CN100503744C - Method for preparing nano silver grain, and prepared nano silver grain - Google Patents
Method for preparing nano silver grain, and prepared nano silver grain Download PDFInfo
- Publication number
- CN100503744C CN100503744C CNB2006100255449A CN200610025544A CN100503744C CN 100503744 C CN100503744 C CN 100503744C CN B2006100255449 A CNB2006100255449 A CN B2006100255449A CN 200610025544 A CN200610025544 A CN 200610025544A CN 100503744 C CN100503744 C CN 100503744C
- Authority
- CN
- China
- Prior art keywords
- chitosan
- nano silver
- solution
- silver grain
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Medicinal Preparation (AREA)
- Cosmetics (AREA)
Abstract
This invention discloses a method for preparing Ag nanoparticles. The method comprises: (1) mixing acid solution of chitosan and AgNO3 solution to obtain a mixed solution; (2) adjusting the pH value to 3.0-5.0; (3) irradiating without oxygen. The deacetylation degree of chitosan is greater than or equal to 70%, and the average molecular weight is less than or equal to 20000. The concentration of chitosan in the mixed solution is 0.001-0.05 wt. %, and that of AgNO3 is 0.01-23.5 mM. The obtained Ag nanoparticles have such advantages as small average particle size, uniform particle size distribution, high solid content, high water solubility, and high biocompatibility.
Description
Technical field
The present invention relates to a kind of preparation method of Nano silver grain and the Nano silver grain that makes.
Background technology
Nano silver grain has good antimicrobial property and photoelectrochemical behaviour, is used widely in nano-catalytic carrier, solar energy converting, biosensor and various anti-biotic material.The method for preparing Nano silver grain has a variety of, as chemical reduction method, evaporation sputtering method and radiation reduction method.In these preparation process, two difficult problems that are difficult to overcome are exactly to prevent to form the argent of nanoparticle by the stable dispersion of air or institute's oxidation of other material and Nano silver grain.The effective ways that solve these two difficult problems are exactly to modify in the nanoparticle surface for preparing, and promptly load one deck polymer substance or charged group on the surface of Nano silver grain make to be difficult between the nanoparticle taking place to reunite and the formation stable dispersion.But, when Nano silver grain is modified, should consider the application of Nano silver grain, effectively coat again and make its stable dispersion, this has proposed certain conditions to the selection that coats material (coating), has also limited to the range of choice that coats material greatly.Using the polymer substance that is widely used in the coated with silver nanoparticle has the straight-chain paraffin and the dendritic compound of straight chain alcohols, mercaptan, band amino or carboxyl.Yet these Nano silver grain solubleness in water that coat the material preparation are very little even insoluble, therefore limited the further use of Nano silver grain.The water miscible research of more existing at present raising Nano silver grains, its coating has alcohols, pyridines or tree type polymer, if the interior residual a spot of coating that has of Nano silver grain product then has the potential bio-toxicity.
On the other hand, be raw material with chitin or chitosan, adopt different methods to reduce behind its molecular-weight average resulting degradation of polysaccharide and have good antimicrobial property and be widely studied and report.Because chitin or chitosan are natural cation high molecular materials, its basic molecular structure is hexa-atomic sugar ring, therefore it has good consistency and biological activity to organism, and market product has been arranged, and is the additive of major ingredient as containing in makeup, food, the animal-feed with the chitosan.
Summary of the invention
The objective of the invention is to solve the problem such as water-soluble, biocompatibility of Nano silver grain in the prior art, a kind of preparation method of Nano silver grain is provided, is coating in the method with the chitosan, and this method specifically comprises the steps:
1) acid solution of chitosan is mixed with silver nitrate solution mixed solution, wherein, the deacetylation of chitosan 〉=70%, molecular-weight average≤20,000, in this mixed solution, the concentration of chitosan is 0.001～0.05wt%, and the concentration of Silver Nitrate is 0.01～23.5mM;
2) regulate pH to 3.0～5.0;
3) under oxygen free condition, carry out irradiation.
