CN103406550B - Method for preparing silver micro-powder for electronic paste of pressure sensitive element - Google Patents
Method for preparing silver micro-powder for electronic paste of pressure sensitive element Download PDFInfo
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- CN103406550B CN103406550B CN201310374375.XA CN201310374375A CN103406550B CN 103406550 B CN103406550 B CN 103406550B CN 201310374375 A CN201310374375 A CN 201310374375A CN 103406550 B CN103406550 B CN 103406550B
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Abstract
The invention discloses a method for preparing silver micro-powder for electronic paste of a pressure sensitive element. The method includes the steps: (1) liquid preparation: placing solid crystals of silver nitrate into a reaction kettle, adding enough water into the reaction kettle and stirring the solid crystals and the water into a 0uniform water solution to prepare an A solution; placing solid powder of soda into a batching kettle, adding enough water into the batching kettle and stirring the solid powder and the water into a uniform water solution to prepare a B solution; taking gelatin as a surface coating agent, adding enough ethyl alcohol and uniformly stirring and dissolving the gelatin to prepare a C solution; preparing a water solution comprising, by weight, 37% of ascorbic acid and maintaining the normal temperature to prepare a D solution; (2) reaction: sequentially adding the C solution and the D solution into the B solution to form A1 mixed solution, firstly standing the A1 mixed solution for 15 min, stopping for 10min, and continuously and uniformly placing the A1 mixed solution into the A solution; (3) rinsing; (4) drying and crushing. The silver micro-powder can realize loose agglomeration of netted flocculent structures, and final products can achieve concentrated grain distribution and high surface activity.
Description
Technical field
The present invention relates to the production method of micro silver powder, especially a kind of production method of pressure cell electric slurry super fine silver powder.
Background technology
Developing rapidly of electronics and information industry, has driven the development of electric slurry and micro silver powder (super fine silver powder) industry.In argent conductor, electrical conductivity is the highest, and the application performance of excellence, has the status that can not be substituted in the electronics industry.Therefore, silver powder and electric slurry series of products thereof are most widely used a kind of noble metal powder maximum with consumption in electronics industry, is the fundamental sum key function material producing various electronic component products.Electric slurry product integrates metallurgy, chemical industry, electronic technology, a kind of electronic functional material of high-tech, mainly for the manufacture of thick film integrated circuit, resistor, resistor network, capacitor, MLCC, conductor ink, electrode of solar battery, LED cold light source, OLED(OLED), printing and high-resolution electric conductor, thin film switch/flexible circuit, conducting resinl, sensitive components and other electronic devices and components.Because silver is noble metal, silver ion is easily reduced to elemental silver simultaneously, and therefore liquid phase reduction is the main method preparing silver powder at present.Water-soluble by silver salt (silver nitrate etc.), add chemical reducing agent (as hydrazine hydrate etc.), deposit silver powder, through rinsing, oven dry and obtain silver-colored reduced powder, average grain diameter is between 0.1-10um, and the control of the selection of reducing agent, reaction condition, the use of interfacial agent, can prepare the micro silver powder (as particle mean size, apparent density, specific area) of different physicochemical characteristic, there is following intrinsic problem due to the restriction of the difference in production technology and reducing condition in present most of micro silver powder:
1. apparent density is higher, and in electric slurry system, dispersive property is inadequate, and sintering silver layer crystalline phase is uneven so that reduce the electric conductivity of slurry;
2. specific area is not high, and sintering activity is undesirable, and silver powder sintering is insufficient, and sintered surface is coarse, silver layer tack is bad so that reduce the solderability of slurry.
Therefore most of micro silver powder is not suitable for applying in pressure cell electric slurry.
Summary of the invention
The technical problem to be solved in the present invention is that existing micro silver powder exists the problems such as apparent density is higher, specific area is not high and is not suitable for applying in pressure cell electric slurry, provides a kind of method preparing silver micro-powder for electronic paste of pressure sensitive element for this reason.
