CN101214555A - Method for preparing spherical nano silver powder - Google Patents
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- CN101214555A CN101214555A CNA2008100466909A CN200810046690A CN101214555A CN 101214555 A CN101214555 A CN 101214555A CN A2008100466909 A CNA2008100466909 A CN A2008100466909A CN 200810046690 A CN200810046690 A CN 200810046690A CN 101214555 A CN101214555 A CN 101214555A
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Abstract
The invention relates to a method for preparing a spherical nanometer sliver powder. A method for preparing a spherical nanometer sliver powder is characterized in that the invention includes the following steps: 1) spraying and pyrolyzing: a, dissolving silver nitrate with one of the three: {1}magnesium nitrate, {2}nickel nitrate, {3}copper nitrate into water to prepare into a water liquor with a consistency of 10 to 40wt percent; the mol ratio of magnesium ion, nickel ion or copper ion in the liquor is 0.05 to 1 :4; then spraying for pyrogenation; b, under the existence of a dispersant and protecting agent, adding into a non-water ethanol to disperse to acquire a mixture; 2) preparing the spherical nanometer sliver powder: a, dripping acid liquor into the mixture and adjusting a PH value between 3 to 5 to acquire a suspension containing the spherical nanometer sliver powder; b, pumping filtration, washing and drying to acquire the spherical nanometer sliver powder. The preparing method is simple and easy to be controlled, has no pollution and low cost, is suitable for industrialization scale production. The prepared spherical nanometer sliver powder belongs to the nanometer grade and the powder has uniform distribution of the grain diameter, regular shape and high yield.
Description
Technical field
The present invention relates to a kind of preparation method of spherical nano-silver powder.
Background technology
Silver atoms ordinal number 47, atomic weight 107.9, the peripheral electron 4d that arranges
105s
1, be positioned at period 5 IB family.Atomic radius 144.4 micromicrons, Ag radius 126 micromicrons, the first ionization energy 735kJ/mol, electronegativity 1.9.Good ductility and heat transfer electric conductivity are arranged.Density 10.5g/cm
3, 961.93 ℃ of fusing points, 2213 ℃ of boiling points.Chemical property is stable, not with the reaction of oxygen G﹠W, not with hydrochloric acid, dilute sulfuric acid and highly basic reaction.Can be dissolved in nitric acid or hot concentrated sulfuric acid.When having air and oxygen to exist, be dissolved in potassium cyanide solution, can be with sulphur or hydrogen sulfide reaction.Along with deepening continuously of nano materials research, the special nature of various nano particles is understood by people gradually.Advantages such as nano-silver powder has little, the very high surface-active of granularity, surface energy, catalytic performance, electrical and thermal conductivity performance and antibiotic and sterilizing activity, fusing point is low, sintering character is good have wide practical use in fields such as catalyst material, electron ceramic material, antistatic material, low temperature superconducting material, electric slurry, bio-sensing modulator material and inorganic antiseptic, deodorizing and the ultraviolet functional materials of absorption portion.
Both at home and abroad for the existing many reports of the achievement in research of nano-silver powder, main preparation method has physical vapor evaporation agglutination, electron beam evaporation, sputtering method, X-ray ray induction, heat plasma, sol-gel, microwave plasma method, mechanical milling method, laser high-temperature combustion method, chemical vapour deposition technique, polymer protection chemical reduction method, electrolysis, melt atomization, liquid phase chemical or solid state chemistry reducing process etc. at present.(1. Chu Guang, poplar natural feet, Liu Weifeng etc.The preparation of nano-silver powder and application study progress thereof.Noble metal, 2006,27 (1): 57-63; 2.H.H.Nersisyan, J.H.Lee, H.T.Son, etal.Mater Res Bull 38 (2003) 949; 3.N.H.H.Abu Bakar, J.Ismail, et al.Mater ChemPhys 104 (2007) 276; 4.N.Singh, P.K.Khanna.Mater Chem Phys 104 (2007) 367; 5.A.L.Pickering, G.J.T.Cooper, D.L.Long, et al.Polyhedron 23 (2004) 2075; 6.Z.Q.Niu F.Yan.Vib Spectrosc 43 (2007) 415; 7.S.Remita, P.Fontaine, E.Lacaze, et al.NuclInstrum Meth B 263 (2007) 436; 8.S.P.Wu, S.Y.Meng.Mater Chem Phys 89 (2005) 423; 9.A.I.Korchagin, N.K.Kuksanov, A.V.Lavrukhin, et al.Vacuum 77 (2005) 485; 10.J.L.H Chau, M.K.Hsu, C.C.Hsieh, et al.Mater Lett 59 (2005) 905; 11.R.Li, D.J.Kim, K.Yu, et al.J Mater Process Tech 137 (2003) 55-59. etc.) can prepare the nano-silver powder of multiple shapes such as sphere, sheet, dendroid by these methods.
