CN101487132B - Flexible visible light frequency band silver dendritic structure composite material and preparation thereof - Google Patents
Flexible visible light frequency band silver dendritic structure composite material and preparation thereof Download PDFInfo
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- CN101487132B CN101487132B CN2008100173221A CN200810017322A CN101487132B CN 101487132 B CN101487132 B CN 101487132B CN 2008100173221 A CN2008100173221 A CN 2008100173221A CN 200810017322 A CN200810017322 A CN 200810017322A CN 101487132 B CN101487132 B CN 101487132B
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Abstract
The invention relates to a flexible composite material with a silver branch-shaped structure at the visible light frequency band and a preparation method thereof, in particular to a two-dimensional nano-silver branch which is prepared on ITO flexible transparent conductive film substrate and a sandwich composite material of silver branch, SiO2 film and silver branch formed by chemically electrodepositing a SiO2 film with the thickness of 100nm on the surface of the silver branch and laminating and assembling another layer of two-dimensional silver branch. The sandwich composite material is provided with a plurality of adsorption peaks within the visible light frequency bands of 360-800nm and the transmission curve is in a zigzag shape.
Description
Technical field
The present invention relates to visible light frequency band silver dendritic structure composite material of a kind of flexibility and preparation method thereof, be particularly related to a kind of nanometer silver branch of the lack of alignment for preparing by chemical electro-deposition in the flexible and transparent substrate and " sandwich " multilayered structure that silica membrane is formed, the matrix material of this flexibility has special light transmission behavior at visible light wave range.
Background technology
Since the nanotechnology proposition, metal nano material is an important component part in current research in nanotechnology field always, the metal nano material of different structure size is because its significant physical and chemical performance and at optics, electricity, and aspect potential application such as magnetics etc. are subject to people's attention.Wherein, the preparation of argent dendritic structure more causes people's extensive concern with research.The chemical process of the nanometer tree branches structure of preparation silver mainly contains electrochemical process, sonochemical method, micro emulsion method, photochemical method, substitution method and template etc. at present.Compare with the preparation method of above-mentioned nanometer tree branches structure, the chemical electro-deposition method have restriction that grain-size little (in the 10-100nm), density height, nano crystal material be subjected to size and dimension less, do not have the numerous and diverse subsequent process of sol-gel, can directly obtain a series of advantages such as large batch of nano crystal material.Up to now, most silver nanostructured all be to be grown in the solution or on the rigid basement, not easily separated purification or the crooked optics that is assembled into specified shape.The present invention adopts the chemical electro-deposition method to prepare nanometer silver dendritic structure about 100nm on the conductive film of flexible and transparent, and tested its transmission behavior at visible light wave range, find that it has a plurality of absorption peaks at 360-800nm wavelength place, to the preparation of flexible optical device and performance study with significant.
Summary of the invention
The matrix material that the purpose of this invention is to provide a kind of nanometer silver branch of the lack of alignment that in the flexible and transparent substrate, prepares by the chemical electro-deposition method.This material is combined according to " silver tree branch-silica membrane-silver tree branch " three layers of mode by nanometer silver branch and silica membrane, and it has special light transmission behavior in the 360-800nm frequency range.
Description of drawings
The surface topography sem photograph of the nanometer silver branch sample of Fig. 1 preparation;
(a) (b) deposition voltage is 0.9V, and (c) (d) deposition voltage is 1.1V.
The different depositing time silica membrane of Fig. 2 cross section and surperficial sem photograph (a) 10s cross section; (b) 6s surface.
Fig. 3 " silver tree branch-silica membrane-silver tree branch " three-decker assembling process.
Fig. 4 conductive film, the visible light wave range transmission curve (a) of silver tree branch structure and silica membrane is attached with the ito thin film of silica membrane; (b) blank ito thin film; (c) be attached with the ito thin film of nanometer silver branch; (d) be attached with the ito thin film of nanometer silver branch, silica membrane.
" sandwich " structure, visible light wave band transmission curve of Fig. 5 " silver tree branch-silica membrane-silver tree branch ", (a) the deposition voltage 1.1V of silver tree branch, interelectrode distance 0.6mm; (b) the deposition voltage 0.9V of silver tree branch, interelectrode distance 0.6mm; (c) the deposition voltage 0.9V of silver tree branch, interelectrode distance 0.35mm.