Technical scheme of the present invention is: the method preparing silver micro-powder for electronic paste of pressure sensitive element, and it comprises the following steps:
(1) dosing: put into silver nitrate solid crystals in a kettle. and add enough water and stir into the uniform aqueous solution, holding temperature is 35 DEG C-45 DEG C, and pH value, 4 ~ 5, is made into solution A; In batching kettle, put into soda ash solid state powder and add enough water and stir into the uniform aqueous solution, holding temperature is 40 DEG C-50 DEG C, and pH value, 12 ~ 13, is made into B solution; Make surface capping agents with gelatin and add enough alcohol stirring and dissolving evenly, being made into C solution; Preparation is the aqueous solution of 37% containing ascorbic acid quality and maintains normal temperature, is made into solution D;
(2) react: successively C, solution D are added in B solution, form A1 mixed solution, then A1 mixed solution is first placed 15min and stop 10min, then continuous uniform puts into solution A, the accumulative tapping time is 50min, record course of reaction initial time and temperature, terminal pH value, and detection reaction terminal is with or without free silver ions;
(3) rinsing: confirm without after silver ion, add water cooling and stirring, precipitates and to remove supernatant after 10min and to add water cleaning again; Filter vat is put into for subsequent use when being washed till electrical conductivity <30 μ S/cm;
(4) fragmentation is dried: the silver powder after being filtered dry again dispersed with stirring is even, baking oven is loaded by every disc gage amount, temperature 60 C-100 DEG C is dried after 3-15h, with the silver powder agglomerate of High Rotation Speed mandrel rod pulverizer after crushing drying in short-term, and obtained silver micro-powder for electronic paste of pressure sensitive element.
In step described in such scheme (1), the mass ratio of silver nitrate solid crystals and water is 1:10, the quality of soda ash solid state powder is 50% of silver nitrate solid crystals quality, the mass ratio of soda ash solid state powder and water is 1:6, its amount of gelatin is 0.5% of silver nitrate solid crystals quality, and its amount of ascorbic acid is 40% of silver nitrate solid crystals quality.
In such scheme, in step (3), each sedimentation time is 10-30min, and the silver powder agglomerate time that step (4) high speed rotates after mandrel rod pulverizer crushing drying is 5s.
In the present invention, this kind of silver powder adopts the design of above-mentioned production technology, particle is wrapped up while generating simple substance galactic nucleus owing to being based on fast reaction under solutions of weak acidity, can make between micro silver powder, to realize loose net flocculent structure to reunite, final products have the size distribution and higher surface-active comparatively concentrated, and apparent density can be controlled in 0.8g/cm
3below, specific area can reach 3.5m
2/ g, and the requirement of the selection of technological parameter and technical process can realize concentrating fast reacting and the stability of system in course of reaction.
Accompanying drawing explanation
Fig. 1 is the micro silver powder microcosmic schematic diagram that the present invention makes.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:(1) dosing: put into silver nitrate solid crystals in a kettle. and add enough water and stir into the uniform aqueous solution, the mass ratio of silver nitrate solid crystals and water is 1:10, and holding temperature is 35 DEG C, and pH value, 4, is made into solution A; In batching kettle, put into soda ash solid state powder and add enough water and stir into the uniform aqueous solution, the quality of soda ash solid state powder is 50% of silver nitrate solid crystals quality, and the mass ratio of soda ash solid state powder and water is 1:6, and holding temperature is 40 DEG C, pH value, 12, is made into B solution; Make surface capping agents with gelatin and add enough alcohol stirring and dissolving evenly, its amount of gelatin is silver nitrate solid crystals quality 0.5%, being made into C solution; Preparation is the aqueous solution of 37% containing ascorbic acid quality and maintains normal temperature, and its amount of ascorbic acid is 40% of silver nitrate solid crystals quality, is made into solution D;
(2) react: successively C, solution D are added in B solution, form A1 mixed solution, then A1 mixed solution is first placed 15min and stop 10min, then continuous uniform puts into solution A, the accumulative tapping time is 50min, record course of reaction initial time and temperature, terminal pH value, and detection reaction terminal is with or without free silver ions;
(3) rinsing: confirm without after silver ion, add water cooling and stirring, precipitates and to remove supernatant after 10min and to add water cleaning again; Each sedimentation time is 10min, puts into filter vat for subsequent use when being washed till electrical conductivity <30 μ S/cm;
(4) fragmentation is dried: the silver powder after being filtered dry again dispersed with stirring is even, loads baking oven by every disc gage amount, after temperature 60 C dries 3h, with the silver powder agglomerate of High Rotation Speed mandrel rod pulverizer in 5s after crushing drying, obtained silver micro-powder for electronic paste of pressure sensitive element.