Simultaneously, the report that adopts chemical reduction method, spray pyrolysis method to prepare super fine silver powder or compound silver powder is also arranged.
(1) preparation method of superfine spherical silver powder
A kind of preparation method of superfine spherical silver powder comprises preparation liquor argenti nitratis ophthalmicus, reducing agent, and this method may further comprise the steps: the concentration of adjusting liquor argenti nitratis ophthalmicus; The pH value of regulating liquor argenti nitratis ophthalmicus is to 1-7; Preparation reducing agent mixed solution; After the reducing agent mixed solution is adjusted to close temperature with liquor argenti nitratis ophthalmicus, under stirring condition, the reducing agent mixed solution mixed with liquor argenti nitratis ophthalmicus and react; Spend the reacted sediment of deionised water, use absolute ethanol washing 1-2 time again; Under 50-80 ℃ of vacuum, dry, just can get the ball shape silver powder of the different-grain diameter of 0.3-3.0 μ m.(Liu Bingning, Zhang Wenhua, Li Haibiao, Ma Shuzhen.The preparation method of superfine spherical silver powder, publication number: CN1387968, the applying date: May 26 calendar year 2001);
(2) be experimental raw to analyze pure silver nitrate, further do not purify, adopt deionized water to be mixed with solution.Adopt vertical spraying thermal decomposition experimental provision, prepared soccer star's ultra-fine silver powder.(Liu Zhihong, Liu Zhiyong, Li Qihou, Wu Houping, Zhang Duomo.Spray heating decomposition prepares super fine silver powder and pattern control thereof.The China YouSe Acta Metallurgica Sinica, 2007,17 (1): 149-155);
(3) be raw material with silver nitrate, silver nitrate and nickel nitrate mixed solution respectively, adopt the spray pyrolysis technology to prepare super fine silver powder and silver-colored nickel composite powder.(S.Y.Yang，S.G.Kim.Characterization?of?silver?and?silver/nickelcomposite?particles?prepared?by?spray?pyrolysis.Powder?Technology?146(2004)185-192)；
(4) be raw material with copper nitrate and silver nitrate, adopt the spray pyrolysis technology to prepare the Ag/CuO super fine composite powder.(D.Majumdar，H.D.Glicksman，T.T.Kodas.Generation?and?sintering?characteristics?ofsilver-copper(II)/oxide?composite?powders?made?by?spray?pyrolysis.PowderTechnology110(2000)76-81)；
The problem of preparation nano-silver powder existence mainly contains at present: the silver powder average grain diameter does not reach Nano grade; Silver powder particle diameter skewness, pattern are irregular; Lower, the separation difficulty of process recovery ratio of preparation silver powder is difficult to realize large-scale industrial production.In these methods, spray heating decomposition is because equipment and process are simple, and the silver powder degree of crystallinity height of preparation, good sphericity, any surface finish are specially adapted to the preparation of the micro aluminum powder of electronic applications, tool wide application prospect.But the relevant report that adopts spray pyrolysis to prepare nano-silver powder is not seen so far.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of spherical nano-silver powder, this preparation method is simple, pollution-free, cost is low, is suitable for industrial-scale production, and prepared spherical nano-silver powder is a Nano grade, and powder diameter is evenly distributed, the yield height.
