CN101972855B - Method for preparing silver micro-powder for high-temperature sintering silver pastes - Google Patents
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Abstract
The invention discloses a method for preparing silver micro-powder for high-temperature sintering silver pastes, which comprises the following steps: preparing a colloidal liquid silver system, a colloidal reduction system and protection solution firstly; then mixing the three. In the invention, a sol gel process and a solution chemical reduction method are used to effectively control the reaction process, so that the industrialized production can be performed stably, and the uniform reaction under the condition of production enlarging still can be ensured, thereby greatly improving the uniformities of shapes and other superficial characteristics of silver particles generated by reaction, and eventually generating flocculating soft silver powder wodges which are easy to carry out post-processing such as collecting and washing, and the like.
Description
Technical field
The present invention relates to a kind of preparation of functional micro silver powder, its preparation method is suitable for industry and goes up the large-scale production micro silver powder.The use of can arranging in pairs or groups in proportion of preparation gained micro silver powder is to satisfy the preparation of electric slurry.
Background technology
Metal ultrafine powder itself possesses superior catalytic performance, magnetic property, electrical property etc., thereby aspect industry such as aerospace, atomic energy, electronics, powder metallurgy, chemistry and medical science, the bioengineering application is more and more widely being arranged.
Wherein micro silver powder is owing to have good electric conductivity and application performance, and application is very extensive in fields such as electronics and electronic materials, in electronics industry, has the status that can not be substituted.Micro silver powder is mainly used in the preparation conductive silver paste, and electronics silver slurry series of products are to use in the electronics industry the most extensively and the maximum a kind of noble metal slurry of consumption, are the critical materials of producing various electronic devices and components.Micro silver powder also in physical property, all has strict demand like granule-morphology, dispersiveness, diameter of particle, size distribution, surface property, crystallinity, tap density etc. except that chemical composition, impurity content etc. has higher requirements.The performance of micro silver powder directly determines key technologies such as conductance and the compactness after the conductive silver paste film forming.
The preparation method of micro silver powder has a variety of, mainly contains vapor phase method, liquid phase method and solid phase method.The vapor phase method investment is big, energy consumption is high, productive rate is low; The micro silver powder particle diameter of solid phase method preparation is bigger than normal and particle size distribution range is wide; Liquid phase method is the method that the most general being used at present prepares micro silver powder.And liquid phase method divides chemical reducing process, electrochemical deposition method, electrolysis, sputtering method, sol-gal process etc.Produce micro silver powder in the industry and adopt the liquid phase chemical reduction method mostly.
The principle that the liquid phase chemical reduction legal system is equipped with micro silver powder is with reducing agent silver to be deposited out with powder type from its salt or the complex aqueous solution or organic system.Chemical reduction method prepares the key of micro silver powder; To search out a suitable chemical reaction condition exactly: one, select corresponding reaction material to come the nucleation and the nucleus growth speed of powder are controlled; Reducing agent commonly used has formaldehyde, ascorbic acid, glycerine, organic amine, unsaturated alcohol, natrium citricum, hydrazine and hydrazine derivative etc., the general hydrazine hydrates that adopt more.Two, the effective dispersant of selection can be eliminated multiple nucleation and increase the merging speed of nucleus before reaching critical radius, thereby reduces the reunion between powder granule.Generally select long-chain protective agents such as gelatin, gum arabic, polyvinyl alcohol, PVP, Sodium Polyacrylate for use.
Electronation silver powder belongs to a silver-colored solids precipitation process; Its process comprises reaction nucleation and two processes of crystalline growth; Owing to be reacted into nuclear process is quick moment reaction (Millisecond); Must make reactant moment in reactor reach molecular level and else realize promptly evenly that microcosmic mixes, just can make the final silver powder pattern maybe be consistent.
