CN101328025A - Preparation of multielement codoped nanaotitania film - Google Patents
Preparation of multielement codoped nanaotitania film Download PDFInfo
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- CN101328025A CN101328025A CNA2008101200654A CN200810120065A CN101328025A CN 101328025 A CN101328025 A CN 101328025A CN A2008101200654 A CNA2008101200654 A CN A2008101200654A CN 200810120065 A CN200810120065 A CN 200810120065A CN 101328025 A CN101328025 A CN 101328025A
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Abstract
The invention discloses a method for preparing a multielement co-doped nano titanium dioxide film comprising the following steps: 1) adding ferric nitrate nonahydrate, silver nitrate and guanidine hydrochloride solid into abatase titanium dioxide solution to prepare a mixed solution; 2) sustainably magnetically stirring the mixed solution under the water bath condition and obtaining an uniform sol; 3) storing the sol at room temperature for 10-12 days to obtain aging solution, preparing a coating glass slide by the aging solution and drying; 4) heat-treating the dried coating glass slide at 350-450 DEG C for 1 hour to obtain the multielement co-doped nano titanium dioxide film. The titanium dioxide film of the invention has functions of achievement the red shift of the ultraviolet absorbance, visible light response of the photocatalysis and no light antibacteria.
Description
Technical field
The present invention relates to a kind of preparation method of multielement codoped nanaotitania film.
Background technology
Nano-titanium dioxide film is a kind of important functional material, in the storage of sun power and the aspects such as environmental treatment of utilization, photochemistry conversion and organic pollutant important application prospects is arranged.The preparation method of nano-titanium dioxide film is numerous, and wherein the method for manufacturing thin film based on sol-gel method is to study more titanium deoxid film preparation method at present.The advantage of this method is an easy big area film forming and being fixed on the matrix of complicated shape, adopts sol-gel method to prepare the existing reported in literature of film in surface of ordinary glass at present; It is raw material that these class methods all adopt presoma such as butyl (tetra) titanate, utilize the sol-gel method process to prepare TiO 2 sol, and apply, thus the preparation titanium deoxid film.This method needs higher thermal treatment temp could remove impurity such as organism, thus to body material particularly the thermal stability of glass claim.
On the other hand, because titanium dioxide forbidden band energy gap (rutile be 3.0eV mutually, be 3.2eV mutually with anatase octahedrite) broad, so ability display light catalytic activity under UV-irradiation only, and very weak to the response of visible light.But ultraviolet radiation is harmful, and general environment for use does not possess strong UV-irradiation condition; But radiation of visible light realizes easily that but because the sunlight main component is visible light, and the ultraviolet composition only accounts for 5%.Therefore, a lot of researchs recent years are exactly to wish to make it at visible region stronger absorption be arranged also by titanium dioxide is carried out doping vario-property or sensitization, improve promptly that it is visible light-responded.The research of relevant multi-element doping titanium deoxid film is on the low side, does not see relevant patent and bibliographical information.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of preparation method of multi-element doping nano-titanium dioxide film, adopts the titanium deoxid film of this method preparation to have functions such as the red shift that can realize ultraviolet absorption, light-catalysed visible light-responded and unglazed photograph be antibiotic.
In order to reach above purpose, the invention provides a kind of preparation method of multi-element doping nano-titanium dioxide film, may further comprise the steps:
1), in anatase type TiO 2 sol, adds nine water iron nitrates, Silver Nitrate and Guanidinium hydrochloride solid, one-tenth mixing solutions; The mol ratio of the iron in the nine water iron nitrates, the silver in the Silver Nitrate, the nitrogen in the Guanidinium hydrochloride and the titanium in the anatase type TiO 2 sol is respectively 0.08～0.8: 0.02～0.12: 6～30: 100;
2), above-mentioned mixing solutions is continued magnetic agitation under water bath condition, churning time is 60～80 minutes, and bath temperature is 45～55 ℃, obtains uniform sol;
3), above-mentioned colloidal sol normal temperature deposited 10～12 days after, colloidal sol after the ageing; Then colloidal sol after the above-mentioned ageing is utilized dip-coating method to apply on glass basis and form film, slide glass becomes to film; Then the above-mentioned slide glass of filming was dried 15 minutes at 80～100 ℃;
4), the slide glass thermal treatment under 350～450 ℃ of temperature of filming after the above-mentioned oven dry was got multielement codoped nanaotitania film after 1 hour.
