CN102212847A - Method for preparing nanometer silver granules - Google Patents
Method for preparing nanometer silver granules Download PDFInfo
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- CN102212847A CN102212847A CN2011101141450A CN201110114145A CN102212847A CN 102212847 A CN102212847 A CN 102212847A CN 2011101141450 A CN2011101141450 A CN 2011101141450A CN 201110114145 A CN201110114145 A CN 201110114145A CN 102212847 A CN102212847 A CN 102212847A
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Abstract
The invention discloses a method for preparing silver nanometer granules with dendritic structures, and belongs to the technical field of nanometer materials. In the method, the silver nanometer granules with the dendritic structures are deposited on the surface of a titanium sheet by utilizing silver-ammonia complex ion dilute solution without supporting electrolytes in a constant potential step method. The method comprises the following processes that: a silver-ammonia complex is formed by taking silver nitrate as a silver ion source and adding ammonia water to control the growth speed and growth direction of crystal nuclei so as to control the sizes and shapes of the granules; and factors such as potential, concentration, metal ion additives with different valence states and the like are changed to control the shapes of the silver nanometer granules. The method is simple in a process, non-pollution and high in safety, does not have public hazards, and is a new method for the novel nanometer granules with the special dendritic structures.
Description
Technical field
The present invention relates to electrochemical deposition method and prepare technical field of nano material, especially, provide a kind of preparation method of dendroid silver nano-grain.
Background technology
The nanometer silver material has very stable physics and chemical property, its application prospect is very extensive, can be used as the antiseptic-germicide in biology and the medical field and have application widely, as in Department of Burn, nanometer silver often can be used as immunomodulator and promotes wound healing and treatment immunogenicity tetter.In addition, nanometer silver can be used as low temperature thermally conductive material, electrocondution slurry in that application is also arranged aspect electronics, the optics.In chemical reaction, nanometer silver can be used as multiple catalyst for reaction, and (the nanometer silver electrode is compared with common silver electrode, its catalytic activity is tens times even hundreds of times of common silver electrode), as PARA FORMALDEHYDE PRILLS(91,95), acetaldehyde, hydrazine hydrate, hydrogen peroxide, glucose etc. good catalytic activity is arranged all, can be used as the sensitive electrochemical sensor and be applied to the detection of these materials.In other field, also be widely used,, can change some characteristic of chemical fabrics, and give very strong sterilizing ability as in chemical fibre, adding a spot of nanometer silver.
Summary of the invention
The objective of the invention is in the silver ammino ion solution of lower concentration, prepare silver nano-grain with dendritic structure by the control sedimentation potential.
A kind of preparation method of dendroid silver nano-grain is characterized in that, the method comprising the steps of:
(1) preparation silver ammino ion solution: take by weighing 0.13-0.26 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters, disappear until precipitation to wherein adding strong aqua again, formed solution is silver ammino ion solution, and then makes the concentration of the silver ammino ion of formation reach 0.015-0.03 mol/L by thin up; Process for preparation carries out in the darkroom, and the silver ammino ion solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.
(2) adopt the constant potential electro-deposition method that silver ammino ion is reduced to simple substance silver, form the dendroid silver nano-grain: with silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, sedimentation potential between-0.8 V--0.3 V, depositing time 300s.
Adding concentration in described silver ammino ion solution is the metal ion additive of 0.01mol/L.
Described metal ion additive is Ca (NO
3)
2Or KNO
3
Beneficial effect: change the concentration of sedimentary current potential, solution, the metal ion additive of different valence state, can obtain difform dendritic nano-silver particle;
Figure of description
Fig. 1 is that sedimentation potential is-0.7 V, the sem photograph when silver ammino ion concentration is 0.03mol/L;
Fig. 2 is that sedimentation potential is that-0.3 V, silver ammino ion concentration are the sem photograph of 0.03mol/L;
Fig. 3 is the sem photograph of sedimentation potential when being-0.5 V;
Fig. 4 is the Ca that adds 0.01 mol/L
2+The time sem photograph.
Fig. 5 is the K that adds 0.01mol/L
+The time sem photograph;
Fig. 6 is that sedimentation potential is-0.8 V, the sem photograph when silver ammino ion concentration is 0.015 mol/L;
Fig. 7 is that sedimentation potential is-0.8 V, the sem photograph when silver ammino ion concentration is 0.02mol/L;
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Embodiment
Embodiment 1
Take by weighing 0.26 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.03mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.With above-mentioned silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.7 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 1.
Embodiment 2
Take by weighing 0.2 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.03mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.With above-mentioned silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.3 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 2.
