CN1557588A - Method for manufacturing nano-silver - Google Patents
Method for manufacturing nano-silver Download PDFInfo
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- CN1557588A CN1557588A CNA2004100157894A CN200410015789A CN1557588A CN 1557588 A CN1557588 A CN 1557588A CN A2004100157894 A CNA2004100157894 A CN A2004100157894A CN 200410015789 A CN200410015789 A CN 200410015789A CN 1557588 A CN1557588 A CN 1557588A
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Abstract
The present invention is nano silver preparing process and belongs to the field of nano material preparing technology in radiochemistry. The technological process includes adopting silver nitrate as silver source, isopropanol as oxidant clearer in water solution, hydrophilic suitable for PVA for controlling the crystal kernel growth speed and grain size and electronic accelerator to produce electron beam for irradiation treatment; washing irradiated solution, centrifugal separation and stoving to obtain black nano silver powder. The present invention has simple technological process, short production period, no pollution and high safety, and the prepared nano silver grain is spherical, homogeneous in size and good in dispersivity.
Description
Technical field
The present invention relates to a kind of manufacture method of Nano Silver, that is to say a kind of preparation method of silver-colored ultramicron, belong to radiation chemistry and make nano material technology field.
Background technology
The application prospect of Nano Silver is boundless, it can be as the conductive silver paste in the integrated circuit, if in chemical fibre, add a spot of Nano Silver, can change some performance of chemical fabrics, and has very strong sterilizing ability, nanocrystalline silver is high by 30% than traditional material as the effectiveness of heat exchanger of dilution refrigeration machine, Nano Silver useful as catalysts also in addition, photomechanical production and enhancing Raman spectrum etc., Nano Silver is entrained in semiconductor or the insulator, then can obtain bigger third-order nonlinear susceptibility, utilize this characteristic can make photoelectric device such as photoswitch.Main at present chemical deposition, photopolymerization-reducing process, mechanical milling method, sputtering method, condensation of gas method, electrode method, galvanoplastic, vapour deposition method, chemistry redox method, the plasma oxidation of adopting of the preparation method of Nano Silver---reduction round-robin method etc.These methods are each has something to recommend him, need difference, can take different preparation methods.Preparing nano material with the irradiation chemical technology is a kind of newer method, and more widely used at present is the gamma-rays radiation method, and it is to utilize cobalt
60The gamma-ray irradiation reaction system that the Co isotope discharges, to obtain nano material, some shortcoming of this method: one,
60The Co isotope is a radioactive substance, when it can not be utilized, will become radwaste, and is unfavorable to environment and safety; Its two, prepare nano material discontinuous often with gamma-rays, can not produce continuously.From present circumstances, yet there are no other radiation sources that are fit to and prepare the Nano Silver material.
Summary of the invention
The objective of the invention is by other radiation sources, i.e. the electron beam of electron accelerator generation prepares Nano Silver as radiation source.
The manufacture method of a kind of Nano Silver of the present invention mainly adopts radiation chemistry to prepare, and it is characterized in that this method has following technical process and processing step:
A. at first, take by weighing a certain amount of silver nitrate, it is dissolved in the distilled water, make the concentration of its silver ion reach 0.005-0.02mol/100ml with FA1004 upper utensil type electronic balance; Add hydrophilic surface active agent polyvinyl alcohol (PVA) then, addition is 0.5-1 gram/100ml; Add the isopropyl alcohol (IPA) as oxidative free radical OH scavenger after stirring again, addition is 10-50ml/100ml; Process for preparation carries out in the darkroom, and the solution for preparing is placed in the light resistant container, treats irradiation;
B. the above-mentioned airtight container that fills the solution for preparing is placed under the radiation of the electron beam that the insulating core electron accelerator produces and carries out radiation treatment, its irradiation dose is 1-50Mrad;
C. use the sample of absolute ethanol washing then, and in the centrifugation of high speed centrifugation machine, repeated multiple times is to remove unreacted ion and hydrophilic surfactant polyvinyl alcohol (PVA) in the solution through irradiation;
D. sample is dried in vacuum drying chamber, temperature is 60 ℃, and drying time is 10-16 hour, finally can get the Nano Silver powder of black.