How when producing in batches, controlling its size, size distribution and pattern is even more important for producing micro silver powder.Patent about the micro silver powder preparation has much both at home and abroad; But less to silver powder particles pattern and uniformity control set forth; And most of silver powder preparations are not tight to the technology controlling and process of course of reaction and selection all from selecting suitable dispersant, protective agent to start with, and are difficult to be amplified to industrial process.Publication number CN1266761A preparation method processes silver ammino solution with silver nitrate, slowly adds in the reducing solution that is made into by reducing agent and protective agent then, prepares nano silver colloidal sol, and the high speed centrifugation separation, leaches silver powder, washs, drying again.This method is unfavorable for the control of silver powder granularity, and the high speed centrifugation separating energy consumption is big, and is high to equipment requirements, and Separation of Solid and Liquid is collected difficulty, is difficult to satisfy industrialization and produces for large quantities of times; Publication number CN1785558 preparation method is employed in the oxidation-reduction process liquor argenti nitratis ophthalmicus is added drop-wise in reducing agent and the dispersant; PH value with the ammoniacal liquor regulator solution prepares micron order silver powder simultaneously, makes the micron grade ball shape silver powder of the different-grain diameter of 0.1～3.0 μ m.This method has been strengthened the stable control of pH value in the course of reaction; Make whole process of preparation in more stable controlled range; Help amplify producing, but along with the amplification of batch output, this method exists local reaction concentration and W-response concentration difference constantly to widen; Owing to be reacted into nuclear process is quick moment reaction (Millisecond), amplifies the uniformity that the concentration difference of producing and producing will directly influence silver powder.
Summary of the invention
For addressing the above problem; The object of the invention is exactly the deficiency to prior art; Provide a kind of high-temperature sintered silver paste to use the micro silver powder preparation method; Its technological process is simple, technology amplify stable, controllability is strong, be easy to suitability for industrialized production, the micro silver powder of preparing simultaneously is applicable to the conductive filler of piezoelectricity, high temperature sintering slurry such as pressure-sensitive.
The present invention is achieved in that a kind of high-temperature sintered silver paste uses the micro silver powder preparation method, it is characterized in that may further comprise the steps:
(1) the preparation silver ammino solution adds macromolecule thickener solution, and fully stirring and dissolving forms the silvering solution system of colloidal sol shape;
(2) preparation is fully stirred the reduction system that forms the colloidal sol shape by the reduction system of reducing agent, NaOH and macromolecule thickener solution composition;
(3) preparation contains the protection solution of macromolecule space obstacle agent;
(4) the silvering solution system of step (1) gained is mixed in the protection solution that directly is added to step (3) gained with the reduction system of step (2) gained, constantly stir in the adition process;
(5) stop to stir and ageing behind reinforced the finishing, obtain flocculence micro silver powder slurries;
(6) Separation of Solid and Liquid, washing, post processing are separated soft-agglomerated, dry.
In the said step (1), the content range of silver ion is 10-50g/L in the silvering solution system, more preferably is selected as 20-30g/L.
In said step (1) and the step (2), macromolecule thickener solution is selected from a kind of or mixed solution in Arabic gum, gelatin, polyanion cellulose, methylcellulose, the sodium carboxymethylcellulose.
In said step (1) and the step (2), the mass ratio of macromolecule thickener and silver ion is 0.1～10: 100, more preferably is selected as 2～5: 100.
Said step (2), in whole reduction system, reducing agent is selected from one or more mixing of vitamin C, formaldehyde, hydrazine hydrate, formic acid, sodium borohydride, and in whole reduction system, reducing agent is 1: 1～20 with the mass ratio of silver; The mass ratio of silver ion and NaOH is 4～6: 1.
The macromolecule space obstacle agent of said step (3) is selected from polyvinyl alcohol or polyvinylpyrrolidone.
In the said step (4), the silvering solution system is mixed through pressurization and stream with reduction system.Pressure limit is preferably 0.03-0.05Mpa in 0.01-0.1Mpa
In the said step (4), silvering solution system, reduction system, protection solution three's reaction ratio is 3.5～4.5: 3.5～4.5: 2.
In the said step (4), the rotating speed of stirring is 60-100r/min.
In the said step (5), digestion time is 20-40min.
The present invention is used through adopting sol-gal process and liquid phase chemical reduction method; Course of reaction has been carried out effective control; Can be stable carry out suitability for industrialized production, but and guarantee to amplify and produce down still homogeneous reaction, improve the silver-colored granule-morphology that reaction generates and the homogeneity of other signs greatly; The final soft-agglomerated silver powder of flocculence that generates is easy to collect washing and waits post processing.
Description of drawings
Fig. 1 is the Electronic Speculum figure of the embodiment of the invention 1 obtained silver powder;
Fig. 2 is the Electronic Speculum figure of the embodiment of the invention 2 obtained silver powder;
Fig. 3 is the Electronic Speculum figure of the embodiment of the invention 3 obtained silver powder.
The specific embodiment
The present invention is that a kind of high-temperature sintered silver paste is used the micro silver powder preparation method, may further comprise the steps:
(1) the preparation silver ammino solution adds macromolecule thickener solution, and fully stirring and dissolving forms the silvering solution system of colloidal sol shape.Wherein, macromolecule thickener solution is selected from a kind of or mixed solution in Arabic gum, gelatin, polyanion cellulose, methylcellulose, the sodium carboxymethylcellulose.
