CN1916235A - Method for preparing composite film of silver Nano granule / titanium dioxide - Google Patents
Method for preparing composite film of silver Nano granule / titanium dioxide Download PDFInfo
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- CN1916235A CN1916235A CN 200610053281 CN200610053281A CN1916235A CN 1916235 A CN1916235 A CN 1916235A CN 200610053281 CN200610053281 CN 200610053281 CN 200610053281 A CN200610053281 A CN 200610053281A CN 1916235 A CN1916235 A CN 1916235A
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- silver
- titanium dioxide
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Abstract
This invention discloses a method for preparing Ag/TiO2 composite film. The method coprises: (1) dissolving Ti compound in an organic solvent to obtain solution A; (2) mixing water, complexing agent, organic solvent and AgNO3 powder to obtain solution B; (3) dropping solution B into solution A, and strring to obtain a stable sol; (4) coating the sol onto a clean carrier by soaking and drawing, and treating at 450-600 deg.C to obtain Ag/TiO2 film. The method and equipment in this invention is simple. The content of Ag in the film is high, thus the obtained Ag/TiO2 film has good photocatalytic performance and high conductivity.
Description
Technical field
The present invention relates to a kind of method for preparing composite film of silver Nano granule/titanium dioxide.
Background technology
Metal-oxide semiconductor (MOS) titanium dioxide (TiO
2) be semiconductor material with wide forbidden band, energy gap is about 3.2～3.41eV, and is transparent in 0.35～12 mum wavelength interval, the specific refractory power height, and have characteristic of mechanical property height, stable chemical performance or the like.TiO at the UV-light wave band
2Has photocatalysis characteristic, at numerous photocatalyst (TiO
2, ZnO, Fe
2O
3, CdS etc.) in, TiO
2Nontoxic with it, catalytic activity is high, good stability, characteristics such as cheap and easy to get are subject to people's attention.Utilize it that organic pollutant in water is carried out photocatalytic degradation, finally generate nonpoisonous and tasteless CO
2, H
2O and some simple inorganicss.But TiO
2Can only absorb the light of ultraviolet band, make its photocatalysis efficiency under daily condition low.TiO
2Not only have photocatalysis characteristic, the super water-wet behavior of photoinduction, but also have unique electrical property.Pure TiO
2Be N-type semiconductor, when nonstoichiometry, exist the oxygen room (with TiO
2-xExpression).In recent years, TiO
2Use as electronic material, sensitive material more and more is subject to people's attention. especially aspect sensor material, as TiO
2Oxygen-sensing sensor, TiO
2Temp-sensitive sensor, TiO
2Widespread uses such as electrochemistry pH transmitter.But pure TiO
2The intrinsic resistance of material itself big (＞10
3Ω), be difficult to accurate measurement.Silver (Ag) mixes or the titanium dioxide of compound Ag is to improve TiO
2An effective way of material light catalysis property and electroconductibility.But because the Ag ion is easily at TiO
2Separate out in the colloidal sol and precipitate, cause the titanium dioxide research work of mixing silver or compound silver to rest on the lower state of silver content (the atomic percent At% of Ag＜2) always.So, if can prepare the titania powder of high silver content (At%＞2) or film mixes for research silver or the photocatalysis performance or the conductivity of the titanium dioxide of compound silver all have important meaning.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing the silver/titanium dioxide laminated film of high silver content.
The method of the silver/titanium dioxide laminated film of preparation high silver content of the present invention, step is as follows:
1) with the compound dissolution of titanium in organic solvent, the compound of titanium and the mol ratio of organic solvent are 1: 4～15, mixture is put into ice-water bath stirs, A liquid;
2) water, complexing agent, organic solvent and Silver Nitrate powder 1: 0.1 in molar ratio～1: 6～18: 0.2～1.5 are mixed and constantly stirring, all dissolve, get B liquid up to Silver Nitrate;
3) B liquid is dropwise splashed in the A liquid that always is placed on ice-water bath, continue then to stir, up to the colloidal sol that obtains colour stable, again that colloidal sol is stand-by in-10～20 ℃ of following ageings;
4) carrier impregnation after will cleaning lifts in above-mentioned colloidal sol, and pull rate is controlled at 1～10cm/min, has whenever lifted one deck, in 450～600 ℃ of following thermal treatment 5～60min, obtains Ag/TiO
2Film.