Low molecular chitosan with molecular-weight average≤20,000 in step 1) is that coating has following advantage: A) good water-solubility, B) excellent biological compatibility, C) good antimicrobial property, D) lifeless matter toxicity.Therefore, in the present invention, the molecular-weight average of chitosan is the smaller the better, is preferably the chitosan of molecular-weight average≤15,000.The chitosan of this low average molecular weight can be by obtaining behind the solid-state irradiation-induced degradation, as through 50～300kGy dosage
60The solid-state irradiation-induced degradation in Co source obtains, the molecular-weight average of this chitosan generally all is not more than 20,000, the preparation method of low average molecular weight chitosan specifically can be with reference to following document (Long Dewu, Wu Guozhong etc., the research of radiation method degrade chitosan and bacteriostasis property thereof, polymer material science and engineering, 21 (2005) 240-242).
In the step 1), as long as the acid solution of chitosan comprises that all can dissolve the acid solution of chitosan, as long as chitosan can be dissolved in wherein fully.The acid of conventional dissolving chitosan has acetic acid and/or hydrochloric acid in the prior art, is preferably acetic acid, and for example chitosan is dissolvable in water in 0.01%～0.05% the acetum, is preferably to be dissolved in 0.02% the acetum.
In the present invention, the deacetylation of chitosan requires 〉=70%, and too low meeting causes the water-soluble of Nano silver grain and dispersion stabilization variation.
In this mixed solution, the concentration of chitosan can be 0.001～0.05wt%, and the concentration of chitosan is too low, does not reach the effect of stablizing Nano silver grain, and the concentration of chitosan is too high, and Nano silver grain is easily reunited.Therefore chitosan can obtain the Nano silver grain that dispersion stabilization is good and uniform particle diameter distributes in this concentration range in reaction system.
In step 1), the concentration of Silver Nitrate can be 0.01～23.5mM in the mixed solution.The concentration of Silver Nitrate is too low, and the productive rate of Nano silver grain is too low; Concentration is too high, and the median size of Nano silver grain is bigger, and also heterogeneity of the size distribution of Nano silver grain.Therefore, more preferably 0.03～20mM of the concentration of Silver Nitrate.
Step 2) in, regulates pH to 3.0～5.0 and can make that the chitosan dissolved is better, be preferably and regulate pH to 3.0.
In the step 3), be meant under the described oxygen free condition to feed rare gas element that the rare gas element here can be nitrogen and/or argon gas etc., but nitrogen is cheap and easy to get with under the condition of removing oxygen, preferably it.
In the step 3), described irradiation can be that the gamma ray projector of 3～15kGy or ultraviolet source that λ is 190～250nm carry out irradiation with irradiation dose.
Described gamma ray projector has multiple, still
60The Co source is cheap and easy to get, preferred it, in the middle of test, ultraviolet source can generate Nano silver grain so that chitosan and Silver Nitrate react also applicable to the present invention, this ultraviolet source is preferably the ultraviolet source that λ is 190～250nm, irradiation time is 20～40min/1mL reaction solution, and the irradiation time of ultraviolet source decides according to what and silver nitrate concentration of load responsive fluid, if silver nitrate concentration of the present invention is 10
-4In the M order of magnitude scope, irradiation time is generally at the 30min/1mL reaction solution, suitably increases irradiation time when silver nitrate concentration is big, and silver nitrate concentration hour suitably reduces irradiation time.And under the same silver nitrate concentration, different irradiation times can influence the particle diameter of Nano silver grain, and irradiation time length can make particle increase, and the time, short particle was then corresponding smaller.In the middle of this irradiation reaction process, gamma-rays or ultraviolet irradiation cause the further degraded of chitosan and silver ions are reduced.
In a preferred embodiment of the present invention, can carry out drying with obtaining solution behind the irradiation, can obtain the exsiccant Nano silver grain.
Another object of the present invention provides the Nano silver grain that preparation method of the present invention makes.
The median size of this Nano silver grain preferably is 5～20nm.
The solid content of this Nano silver grain preferably is 0.4wt%, and the solid content of indication is meant the massfraction of argent in silver nano-particle solution here.