Above-mentioned concentration of silver ions optimum is 0.0015-0.02mol/100ml; Surface active agent polyvinyl alcohol (PVA) optimum addition is 0.7-0.8 gram/100ml; Isopropyl alcohol (IPA) optimum addition is 30-40ml/100ml.
The irradiation dose optimum of above-mentioned electron accelerator electron beam is 25-30Mrad.
The inventive method mainly adopts the source of silver nitrate as silver ion, the H aqueous electron e that utilizes the industrial electronic accelerator that aqueous solution ionization is produced
- AgDeng having reproducibility particle and free radical, silver ion progressively is reduced into silver atoms, silver atoms is gathered into nucleus, controls the size of the growth rate of nucleus with the control particle by hydrophilic surfactant active's polyvinyl alcohol (PVA), makes crystal grain reach nanoscale.
In the preparation process of the inventive method, the adding of surface active agent polyvinyl alcohol (PVA), can carry out surface modification to particle, cover one layer of polymeric at particle surface, so not only can control the growth of particle nucleation, and the particle aggregation phenomenon that takes place owing to the high surface energy of metallic atom particle, high chemical energy can prevent solution evaporation the time.The effect that adds isopropyl alcohol (TPA) is to remove oxidative free radical OH.
The present invention has plurality of advantages: 1. can not use any catalyst just can make at normal temperatures and pressures.2. adopt electron beam to prepare the nanometer copper product as the method for radiation source, its technological process is simple, sets up the mode of production of continous way easily, and with short production cycle.3. electron accelerator cuts out, and electron beam disappears, thus pollution-free, nuisanceless, help environmental protection, and security is good, 4. Zhi Bei nano-Ag particles is spherical in shape, and size is even, good dispersion.
The specific embodiment
After now the embodiment of the inventive method being described in
Embodiment one: the concrete preparation process of present embodiment is as follows:
A. at first, take by weighing a certain amount of silver nitrate, it is dissolved in the distilled water, make the concentration of its silver ion reach 0.01mol/100ml with FA1004 upper utensil type electronic balance; Add hydrophilic surface active agent polyvinyl alcohol (PVA) then, addition is 0.7 gram/100ml; Add oxidative free radical OH free radical scavenger isopropyl alcohol (IPA) after stirring again, addition is 2ml/100ml; Process for preparation carries out in the darkroom, and the solution for preparing is placed in the light resistant container, treats irradiation;
B. the above-mentioned colloidal solution for preparing is carried out radiation treatment under the radiation of the electron beam that the insulating core electron accelerator produces, its irradiation dose is 20Mrad;
C. wash irradiated sample with absolute alcohol then, and in the centrifugation of high speed centrifugation machine, repeated multiple times is to remove unreacted ion and hydrophilic surfactant polyvinyl alcohol (PVA) in the solution;
D. sample is dried in vacuum drying chamber, temperature is 60 ℃, and drying time is 10 hours, finally can get the Nano Silver powder of black.
Prepared style is carried out every characteristic test, and test case and result thereof are as follows:
With x x ray diffraction analysis x (XRD), can determine that from diffraction peak prepared black powder is a Nano Silver.
Utilize Hitachi 800 high resolution transmission electron microscopies (TEM) to observe, the particle that can see prepared Nano Silver is sphere, even particle size, and its particle diameter is distributed between the 20nm-40nm.
By the fusing point of NETZSCH STA 409 PG/PC type thermal analyzer test materials, the fusing point of prepared nanometer copper is 128.5 ℃, and the fusing point of common copper is 961.6 ℃.This shows that when the copper particle reaches nanoscale very big change takes place the performance of material.Therefore can utilize this performance of material that Nano Silver is made low-melting electric slurry, can carry out sintering at low temperatures and carry out the nanometer welding.