The compound of above-mentioned titanium can be butyl (tetra) titanate, titanium chloride or isopropyl titanate.Said organic solvent can be ethanol, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, ethylene glycol phenyl ether, Benzenediol methyl ether or propyl alcohol.Complexing agent can adopt diethanolamine, citric acid, hydroxylated cellulose (HPC) or polyoxyethylene glycol (PEG).Said carrier can be simple glass sheet, quartz glass plate or ceramic plate.
Be coated in the Ag/TiO on the carrier
2The thickness of film can be controlled by speed that lifts and number of times.
Beneficial effect of the present invention is:
The present invention adopts the sol-gel dip-coating method to prepare Ag/TiO
2Film, method and use equipment are simple; Prepared Ag/TiO
2In the film, the content height of Ag: the At% of Ag can reach 10.36.The high Ag/TiO of this Ag content
2Film has the TiO than low Ag content (At%＜2)
2Film and do not contain the TiO of Ag
2Better photocatalysis performance of film and electroconductibility.
Description of drawings
Fig. 1 is Ag/TiO
2The X ray diffracting spectrum of film;
Fig. 2 is Ag/TiO
2The photo of taking under the backscattered electron pattern of film.
Embodiment
Further specify the present invention below in conjunction with specific examples.
1) butyl (tetra) titanate and ethanol were mixed in the container in 1: 6 in molar ratio, and container are put into ice-water bath stir 30min, obtain A liquid,
2) with water, diethanolamine, ethanol and Silver Nitrate powder 1: 1: 12 in molar ratio: 0.6 mixes and constantly stirs, and all dissolves up to Silver Nitrate, obtains B liquid.
3) B liquid is dropwise splashed in the A liquid that always is placed on ice-water bath, continue then to stir, up to the colloidal sol that obtains colour stable, again that colloidal sol is stand-by in 4 ℃ of following ageings;
4) clean quartz glass plate is immersed in the above-mentioned colloidal sol lifts, pull rate is controlled at 2cm/min, has whenever lifted one deck, in 450 ℃ of following thermal treatment 30min, obtains Ag/TiO
2Film.
Prepared Ag/TiO
2The XRD figure of film is composed as shown in Figure 1, and film is made up of the titanium dioxide and the argent of anatase octahedrite phase.Ag/TiO
2The BSE photo of film as shown in Figure 2, the high zone of brightness is Ag, as seen from the figure, silver is dispersed in TiO
2In.Prepared Ag/TiO
2The content At% of Ag is 8.36 in the film.
1) titanium chloride and ethylene glycol monomethyl ether were mixed in the container in 1: 15 in molar ratio, and container are put into ice-water bath stir 30min, obtain A liquid,
2) with water, citric acid, ethylene glycol monomethyl ether and Silver Nitrate powder 1: 0.1: 18 in molar ratio: 1.5 mix and constantly stir, and all dissolve up to Silver Nitrate, obtain B liquid.
3) B liquid is dropwise splashed in the A liquid that always is placed on ice-water bath, continue then to stir, up to the colloidal sol that obtains colour stable, again that colloidal sol is stand-by in-4 ℃ of following ageings;
4) clean simple glass sheet is immersed in the above-mentioned colloidal sol lifts, pull rate is controlled at 8cm/min, has whenever lifted one deck, in 600 ℃ of following thermal treatment 10min, obtains Ag/TiO
2Film.
Prepared Ag/TiO
2The content At% of Ag is 10.36 in the film.
Embodiment 3
1) isopropyl titanate and propylene glycol monomethyl ether were mixed in the container in 1: 4 in molar ratio, and container are put into ice-water bath stir 30min, obtain A liquid,
2) with water, polyoxyethylene glycol, propylene glycol monomethyl ether and Silver Nitrate powder 1: 0.5: 6 in molar ratio: 0.2 mixes and constantly stirs, and all dissolves up to Silver Nitrate, obtains B liquid.
