CN103909273A - Method for preparing triangular micro-nano silver powder - Google Patents
Method for preparing triangular micro-nano silver powder Download PDFInfo
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- CN103909273A CN103909273A CN201410090376.6A CN201410090376A CN103909273A CN 103909273 A CN103909273 A CN 103909273A CN 201410090376 A CN201410090376 A CN 201410090376A CN 103909273 A CN103909273 A CN 103909273A
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Abstract
The invention discloses a method for preparing triangular micro-nano silver powder. The method comprises the following steps: dissolving polyvinylpyrrolidone into an alcohol solvent to obtain 0.001-0.1g/mL of polyvinylpyrrolidone solution; adding chlorate into the polyvinylpyrrolidone solution till the concentration of chloride ions is 10<-5>-10<-2>mol/L; uniformly stirring; adding silver nitrate till the concentration is 0.001-0.2g/mL; dissolving, and transferring into a reaction kettle; heating to 120 DEG C, and reacting for 0.1-5 hours; heating to 160 DEG C, and reacting for 1-5 hours; cooling; repeatedly centrifuging and washing by using absolute ethyl alcohol to obtain the triangular micro-nano silver powder. By adopting the method, the shape and size of silver powder can be adjusted, and triangular and triangular-conical silver powder of multiple scales within the micro-nano scale range can be prepared.
Description
Technical field:
The invention belongs to metal material field, be specifically related to a kind of method of preparing the micro-nano silver powder of triangular shape.
Background technology:
Silver powder is a kind of metal dust being most widely used in electronics industry, has good conduction, thermal conductivity, and its quality directly or indirectly affects slurry and finally forms the performance of conductor.The preparation method of silver powder mainly contains Physical and chemical method.
Chemical method is with reducing agent, silver form with powder from its salt or complex solution to be deposited.The principal element that determines chemical deposition process has solution concentration, pH value, reaction temperature, reducing agent to add speed, whipped form and speed etc.Reducing agent has conclusive impact to the form of prepared silver powder, and except to silver powder particle diameter, different reducing agents also presents larger difference to the surface of silver powder point dimension, and patent of the present invention has adopted two kinds of comparatively special alcohol as reducing agent.Dispersant is also larger on the form impact of silver powder.
Triangular shape nano silver particles has good electric conductivity, and unique plasma resonance optical property has important application in the industry such as optics, microelectronics.
Patents: CN102133645A, South China Science & Engineering University, a kind of preparation method of eco-friendly micron order triangle silver strip.
Summary of the invention:
The object of this invention is to provide a kind of technique simple, the system extent of reaction is high, and prepared silver powder shape and size homogeneity is high, the method for what production cost was low the prepare micro-nano silver powder of triangular shape.
The method of preparing the micro-nano silver powder of triangular shape of the present invention, is characterized in that, comprises the following steps:
Polyvinylpyrrolidone (PVP) is dissolved in alcoholic solvent, makes the polyvinylpyrrolidonesolution solution of 0.001-0.1g/mL, add chlorate in polyvinylpyrrolidonesolution solution, the concentration that makes chlorion is 10
-5-10
-2mol/L, stirs, and adds silver nitrate, and making its concentration is 0.001-0.2g/mL, after dissolving, proceed in reactor, be heated to 120 DEG C of reaction 0.1-5 hour, then be heated to 160 DEG C of reaction 1-5 hour, cooling, with absolute ethyl alcohol centrifuge washing several, obtain the micro-nano silver powder of triangular shape.
Described alcoholic solvent is 1,3 butanediol or 2,4 pentanediols or both mixed solvents.
Described polyvinylpyrrolidone (PVP), its relative molecular weight is preferably Mr=6000～15000.
Described chlorate is: NaCl, CuCl, CuCl
2, KCl, CaCl
2, ZnCl
2, MgCl
2, FeCl
3in a kind of or its combination, preferably CuCl.
Described uses absolute ethyl alcohol centrifuge washing for several times, and its centrifugation revolution is 2000～6000r/min, and centrifugation time is 5～15min, and centrifugal number of times is 2-4 time.
The method of preparing the micro-nano silver powder of triangular shape of the present invention, it can carry out modulation to the shape and size of silver powder, can prepare the silver powder of multiple yardstick within the scope of triangle sheet and triangle taper and micro/nano level.The micro-nano silver powder of triangular shape preparing, in the time being in contact with one another, can provide large contact surface long-pending, reduce interplanar distance, thereby reduce then to wear resistance and lumped resistance, in the time preparing the products such as conducting resinl, can effectively improve the electric conductivity of conducting resinl, therefore the silver-colored use amount of comparable corresponding minimizing, has the value of industrialization promotion.This method technique is simple simultaneously, and the system extent of reaction is high, and prepared silver powder shape and dimensional homogeneity are high, and production cost is low.
Brief description of the drawings:
Fig. 1 is the ESEM picture of the silver powder sample that makes of embodiment 1;
Fig. 2 is the ESEM picture of the silver powder sample that makes of embodiment 2;
Fig. 3 is the ESEM picture of the silver powder sample that makes of embodiment 3;
Fig. 4 is the ESEM picture of the silver powder sample that makes of embodiment 4.