Embodiment 2:(1) dosing: put into silver nitrate solid crystals in a kettle. and add enough water and stir into the uniform aqueous solution, the mass ratio of silver nitrate solid crystals and water is 1:10, and holding temperature is 45 DEG C, and pH value, 5, is made into solution A; In batching kettle, put into soda ash solid state powder and add enough water and stir into the uniform aqueous solution, the quality of soda ash solid state powder is 50% of silver nitrate solid crystals quality, and the mass ratio of soda ash solid state powder and water is 1:6, and holding temperature is 50 DEG C, pH value, 13, is made into B solution; Make surface capping agents with gelatin and add enough alcohol stirring and dissolving evenly, its amount of gelatin is silver nitrate solid crystals quality 0.5%, being made into C solution; Preparation is the aqueous solution of 37% containing ascorbic acid quality and maintains normal temperature, and its amount of ascorbic acid is 40% of silver nitrate solid crystals quality, is made into solution D;
(2) react: successively C, solution D are added in B solution, form A1 mixed solution, then A1 mixed solution is first placed 15min and stop 10min, then continuous uniform puts into solution A, the accumulative tapping time is 50min, record course of reaction initial time and temperature, terminal pH value, and detection reaction terminal is with or without free silver ions;
(3) rinsing: confirm without after silver ion, add water cooling and stirring, precipitates and to remove supernatant after 10min and to add water cleaning again; Each sedimentation time is 30min, puts into filter vat for subsequent use when being washed till electrical conductivity <30 μ S/cm;
(4) fragmentation is dried: the silver powder after being filtered dry again dispersed with stirring is even, loads baking oven by every disc gage amount, after temperature 100 DEG C dries 15h, with the silver powder agglomerate of High Rotation Speed mandrel rod pulverizer in 5s after crushing drying, obtained silver micro-powder for electronic paste of pressure sensitive element.
This kind of silver powder adopts the design of above-mentioned production technology, particle is wrapped up while generating simple substance galactic nucleus owing to being based on fast reaction under solutions of weak acidity, can make between micro silver powder, to realize loose net flocculent structure to reunite, final products have the size distribution and higher surface-active comparatively concentrated, apparent density can be controlled in below 0.8g/cm3, specific area can reach 3.5m2/g,, and the requirement of the selection of technological parameter and technical process can realize concentrating fast reacting and the stability of system in course of reaction.
In order to prevent in reaction vessel, metal erosion is on the impact of micro silver powder product quality, and above-mentioned reactor, batching kettle material are 321 stainless steels.
Analyze this kind of micro silver powder of batch production after testing, its index parameter is as shown in the table:
| D10 | D50 | D90 | Dav | Pine ratio | Shake close | Scaling loss | Moisture content | Specific area |
| 0.215um | 0.593um | 1.213um | 0.664um | 0.8m 2/g | 1.69g/cm 3 | 0.67% | 0.07% | 3.53m2/g |
Above in conjunction with the embodiments to invention has been exemplary description; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the improvement of the various unsubstantialities that method of the present invention is conceived and technical scheme is carried out; or design of the present invention and technical scheme directly applied to other occasion, all within protection scope of the present invention without to improve.