Positive progressive effect of the present invention is: the median size of the Nano silver grain that method of the present invention makes is little, homogeneity good, dispersion stabilization is good, solid content is high, have no side effect, and have well water-soluble and biocompatibility, preparation method of the present invention also is easy to control the Nano silver grain that obtains the size distribution homogeneous.
Description of drawings
The TEM figure of the Nano silver grain that Figure 1A makes for the embodiment of the invention 1;
The size distribution column synoptic diagram of the Nano silver grain that Figure 1B makes for the embodiment of the invention 1;
The height of pillar is represented among the figure: the Nano silver grain of this size shared mark (proportion, the frequency of Chu Xianing in other words in other words) in the Nano silver grain of all countings.
Fig. 2 A is the TEM figure of the Nano silver grain that makes of the embodiment of the invention 2;
Fig. 2 B is the size distribution column synoptic diagram of the Nano silver grain that makes of the embodiment of the invention 2;
Fig. 3 A is the TEM figure of the Nano silver grain that makes of the embodiment of the invention 3;
Fig. 3 B is the size distribution column synoptic diagram of the Nano silver grain that makes of the embodiment of the invention 3;
Fig. 4 A is the TEM figure of the Nano silver grain that makes of the embodiment of the invention 4;
Fig. 4 B is the size distribution column synoptic diagram of the Nano silver grain that makes of the embodiment of the invention 4;
The TEM figure of the Nano silver grain that Fig. 5 makes for the embodiment of the invention 5;
Fig. 6 is the maximal ultraviolet absorption spectrogram of Nano silver grain of the present invention;
Fig. 7 is the potential ph diagram ph of Nano silver grain of the present invention under different pH.
Embodiment
According to document (Long Dewu, Wu Guozhong etc., the research of radiation method degrade chitosan and bacteriostasis property thereof, polymer material science and engineering, 21 (2005) 240-242) the preparation chitosan is as coating of the present invention, concrete steps are as follows: the chitosan of deacetylation 〉=70% is carried out solid-state irradiation-induced degradation through cobalt-60 source of 300kGy dosage, obtain molecular-weight average and be about 15,000 chitosan.
The chitosan of deacetylation 〉=70% is carried out solid-state irradiation-induced degradation through cobalt-60 source of 100kGy dosage, obtain molecular-weight average and be about 20,000 chitosan.
Embodiment 1
With above-mentioned deacetylation 〉=70%, molecular-weight average is that about 20,000 chitosan is dissolved in 0.02% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, contain 0.005wt% chitosan and 2.0 * 10 in this mixed solution
-3Mol.L
-1Silver Nitrate.This mixed solution is regulated pH to 3.0 with acetic acid again; Feed purity nitrogen and carry out deoxygenation, use
60Irradiation is carried out in the Co source, and irradiation dose 10kGy obtains brown yellow solution; This drips of solution is carried out drying on copper mesh, scan with transmission electron microscope afterwards, shown in result such as Figure 1A (TEM amplifies 40,000 times, and scale is 50nm among the figure), size distribution is shown in Figure 1B.
The result shows: can find out that from Figure 1A the particle diameter ratio of the Nano silver grain that preparation method of the present invention makes is more even, Figure 1B can prove that also particle diameter is homogeneous and distributes, and median size is 16nm.
With above-mentioned deacetylation 〉=70%, molecular-weight average is that about 20,000 chitosan is dissolved in 0.01% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, contain 0.005wt% chitosan and 1.0 * 10 in this mixed solution
-3Mol.L
-1Silver Nitrate, this mixed solution is regulated pH to 3.0 with acetic acid again; Feed purity nitrogen and carry out deoxygenation, use
60Irradiation is carried out in the Co source, and irradiation dose 10kGy obtains yellow solution; This drips of solution is carried out drying on copper mesh, scan with transmission electron microscope afterwards, shown in result such as Fig. 2 A (amplify 40,000 times, scale is 50nm among the figure), size distribution is shown in Fig. 2 B.
The result shows: can find out that from Fig. 2 A the particle diameter ratio of the Nano silver grain that preparation method of the present invention makes is more even, Fig. 2 B can prove that also particle diameter is homogeneous and distributes, and the Nano silver grain median size is 10nm.