(2) preparation is fully stirred the reduction system that forms the colloidal sol shape by the reduction system of reducing agent, NaOH and macromolecule thickener solution composition.In the system, reducing agent can be selected one or more of vitamin C, formaldehyde, hydrazine hydrate, formic acid, sodium borohydride for use, and reducing agent is 1: 1～20 with the mass ratio of silver; The mass ratio of silver ion and NaOH is 4～6: 1.Best, reducing agent is 1: 1.2～15 with the mass ratio of silver; The mass ratio of silver ion and NaOH is 5: 1.
(3) preparation contains the protection solution of macromolecule space obstacle agent.The agent of macromolecule space obstacle is optional from polyvinyl alcohol or polyvinylpyrrolidone.
(4) the silvering solution system of step (1) gained is mixed in the protection solution that directly is added to step (3) gained with the reduction system of step (2) gained, constantly stir in the adition process.The rotating speed that stirs is preferably 60-100r/min.Silvering solution system, reduction system, protection solution three's reaction ratio is 3.5～4.5: 3.5～4.5: 2, and the best is 4: 4: 2.
(5) stop to stir and ageing behind reinforced the finishing, the preferred 20-40min of digestion time obtains flocculence micro silver powder slurries;
(6) soft-agglomerated, drying etc. is separated in Separation of Solid and Liquid, washing, post processing.
The present invention is used through adopting sol-gal process and liquid phase chemical reduction method, and course of reaction has been carried out effective control, can be stable carry out suitability for industrialized production.The present invention is used through agent of anionic cellulose isosol and polyvinylpyrrolidone dispersant, uses the generation of flocculant stopping reaction silver particle, uses dispersant that the silver-colored particle that generates is disperseed protection simultaneously, prevents the silver powder reunion.Consumption and mixing speed through regulating flocculant are reacted with stable control; Making silver ion mix, react nucleation with reduction system slows down; The flocculant that is adopted simultaneously has parcel and space obstacle effect to generating silver-colored particle, thus the silver-colored granule-morphology that better control reaction generates and the homogeneity of other signs.Simultaneously, the present invention can change reaction solution viscosity generates silver-colored particle with the control reaction granularity and reunion degree through regulating flocculant addition.The present invention can make the uniformity that can guarantee reaction in the reaction system that is reflected at different scales through the cocurrent adding material mode.Quantity that can corresponding adjusting charge door is to satisfy industrial amplification.
(1) take by weighing the 50g polyanion cellulose and be dissolved in the 1000ml deionized water, fully stirring and dissolving becomes the colloidal sol body A of 5% mass ratio.
(2) take by weighing 40g and analyze pure AgNO
3Be dissolved in the 200ml deionized water, be made into liquor argenti nitratis ophthalmicus; The ammoniacal liquor 30-40ml that adds 25-28% obtains silver ammino solution till making to the liquor argenti nitratis ophthalmicus solution change clarification by muddiness.Add 20ml again and joined Sol A, fully mix the silver sol system that obtains after the adding deionized water is diluted to 400ml.
(3) taking by weighing the analytically pure NaOH of 5g is dissolved in the 200ml deionized water; Stir and to add 80% the pure hydrazine hydrate 5ml of analysis after the fully dissolving respectively, add 20ml and joined colloidal sol body A, add deionized water at last and be diluted to fully to mix behind the 400ml and obtain reducing sol system.
(4) take by weighing 1.5g polyvinylpyrrolidone PVP heating and be dissolved in the 200ml deionized water, be made into protection solution.
(5) with the silvering solution system for preparing and reduction system through under 0.1Mpa pressure and stream mix and be added in the protection solution that contains polyvinylpyrrolidone PVP, and mix in the 80r/min rotating speed.Stopping to stir also behind reinforced the finishing, ageing 30min obtains polymolecularity, evengranular flocculence micro silver powder slurries.Whole reaction system can be accomplished down at 25-30 ℃.
(6) after reaction finishes, to the micro silver powder slurries filter Separation of Solid and Liquid with deionized water cleaning silver powder to electrical conductivity≤20us/cm, use soaked in absolute ethyl alcohol again 2 times, filter and drain.
(7) silver powder that will wet obtains the micro silver powder product through 75 ℃ of infra-red dryings after 30 hours.Product carries out SEM, granularity and specific area measuring, silver powder Electronic Speculum uniform particles, and grain diameter is (as shown in Figure 1) between 0.1-0.3um; Products obtained therefrom particle mean size 0.3-0.5um, narrow distribution range; Specific area 7.0-7.5m
2/ g.