3) B liquid is dropwise splashed in the A liquid that always is placed on ice-water bath, continue then to stir, up to the colloidal sol that obtains colour stable, again that colloidal sol is stand-by in 20 ℃ of following ageings;
4) clean ceramic plate is immersed in the above-mentioned colloidal sol lifts, pull rate is controlled at 2cm/min, has whenever lifted one deck, in 500 ℃ of following thermal treatment 30min, obtains Ag/TiO
2Film.
Prepared Ag/TiO
2The content At% of Ag is 3.64 in the film.
Embodiment 4
1) isopropyl titanate and propyl alcohol were mixed in the container in 1: 4 in molar ratio, and container are put into ice-water bath stir 30min, obtain A liquid,
2) with water, polyoxyethylene glycol, propyl alcohol and Silver Nitrate powder 1: 0.5: 9 in molar ratio: 0.4 mixes and constantly stirs, and all dissolves up to Silver Nitrate, obtains B liquid.
3) B liquid is dropwise splashed in the A liquid that always is placed on ice-water bath, continue then to stir, up to the colloidal sol that obtains colour stable, again that colloidal sol is stand-by in 10 ℃ of following ageings;
4) clean ceramic plate is immersed in the above-mentioned colloidal sol lifts, pull rate is controlled at 6cm/min, has whenever lifted one deck, in 550 ℃ of following thermal treatment 20min, obtains Ag/TiO
2Film.
Prepared Ag/TiO
2The content At% of Ag is 7.64 in the film.
Claims (5)
1. method for preparing the silver/titanium dioxide laminated film is characterized in that may further comprise the steps:
1) with the compound dissolution of titanium in organic solvent, the compound of titanium and the mol ratio of organic solvent are 1: 4～15, mixture is put into ice-water bath stirs, A liquid;
2) water, complexing agent, organic solvent and Silver Nitrate powder 1: 0.1 in molar ratio～1: 6～18: 0.2～1.5 are mixed and constantly stirring, all dissolve, get B liquid up to Silver Nitrate;
3) B liquid is dropwise splashed in the A liquid that always is placed on ice-water bath, continue then to stir, up to the colloidal sol that obtains colour stable, again that colloidal sol is stand-by in-10～20 ℃ of following ageings;
4) carrier impregnation after will cleaning lifts in above-mentioned colloidal sol, and pull rate is controlled at 1～10cm/min, has whenever lifted one deck, in 450～600 ℃ of following thermal treatment 5～60min, obtains Ag/TiO
2Film.
2. the method for preparing the silver/titanium dioxide laminated film according to claim 1, the compound that it is characterized in that said titanium are butyl (tetra) titanate, titanium chloride or isopropyl titanate.
3. the method for preparing the silver/titanium dioxide laminated film according to claim 1 is characterized in that said organic solvent is ethanol, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, ethylene glycol phenyl ether, Benzenediol methyl ether or propyl alcohol.
4. the method for preparing the silver/titanium dioxide laminated film according to claim 1 is characterized in that said complexing agent is diethanolamine, citric acid, hydroxylated cellulose (HPC) or polyoxyethylene glycol (PEG).
5. the method for preparing the silver/titanium dioxide laminated film according to claim 1 is characterized in that said carrier is simple glass sheet, quartz glass plate or ceramic plate.