Embodiment two: the concrete preparation process of present embodiment is as follows:
A. at first, take by weighing a certain amount of silver nitrate, it is dissolved in the distilled water, make the concentration of its silver ion reach 0.02mol/100ml with FA1004 upper utensil type electronic balance; Add hydrophilic surface active agent polyvinyl alcohol (PVA) then, addition is 1 gram/100ml; Add oxidative free radical OH free radical scavenger isopropyl alcohol (IPA) after stirring again, addition is 40ml/100ml; Process for preparation carries out in the darkroom, and the solution for preparing is placed in the light resistant container, treats irradiation;
B. the above-mentioned colloidal solution for preparing is carried out radiation treatment under the radiation of the electron beam that the insulating core electron accelerator produces, its irradiation dose is 40Mrad;
C. wash irradiated sample with absolute alcohol then, and in the centrifugation of high speed centrifugation machine, repeated multiple times is to remove unreacted ion and hydrophilic surfactant polyvinyl alcohol (PVA) in the solution;
D. sample is dried in vacuum drying chamber, temperature is 60 ℃, and drying time is 16 hours, finally can get the Nano Silver powder of black.
Claims (3)
1. the manufacture method of a Nano Silver mainly adopts radiation chemistry to prepare, and it is characterized in that this method has following technical process and processing step:
A. at first, take by weighing a certain amount of silver nitrate, it is dissolved in the distilled water, make the concentration of its silver ion reach 0.005-0.02mol/100ml with FA1004 upper utensil type electronic balance; Add hydrophilic surface active agent polyvinyl alcohol (PVA) then, addition is 0.5-1 gram/100ml; Add the isopropyl alcohol (IPA) as oxidative free radical OH scavenger after stirring again, addition is 10-50ml/100ml; Process for preparation carries out in the darkroom, and the solution for preparing is placed in the light resistant container, treats irradiation;
B. the above-mentioned airtight container that fills the solution for preparing is placed under the radiation of the electron beam that the insulating core electron accelerator produces and carries out radiation treatment, its irradiation dose is 1-50Mrad;
C. use the sample of absolute ethanol washing then, and in the centrifugation of high speed centrifugation machine, repeated multiple times is to remove unreacted ion and hydrophilic surfactant polyvinyl alcohol (PVA) in the solution through irradiation;
D. sample is dried in vacuum drying chamber, temperature is 60 ℃, and drying time is 10-16 hour, finally can get the Nano Silver powder of black.
2. the manufacture method of a kind of Nano Silver according to claim 1 is characterized in that, described concentration of silver ions optimum is 0.0015-0.02mol/100ml; Surface active agent polyvinyl alcohol (PVA) optimum addition is 0.7-0.8 gram/100ml; Isopropyl alcohol (IPA) optimum addition is 30-40ml/100ml.
3. the manufacture method of a kind of Nano Silver according to claim 1 is characterized in that, the irradiation dose optimum of described electron accelerator electron beam is 25-30Mrad.