Detailed description of the invention:
Following examples are to further illustrate of the present invention, instead of limitation of the present invention.
Embodiment 1:
Polyvinylpyrrolidone (PVP, relative molecular mass Mr=6000) 2g is dissolved in 1,3 butanediol of 20mL, adds 0.2mL after dissolving again, (concentration of the concentration that makes chlorion in whole reaction liquid is 10 for the CuCl aqueous solution of 1.0mol/L
-2mol/L), after stirring, then dissolve in the AgNO of 4g
3, after dissolving, proceed to reactor, be heated to 120 DEG C of reactions 0.1 hour, then be heated to 160 DEG C of reactions 5 hours.After cooling, wash twice of centrifugation (rotating speed 4000r/min, each 10min), silver powder precipitation is carried out absolute ethanol washing centrifugal twice (rotating speed 4000r/min, each 10min) again, obtains silver powder sample (the micro-nano silver powder of triangular shape).Observe (Fig. 1) by SEM, the silver powder of gained approaches 100% for the conical surface is the submicron order triangular pyramidal silver powder of nearly isosceles right triangle, right angle length of side 300nm to 400nm, and dimensional homogeneity is good.
Embodiment 2:
Polyvinylpyrrolidone (PVP, relative molecular mass Mr=10000) 0.02g is dissolved in 2,4 pentanediols of 20mL, after dissolving, adds 0.2mL, 10
-3(concentration of the concentration that makes chlorion in whole reaction liquid is 10 for the NaCl aqueous solution of mol/L
-5mol/L), after stirring, then dissolve in the AgNO of 0.02g
3, after dissolving, proceed to reactor, be heated to 120 DEG C of reactions 5 hours, then be heated to 160 DEG C of reactions 1 hour.After cooling, wash twice of centrifugation (rotating speed 4000r/min, each 10min), collect silver powder precipitation and carry out again absolute ethanol washing centrifugal twice (rotating speed 4000r/min, each 10min), obtain silver powder sample (the micro-nano silver powder of triangular shape).Observe (Fig. 2) by SEM, the silver powder shape of gained approaches 100% and presents triangular cone table shape, and wherein upper and lower surface is equilateral triangle, side is isosceles trapezoid, and size is at submicron order, upper bottom surface length of side 200nm to 300nm, bottom surface length of side 400nm to 500nm, thickness 200nm to 250nm.
Embodiment 3:
Polyvinylpyrrolidone (PVP, relative molecular mass Mr=15000) 0.6g is dissolved in to 1,3 butanediol of 20mL and the mixed solution of 2,4 pentanediols (volume ratio is 7:3), after dissolving, adds 0.2mL, the FeCl of 0.1mol/L
3(concentration of the concentration that makes chlorion in whole reaction liquid is 3 × 10 to the aqueous solution
-3mol/L), after stirring, then dissolve in the AgNO of 0.17g
3, after dissolving, proceed to reactor, be heated to 120 DEG C of reactions 2 hours, then be heated to 160 DEG C of reactions 3 hours.After cooling, wash twice of centrifugation (rotating speed 4000r/min, each 10min), the centrifugal silver powder precipitation of collecting is carried out absolute ethanol washing centrifugal once (rotating speed 4000r/min, each 10min) again, obtains silver powder sample (the micro-nano silver powder of triangular shape).Observe (Fig. 3) by SEM, the silver powder shape of gained approximately 95% presents triangular pyramidal, and wherein the conical surface is nearly isosceles right triangle; Size is at submicron order, right angle length of side 300nm to 400nm, and dimensional homogeneity is good.Separately have an appointment 5% for nearly triangle or random silver powder.
Embodiment 4:
Polyvinylpyrrolidone (PVP, relative molecular mass Mr=10000) 0.12g is dissolved in to 1,3 butanediol of 20mL and the mixed solution of 2,4 pentanediols (volume ratio is 3:7), after dissolving, adds 0.2mL, the CaCl of 0.05mol/L
2(concentration of the concentration that makes chlorion in whole reaction liquid is 10 to the aqueous solution
-3mol/L), after stirring, then dissolve in the AgNO of 1.2g
3, after dissolving, proceed to reactor, be heated to 120 DEG C of reactions 2.5 hours, then be heated to 160 DEG C of reactions 5 hours.After cooling, wash twice of centrifugation (rotating speed 4000r/min, each 10min), the centrifugal silver powder precipitation of collecting is carried out absolute ethanol washing centrifugal twice (rotating speed 4000r/min, each 10min) again, obtains silver powder sample (the micro-nano silver powder of triangular shape).Observe (Fig. 4) by SEM, the silver powder shape of gained approximately 80% presents triangular shape, and its triangular shape is the mixing of pyrometric cone, triangular cone table and triangular piece powder, and triangle silver powder size dimension concentrates on 1 μ m to 3 μ m.Separately have an appointment 20% polygon and circular piece powder is present in system.
