CN1709618A - Method for preparing nano or submicron silver powder - Google Patents
Method for preparing nano or submicron silver powder Download PDFInfo
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- CN1709618A CN1709618A CN 200510010904 CN200510010904A CN1709618A CN 1709618 A CN1709618 A CN 1709618A CN 200510010904 CN200510010904 CN 200510010904 CN 200510010904 A CN200510010904 A CN 200510010904A CN 1709618 A CN1709618 A CN 1709618A
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Abstract
The present invention relates to a method of nm or sub-micron silver farina's preparation. Firstly, it makes silver nitrate dissolve in deionized water and dilute to 0.1~mol/L. Then in the condition of reduction temperature between 20 Deg. C and 50 Deg. C, stirring up in high speed, alkalescence and in the protection of surfactant, reducing the silver in the silver nitride solution to silver farina by organic reductant. Finally, after filtrating and abstersion, put created silver farina into vacuum oven and dry to get nm or sub-micron silver farina. The invention does not use complxer such as ammonia to complex the silver ion in the solution, but directly make nm or demicron silver farina by organic reductant. Advantages: simple technics, cheap production cost, less circumstance polutting, nm or perfect dispersing of demicron silver farina, granule bulk's uniformity and so on.
Description
Technical field; The present invention relates to the preparation method of a kind of nanometer, submicron silver powder, belong to materials science field.
Background technology: nano-silver powder has many particular performances,, surface big as specific area can and surface-active height, sintering temperature low etc., be widely used in fields such as electronics, metallurgy, chemical industry, medicine, military project, Aeronautics and Astronautics, medical, anti-biotic material, super low temperature refrigeration.
At present, the preparation method of nano-silver powder mainly contains physics method and chemical method.The physics method generally adopts vacuum evaporation-condensation method, vacuum sputtering and plasma sputtering method, has that equipment investment is big, productive rate is low, energy consumption is big and shortcoming such as cost height.Chemical method generally is with silver nitrate (AgNO
3) be raw material, adding ammoniacal liquor makes silver ion complexation form silver ammino ion to reduce the concentration of the silver ion in the solution, use hydrogen peroxide, hydrazine hydrate, triethanolamine, natrium citricum, ascorbic acid etc. silver to be precipitated out then, but the use of ammoniacal liquor make operating environment than variation as reducing agent.
Summary of the invention: the purpose of this invention is to provide a kind of be raw material with the silver nitrate, do not use complexing agent such as ammoniacal liquor that the silver ion in the solution is carried out complexing, and directly prepare the preparation method of nanometer or submicron silver powder with organic reducing agent.
The present invention prepares the method for nanometer or submicron silver powder; be earlier with silver nitrate with deionized water dissolving and be diluted to 0.1～1mol/L; it is 20～50 ℃ at reduction temperature then; under the protection of high-speed stirred, alkali condition and surfactant; with organic reducing agent silver being reduced into nanometer or submicron silver powder from liquor argenti nitratis ophthalmicus (adds organic reducing agent and carries out reduction reaction in liquor argenti nitratis ophthalmicus; restore fully to silver); filter then, wash, dry, obtain the nanometer or the submicron silver powder of good dispersion and even particle size.The washing of silver powder spends deionised water earlier 5～8 times, again with absolute alcohol washing 2～3 times.
The alkaline matter that adds in liquor argenti nitratis ophthalmicus can be NaOH, KOH, Na
2CO
3, K
2CO
3Deng, its concentration can be 2～4mol/L, and addition should guarantee that the reduction reaction endpoint pH reaches 9.0～11.8; Used reducing agent can be any in formic acid, formaldehyde, ethylene glycol or the glycerine (glycerine), also can be wherein any two kinds mixed liquor; Used surfactant (dispersant) can be any in polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) or the soil temperature 80, it also can be wherein any two kinds mixture, its concentration is 2～4%, and adding total amount is that every kilogram of silver adds 8.02～12.04 grams (8.02～12.04g/kg-Ag); The mixing speed of course of reaction is 800～2900 rev/mins, and the time that reduction reaction is carried out can be 20～40 minutes, till restoring fully to silver; The bake out temperature of silver powder in vacuum drying oven can be 60～80 ℃, drying time and can be 12～36 hours (specifically determine according to actual needs, be as the criterion by oven dry with silver powder).
The present invention is raw material with the silver nitrate, do not use complexing agent such as ammoniacal liquor that the silver ion in the solution is carried out complexing, and directly prepares nanometer or submicron silver powder with organic reducing agent, simplified technological process, avoided complexing agents such as ammoniacal liquor to producing and the influence of environment.Have that technology is simple, production cost is low, environmental pollution is little, the advantage of gained nanometer or submicron silver powder good dispersion and even particle size.
Description of drawings:
Accompanying drawing is a process chart of the present invention.