Claims (2)
1. prepare the method for silver micro-powder for electronic paste of pressure sensitive element, it is characterized in that it comprises the following steps:
(1) dosing: put into silver nitrate solid crystals in a kettle. and add enough water and stir into the uniform aqueous solution, the mass ratio of silver nitrate solid crystals and water is 1:10, and holding temperature is 35 DEG C-45 DEG C, and ph value, 4 ~ 5, is made into solution A; In batching kettle, put into soda ash solid state powder and add enough water and stir into the uniform aqueous solution, the quality of soda ash solid state powder is 50% of silver nitrate solid crystals quality, and the mass ratio of soda ash solid state powder and water is 1:6, and holding temperature is 40 DEG C-50 DEG C, ph value, 12 ~ 13, is made into B solution; Make surface capping agents with gelatin and add enough alcohol stirring and dissolving evenly, its amount of gelatin is silver nitrate solid crystals quality 0.5%, being made into C solution; Preparation is the aqueous solution of 37% containing ascorbic acid quality and maintains normal temperature, and its amount of ascorbic acid is 40% of silver nitrate solid crystals quality, is made into solution D;
(2) react: when A, B solution temperature reach setting, successively C, solution D are added in B solution, form A1 mixed solution, then A1 mixed solution is first placed 15min and stop 10min, then continuous uniform puts into solution A, the accumulative tapping time is 50min, record course of reaction initial time and temperature, terminal pH value, and detection reaction terminal is with or without free silver ions;
(3) rinsing: confirm without after silver ion, add water cooling and stirring, precipitates and to remove supernatant after 10min and to add water cleaning again; Filter vat is put into for subsequent use when being washed till electrical conductivity <30 μ S/cm;
(4) fragmentation is dried: the silver powder after being filtered dry again dispersed with stirring is even, baking oven is loaded by every disc gage amount, temperature 60 C-100 DEG C is dried after 3-15h, with the silver powder agglomerate of High Rotation Speed mandrel rod pulverizer after crushing drying in short-term, and obtained silver micro-powder for electronic paste of pressure sensitive element.
2. prepare the method for silver micro-powder for electronic paste of pressure sensitive element as claimed in claim 1, it is characterized in that the silver powder agglomerate time after described step (4) high speed rotation mandrel rod pulverizer crushing drying is 5s.
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| CN103846452B (en) * | 2014-03-19 | 2016-01-06 | 中科铜都粉体新材料股份有限公司 | Prepare the method for solar panel micro silver powder |
| CN110449572B (en) * | 2019-08-08 | 2021-07-20 | 湖南诺尔得材料科技有限公司 | Preparation method of functional silver powder for electronic paste |
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| CN1227148A (en) * | 1999-01-19 | 1999-09-01 | 沈阳黎明发动机制造公司 | High purity high dispersiveness spherical super fine silver powder and its producing method |
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| CN101733410A (en) * | 2009-12-31 | 2010-06-16 | 广东风华高新科技股份有限公司 | Preparation method of high dispersibility superfine silver powder with adjustable grain diameter |
| CN102528069A (en) * | 2010-12-10 | 2012-07-04 | 比亚迪股份有限公司 | Preparation method for silver powder |
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| JP2010077493A (en) * | 2008-09-26 | 2010-04-08 | Dowa Electronics Materials Co Ltd | Silver powder and method for producing the same |
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| US4979985A (en) * | 1990-02-06 | 1990-12-25 | E. I. Du Pont De Nemours And Company | Process for making finely divided particles of silver metal |
| CN1227148A (en) * | 1999-01-19 | 1999-09-01 | 沈阳黎明发动机制造公司 | High purity high dispersiveness spherical super fine silver powder and its producing method |
| CN101554664A (en) * | 2009-05-20 | 2009-10-14 | 广东风华高新科技股份有限公司 | Method for preparing nano-scale silver powder |
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