Embodiment 3
With above-mentioned deacetylation 〉=70%, molecular-weight average is that about 15,000 chitosan is dissolved in 0.03% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, contain 0.005wt% chitosan and 5.0 * 10 in this mixed solution
-4Mol.L
-1Silver Nitrate, this mixed solution is regulated pH to 3.0 with acetic acid again; Feed purity nitrogen and carry out deoxygenation, use
60Irradiation is carried out in the Co source, and irradiation dose 10kGy obtains bright yellow solution; This drips of solution is carried out drying on copper mesh, scan with transmission electron microscope afterwards, shown in result such as Fig. 3 A (TEM amplifies 40,000 times, and scale is 50nm among the figure), size distribution is shown in Fig. 3 B.
The result shows: can find out that from Fig. 3 A the particle diameter ratio of the Nano silver grain that preparation method of the present invention makes is more even, Fig. 3 B can prove that also particle diameter is homogeneous and distributes, and the Nano silver grain median size is 8nm.
With above-mentioned deacetylation 〉=70%, molecular-weight average is that about 15,000 chitosan is dissolved in 0.05% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, contain 0.005wt% chitosan and 3.0 * 10 in this mixed solution
-4Mol.L
-1Silver Nitrate, this mixed solution is regulated pH to 3.0 with acetic acid again; Feed purity nitrogen and carry out deoxygenation, use
60Irradiation is carried out in the Co source, and irradiation dose 10kGy obtains bright yellow solution; This drips of solution is carried out drying on copper mesh, scan with transmission electron microscope afterwards, shown in result such as Fig. 4 A (TEM amplifies 40,000 times, and scale is 50nm among the figure), size distribution is shown in Fig. 4 B.
The result shows: can find out that from Fig. 4 A and 4B the Nano silver grain that preparation method of the present invention makes is compared with embodiment 1～3, particle diameter is littler, and median size is 5nm, and this explanation can be regulated and control the particle diameter of Nano silver grain by the concentration of regulating silver ion solution.
With above-mentioned deacetylation 〉=70%, molecular-weight average is 20, chitosan about 000 is dissolved in 0.02% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, the Silver Nitrate that contains 0.01wt% chitosan and 0.4wt% (being 23.5mM) in this mixed solution, this mixed solution are regulated pH to 3.0 with acetic acid again; Feed purity nitrogen and carry out deoxygenation, use
60Irradiation is carried out in the Co source, and irradiation dose 10kGy obtains brown solution; This drips of solution is carried out drying on copper mesh, scan with transmission electron microscope afterwards, shown in result such as Fig. 5 (amplify 20,000 times, scale is 100nm among the figure).
The result shows: the size of Nano silver grain is about 6～20nm.
With above-mentioned deacetylation 〉=70%, molecular-weight average is 20, chitosan about 000 is dissolved in 0.04% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, ultimate density is chitosan 0.001wt% and Silver Nitrate 2.0 * 10 in the mixed solution
-5Mol.L
-1Logical purity nitrogen deoxygenation is carried out irradiation with the 250nm ultraviolet ray, and irradiation 30min obtains bright yellow solution.
Embodiment 7
With above-mentioned deacetylation 〉=70%, molecular-weight average is that about 15,000 chitosan is dissolved in 0.02% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, the mixed solution ultimate density is chitosan 0.05wt% and Silver Nitrate 1.0 * 10
-5Mol.L
-1Logical purity nitrogen deoxygenation is carried out irradiation with λ for the 190nm ultraviolet ray, and irradiation 30min obtains bright yellow solution.
With above-mentioned deacetylation 〉=70%, molecular-weight average is 20, chitosan about 000 is dissolved in 0.03% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, ultimate density is chitosan 0.005wt% and Silver Nitrate 3.0 * 10 in the mixed solution
-5Mol.L
-1Logical purity nitrogen deoxygenation is used
60Irradiation is carried out in the Co source, and irradiation dose 15kGy obtains bright yellow solution.