To achieve these goals, technical scheme of the present invention is: a kind of preparation method of spherical nano-silver powder is characterized in that it comprises the steps:
1), spray pyrolysis:
A. with silver nitrate and one of following three kinds: 1. magnesium nitrate, 2. nickel nitrate, 3. copper nitrate, soluble in waterly be mixed with the aqueous solution that concentration is 10～40wt.% (mass concentration), the mol ratio of silver ion and magnesium ion, nickel ion or copper ion is 0.05～1: 4 in the solution; Then with silver nitrate and one of following three kinds: 1. magnesium nitrate, 2. nickel nitrate, the 3. aqueous solution spray pyrolysis of copper nitrate, pyrolysis temperature is 600～800 ℃, liquid inventory is controlled to be 336～500 milliliters/hour, carrier gas flux is 0.28MPa～0.32MPa, ambiance is an air, the composite precursor powder of De Yin and magnesia, nickel oxide or cupric oxide; Liquid inventory is controlled the precursor powder granularity at 10nm～1.0 μ m when concentration by regulating silver nitrate and magnesium nitrate, nickel nitrate or copper nitrate aqueous solution and spray pyrolysis;
B. with the composite precursor powder of silver and magnesia, nickel oxide or cupric oxide in the presence of dispersant and protective agent, add ultrasonic dispersion 10～30 minutes (employing magnetic stirrer) in the absolute ethyl alcohol, must mixture; Wherein, dispersant and protective agent are polyvinylpyrrolidone, and the mass ratio of polyvinylpyrrolidone and silver nitrate is 1: 10～50, and the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 1～5wt.%;
2) preparation of spherical nano-silver powder:
A. be that 5～10% acid solution is added drop-wise in the mixture that step 1) b obtains with mass concentration, regulating the pH value is 3～5, must contain the suspension of spherical nano-silver powder;
The suspension suction filtration that b. will contain spherical nano-silver powder, through 2～3 washings, the vacuum drying of absolute ethyl alcohol, vacuum drying temperature is controlled at 50～70 ℃, obtains spherical nano-silver powder again.
Described acid solution is hydrochloric acid solution, sulfuric acid solution or ammonium chloride solution.
Magnesium nitrate, nickel nitrate or copper nitrate template have played inhibitor and protectant effect, can control particle size and evenly distribution.The oxide that magnesium nitrate, nickel nitrate or copper nitrate decompose separates prevention with silver-colored particle, and it is grown up.Be not lose in the silver nitrate decomposable process, so very high yield is arranged.
The invention has the beneficial effects as follows: the particle diameter of the spherical nano-silver powder of preparation is evenly distributed, degree of crystallinity height, pattern rule, good sphericity, any surface finish, the process recovery ratio height of preparation silver powder; The controllable granularity of spherical nano-silver powder is built in 10nm～100nm.The present invention is simple and direct, easy to control because of its technology, do not pollute, cost of investment is low, is suitable for industrial-scale production.
The present invention has wide practical use in fields such as catalyst material, electron ceramic material, antistatic material, low temperature superconducting material, electric slurry, bio-sensing modulator material, inorganic antiseptic, deodorizing and the ultraviolet functional materials of absorption portion.
Description of drawings
Fig. 1 is preparation technology's flow chart of spherical nano-silver powder;
Fig. 2 is the X ray diffracting spectrum of spherical nano-silver powder;
Fig. 3 a is the field emission scanning electron microscope figure of silver and magnesian composite precursor powder;
Fig. 3 b is the field emission scanning electron microscope figure of spherical nano-silver powder.