The specific embodiment: the invention will be further described below in conjunction with drawings and Examples.
Embodiment 1: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.1mol/L, under the condition of 25 ℃ of room temperatures and high-speed stirred (1000 rev/mins), adding 5ml formic acid and 6ml concentration and be the NaOH solution 140ml that 2% polyvinyl alcohol (PVA) solution (the PVA consumption is 11.11g/kg-Ag) and concentration is 2M reduces, recovery time is 30 minutes, reaction end pH=10.9, gained silver powder spends deionised water 6 times, again with absolute alcohol washing 3 times, under 70 ℃, carry out vacuum drying 24 hours, can obtain the nano-silver powder that average grain diameter is 70nm, direct yield is 99.3%.
Embodiment 2: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.3mol/L, at reduction temperature (2900 rev/mins) under the condition of 50 ℃ and high-speed stirred, adding 10ml formaldehyde and 13ml concentration and be the NaOH solution 420ml that 2% polyvinyl alcohol (PVA) solution (the PVA consumption is 8.02g/kg-Ag) and concentration is 2M reduces, recovery time is 20 minutes, reaction end pH=11.8, gained silver powder spends deionised water 8 times, again with absolute alcohol washing 3 times, under 65 ℃, carry out vacuum drying 36 hours, can obtain the nano-silver powder that average grain diameter is 80nm, direct yield is 99.3%.
Embodiment 3: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.5mol/L, under the condition of 25 ℃ of room temperatures and high-speed stirred (2000 rev/mins), adding 10ml ethylene glycol and 14ml concentration and be the NaOH solution 700ml that 4% soil temperature 80 (soil temperature 80 consumptions are 10.37g/kg-Ag) and concentration is 2M reduces, recovery time is 30 minutes, reaction end pH=10.5, gained silver powder spends deionised water 7 times, again with absolute alcohol washing 3 times, under 70 ℃, carry out vacuum drying 12 hours, can obtain the nano-silver powder that average grain diameter is 53nm, direct yield is 99.6%.
Embodiment 4: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.1mol/L, at reduction temperature (1500 rev/mins) under the condition of 40 ℃ and high-speed stirred, adding 5ml glycerine and 5ml concentration and be the KOH solution 140ml that 2% polyvinylpyrrolidone (PVP) solution (the PVP consumption is 9.26g/kg-Ag) and concentration is 2M reduces, recovery time is 25 minutes, reaction end pH=10.2, gained silver powder spends deionised water 6 times, again with absolute alcohol washing 3 times, under 80 ℃, carry out vacuum drying 12 hours, can obtain the nano-silver powder that average grain diameter is 100nm, direct yield is 99.4%.
Embodiment 5: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.3mol/L, be (1200 rev/mins) under the condition of 20 ℃ and high-speed stirred at reduction temperature, adding 5ml formic acid and 6ml ethylene glycol and 13ml concentration and be 3% polyvinylpyrrolidone (PVP) solution (the PVP consumption is 12.04g/kg-Ag) and concentration is the Na of 4M
2CO
3Solution 450ml reduces, and the recovery time is 40 minutes, reaction end pH=9.8, gained silver powder spends deionised water 7 times, with absolute alcohol washing 2 times, carries out vacuum drying 20 hours under 70 ℃ again, can obtain the nano-silver powder that average grain diameter is 67nm, direct yield is 99.5%.
Embodiment 6: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.3mol/L, under the condition of 25 ℃ of room temperatures and high-speed stirred (1000 rev/mins), adding 5ml formaldehyde and 2ml glycerine and 12ml concentration and be 2.5% polyvinyl alcohol (PVA) solution (the PVA consumption is 9.26g/kg-Ag) and concentration is the K of 3M
2CO
3Solution 650ml reduces, and the recovery time is 30 minutes, reaction end pH=9.6, gained silver powder spends deionised water 8 times, with absolute alcohol washing 3 times, carries out vacuum drying 36 hours under 60 ℃ again, can obtain the nano-silver powder that average grain diameter is 86nm, direct yield is 99.4%.
Embodiment 7: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 0.2mol/L, at reduction temperature (2500 rev/mins) under the condition of 35 ℃ and high-speed stirred, adding 10ml glycerine, concentration and be 2% polyvinyl alcohol (PVA) and each 5ml of polyvinylpyrrolidone (PVP) solution (PVA and PVP consumption are 4.63g/kg-Ag respectively, and the summation of the two is 9.26g/kg-Ag) and concentration is the Na of 2M
2CO
3Solution 390ml reduces, and the recovery time is 30 minutes, reaction end pH=9.0, gained silver powder spends deionised water 7 times, with absolute alcohol washing 3 times, carries out vacuum drying 16 hours under 75 ℃ again, can obtain the nano-silver powder that average grain diameter is 83nm, direct yield is 99.2%.