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| CNA2004100157894A CN1557588A (en) | 2004-01-13 | 2004-01-13 | Method for manufacturing nano-silver |
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| CNA2004100157894A CN1557588A (en) | 2004-01-13 | 2004-01-13 | Method for manufacturing nano-silver |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100393455C (en) * | 2005-12-23 | 2008-06-11 | 西安交通大学 | Preparation method of colloidal silver nanometer granule |
| CN100396408C (en) * | 2005-07-29 | 2008-06-25 | 云南铜业股份有限公司 | Production technology of high purity granular silver |
| CN100503744C (en) * | 2006-04-07 | 2009-06-24 | 中国科学院上海应用物理研究所 | Method for preparing nano silver grain, and prepared nano silver grain |
| CN101817086A (en) * | 2010-04-14 | 2010-09-01 | 中国科学院生态环境研究中心 | Novel process for converting silver-containing scarp to nano-silver |
| CN101200553B (en) * | 2006-12-14 | 2011-02-16 | 中国科学院理化技术研究所 | Silver particles/polyvinyl alcohol composite film as well as preparation method and uses thereof |
| CN102069193A (en) * | 2011-01-17 | 2011-05-25 | 华东理工大学 | Method for preparing granularity-controllable narrow-distribution spherical easily-dispersible silver powder through radiation reduction |
| CN102161092A (en) * | 2011-03-22 | 2011-08-24 | 中科院广州化学有限公司 | Nano silver capable of being dispersed in hydrophilic system and preparation method thereof |
| CN102310200A (en) * | 2011-08-24 | 2012-01-11 | 明基材料有限公司 | Nano silver particle forming method |
| CN103231067A (en) * | 2013-04-19 | 2013-08-07 | 河海大学 | Method for preparing nanometer metal particles |
| CN103341637A (en) * | 2013-07-10 | 2013-10-09 | 洛阳师范学院 | Silver microfibre and method for manufacturing silver microfibre |
| CN105597778A (en) * | 2015-11-17 | 2016-05-25 | 江苏大学 | Strontium ferrite-loaded nano silver composite material and preparing method thereof |
-
2004
- 2004-01-13 CN CNA2004100157894A patent/CN1557588A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100396408C (en) * | 2005-07-29 | 2008-06-25 | 云南铜业股份有限公司 | Production technology of high purity granular silver |
| CN100393455C (en) * | 2005-12-23 | 2008-06-11 | 西安交通大学 | Preparation method of colloidal silver nanometer granule |
| CN100503744C (en) * | 2006-04-07 | 2009-06-24 | 中国科学院上海应用物理研究所 | Method for preparing nano silver grain, and prepared nano silver grain |
| CN101200553B (en) * | 2006-12-14 | 2011-02-16 | 中国科学院理化技术研究所 | Silver particles/polyvinyl alcohol composite film as well as preparation method and uses thereof |
| CN101817086A (en) * | 2010-04-14 | 2010-09-01 | 中国科学院生态环境研究中心 | Novel process for converting silver-containing scarp to nano-silver |
| CN102069193B (en) * | 2011-01-17 | 2012-07-04 | 华东理工大学 | Method for preparing granularity-controllable narrow-distribution spherical easily-dispersible silver powder through radiation reduction |
| CN102069193A (en) * | 2011-01-17 | 2011-05-25 | 华东理工大学 | Method for preparing granularity-controllable narrow-distribution spherical easily-dispersible silver powder through radiation reduction |
| CN102161092A (en) * | 2011-03-22 | 2011-08-24 | 中科院广州化学有限公司 | Nano silver capable of being dispersed in hydrophilic system and preparation method thereof |
| CN102161092B (en) * | 2011-03-22 | 2013-03-06 | 中科院广州化学有限公司 | Nano silver capable of being dispersed in hydrophilic system and preparation method thereof |
| CN102310200A (en) * | 2011-08-24 | 2012-01-11 | 明基材料有限公司 | Nano silver particle forming method |
| CN102310200B (en) * | 2011-08-24 | 2014-09-03 | 明基材料有限公司 | Nano silver particle forming method |
| CN103231067A (en) * | 2013-04-19 | 2013-08-07 | 河海大学 | Method for preparing nanometer metal particles |
| CN103231067B (en) * | 2013-04-19 | 2015-08-26 | 河海大学 | A kind of preparation method of nano-metal particle |
| CN103341637A (en) * | 2013-07-10 | 2013-10-09 | 洛阳师范学院 | Silver microfibre and method for manufacturing silver microfibre |
| CN105597778A (en) * | 2015-11-17 | 2016-05-25 | 江苏大学 | Strontium ferrite-loaded nano silver composite material and preparing method thereof |
| CN105597778B (en) * | 2015-11-17 | 2018-06-19 | 江苏大学 | A kind of strontium ferrite loading nano silvery composite material and preparation method thereof |
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