Improvement as the preparation method of multielement codoped nanaotitania film of the present invention: in the step 3), on glass basis, apply 2～4 layers continuously, form 2～4 layers film.
The present invention is raw material with the anatase type TiO 2 sol, introduces iron ion (Fe
3+), silver ions (Ag
+) and nitrogen element (N), thereby make the equally distributed titanium dioxide nano sol of doped element; And further pass through dip-coating method, thereby obtain being deposited on the titanium deoxid film on the glass basis.In preparation method of the present invention, iron ion and silver ions are respectively from nine water iron nitrate and Silver Nitrates, and Guanidinium hydrochloride is responsible for providing the nitrogen element.
Anatase type TiO 2 sol can be prepared by the CN101054202 disclosed method; Also can directly buy anatase titanium dioxide, adopt deionized water to disperse to prepare and get, nano titanium oxide can be purchased the ten thousand scape novel material company limiteds in Hangzhou.
Preparation method of the present invention conscientiously studies with a large amount of tests resulting through the contriver.The present invention introduces iron, nitrogen, three kinds of elements of silver on the basis of the TiO 2 sol that contains anatase nanocrystal, be prepared into the multi-element doping titanium deoxid film, and it has the red shift that can realize ultraviolet absorption, light-catalysed function such as visible light-responded.Get 3 slide glasss that are loaded with multielement codoped nanaotitania film of the inventive method gained and put into about 10～12 rhodamine B solution medium ultraviolet illumination that restrain 3.0 mg/litre after 30 minutes, the degradation rate of rhodamine can reach 40%～60%; If illumination is 2.5 hours under sunlight, then the degradation rate of rhodamine can reach 80～85%.
Embodiment
Embodiment 1, a kind of multi-element doping nano-titanium dioxide film, concrete preparation method is as follows:
1), get 60 grams and contain the TiO 2 sol of anatase nanocrystal, add nine water iron nitrates, the mol ratio that makes Fe and Ti is 0.08: 100; Add Silver Nitrate, the mol ratio that makes Ag and Ti is 0.04: 100; Add Guanidinium hydrochloride, the mol ratio that makes N and Ti is 30: 100; Obtain mixing solutions thus;
2), above-mentioned mixing solutions is continued magnetic agitation under water bath condition, churning time is 60 minutes, and bath temperature is 55 ℃, obtains even clarifying colloidal sol;
3), above-mentioned colloidal sol normal temperature deposited 10 days after, colloidal sol after the ageing; Then colloidal sol after the above-mentioned ageing is utilized dip-coating method on dipping pulling film forming machine, to prepare film, be specially: on every sheet glass matrix, apply 2～4 layers continuously respectively, form 2～4 layers film, thereby obtain to film slide glass; Then with the above-mentioned slide glass of filming 80～100 ℃ drying in oven 15 minutes;
4), the slide glass thermal treatment under 350～450 ℃ of temperature of filming after the above-mentioned oven dry was prepared the thin film of titanium oxide of iron, nitrogen, silver-colored multi-element doping after 1 hour.
According to step 1) and step 2) preparation and the solid load of multi-element doping titanium dioxide nano sol be approximately 0.5%～2%, the colloidal sol particle diameter is approximately 30～100 nanometers.
Get 3 slide glasss that are loaded with multielement codoped nanaotitania film of step 4) gained and put into about 10～12 rhodamine B solution medium ultraviolet illumination that restrain 3.0 mg/litre after 30 minutes, the degradation rate of rhodamine can reach 40%～60%; If illumination is 2.5 hours under sunlight, then the degradation rate of rhodamine can reach 80～85%.