Embodiment
1.ITO the preparation of nanometer silver branch on the film: 1.2g PEG-20000 is joined (concentration is 12mM) in the 5ml ultrapure water, the dissolving back adds 3ml silver nitrate solution (concentration is 0.59mM), 4 ℃ of following ageings obtained brown heavy-gravity electrolytic solution more than 24 hours, and its cryopreservation is stand-by.Adopt the two electrodes system, the metal silver strip is an anode, 10 * 40mm
2The ITO conductive film be negative electrode, the two-plate spacing is 0.3-0.6mm.With suction pipe electrolytic solution is added drop-wise to the pole plate edge, by capillary action, electrolytic solution can be sucked between the two-plate automatically, the control deposition voltage is 0.9V-1.3V, and depositing time is 3-5min, after electrodeposition process finishes, sample surfaces is washed with a large amount of ultrapure waters, dry up, make the nanometer silver branch.
2. " silver tree branch-silica membrane " double-deck preparation: the 0.17g SODIUMNITRATE is dissolved in (concentration is 0.1M) in the 20ml ultrapure water, and dripping hydrochloric acid is to pH=3 under stirring.After this, add the 1.585g cetyl trimethylammonium bromide, treat that it fully dissolves the ethanolic soln (concentration is 0.68M) that the back adds the 20ml tetraethoxy, get electrolytic solution behind the stirring 3h.Adopt the two electrodes system, graphite flake is an anode, and the ITO conductive film that deposits the silver tree branch is a negative electrode, and polar plate spacing is 0.5mm, and deposition voltage is 2.0V, and depositing time is 3-10s.After electrodeposition process finishes, sample surfaces is washed with a large amount of ultrapure waters rapidly.Can obtain the silicon dioxide layer that light transmission is good and smooth surface is smooth on the surface of silver tree branch, just " silver tree branch-silica membrane " bilayer structure.
3. the preparation of " silver tree branch-silica membrane-silver tree branch " three-decker: the assembling process of " sandwich " matrix material as shown in Figure 3, behind the certain thickness silica membrane of galvanic deposit on the surface of two-dimensional nano silver tree branch with other superimposed silver tree branch, silica membrane and silver tree branch " sandwich " matrix material of being assembled into of one deck two-dimensional nano silver tree branch.
4. the visible light transmissive property testing of three-decker: adopt UV-9300 type ultraviolet-visible pectrophotometer, the vertical visible light transmissivity characteristic during by this " sandwich " structure of test light wave.Test result shows that it has a plurality of absorption peaks to occur between 360nm～800nm, the test curve indentation shows the transmission performance that it is special.
The performance of implementation procedure of the present invention and material is by embodiment and description of drawings:
Embodiment one: in the process of preparation nanometer silver branch, the control deposition voltage is 0.9v, polar plate spacing is 0.6mm, depositing time 5min, after electrodeposition process finishes, sample surfaces is washed with a large amount of ultrapure waters, dry up, make as about modular construction 100 nanometers of accompanying drawing 1 (a) shown in (b), unordered nanometer silver branch of arranging.In " silver tree branch-silica membrane " double-deck preparation process, graphite flake is an anode, and the ITO conductive film that deposits the silver tree branch is a negative electrode, and polar plate spacing is 0.5mm, and deposition voltage is 2.0V, and depositing time is 6s.After electrodeposition process finishes, sample surfaces rapidly with a large amount of ultrapure water flushings, is dried up, make the thickness 100 nanometer left and right sides smooth surfaces shown in Fig. 2 (aII), Fig. 2 (b), the silica membrane of compact structure.Nanometer silver branch and " silver tree branch-silica membrane " bilayer structure of preparation is superimposed in opposite directions and fixes, can obtain " silver tree branch-silica membrane-silver tree branch " three-decker with ordinary plate glass.In the process of test three-decker, use UV-9300 type ultraviolet-visible pectrophotometer, transmitance when propagating in air with light wave is 100%, is 0% when seeing through with light zero, can be in a plurality of transmission peaks that obtain in 360nm～800nm scope shown in accompanying drawing 5 (b).