The specific embodiment
Embodiment 1:
As shown in Figure 1, with 10 gram silver nitrate (AgNO
3) and 1208 gram magnesium nitrate { Mg (NO
3)
2Raw material is dissolved in 10962 milliliters the distilled water, through 600 ℃ of air atmosphere spray pyrolysis, liquid inventory is 336 milliliters/hour, gas carrier flow 0.28MPa, make silver and magnesian composite precursor powder, place it in 100 milliliters of ethanol solutions that are dissolved with 1 gram protective agent and polyethylene of dispersing agent pyrrolidones, adopt ultrasonic dispersion 10 minutes (employing magnetic stirrer), get mixture; Configuration quality concentration is 5% hydrochloric acid solution, is added drop-wise in the mixture, and regulating the pH value is 3; After drip finishing, behind the powder suction filtration in the solution, after 2 washings of absolute ethyl alcohol, vacuum drying, vacuum drying temperature is controlled at 50 ℃, and (granularity is 10nm～100nm) to obtain spherical nano-silver powder.
Fig. 2, Fig. 3 a, Fig. 3 b are that embodiment 1 obtains, and illustrate that the present invention can obtain that particle diameter is evenly distributed, the Nano Silver powder of pattern rule.
Embodiment 2:
With 50 gram silver nitrate (AgNO
3) and 302 gram magnesium nitrate { Mg (NO
3)
2Raw material is dissolved in 528 milliliters the distilled water, through 800 ℃ of air atmosphere spray pyrolysis, liquid inventory is 500 milliliters/hour, gas carrier flow 0.32MPa, make silver and magnesian composite precursor powder, place it in 100 milliliters of ethanol solutions that are dissolved with 5 gram protective agents and polyethylene of dispersing agent pyrrolidones, adopt ultrasonic dispersion 30 minutes (employing magnetic stirrer), get mixture; Configuration quality concentration is 15% sulfuric acid solution, is added drop-wise in the mixture, and regulating the pH value is 3; After drip finishing, behind the powder suction filtration in the solution, after 3 washings of absolute ethyl alcohol, vacuum drying, vacuum drying temperature is controlled at 70 ℃, and (granularity is 10nm～100nm) to obtain spherical nano-silver powder.
Embodiment 3:
With 50 gram silver nitrate (AgNO
3) and 3424 gram nickel nitrate { Ni (NO
3)
2Raw material is dissolved in 13896 milliliters the distilled water, through 800 ℃ of air atmosphere spray pyrolysis, liquid inventory is 500 milliliters/hour, gas carrier flow 0.32MPa, make the composite precursor powder of silver and nickel oxide, place it in 100 milliliters of ethanol solutions that are dissolved with 5 gram protective agents and polyethylene of dispersing agent pyrrolidones, adopt ultrasonic dispersion 30 minutes (employing magnetic stirrer), get mixture; Configuration quality concentration is 10% ammonium chloride solution, is added drop-wise in the mixture, and regulating the pH value is 4; After drip finishing, behind the powder suction filtration in the solution, after 3 washings of absolute ethyl alcohol, vacuum drying, vacuum drying temperature is controlled at 70 ℃, and (granularity is 10nm～100nm) to obtain spherical nano-silver powder.
Embodiment 4:
With 50 gram silver nitrate (AgNO
3) and 685 gram nickel nitrate { Ni (NO
3)
2Raw material is dissolved in 6615 milliliters the distilled water, through 600 ℃ of air atmosphere spray pyrolysis, liquid inventory is 336 milliliters/hour, gas carrier flow 0.28MPa, make the composite precursor powder of silver and nickel oxide, place it in 100 milliliters of ethanol solutions that are dissolved with 1 gram protective agent and polyethylene of dispersing agent pyrrolidones, adopt ultrasonic dispersion 10 minutes, get mixture; Configuration quality concentration is 5% ammonium chloride solution, is added drop-wise in the mixture, and regulating the pH value is 4; After drip finishing, behind the powder suction filtration in the solution, after 2 washings of absolute ethyl alcohol, vacuum drying, vacuum drying temperature is controlled at 50 ℃, and (granularity is 10nm～100nm) to obtain spherical nano-silver powder.