Embodiment 2, a kind of multi-element doping nano-titanium dioxide film, concrete preparation method is as follows:
1), get 60 the gram contain the anatase octahedrite Nano sol, add nine water iron nitrates, the mol ratio that makes Fe and Ti is 0.8: 100; Add Silver Nitrate, the mol ratio that makes Ag and Ti is 0.02: 100; Add Guanidinium hydrochloride, the mol ratio that makes N and Ti is 6: 100; Obtain mixing solutions thus;
2), above-mentioned mixing solutions is continued magnetic agitation under water bath condition, churning time is 80 minutes, and bath temperature is 45 ℃, obtains even clarifying colloidal sol;
3), above-mentioned colloidal sol normal temperature deposited 11 days after, colloidal sol after the ageing; Then colloidal sol after the above-mentioned ageing is utilized dip-coating method on dipping pulling film forming machine, to prepare film, be specially: on every sheet glass matrix, apply 2～4 layers continuously respectively, form 2～4 layers film, thereby obtain to film slide glass; Then with the above-mentioned slide glass of filming 80～100 ℃ drying in oven 15 minutes;
4), the slide glass thermal treatment under 350～450 ℃ of temperature of filming after the above-mentioned oven dry was prepared the thin film of titanium oxide of iron, nitrogen, silver-colored multi-element doping after 1 hour.
According to step 1) and step 2) preparation and the solid load of multi-element doping titanium dioxide nano sol be approximately 0.5%～2%, the colloidal sol particle diameter is approximately 30～100 nanometers.
Get 3 slide glasss that are loaded with multielement codoped nanaotitania film of step 4) gained and put into about 10～12 rhodamine B solution medium ultraviolet illumination that restrain 3.0 mg/litre after 30 minutes, the degradation rate of rhodamine can reach 40%～60%; If illumination is 2.5 hours under sunlight, then the degradation rate of rhodamine can reach 80～85%.
Embodiment 3, a kind of multi-element doping nano-titanium dioxide film, concrete preparation method is as follows:
1), get 60 the gram contain anatase sol, add nine water iron nitrates, the mol ratio of Fe and Ti was respectively 0.4: 100; Add Silver Nitrate, the mol ratio that makes Ag and Ti is 0.12: 100; Add Guanidinium hydrochloride, the mol ratio that makes N and Ti is 10: 100; Obtain mixing solutions thus;
2), above-mentioned mixing solutions is continued magnetic agitation under water bath condition, churning time is 70 minutes, and bath temperature is 50 ℃, obtains even clarifying colloidal sol;
3), above-mentioned colloidal sol normal temperature deposited 12 days after, colloidal sol after the ageing; Then colloidal sol after the above-mentioned ageing is utilized dip-coating method on dipping pulling film forming machine, to prepare film, be specially: on every sheet glass matrix, apply 2～4 layers continuously respectively, form 2～4 layers film, thereby obtain to film slide glass; Then with the above-mentioned slide glass of filming 80～100 ℃ drying in oven 15 minutes;
4), the slide glass thermal treatment under 350～450 ℃ of temperature of filming after the above-mentioned oven dry was prepared the thin film of titanium oxide of iron, nitrogen, silver-colored multi-element doping after 1 hour.
According to step 1) and step 2) preparation and the solid load of multi-element doping titanium dioxide nano sol be approximately 0.5%～2%, the colloidal sol particle diameter is approximately 30～100 nanometers.