Embodiment 8: with the liquor argenti nitratis ophthalmicus 1000ml of deionized water preparation 1mol/L, under the condition of 45 ℃ of room temperatures and high-speed stirred (800 rev/mins), adding 25ml formic acid and 15ml concentration and be the KOH solution 350ml that 3% polyvinylpyrrolidone (PVP) solution (the PVP consumption is 8.33g/kg-Ag) and concentration is 4M reduces, recovery time is 30 minutes, reaction end pH=11.3, gained silver powder spends deionised water 7 times, again with absolute alcohol washing 3 times, under 70 ℃, carry out vacuum drying 24 hours, can obtain average grain diameter is the submicron order silver powder of 0.24 μ m, and direct yield is 99.7%.
Claims (8)
1, the preparation method of a kind of nanometer, submicron silver powder; it is characterized in that earlier silver nitrate with deionized water dissolving and be diluted to 0.1～1mol/L; at reduction temperature is under the protection of 20～50 ℃, high-speed stirred, alkali condition and surfactant; with organic reducing agent silver is reduced into nanometer or submicron silver powder from liquor argenti nitratis ophthalmicus; after the silver powder that generates filters, washs, put into the vacuum drying oven oven dry and obtain nanometer or submicron silver powder.
2, the preparation method of nanometer according to claim 1, submicron silver powder is characterized in that alkali condition is that the adding alkaline matter is 9.0～11.8 to reaction end pH value in liquor argenti nitratis ophthalmicus, and the mixing speed of course of reaction is 800～2900 rev/mins.
3, the preparation method of nanometer according to claim 1 and 2, submicron silver powder is characterized in that reducing agent can be any in formic acid, formaldehyde, ethylene glycol or the glycerine, also can be wherein any two kinds mixed liquor.
4, the preparation method of nanometer according to claim 1 and 2, submicron silver powder is characterized in that surfactant is polyvinylpyrrolidone, polyvinyl alcohol or soil temperature 80, also can be wherein any two kinds mixture.
5, the preparation method of nanometer according to claim 4, submicron silver powder is characterized in that surfactant concentrations is 2～4%.
6, the preparation method of nanometer according to claim 5, submicron silver powder, the adding total amount that it is characterized in that surfactant are that every kilogram of silver adds 8.02～12.04 grams.
7, the preparation method of nanometer according to claim 1, submicron silver powder is characterized in that the bake out temperature of silver powder in vacuum drying oven is that 60～80 ℃, drying time are 12～36 hours.
8, the preparation method of nanometer according to claim 1 and 2, submicron silver powder is characterized in that the reduction reaction time is 20～40 minutes.
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| CN100420528C (en) * | 2005-12-28 | 2008-09-24 | 中国科学院理化技术研究所 | Method for preparing redispersible Ag nanoparticle by using silver halide precrystallization reduction process |
| CN100431752C (en) * | 2006-09-30 | 2008-11-12 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
| CN100528427C (en) * | 2007-09-14 | 2009-08-19 | 北京首创纳米科技有限公司 | Method for preparing nanometer silver composite sol |
| CN101610865A (en) * | 2006-12-20 | 2009-12-23 | 派诺尔斯工业服务公司 | Preparation method of stable single dispersion metal silver nano-grain and products thereof |
| CN101053906B (en) * | 2006-04-11 | 2011-02-02 | 三星电机株式会社 | Method for manufacturing nickel nanoparticles |
| CN102009185A (en) * | 2010-12-09 | 2011-04-13 | 中山火炬职业技术学院 | Preparation method of silver nanobelts |
| CN101695757B (en) * | 2009-10-29 | 2011-10-05 | 彩虹集团公司 | Method for preparing aluminium powder with high tap density |
| CN102689021A (en) * | 2012-07-02 | 2012-09-26 | 昆明理工大学 | Method for preparing micron spherical silver powder |
| CN102085574B (en) * | 2009-12-04 | 2012-12-12 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
| CN103143724A (en) * | 2013-03-16 | 2013-06-12 | 安徽工业大学 | Preparation method of nanometer silver colloid in different shapes |
| CN103769608A (en) * | 2014-02-20 | 2014-05-07 | 北京碧水源膜科技有限公司 | Nano-silver sol separating method |
| US8852316B2 (en) | 2008-04-28 | 2014-10-07 | Tata Chemicals Limited | Process for the preparation of silver nano particles |
| CN104325151A (en) * | 2014-10-11 | 2015-02-04 | 中国振华集团云科电子有限公司 | Silver powder preparing method |