Embodiment 9
With above-mentioned deacetylation 〉=70%, molecular-weight average is that about 20,000 chitosan is dissolved in 0.02% the acetic acid, again this solution is mixed with silver nitrate solution mixed solution, contain 0.02wt% chitosan and 20mmol.L in the mixed solution
-1Silver Nitrate; Logical purity nitrogen deoxygenation is used
60Irradiation is carried out in the Co source, and irradiation dose 3kGy obtains bright yellow solution.
The silver nano-particle solution that embodiment 1～4 directly prepares is surveyed absorption spectrum with ultraviolet spectrophotometer, the result as shown in Figure 6, maximum absorption band is about 400nm, along with reducing of nano particle diameter, maximum absorption band moves to 390nm (a among the figure, b, c, d is the silver nano-particle solution of corresponding embodiment 1～4 respectively), this and document (M.Mostafavi, G.R.Dey, L Franc ü ois, J.Belloni, Transient and Stable Silver Clusters Induced by Radiolysis in Methanol, J.Phys.Chem.A 2002,106,10184-10194) report conforms to.
Effect embodiment 1 is water-soluble
Nano silver grain colloidal sol centrifugation 5min under 3000rpm with embodiment 1 makes goes the supernatant liquid suction with suction pipe, adds deionized water again three times, and ultra-sonic dispersion can obtain transparent glassy yellow silver Nano sol.Nano silver grain of the present invention can reach 10
-2M
-1The concentration of (argent).
The Nano silver grain for preparing with embodiment 1～4 is dissolved in the water, and makes its concentration reach 0.08wt%.The result shows: Nano silver grain energy stable dispersion of the present invention is in the aqueous solution.At room temperature, lucifuge can not deposited up to 6 months, and flocculation does not take place or become muddy, keeps the character of transparent colloid.Serious reunion does not take place in the scope of pH2.2～7.3, and this can be confirmed from the Zeta under the condition of different pH (ξ) current potential, and as shown in Figure 7, as can be seen from the figure Nano silver grain colloidal iso-electric point is pH=9.2.
Claims (9)
1, a kind of preparation method of Nano silver grain, this method comprises the steps:
1) acid solution of chitosan is mixed with silver nitrate solution mixed solution, wherein, the deacetylation of chitosan 〉=70%, molecular-weight average≤20,000, in this mixed solution, the concentration of chitosan is 0.001～0.05wt%, and the concentration of Silver Nitrate is 0.01～23.5mM;
2) regulate pH to 3.0～5.0;
3) under oxygen free condition, carry out irradiation.
2, preparation method according to claim 1 is characterized in that: in the step 1), the acid solution of chitosan is meant the acetic acid and/or the hydrochloric acid soln of chitosan.
3, preparation method according to claim 1 and 2 is characterized in that: in the step 1), and the molecular-weight average of chitosan≤15,000; The concentration of Silver Nitrate is 0.03～20mM in this mixed solution.
4, preparation method according to claim 1 and 2 is characterized in that: step 2) in, pH to 3.0 regulated.
5, preparation method according to claim 1 and 2 is characterized in that: in the step 3), described is under oxygen free condition under the condition that feeds the nitrogen deoxygenation.
6, preparation method according to claim 1 and 2 is characterized in that: in the step 3), described irradiation is meant that irradiation dose is that the gamma ray projector of 3～15kGy or ultraviolet source that λ is 190～250nm carry out irradiation.
7, preparation method according to claim 6 is characterized in that: described gamma ray projector is meant
60The Co source; The irradiation time of this ultraviolet source is 20～40min/1mL reaction solution.
8, the Nano silver grain that makes of the described preparation method of a kind of claim 1.