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|---|---|---|---|
| CNB2006100532812A CN100428997C (en) | 2006-09-06 | 2006-09-06 | Method for preparing composite film of silver Nano granule / titanium dioxide |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101693196B (en) * | 2009-10-01 | 2012-01-11 | 徐志兵 | Preparation method of silver/titanium dioxide compound |
| CN102492322A (en) * | 2011-12-09 | 2012-06-13 | 华东理工大学 | Nano-coating for unsaturated evaporation heat transfer surface |
| CN102744059A (en) * | 2012-07-16 | 2012-10-24 | 黑龙江大学 | Preparation method of ordered mesoporous titania/silver photocatalyst |
| CN101760171B (en) * | 2008-12-25 | 2013-08-14 | 西北工业大学 | Optical resonance composite material in noble metal/titanium dioxide micro-nano structure |
| CN103556177A (en) * | 2013-11-05 | 2014-02-05 | 福州大学 | Active-layer-modified titanium substrate conducting material and preparation method thereof |
| CN104258850A (en) * | 2014-09-26 | 2015-01-07 | 苏州纽艾之光净化设备有限公司 | Ag-doped TiO2 nano thin film and composite material containing thin film |
| CN106040211A (en) * | 2016-05-27 | 2016-10-26 | 山东大学 | Preparation method of yellow TiO2 photocatalytic material capable of absorbing visible light |
| CN106057357A (en) * | 2016-06-15 | 2016-10-26 | 浙江大学 | Method for preparing silver nanowire-titanium dioxide composite transparent electrode and transparent electrode |
| CN106784307A (en) * | 2016-11-10 | 2017-05-31 | 河北大学 | One kind is based on TiO2Neurobionics device of neurobionics layer and preparation method thereof |
| CN110563483A (en) * | 2019-10-11 | 2019-12-13 | 南京工业大学 | Low dielectric fused quartz microwave dielectric ceramic surface metallization method |
| CN112547459A (en) * | 2020-11-04 | 2021-03-26 | 东南大学 | Preparation method of composite antibacterial coating aluminum foil |
| CN113149454A (en) * | 2021-05-06 | 2021-07-23 | 东南大学 | Preparation method of colorless transparent antibacterial glass |
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2006
- 2006-09-06 CN CNB2006100532812A patent/CN100428997C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760171B (en) * | 2008-12-25 | 2013-08-14 | 西北工业大学 | Optical resonance composite material in noble metal/titanium dioxide micro-nano structure |
| CN101693196B (en) * | 2009-10-01 | 2012-01-11 | 徐志兵 | Preparation method of silver/titanium dioxide compound |
| CN102492322A (en) * | 2011-12-09 | 2012-06-13 | 华东理工大学 | Nano-coating for unsaturated evaporation heat transfer surface |
| CN102744059A (en) * | 2012-07-16 | 2012-10-24 | 黑龙江大学 | Preparation method of ordered mesoporous titania/silver photocatalyst |
| CN102744059B (en) * | 2012-07-16 | 2014-03-12 | 黑龙江大学 | Preparation method of ordered mesoporous titania/silver photocatalyst |
| CN103556177A (en) * | 2013-11-05 | 2014-02-05 | 福州大学 | Active-layer-modified titanium substrate conducting material and preparation method thereof |
| CN103556177B (en) * | 2013-11-05 | 2016-03-30 | 福州大学 | A kind of active coating Modified Titanium base material electro-conductive material and preparation method thereof |
| CN104258850A (en) * | 2014-09-26 | 2015-01-07 | 苏州纽艾之光净化设备有限公司 | Ag-doped TiO2 nano thin film and composite material containing thin film |
| CN106040211A (en) * | 2016-05-27 | 2016-10-26 | 山东大学 | Preparation method of yellow TiO2 photocatalytic material capable of absorbing visible light |
| CN106040211B (en) * | 2016-05-27 | 2018-07-10 | 山东大学 | A kind of yellow TiO with visible absorption performance2The preparation method of catalysis material |
| CN106057357A (en) * | 2016-06-15 | 2016-10-26 | 浙江大学 | Method for preparing silver nanowire-titanium dioxide composite transparent electrode and transparent electrode |
| CN106784307A (en) * | 2016-11-10 | 2017-05-31 | 河北大学 | One kind is based on TiO2Neurobionics device of neurobionics layer and preparation method thereof |
| CN106784307B (en) * | 2016-11-10 | 2019-01-08 | 河北大学 | One kind being based on TiO2Neurobionics device of neurobionics layer and preparation method thereof |
| CN110563483A (en) * | 2019-10-11 | 2019-12-13 | 南京工业大学 | Low dielectric fused quartz microwave dielectric ceramic surface metallization method |
| CN112547459A (en) * | 2020-11-04 | 2021-03-26 | 东南大学 | Preparation method of composite antibacterial coating aluminum foil |
| CN113149454A (en) * | 2021-05-06 | 2021-07-23 | 东南大学 | Preparation method of colorless transparent antibacterial glass |
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| CN100428997C (en) | 2008-10-29 |
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Granted publication date: 20081029 Termination date: 20170906 |