Embodiment 2
(1) take by weighing the 50g polyanion cellulose and be dissolved in the 1000ml deionized water, fully stirring and dissolving becomes the colloidal sol body A of 5% mass ratio.
(2) take by weighing 40g and analyze pure AgNO
3Be dissolved in the 200ml deionized water, be made into liquor argenti nitratis ophthalmicus; The ammoniacal liquor 30-40ml that adds 25-28% obtains silver ammino solution till making to the liquor argenti nitratis ophthalmicus solution change clarification by muddiness.Add 10ml again and joined Sol A, fully mix the silver sol system that obtains after the adding deionized water is diluted to 400ml.
(3) taking by weighing the analytically pure NaOH of 5g is dissolved in the 200ml deionized water; Stir to add respectively after the fully dissolving and analyze pure formaldehyde 5g, add 10ml and joined colloidal sol body A, add deionized water at last and be diluted to fully to mix behind the 400ml and obtain reducing sol system.
(4) take by weighing 1.5g polyvinylpyrrolidone PVP heating and be dissolved in the 200ml deionized water, be made into protection solution.
(5) with the silvering solution system for preparing and reduction system through under 0.05Mpa pressure and stream mix and be added in the protection solution that contains polyvinylpyrrolidone PVP, and mix in the 80r/min rotating speed.Stopping to stir also behind reinforced the finishing, ageing 30min obtains polymolecularity, evengranular flocculence micro silver powder slurries.Whole reaction system can be accomplished down at 25-30 ℃.
(6) after reaction finishes, to the micro silver powder slurries filter Separation of Solid and Liquid with deionized water cleaning silver powder to electrical conductivity≤20us/cm, use soaked in absolute ethyl alcohol again 2 times, filter and drain.
(7) silver powder that will wet obtains the micro silver powder product through 75 ℃ of infra-red dryings after 30 hours.Product carries out SEM, granularity and specific area measuring, silver powder Electronic Speculum uniform particles, and grain diameter is (as shown in Figure 2) between 0.2-0.3um; Products obtained therefrom particle mean size 0.6-1.5um, narrow distribution range; Specific area 6.0-6.5m
2/ g.
Embodiment 3:
(1) take by weighing the 50g arabia gum and be dissolved in the 1000ml deionized water, fully stirring and dissolving becomes the colloidal sol body B of 5% mass ratio.
(2) take by weighing 40g and analyze pure AgNO
3Be dissolved in the 200ml deionized water, be made into liquor argenti nitratis ophthalmicus; The ammoniacal liquor 30-40ml that adds 25-28% obtains silver ammino solution till making to the liquor argenti nitratis ophthalmicus solution change clarification by muddiness.Add 5ml again and joined sol B, fully mix the silver sol system that obtains after the adding deionized water is diluted to 400ml.
(3) take by weighing the analytically pure NaOH of 5g and be dissolved in the 200ml deionized water, stir to add respectively after the fully dissolving and analyze pure Vc25g, add 5ml and joined colloidal sol body B, add deionized water at last and be diluted to fully to mix behind the 400ml and obtain reducing sol system.
(4) take by weighing 1.5g polyvinylpyrrolidone PVP heating and be dissolved in the 200ml deionized water, be made into protection solution.
(5) with the silvering solution system for preparing and reduction system under 0.03Mpa pressure and stream mix and be added in the protection solution that contains polyvinylpyrrolidone PVP, and mix in the 100r/min rotating speed.Stopping to stir also behind reinforced the finishing, ageing 30min obtains lead fine-powdered silver powder.Whole reaction system can be accomplished down at 25-30 ℃.
(6) after reaction finishes, to the micro silver powder slurries filter Separation of Solid and Liquid with deionized water cleaning silver powder to electrical conductivity≤20us/cm, use soaked in absolute ethyl alcohol again 2 times, filter and drain.
(7) silver powder that will wet obtains the micro silver powder product through 75 ℃ of infra-red dryings after 30 hours.Product carries out SEM, granularity and specific area measuring, silver powder Electronic Speculum uniform particles, and grain diameter is (as shown in Figure 3) between 0.4-0.6um; Products obtained therefrom particle mean size 3-5um, narrow distribution range; Specific area 2.0-3.0m
2/ g.