Embodiment 5:
With 50 gram silver nitrate { AgNO
3And 285 gram copper nitrate { Cu (NO
3)
2Raw material is dissolved in 1340 milliliters the distilled water, through 700 ℃ of air atmosphere spray pyrolysis, liquid inventory is 400 milliliters/hour, gas carrier flow 0.30MPa, make the composite precursor powder of silver and cupric oxide, place it in 100 milliliters of ethanol solutions that are dissolved with 3 gram protective agents and polyethylene of dispersing agent pyrrolidones, adopt ultrasonic dispersion 20 minutes, get mixture; Configuration quality concentration is 5% hydrochloric acid solution, is added drop-wise in the mixture, and regulating the pH value is 5; After drip finishing, behind the powder suction filtration in the solution, after 3 washings of absolute ethyl alcohol, vacuum drying, vacuum drying temperature is controlled at 60 ℃, and (granularity is 10nm～100nm) to obtain spherical nano-silver powder.
Embodiment 6:
With 10 gram silver nitrate AgNO
3With 2845 gram copper nitrate Cu (NO
3)
2Raw material is dissolved in 4282 milliliters the distilled water, through 700 ℃ of air atmosphere spray pyrolysis, liquid inventory is 450 milliliters/hour, gas carrier flow 0.31MPa, make the composite precursor powder of silver and cupric oxide, place it in 100 milliliters of ethanol solutions that are dissolved with 2 gram protective agents and polyethylene of dispersing agent pyrrolidones, adopt ultrasonic dispersion 15 minutes, get mixture; Configuration quality concentration is 10% sulfuric acid solution, is added drop-wise in the mixture, and regulating the pH value is 5; After drip finishing, behind the powder suction filtration in the solution, after 3 washings of absolute ethyl alcohol, vacuum drying, vacuum drying temperature is controlled at 60 ℃, and (granularity is 10nm～100nm) to obtain spherical nano-silver powder.
Embodiment 7:
A kind of preparation method of spherical nano-silver powder, it comprises the steps:
1), spray pyrolysis:
A. be mixed with the aqueous solution that concentration is 10wt.% (mass concentration) with silver nitrate and copper nitrate are soluble in water, the mol ratio of silver ion and copper ion is 0.05: 4 in the solution; With the aqueous solution spray pyrolysis of silver nitrate and copper nitrate, pyrolysis temperature is 600 ℃ then, and liquid inventory is controlled to be 336 milliliters/hour, and carrier gas flux is 0.28MPa, and ambiance is an air, the composite precursor powder of De Yin and cupric oxide;
B. with silver and the composite precursor powder of cupric oxide in the presence of dispersant and protective agent, add ultrasonic dispersion 10 minutes (employing magnetic stirrer) in the absolute ethyl alcohol, must mixture; Wherein, dispersant and protective agent are polyvinylpyrrolidone, and the mass ratio of polyvinylpyrrolidone and silver nitrate is 1: 10, and the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 1wt.%;
2) preparation of spherical nano-silver powder:
A. be that 5% acid solution (ammonium chloride solution) is added drop-wise in the mixture that step 1) b obtains with mass concentration, regulating the pH value is 3, must contain the suspension of spherical nano-silver powder;
Through 2 washings, the vacuum drying of absolute ethyl alcohol, vacuum drying temperature is controlled at 50 ℃, obtains spherical nano-silver powder again for the suspension suction filtration that b. will contain spherical nano-silver powder, the powder behind the suction filtration.