Claims (5)
1. prepare the method for the micro-nano silver powder of triangular shape for one kind, it is characterized in that, comprise the following steps: polyvinylpyrrolidone is dissolved in alcoholic solvent, makes the polyvinylpyrrolidonesolution solution of 0.001-0.1g/mL, add chlorate in polyvinylpyrrolidonesolution solution, the concentration that makes chlorion is 10
-5-10
-2mol/L, stirs, and adds silver nitrate, and making its concentration is 0.001-0.2g/mL, after dissolving, proceed in reactor, be heated to 120 DEG C of reaction 0.1-5 hour, then be heated to 160 DEG C of reaction 1-5 hour, cooling, with absolute ethyl alcohol centrifuge washing several, obtain the micro-nano silver powder of triangular shape.
2. method according to claim 1, is characterized in that, described alcoholic solvent is 1,3 butanediol or 2,4 pentanediols or both mixed solvents.
3. method according to claim 1, is characterized in that, described polyvinylpyrrolidone, and its relative molecular weight is Mr=6000～15000.
4. method according to claim 1, is characterized in that, described chlorate is: NaCl, CuCl, CuCl
2, KCl, CaCl
2, ZnCl
2, MgCl
2, FeCl
3in a kind of or its combination.
5. method according to claim 1, is characterized in that, described uses absolute ethyl alcohol centrifuge washing for several times, and its centrifugation revolution is 2000～6000r/min, and centrifugation time is 5～15min, and centrifugal number of times is 2-4 time.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104972136A (en) * | 2015-07-30 | 2015-10-14 | 哈尔滨工业大学 | Preparation method for sheet type silver nanoparticles |
| CN105140341A (en) * | 2015-07-28 | 2015-12-09 | 李嘉诚 | Fabrication method of thin-film solar cell front electrode |
| CN109290588A (en) * | 2018-11-08 | 2019-02-01 | 南京大学 | A kind of preparation method of monodispersity triangular nano silver |
| CN110899722A (en) * | 2019-12-26 | 2020-03-24 | 无锡晶睿光电新材料有限公司 | Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof |
| CN115805316A (en) * | 2021-09-14 | 2023-03-17 | 中国科学院化学研究所 | Flaky silver nanoparticles, preparation method thereof, conductive silver paste composition and conductive silver paste |
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| CN1935422A (en) * | 2006-09-30 | 2007-03-28 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
| CN101024251A (en) * | 2007-03-08 | 2007-08-29 | 西北工业大学 | Method for preparing nano metal |
| WO2010108158A2 (en) * | 2009-03-20 | 2010-09-23 | Northwestern University | Plasmon mediated, photoinduced synthesis of triangular bipyramids |
| CN102085574A (en) * | 2009-12-04 | 2011-06-08 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
| JP5372450B2 (en) * | 2008-09-25 | 2013-12-18 | 独立行政法人科学技術振興機構 | Method for producing metal nanoparticles |
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| CN1935422A (en) * | 2006-09-30 | 2007-03-28 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
| CN101024251A (en) * | 2007-03-08 | 2007-08-29 | 西北工业大学 | Method for preparing nano metal |
| JP5372450B2 (en) * | 2008-09-25 | 2013-12-18 | 独立行政法人科学技術振興機構 | Method for producing metal nanoparticles |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140341A (en) * | 2015-07-28 | 2015-12-09 | 李嘉诚 | Fabrication method of thin-film solar cell front electrode |
| CN105140341B (en) * | 2015-07-28 | 2017-05-10 | 李嘉诚 | Fabrication method of thin-film solar cell front electrode |
| CN104972136A (en) * | 2015-07-30 | 2015-10-14 | 哈尔滨工业大学 | Preparation method for sheet type silver nanoparticles |
| CN104972136B (en) * | 2015-07-30 | 2017-02-01 | 哈尔滨工业大学 | Preparation method for sheet type silver nanoparticles |
| CN109290588A (en) * | 2018-11-08 | 2019-02-01 | 南京大学 | A kind of preparation method of monodispersity triangular nano silver |
| CN109290588B (en) * | 2018-11-08 | 2021-11-16 | 南京大学 | Preparation method of monodisperse triangular nano silver |
| CN110899722A (en) * | 2019-12-26 | 2020-03-24 | 无锡晶睿光电新材料有限公司 | Thin single crystal flake silver powder synthesized by chemical method and preparation method thereof |
| CN115805316A (en) * | 2021-09-14 | 2023-03-17 | 中国科学院化学研究所 | Flaky silver nanoparticles, preparation method thereof, conductive silver paste composition and conductive silver paste |
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| CN103909273B (en) | 2019-05-24 |
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Effective date of registration: 20210409 Address after: 510000 room 702, No.6-1, courtyard 81, Xianlie Middle Road, Dongshan District, Guangzhou City, Guangdong Province Patentee after: Tian Geng Address before: Unit 407-409, 4th floor, Zone G, science and technology innovation base, No.80, Science City, Langyue Road, Guangzhou Economic and Technological Development Zone, Guangdong 510000 Patentee before: SERVTEK MATERIAL TECHNOLOGY Co.,Ltd. |
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