集团公司 | Environment-friendly silver conductive paste for surface mounting of semiconductor chips and preparation method of environment-friendly silver conductive paste |
| CN102262941B (en) * | 2011-07-19 | 2012-09-19 | 彩虹集团公司 | Method for preparing environment-friendly terminal electrode dipping silver paste for chip inductor |
| CN102642170B (en) * | 2012-05-07 | 2014-06-04 | 广东风华高新科技股份有限公司 | Multilayer ceramic capacitor grinding process and application of multilayer ceramic capacitor grinding process |
| CN104078096A (en) * | 2014-06-04 | 2014-10-01 | 乐凯特科技铜陵有限公司 | Low-cost printed circuit board silver paste and preparation method thereof |
| CN106297955A (en) * | 2016-09-30 | 2017-01-04 | 天津宝兴威科技有限公司 | A kind of nano silver conductive paste |
| CN106531348A (en) * | 2016-09-30 | 2017-03-22 | 天津宝兴威科技有限公司 | Nano silver paste preparation method |
| CN110600162B (en) * | 2019-10-23 | 2021-04-02 | 河南农业大学 | Solar cell conductive paste and preparation method thereof |
| CN111584155B (en) * | 2020-05-29 | 2021-12-03 | 宁波鑫智达新材料有限公司 | Conductive silver paste applied to ceramic filter and preparation method thereof |
| CN113571230B (en) * | 2021-07-21 | 2023-08-29 | 深圳顺络电子股份有限公司 | Conductive silver paste, electrode structure and laminated common mode filter |
| CN116031012B (en) * | 2023-01-10 | 2023-09-22 | 惠州市帕克威乐新材料有限公司 | Nano conductive silver paste and preparation method thereof |
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