Embodiment 8:
A kind of preparation method of spherical nano-silver powder, it comprises the steps:
1), spray pyrolysis:
A. be mixed with the aqueous solution that concentration is 40wt.% (mass concentration) with silver nitrate and nickel nitrate are soluble in water, the mol ratio of silver ion and nickel ion is 1: 4 in the solution; With the aqueous solution spray pyrolysis of silver nitrate and nickel nitrate, pyrolysis temperature is 800 ℃ then, and liquid inventory is controlled to be 500 milliliters/hour, and carrier gas flux is 0.32MPa, and ambiance is an air, the composite precursor powder of De Yin and nickel oxide;
B. with silver and the composite precursor powder of nickel oxide in the presence of dispersant and protective agent, add ultrasonic dispersion 30 minutes (employing magnetic stirrer) in the absolute ethyl alcohol, must mixture; Wherein, dispersant and protective agent are polyvinylpyrrolidone, and the mass ratio of polyvinylpyrrolidone and silver nitrate is 1: 50, and the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 5wt.%;
2) preparation of spherical nano-silver powder:
A. be that 10% acid solution (sulfuric acid solution) is added drop-wise in the mixture that step 1) b obtains with mass concentration, regulating the pH value is 5, must contain the suspension of spherical nano-silver powder;
Through 3 washings, the vacuum drying of absolute ethyl alcohol, vacuum drying temperature is controlled at 70 ℃, obtains spherical nano-silver powder again for the suspension suction filtration that b. will contain spherical nano-silver powder, the powder behind the suction filtration.
The bound value of each raw material of the present invention, and the bound value of technological parameter can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (2)
1. the preparation method of a spherical nano-silver powder is characterized in that it comprises the steps:
1), spray pyrolysis:
A. with silver nitrate and one of following three kinds: 1. magnesium nitrate, 2. nickel nitrate, 3. copper nitrate, soluble in waterly be mixed with the aqueous solution that concentration is 10～40wt.%, the mol ratio of silver ion and magnesium ion, nickel ion or copper ion is 0.05～1: 4 in the solution; Then with silver nitrate and one of following three kinds: 1. magnesium nitrate, 2. nickel nitrate, the 3. aqueous solution spray pyrolysis of copper nitrate, pyrolysis temperature is 600～800 ℃, liquid inventory is controlled to be 336～500 milliliters/hour, carrier gas flux is 0.28MPa～0.32MPa, ambiance is an air, the composite precursor powder of De Yin and magnesia, nickel oxide or cupric oxide;
B. with the composite precursor powder of silver and magnesia, nickel oxide or cupric oxide in the presence of dispersant and protective agent, added in the absolute ethyl alcohol ultrasonic dispersion 10～30 minutes, must mixture; Wherein, dispersant and protective agent are polyvinylpyrrolidone, and the mass ratio of polyvinylpyrrolidone and silver nitrate is 1: 10～50, and the concentration of polyvinylpyrrolidone in absolute ethyl alcohol is 1～5wt.%;
2) preparation of spherical nano-silver powder:
A. be that 5～10% acid solution is added drop-wise in the mixture that step 1) b obtains with mass concentration, regulating the pH value is 3～5, must contain the suspension of spherical nano-silver powder;
The suspension suction filtration that b. will contain spherical nano-silver powder through 2～3 washings, the vacuum drying of absolute ethyl alcohol, obtains spherical nano-silver powder again.
2. the preparation method of a kind of spherical nano-silver powder according to claim 1, it is characterized in that: described acid solution is hydrochloric acid solution, sulfuric acid solution or ammonium chloride solution.
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| CN106610144B (en) * | 2016-12-07 | 2019-10-25 | 桂林电子科技大学 | A kind of method that local surface plasma resonance absorption sunlight prepares steam |
| CN107385210A (en) * | 2017-07-07 | 2017-11-24 | 金川集团股份有限公司 | A kind of nickel nitrate/cobalt liquor system transition and the method for nitric acid reuse |
| CN107385210B (en) * | 2017-07-07 | 2019-08-06 | 金川集团股份有限公司 | A kind of method that nickel nitrate/cobalt liquor system makes the transition with nitric acid reuse |
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| CN109702222B (en) * | 2018-03-30 | 2022-06-10 | 中南大学 | Preparation method of silver zinc oxide or silver copper oxide composite powder and system for implementing preparation method |
| CN110961656A (en) * | 2019-11-18 | 2020-04-07 | 昆明理工大学 | Preparation method of copper-nickel alloy powder |
| CN110961656B (en) * | 2019-11-18 | 2021-07-09 | 昆明理工大学 | Preparation method of copper-nickel alloy powder |
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