CN101468876B - Visible light frequency band silver dendritic structure composite material and preparation thereof - Google Patents
Visible light frequency band silver dendritic structure composite material and preparation thereof Download PDFInfo
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- CN101468876B CN101468876B CN2007103081640A CN200710308164A CN101468876B CN 101468876 B CN101468876 B CN 101468876B CN 2007103081640 A CN2007103081640 A CN 2007103081640A CN 200710308164 A CN200710308164 A CN 200710308164A CN 101468876 B CN101468876 B CN 101468876B
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Abstract
The invention relates to visible light frequency range nanometer composite material, in particular to the three-layer composite material formed by nanometer silver dendritic structures and an insulated thin layer. Through a chemical electrodeposition method, a randomly arranged nanometer silver dendritic structure is prepared on the surface of the ITO conductive glass; and then the insulated thin layer is deposited on the surface of the dendritic structure layer which is combined with the other silver dendritic structure having no insulated thin layer on the surface in the three-layer mode of dendritic silver-insulated thin layer-dendritic silver, so the composite material is obtained. The material can absorb light of various frequencies in the frequency range from 360nm to 800nm. The light transmission curve is indented.
Description
Technical field the present invention relates to a kind of visible light frequency band nano composite material, be particularly related to a kind of nano silver tree dendritic structures of lack of alignment and three-decker material of heat insulating lamina composition and preparation method thereof, this material has the light transmission behavior that is different from traditional material in a plurality of frequency ranges of visible light.
The background technology nano metal material more and more is subject to people's attention owing to have unique character at aspects such as electricity, magnetics, optics, catalysis, and it is widely used at aspects such as high-density magnetic memory device, feds, electroanalysis trace detection.Recently, the dendritic structure of nanotrees also shows its characteristics at the preparation and the aspect of performance of super material (metamaterial).The super material of synthetic generally is to adopt physical method to etch regular metal Nano structure array in substrate, in order to realize the special property of material, but it is because the restriction of etching technics, be difficult to obtain tens nanometers even the metal construction array of small scale more, and with high costs.And by the chemical process people can be fairly simple the metal construction of acquisition nanoscale.With the unordered rarely seen so far report of the nanometer metal structure super material of preparation.Because the singularity of chemical process, this dendritic structure that we obtain is arranged in the ito glass substrate with state of disarray, and the matrix material of being made up of the nanometer metal structure of this lack of alignment has special light transmission behavior at visible light frequency band.It has a plurality of absorption peaks in 360nm～800nm wavelength region, with the light transmission behavior of traditional material very big-difference is arranged, and is significant in chemical process artificial preparation field of novel.
Summary of the invention the purpose of this invention is to provide a kind of nano composite material that realizes by the chemical electro-deposition method.This material is combined according to " dendroid silver-heat insulating lamina-dendroid silver " three layers of mode by the nano silver tree dendritic structures and the siliceous heat insulating lamina of lack of alignment, and it has special optical property in 360～800nm frequency range.
Description of drawings
Fig. 1 prepares silver dendritic structure and heat insulating lamina electrode device synoptic diagram.
The preparation process synoptic diagram of Fig. 2 institute invention three-decker matrix material.
Figure 30 .9V voltage conditions is the stereoscan photograph of preparation silver dendritic structure down.
(a) low multiple stereoscan photograph; (b) higher multiple stereoscan photograph.
Fig. 4 .0.9V voltage conditions is the stereoscan photograph of preparation silver dendritic structure down.
(a) low multiple stereoscan photograph; (b) higher multiple stereoscan photograph.
The transmittance curve of Fig. 5 institute invention three-layer composite structure material sample 1.
(a) blank ito glass; (b) adhere to the ito glass of insulating film; (c) adhere to the ito glass of the dendritic silver of one deck nanotrees;
(d) dendroid silver, insulation film bilayer structure; (e) dendroid silver, insulation film, dendroid silver " sandwich " structure;
The transmittance curve of Fig. 6 institute invention three-layer composite structure material sample 2.