9, Nano silver grain as claimed in claim 8 is characterized in that: the median size of this Nano silver grain is 5～20nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100255449A CN100503744C (en) | 2006-04-07 | 2006-04-07 | Method for preparing nano silver grain, and prepared nano silver grain |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100255449A CN100503744C (en) | 2006-04-07 | 2006-04-07 | Method for preparing nano silver grain, and prepared nano silver grain |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101050315A CN101050315A (en) | 2007-10-10 |
| CN100503744C true CN100503744C (en) | 2009-06-24 |
Family
ID=38781925
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100255449A Expired - Fee Related CN100503744C (en) | 2006-04-07 | 2006-04-07 | Method for preparing nano silver grain, and prepared nano silver grain |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100503744C (en) |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101947654A (en) * | 2010-09-16 | 2011-01-19 | 南京大学 | Method for producing water-soluble fluorescent silver nanoclusters |
| CN102228995B (en) * | 2011-06-30 | 2013-02-13 | 华南理工大学 | Polysaccharide-nano silver sol and preparation method thereof |
| CN102935520B (en) * | 2012-12-05 | 2015-10-28 | 苏州大学 | A kind of modified glucose prepares the method for nano-silver water solution |
| CN103752849B (en) * | 2014-02-13 | 2016-02-24 | 华东理工大学 | Prepare the method for stabilized nanoscale silver |
| CN104815990B (en) * | 2015-04-20 | 2017-05-03 | 西安理工大学 | Method for preparing nanometer sliver colloid with liquid phase reduction method |
| CN105478792B (en) * | 2015-12-05 | 2017-08-04 | 浙江大学 | A kind of environment-friendly preparation method thereof of modification of chitosan nano silver colloidal sol |
| CN105798321A (en) * | 2016-01-29 | 2016-07-27 | 宁波工程学院 | Half-metallic bismuth nanoribbon, half-metallic bismuth nanospheres and preparation method of half-metallic bismuth nanoribbon and half-metallic bismuth nanospheres |
| CN106216709A (en) * | 2016-08-26 | 2016-12-14 | 太原理工大学 | A kind of method preparing O carboxymethyl chitosan parcel nanometer silver |
| CN106417275A (en) * | 2016-08-29 | 2017-02-22 | 太原理工大学 | Method for preparing chitosan encapsulated nano-silver graphene oxide composite antibacterial material |
| CN106942274B (en) * | 2017-03-30 | 2018-03-20 | 安徽省银锂子生物科技发展有限公司 | A kind of high-effective broad-spectrum fungicide of low content Nano silver solution |
| CN108166100A (en) * | 2018-01-22 | 2018-06-15 | 尹淑珍 | Antibacterial thermal insulating clothes |
| CN108339977A (en) * | 2018-02-12 | 2018-07-31 | 太原理工大学 | A kind of preparation method and application of chitosan oligosaccharide nano silver composite antibacterial agent |
| CN112494515B (en) * | 2020-12-28 | 2022-04-15 | 武汉大学 | Silver nano hydrogel for regulating flora-activated immune response and preparation method and application thereof |
| CN112980016B (en) * | 2021-02-08 | 2022-05-24 | 宁波工程学院 | Preparation method of water-soluble chitosan noble metal nano composite material |
| CN113021558B (en) * | 2021-03-17 | 2023-05-02 | 浙江省林业科学研究院 | Preparation method of wear-resistant antibacterial bamboo straw |
| CN116037070A (en) * | 2022-12-19 | 2023-05-02 | 湖北杰明凯林科技有限公司 | Formaldehyde purification material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190042A (en) * | 1997-02-03 | 1998-08-12 | 中国科学技术大学 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
| US20040058013A1 (en) * | 2000-08-22 | 2004-03-25 | Alan Taylor | Preparation of articles having a contact biocidal property |
| CN1509206A (en) * | 2001-04-30 | 2004-06-30 | ѧУ��������Ī˹�ƴ�ѧУ | Colloid solution of metal nanoparticles, metal-polymer nanocompositions and method for preparation thereof |
| CN1557588A (en) * | 2004-01-13 | 2004-12-29 | 上海大学 | Method for manufacturing nano-silver |
-
2006
- 2006-04-07 CN CNB2006100255449A patent/CN100503744C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1190042A (en) * | 1997-02-03 | 1998-08-12 | 中国科学技术大学 | Ultraviolet irradiation process preparing metal and metal oxide superfine powder and metal film |