Above-mentioned three embodiment are easy to industrialization and amplify owing to through the cocurrent adding material mode, can make the uniformity that can guarantee reaction in the reaction system that is reflected at different scales.Quantity that can corresponding adjusting charge door is to satisfy industrial amplification.The silver powder that makes above three kinds of specifications can be satisfied with the conductive filler as high temperature sintering type conductor paste, is applicable to the piezoelectricity of high temperature sintering, pressure-sensitive silver slurry.Different matched combined through three kinds of silver powder are used, and can realize the sintering result of different target.
Claims (3)
1. a high-temperature sintered silver paste is used the micro silver powder preparation method, it is characterized in that may further comprise the steps:
(1) preparation silver ammino solution; Add macromolecule thickener solution; Fully stirring and dissolving forms the silvering solution system of colloidal sol shape; The content range of silver ion is 10-50g/L in the silvering solution system, and macromolecule thickener solution is selected from a kind of or mixed solution in Arabic gum, gelatin, polyanion cellulose, methylcellulose, the sodium carboxymethylcellulose, and the mass ratio of macromolecule thickener and silver ion is 0.1 ~ 10:100;
(2) preparation is by the reduction system of reducing agent, NaOH and macromolecule thickener solution composition; Fully stir the reduction system that forms the colloidal sol shape; Wherein macromolecule thickener solution is selected from a kind of or mixed solution in Arabic gum, gelatin, polyanion cellulose, methylcellulose, the sodium carboxymethylcellulose, and reducing agent is selected from one or more mixing of vitamin C, formaldehyde, hydrazine hydrate, formic acid, sodium borohydride; In whole reduction system, the mass ratio of macromolecule thickener and silver ion is 0.1 ~ 10:100, and reducing agent is 1:1 ~ 20 with the mass ratio of silver; The mass ratio of silver ion and NaOH is 4 ~ 6:1;
(3) preparation contains the protection solution of macromolecule space obstacle agent, and the agent of said macromolecule space obstacle is selected from polyvinyl alcohol or polyvinylpyrrolidone;
(4) be that pressurization and stream mix under the 0.01-0.1MPa with the reduction system of the silvering solution system of step (1) gained and step (2) gained in pressure limit; Directly be added in the protection solution of step (3) gained; Constantly stir in the adition process, wherein silvering solution system, reduction system, protection solution three's reaction ratio is 3.5 ~ 4.5:3.5 ~ 4.5:2;
(5) stop to stir and ageing behind reinforced the finishing, obtain flocculence micro silver powder slurries;
(6) Separation of Solid and Liquid, washing, post processing are separated soft-agglomerated, dry.
2. a kind of high-temperature sintered silver paste according to claim 1 is used the micro silver powder preparation method, it is characterized in that: in the said step (4), the rotating speed of stirring is 60-100r/min.
3. a kind of high-temperature sintered silver paste according to claim 1 is used the micro silver powder preparation method, it is characterized in that: in the said step (5), digestion time is 20-40min.
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| CN106583751A (en) * | 2016-12-29 | 2017-04-26 | 广东羚光新材料股份有限公司 | Preparation method of flat silver powder |
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| CN112191861B (en) * | 2020-09-29 | 2022-12-20 | 湖南中伟新银材料科技有限公司 | Preparation method of conductive silver powder, prepared conductive silver powder and application of conductive silver powder |
| CN114619039B (en) * | 2022-03-15 | 2023-01-31 | 江苏连银新材料有限公司 | Spherical silver powder, preparation method thereof and conductive paste |
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| CN101279376A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Preparation of high dispersed superfine spherical silver powder for conductive silver slurry |
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Address after: 526020 Taihe North Road, Guangdong, Zhaoqing Patentee after: GUANGDONG LINGGUANG NEW MATERIAL Co.,Ltd. Address before: 526020 Taihe North Road, Guangdong, Zhaoqing Patentee before: ZHAOQING LINGGUANG ELECTRONIC CHEMICAL MATERIAL TECHNOLOGY Co.,Ltd. |
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Denomination of invention: Method for preparing silver micro-powder for high-temperature sintering silver pastes Effective date of registration: 20200426 Granted publication date: 20121017 Pledgee: China Co. truction Bank Corp Zhaoqing branch Pledgor: GUANGDONG LINGGUANG NEW MATERIAL Co.,Ltd. Registration number: Y2020440000098 |
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Granted publication date: 20121017 Pledgee: China Co. truction Bank Corp Zhaoqing branch Pledgor: GUANGDONG LINGGUANG NEW MATERIAL Co.,Ltd. Registration number: Y2020440000098 |
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