(a) blank ito glass; (b) adhere to the ito glass of insulating film; (c) adhere to the ito glass of the dendritic silver of one deck nanotrees;
(d) dendroid silver, insulation film bilayer structure; (e) dendroid silver, insulation film, dendroid silver " sandwich " structure;
Embodiment
1. electrolytic solution preparation 1.: 1.2g polyoxyethylene glycol-20000 is added in the 5mL ultrapure water, fully dissolving, in mixed solution, add 3mL silver nitrate solution (massfraction 16.7%), stirring and dissolving, solution becomes viscous liquid, mixed solution is packed, under low temperature, lucifuge condition ageing stand-by more than 24 hours, obtain electrolytic solution 1.;
2. the preparation of dendroid silver: the transparent conducting glass (ito glass) that will be coated with tin indium oxide cleans up and dries, as negative electrode; Get smooth smooth silver strip and clean up and dry, as anode; Conductive glass, silver electrode are formed device as shown in Figure 1, interelectrode distance thickness is that the sheet of moulding of 0.6mm is controlled, and adds electrolytic solution 1., and the control deposition voltage is between 0.7V～0.9V, controlling conduction time is 2～3 minutes, obtains the dendritic silver of nanotrees on the ito glass surface;
3. electrolytic solution preparation 2.: the 0.17g SODIUMNITRATE is dissolved in the 20ml ultrapure water, dripping hydrochloric acid is to pH=3 under stirring, add 1.585g cetyl trimethyl bromination again by (CTAB), fully the dissolving back adds the ethanolic soln (concentration is 0.68M) of 20ml tetraethoxy (TEOS), stir 3h, obtain electrolytic solution 2.;
4. " dendroid silver-insulation layer " double-deck preparation: with the ito glass of depositing silver dendritic structure as negative electrode, choose bright and clean smooth carbon flat board as anode, form device as shown in Figure 1, with electrolytic solution 2. between the two poles of the earth of adding apparatus, the control electrode spacing is 0.6mm, control voltage is 2.5V, controlling conduction time is 6 seconds, can obtain the good and smooth smooth insulation layer of light transmission on the surface of dendroid silver, the about 100nm of thickness of thin layer obtains " dendroid silver, heat insulating lamina " bilayer structure.
5. the preparation of " dendroid silver-insulation layer-dendroid silver " three-decker: the dendroid silver sample of bilayer structure sample and depositing insulating layer is not combined and fixing so that two conducting surfaces are relative, between two-layer ITO conductive glass, just realized dendroid silver, insulation layer, dendroid silver three-decker like this.Adopt UV-9100 type ultraviolet-visible pectrophotometer, test is when the visible light transmissivity characteristic of light wave during vertically by this " sandwich " structure.The difference of itself and traditional material light transmission behavior as can be seen.
The performance of implementation procedure of the present invention and material is by embodiment and description of drawings:
Embodiment one: the ito glass that will handle, silver plate electrode are assembled into reaction unit, as shown in Figure 1.Adding electrolytic solution 1. between two electrodes, is 0.9V condition deposit 2 minutes at deposition voltage, can obtain the silver dendritic structure of lack of alignment on the ito glass surface, and its pattern as shown in Figure 3.With the ito glass of above-mentioned depositing silver dendritic structure as negative electrode, the carbon plate electrode is as anode, be assembled into device as shown in Figure 1, add electrolytic solution 2., at deposition voltage is 2.5V condition deposit heat insulating lamina, obtain " dendroid silver-heat insulating lamina " bilayer structure, heat insulating lamina thickness is approximately 100nm.Descend the ito glass of the dendritic structure of depositing silver of preparation to combine itself and the described the same terms in front, and paste and fix, can obtain " dendroid silver-heat insulating lamina-dendroid silver " three-decker, preparation process as shown in Figure 2.Use UV-9100 type ultraviolet-visible pectrophotometer that this matrix material is carried out the visible light transmissivity test, when light wave vertically passes through this matrix material, it sees through characteristic shown in accompanying drawing 5 (e), in 360nm～800nm scope, there are a plurality of transmission peaks light-wave transmission curve indentation to occur.Accompanying drawing 5 (a)～(d) is for forming the transmitance situation of three-decker each several part.
Embodiment two: the ito glass that will handle, silver plate electrode are assembled into reaction unit, as shown in Figure 1.Between two electrodes, add electrolytic solution 1., at deposition voltage is 0.7V condition deposit 3 minutes, can obtain the silver dendritic structure of lack of alignment on the ito glass surface, its pattern can see that silver dendritic structure is thick than the structure for preparing under the embodiment one described condition as shown in Figure 4; With the ito glass of above-mentioned depositing silver dendritic structure as negative electrode, the carbon plate electrode is as anode, be assembled into device as shown in Figure 1, add electrolytic solution 2., at deposition voltage is 2.5V condition deposit heat insulating lamina, obtain " dendroid silver-heat insulating lamina " bilayer structure, heat insulating lamina thickness is approximately 100nm.Descend the ito glass of the dendritic structure of depositing silver of preparation to combine itself and the described the same terms in front, and paste and fix, can obtain " dendroid silver-heat insulating lamina-dendroid silver " three-decker, preparation process as shown in Figure 2.Use UV-9100 type ultraviolet-visible pectrophotometer that this matrix material is carried out the visible light transmissivity test, when light wave vertically passes through this matrix material, it sees through characteristic shown in accompanying drawing 6 (e), does not find that in 360nm～800nm scope the transmission peaks as matrix material as described in the embodiment one occurs.Accompanying drawing 6 (a)～(d) is for forming the transmitance situation of three-decker each several part.