| US20040058013A1 (en) * | 2000-08-22 | 2004-03-25 | Alan Taylor | Preparation of articles having a contact biocidal property |
| CN1509206A (en) * | 2001-04-30 | 2004-06-30 | ѧУ��������Ī˹�ƴ�ѧУ | Colloid solution of metal nanoparticles, metal-polymer nanocompositions and method for preparation thereof |
| CN1557588A (en) * | 2004-01-13 | 2004-12-29 | 上海大学 | Method for manufacturing nano-silver |
Non-Patent Citations (2)
| Title |
|---|
| 利用还原性多糖合成银纳米粒子. 曹洁明等.化学学报，第63卷第16期. 2005 * |
| 在线性壳聚糖膜内原位还原制备银纳米粒子及银单晶体. 姚素薇等.物理化学学报，第19卷第5期. 2003 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101050315A (en) | 2007-10-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100503744C (en) | Method for preparing nano silver grain, and prepared nano silver grain | |
| Ahmed et al. | Hydroxyethyl cellulose for spontaneous synthesis of antipathogenic nanostructures:(Ag & Au) nanoparticles versus Ag-Au nano-alloy | |
| Qasim et al. | Green synthesis of iron oxide nanorods using Withania coagulans extract improved photocatalytic degradation and antimicrobial activity | |
| Sharma et al. | Silver nanoparticles: green synthesis and their antimicrobial activities | |
| Iravani et al. | Synthesis of silver nanoparticles: chemical, physical and biological methods | |
| Gangadoo et al. | The synthesis and characterisation of highly stable and reproducible selenium nanoparticles | |
| Valodkar et al. | Morphology and antibacterial activity of carbohydrate-stabilized silver nanoparticles | |
| Powar et al. | Cu nanoparticle: Synthesis, characterization and application | |
| CN102198511A (en) | Preparation method of carboxymethyl curdlan polysaccharide-based colloidal aqueous solution containing nano silver particles | |
| CN102228995B (en) | Polysaccharide-nano silver sol and preparation method thereof | |
| Putri et al. | Tuning the photocatalytic activity of nanocomposite ZnO nanorods by shape-controlling the bimetallic AuAg nanoparticles | |
| Sahni et al. | Controlled green synthesis of silver nanoparticles by Allium cepa and Musa acuminata with strong antimicrobial activity | |
| Ayati et al. | Rate redox-controlled green photosynthesis of gold nanoparticles using H 3+ x PMo 12− x V x O 40 | |
| Labanni et al. | The effect of monoethanolamine as stabilizing agent in Uncaria gambir Roxb. mediated synthesis of silver nanoparticles and its antibacterial activity | |
| Kumar et al. | Kinetic and mechanistic studies of the formation of silver nanoparticles by nicotinamide as a reducing agent | |
| Pathania et al. | Studies on anticancerious and photocatalytic activity of carboxymethyl cellulose-cl-poly (lactic acid-co-itaconic acid)/ZnO-Ag nanocomposite | |
| Sagadevan et al. | Exploration of the antibacterial capacity and ethanol sensing ability of Cu-TiO2 nanoparticles | |
| Długosz et al. | Continuous synthesis of metal and metal oxide nanoparticles in microwave reactor | |
| Kuntyi et al. | Sonoelectrochemical synthesis of silver nanoparticles in sodium polyacrylate solution | |
| Vázquez et al. | Electrochemical study, structural characterization and antimicrobial activity of Silver and Copper Oxide (CuO) nanoparticles synthesized by a Green Method Using L-ascorbic Acid and Chitosan | |
| Khachatryan et al. | Formation of nanometal particles in the dialdehyde starch matrix | |
| EP2230321A1 (en) | Process for the preparation of supported metal nanoparticles | |
| Jeevanantham et al. | Green formulation of palladium nanoparticles on photocatalytic behavior of fabric dyes removal and its antibacterial assay | |
| Lyalina et al. | Obtaining of metal nanoparticles using reducing agents and chitosan | |
| KR20020082633A (en) | Preparation and application of ultra fine titania photocalysts doped by transition, lanthanides, and precious metals ion (Au, In, Sn, W, Zn, V, Ce, Eu, Ag) to utilize a solar spectrum (or spectrum of visible range) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090624 Termination date: 20140407 |