| CN104862952A (en) * | 2014-12-31 | 2015-08-26 | 皖西学院 | New preparation technology of permanent antibiosis and mildew prevention waterproof agent |
| CN104985190A (en) * | 2013-10-30 | 2015-10-21 | 江苏理工学院 | Synthetic method of flower-like silver microparticles |
| CN104999091A (en) * | 2015-08-22 | 2015-10-28 | 钱景 | Nano-silver particles and preparation thereof |
| CN105019229A (en) * | 2015-08-22 | 2015-11-04 | 钱景 | Preparation method of silver-carrying antibacterial blended fabric |
| CN105036092A (en) * | 2015-08-07 | 2015-11-11 | 中南大学 | Preparation method of spherical silver selenide particles |
| CN105088752A (en) * | 2015-08-22 | 2015-11-25 | 钱景 | Method for preparing silver-carrying antibacterial blended fabric by instant coffee |
| CN105133300A (en) * | 2015-08-22 | 2015-12-09 | 钱景 | Method for preparing nanosilver and finishing fabric |
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| CN108524540A (en) * | 2018-06-07 | 2018-09-14 | 同济大学 | A kind of composition and its application containing gentamicin and nano silver |
| CN110947980A (en) * | 2019-12-24 | 2020-04-03 | 长沙新材料产业研究院有限公司 | Preparation method of micron/submicron silver powder |
| CN111036936A (en) * | 2019-12-21 | 2020-04-21 | 浙江加州国际纳米技术研究院台州分院 | Method for improving yield of silver nanoparticles synthesized by polyol method |
| CN111804927A (en) * | 2019-04-10 | 2020-10-23 | 近镒生技股份有限公司 | Nano silver particle, porous material composition and preparation method thereof |
| CN114472917A (en) * | 2022-02-11 | 2022-05-13 | 西安汇创贵金属新材料研究院有限公司 | Preparation method of high-dispersity submicron silver powder |
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| CN115740480A (en) * | 2022-11-03 | 2023-03-07 | 云南驰宏锌锗股份有限公司 | Preparation method of superfine spherical silver powder |
-
2005
- 2005-07-08 CN CN 200510010904 patent/CN1709618A/en active Pending
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| CN100420528C (en) * | 2005-12-28 | 2008-09-24 | 中国科学院理化技术研究所 | Method for preparing redispersible Ag nanoparticle by using silver halide precrystallization reduction process |
| CN101053906B (en) * | 2006-04-11 | 2011-02-02 | 三星电机株式会社 | Method for manufacturing nickel nanoparticles |
| CN100431752C (en) * | 2006-09-30 | 2008-11-12 | 南京大学 | Method for preparing single dispersion triangular nano silver slice |
| CN101610865A (en) * | 2006-12-20 | 2009-12-23 | 派诺尔斯工业服务公司 | Preparation method of stable single dispersion metal silver nano-grain and products thereof |
| CN100528427C (en) * | 2007-09-14 | 2009-08-19 | 北京首创纳米科技有限公司 | Method for preparing nanometer silver composite sol |
| US8852316B2 (en) | 2008-04-28 | 2014-10-07 | Tata Chemicals Limited | Process for the preparation of silver nano particles |
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| CN102085574B (en) * | 2009-12-04 | 2012-12-12 | 深圳先进技术研究院 | Water-dispersible silver nanometer particles and preparation method thereof |
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| CN102009185A (en) * | 2010-12-09 | 2011-04-13 | 中山火炬职业技术学院 | Preparation method of silver nanobelts |
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| CN103143724B (en) * | 2013-03-16 | 2015-04-22 | 安徽工业大学 | Preparation method of nanometer silver colloid in different shapes |
| CN104985190B (en) * | 2013-10-30 | 2017-06-13 | 江苏理工学院 | Synthetic method of flower-like silver microparticles |
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| CN106521942B (en) * | 2016-12-01 | 2019-01-01 | 盐城工学院 | The method of allantoin application method and fabricated in situ nano-silver antibacterial finishing textile |
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| CN108524540A (en) * | 2018-06-07 | 2018-09-14 | 同济大学 | A kind of composition and its application containing gentamicin and nano silver |
| CN111804927A (en) * | 2019-04-10 | 2020-10-23 | 近镒生技股份有限公司 | Nano silver particle, porous material composition and preparation method thereof |
| CN111036936A (en) * | 2019-12-21 | 2020-04-21 | 浙江加州国际纳米技术研究院台州分院 | Method for improving yield of silver nanoparticles synthesized by polyol method |
| CN110947980A (en) * | 2019-12-24 | 2020-04-03 | 长沙新材料产业研究院有限公司 | Preparation method of micron/submicron silver powder |
| CN114472917A (en) * | 2022-02-11 | 2022-05-13 | 西安汇创贵金属新材料研究院有限公司 | Preparation method of high-dispersity submicron silver powder |
| CN115464147A (en) * | 2022-09-16 | 2022-12-13 | 北京曙光航空电气有限责任公司 | Silver powder manufacturing method |
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