Embodiment 3
Take by weighing 0.13 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.015mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.With above-mentioned silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.8 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 3.
Embodiment 4
Take by weighing 0.26 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.03mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.Adding concentration in above-mentioned silver ammino ion solution is the Ca (NO of 0.01mol/L
3)
2, making its concentration is 10mmol/L, with this silver ammino ion+Ca
2+Mixed solution is an ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.7 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 4.
Embodiment 5
Take by weighing 0.26 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.03mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.Adding concentration in above-mentioned silver ammino ion solution is the KNO of 0.01mol/L
3, making its concentration is 10mmol/L, with this silver ammino ion+K
+Mixed solution is an ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.7 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 5.
Embodiment 6
Take by weighing 0.13 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.015mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.With this silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.8 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 6.
Embodiment 7
Take by weighing 0.26 g Silver Nitrate, it is dissolved in about 10 ml redistilled waters,, and then make the concentration of the silver ammino ion of formation reach 0.02mol/L by thin up again to wherein adding strong aqua till precipitation does not generate; Process for preparation carries out in the darkroom, and the solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container.With this silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, is down potentiostatic deposition 300 seconds of-0.8 V (with respect to silver electrode) at current potential, formed dendroid silver nano-grain is deposited on titanium plate surface, its sem photograph is seen Fig. 7.
Claims (3)
1. the preparation method of a dendroid silver nano-grain is characterized in that, the method comprising the steps of:
(1) preparation silver ammino ion solution: take by weighing the 0.13-0.26g Silver Nitrate, it is dissolved in about 10 ml redistilled waters, disappear until precipitation to wherein adding strong aqua again, formed solution is silver ammino ion solution, and then makes the concentration of the silver ammino ion of formation reach 0.015-0.03 mol/L by thin up; Process for preparation carries out in the darkroom, and the silver ammino ion solution for preparing is wrapped with the plastics bag of black, is placed in the light resistant container;
(2) adopt the constant potential electro-deposition method that silver ammino ion is reduced to simple substance silver, form the dendroid silver nano-grain: with silver ammino ion solution is ionogen, with geometric area 0.4cm
2The titanium sheet be working electrode, platinized platinum is a supporting electrode, silver electrode is a reference electrode, sedimentation potential between-0.8 V-0.3 V, depositing time 300s.
2. the preparation method of dendroid silver nano-grain according to claim 1 is characterized in that, adding concentration in silver ammino ion solution is the metal ion additive of 0.01mol/L.
3. the preparation method of dendroid silver nano-grain according to claim 2 is characterized in that, described metal ion additive is Ca (NO
3)
2Or KNO
3
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719858A (en) * | 2012-06-01 | 2012-10-10 | 西安交通大学 | Preparation method of dendritic nano silver |
| CN105908220A (en) * | 2016-05-06 | 2016-08-31 | 上海应用技术学院 | Method for manufacturing micro-nano-silver dendritic crystal through liquid-phase electrodeposition |
| CN106757173A (en) * | 2016-11-25 | 2017-05-31 | 电子科技大学 | A kind of preparation method of the micro-nano crystal of silver-colored polyhedron without surface ligand |
| CN110644017A (en) * | 2019-11-14 | 2020-01-03 | 常州工程职业技术学院 | Dendritic silver-iron oxide composite photoelectrode and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719858A (en) * | 2012-06-01 | 2012-10-10 | 西安交通大学 | Preparation method of dendritic nano silver |
| CN102719858B (en) * | 2012-06-01 | 2015-04-29 | 西安交通大学 | Preparation method of dendritic nano silver |
| CN105908220A (en) * | 2016-05-06 | 2016-08-31 | 上海应用技术学院 | Method for manufacturing micro-nano-silver dendritic crystal through liquid-phase electrodeposition |
| CN105908220B (en) * | 2016-05-06 | 2018-03-30 | 上海应用技术学院 | A kind of method that liquid electrodeposition prepares micro-nano silver dendrite |
| CN106757173A (en) * | 2016-11-25 | 2017-05-31 | 电子科技大学 | A kind of preparation method of the micro-nano crystal of silver-colored polyhedron without surface ligand |
| CN110644017A (en) * | 2019-11-14 | 2020-01-03 | 常州工程职业技术学院 | Dendritic silver-iron oxide composite photoelectrode and preparation method thereof |
| CN110644017B (en) * | 2019-11-14 | 2021-03-19 | 常州工程职业技术学院 | Dendritic silver-iron oxide composite photoelectrode and preparation method thereof |
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| CN102212847B (en) | 2012-10-31 |
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