Claims (2)
1. visible light frequency band silver dendritic structure composite material, its principal character is that to adopt the chemical electro-deposition method be that the preparation process of substrate preparation " dendroid silver-heat insulating lamina-dendroid silver " 3-layer composite material is with the ITO conductive glass, with the 1.2g molecular weight is that 20000 polyoxyethylene glycol adds fully dissolving in the 5mL ultrapure water, adding the 3mL massfraction in mixed solution is 16.% silver nitrate solution stirring and dissolving, solution becomes viscous liquid, mixed solution is packed, ageing obtained electrolytic solution more than 24 hours under 4 ℃ of lucifuge conditions, again with the ITO conductive glass as negative electrode, with smooth smooth dull and stereotyped silver electrode as anode, in interelectrode distance is 0.6mm, deposition voltage is 0.9V condition deposit 2min, obtain the nano silver tree dendritic structures of lack of alignment on the ito glass surface, behind two silver dendritic structure samples of same deposition condition preparation, the 0.17g SODIUMNITRATE is dissolved in the 20ml ultrapure water, dripping hydrochloric acid is to pH=3 under stirring, add the 1.585g cetyl trimethylammonium bromide again, fully the dissolving back adds the ethanolic soln stirring 3h of 20ml tetraethoxy as electrolytic solution, with the ito glass of a slice depositing silver dendritic structure as negative electrode, smooth smooth carbon dioxide process carbon electrode is as anode, in interelectrode distance is 0.6mm, deposition voltage is 2.5V condition deposit 6s, obtain the insulation layer of thickness 100nm, with the combination of the ito glass of another sheet depositing silver dendritic structure and be fixed together, obtain " dendroid silver-heat insulating lamina-dendroid silver " three-decker then.
2. a kind of according to claim 1 visible light frequency band silver dendritic structure composite material is characterized in that this material has special absorption behavior to visible light, and it has absorption in 360nm～800nm frequency range to the light of multiple frequency, the transmission curve indentation.
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| CN2007103081640A CN101468876B (en) | 2007-12-28 | 2007-12-28 | Visible light frequency band silver dendritic structure composite material and preparation thereof |
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| CN2007103081640A CN101468876B (en) | 2007-12-28 | 2007-12-28 | Visible light frequency band silver dendritic structure composite material and preparation thereof |
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| CN101468876B true CN101468876B (en) | 2011-12-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102212847B (en) * | 2011-05-04 | 2012-10-31 | 湖南科技大学 | Method for preparing nanometer silver granules |
| CN104819975A (en) * | 2015-05-21 | 2015-08-05 | 中北大学 | Filter-paper-based silver-dendrite surface-enhanced Raman scattering active substrate and production method thereof |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6331119B1 (en) * | 1999-12-28 | 2001-12-18 | International Business Machines Corporation | Conductive adhesive having a palladium matrix interface between two metal surfaces |
| CN1569713A (en) * | 2004-05-08 | 2005-01-26 | 上海耀华皮尔金顿玻璃股份有限公司 | Double silver low-emissivity coated glass based on composite dielectric layer |
| CN1892945A (en) * | 2005-07-01 | 2007-01-10 | 松下电器产业株式会社 | Movable contact assembly, method of manufacturing the same, and switch using the same |
| CN1925209A (en) * | 2005-09-02 | 2007-03-07 | 西北工业大学 | Minus magnetism conducting rate material constituted of branch shape structural unit |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6331119B1 (en) * | 1999-12-28 | 2001-12-18 | International Business Machines Corporation | Conductive adhesive having a palladium matrix interface between two metal surfaces |
| CN1569713A (en) * | 2004-05-08 | 2005-01-26 | 上海耀华皮尔金顿玻璃股份有限公司 | Double silver low-emissivity coated glass based on composite dielectric layer |
| CN1892945A (en) * | 2005-07-01 | 2007-01-10 | 松下电器产业株式会社 | Movable contact assembly, method of manufacturing the same, and switch using the same |
| CN1925209A (en) * | 2005-09-02 | 2007-03-07 | 西北工业大学 | Minus magnetism conducting rate material constituted of branch shape structural unit |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2006-28606A 2006.02.02 |
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