Embodiment two: in the process of preparation nanometer silver branch, the control deposition voltage is 1.1v, and polar plate spacing is 0.6mm, depositing time is 5min, and electrodeposition process washes sample surfaces after finishing with a large amount of ultrapure waters, dry up, make as the nanometer silver branch of accompanying drawing 1 (c) shown in (d).Assembling of " silver tree branch-silica membrane " double-deck preparation process, " silver tree branch-silica membrane-silver tree branch " three-decker and the test of visible light wave range optical transmission are with embodiment one.Can obtain the transmission curve shown in accompanying drawing 5 (a).
Embodiment three: in the process of preparation nanometer silver branch, the control deposition voltage is 0.9v, and polar plate spacing is 0.35mm, and depositing time is 2min, and electrodeposition process washes sample surfaces after finishing with a large amount of ultrapure waters, dry up, and makes the nanometer silver branch.Assembling of " silver tree branch-silica membrane " double-deck preparation process, " silver tree branch-silica membrane-silver tree branch " three-decker and the test of visible light wave range optical transmission are with embodiment one.Can obtain a plurality of transmission peaks shown in accompanying drawing 5 (c).
Claims (1)
1. the visible light frequency band silver dendritic structure composite material of a flexibility, sandwich matrix material by tin indium oxide (ITO) flexible transparent conductive film, silver tree branch and silica membrane is formed, its principal character is to adopt the chemical electro-deposition method to prepare nanometer silver branch and silica membrane, wherein, (1) the chemical electro-deposition preparation process of nanometer silver branch is, adopt the two electrodes system, the metal silver strip is an anode, 10 * 40mm
2The ITO conductive film be negative electrode, the two-plate spacing is 0.3-0.6mm, concentration is that 0.59mM Silver Nitrate, PEG-20000 mixing solutions are electrolytic solution, and deposition voltage is 0.9-1.3V condition deposit 3-5min, obtains the nano silver tree dendritic structures of lack of alignment on the flexible transparent conductive film surface; (2) " silver tree branch-silica membrane " double-deck preparation process is, the 0.17g SODIUMNITRATE is dissolved in the 20ml ultrapure water, sodium nitrate concentration is 0.1M, dripping hydrochloric acid is to pH=3 under stirring, after this, add 1.585g hexadecyl trimethyl ammonium bromide (CTAB), treat that it fully dissolves the ethanolic soln that the back adds 20ml tetraethoxy (TEOS), the ethanolic soln concentration of tetraethoxy is 0.68M, makes electrolytic solution behind the stirring 3h, adopts the two electrodes system, graphite flake is an anode, the above-mentioned ITO conductive film that deposits the silver tree branch is a negative electrode, and polar plate spacing is 0.5mm, and deposition voltage is 2.0V, depositing time is 6s, after electrodeposition process finishes, sample surfaces rapidly with a large amount of ultrapure water flushings, is obtained " silver tree branch-silica membrane " bilayer structure; (3) preparation process of " silver tree branch-silica membrane-silver tree branch " three-decker is, with the face-to-face stack combinations of ITO conductive film of above-mentioned " silver tree branch-silica membrane " bilayer structure and above-mentioned depositing silver branch, fixing, obtain flexible " silver tree branch-silica membrane-silver tree branch " three-decker, this flexible materials has absorption in 360nm～800nm frequency range to the light of multiple frequency, the transmission curve indentation.
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| CN103103608A (en) * | 2011-11-09 | 2013-05-15 | 中国科学院合肥物质科学研究院 | Film formed by silver nanosheets and preparation method and application of film |
| CN103088382B (en) * | 2013-03-01 | 2016-02-17 | 浙江大学 | A kind of preparation method of light-operated local plating silica membrane |
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| CN101003907A (en) * | 2006-12-14 | 2007-07-25 | 南京大学 | Method for preparing metal and dielectric composite grains of silicon dioxide coated by Nano silver |
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| CN101003907A (en) * | 2006-12-14 | 2007-07-25 | 南京大学 | Method for preparing metal and dielectric composite grains of silicon dioxide coated by Nano silver |
Non-Patent Citations (3)
| Title |
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| Xudong Zhang等.Synthesis of monodisperse and spherical YAG nanopowderby a mixed solvothermal method.Journal of Alloys and Compounds372.2004,372300-303. * |
| 邵丽等.超声化学法制备树枝状纳米银的研究.无机化学学报23 10.2007,23(10),1824-1828. |
| 邵丽等.超声化学法制备树枝状纳米银的研究.无机化学学报23 10.2007,23(10),1824-1828. * |
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