Get 3 slide glasss that are loaded with multielement codoped nanaotitania film of step 4) gained and put into about 10～12 rhodamine B solution medium ultraviolet illumination that restrain 3.0 mg/litre after 30 minutes, the degradation rate of rhodamine can reach 40%～60%; If illumination is 2.5 hours under sunlight, then the degradation rate of rhodamine can reach 80～85%.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (2)
1, a kind of preparation method of multielement codoped nanaotitania film is characterized in that may further comprise the steps:
1), in anatase type TiO 2 sol, adds nine water iron nitrates, Silver Nitrate and Guanidinium hydrochloride solid, one-tenth mixing solutions; The mol ratio of the iron in the described nine water iron nitrates, the silver in the Silver Nitrate, the nitrogen in the Guanidinium hydrochloride and the titanium in the anatase type TiO 2 sol is respectively 0.08～0.8: 0.02～0.12: 6～30: 100;
2), above-mentioned mixing solutions is continued magnetic agitation under water bath condition, churning time is 60～80 minutes, and bath temperature is 45～55 ℃, uniform sol;
3), above-mentioned colloidal sol normal temperature deposited 10～12 days after, colloidal sol after the ageing; Then colloidal sol after the above-mentioned ageing is utilized dip-coating method to apply on glass basis and form film, slide glass becomes to film; Then the above-mentioned slide glass of filming was dried 15 minutes at 80～100 ℃;
4), the slide glass thermal treatment under 350～450 ℃ of temperature of filming after the above-mentioned oven dry was got multielement codoped nanaotitania film after 1 hour.
2, the preparation method of multielement codoped nanaotitania film according to claim 1 is characterized in that: in the described step 3), apply 2～4 layers continuously on glass basis, form 2～4 layers film.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791562A (en) * | 2010-03-25 | 2010-08-04 | 东华大学 | Method for preparing ferrum-fluorine-codoped nano-titanium dioxide visible light photocatalyst |
| CN102219281A (en) * | 2010-04-13 | 2011-10-19 | 中国水利水电科学研究院 | Photocatalytic water purification device and manufacturing method of photocatalytic water purification device |
| CN102587610A (en) * | 2012-01-31 | 2012-07-18 | 南昌大学 | Visible-light response self-cleaning fluorocarbon aluminum veneer with nitrogen-doped nanometer titanium dioxide film coated on surface |
| CN103143372A (en) * | 2013-03-20 | 2013-06-12 | 郑州大学 | Preparation method for iron, cobalt and nitrogen co-doped modified TiO2/SO42-visible light photocatalyst |
| CN104852032A (en) * | 2015-03-31 | 2015-08-19 | 浙江大学 | Preparation method of silver-loaded titanium dioxide anode material |
| CN108411309A (en) * | 2018-03-28 | 2018-08-17 | 中国石油大学(北京) | A kind of preparation method of iron oxide composite titanium dioxide thin film light anode for photoproduction cathodic protection |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323752C (en) * | 2005-04-30 | 2007-07-04 | 中国地质大学（武汉） | Manufacture of Ag+-Fe+ dosed TiO2 weakly exciting catalytic luminating film |
| CN101037553B (en) * | 2007-02-13 | 2010-04-21 | 云南大学 | Preparation and application method of optically catalysed environment protection type coating |
-
2008
- 2008-07-17 CN CN2008101200654A patent/CN101328025B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791562A (en) * | 2010-03-25 | 2010-08-04 | 东华大学 | Method for preparing ferrum-fluorine-codoped nano-titanium dioxide visible light photocatalyst |
| CN102219281A (en) * | 2010-04-13 | 2011-10-19 | 中国水利水电科学研究院 | Photocatalytic water purification device and manufacturing method of photocatalytic water purification device |
| CN102219281B (en) * | 2010-04-13 | 2013-07-10 | 中国水利水电科学研究院 | Photocatalytic water purification device and manufacturing method of photocatalytic water purification device |
| CN102587610A (en) * | 2012-01-31 | 2012-07-18 | 南昌大学 | Visible-light response self-cleaning fluorocarbon aluminum veneer with nitrogen-doped nanometer titanium dioxide film coated on surface |
| CN102587610B (en) * | 2012-01-31 | 2014-10-29 | 南昌大学 | Visible-light response self-cleaning fluorocarbon aluminum veneer with nitrogen-doped nanometer titanium dioxide film coated on surface |
| CN103143372A (en) * | 2013-03-20 | 2013-06-12 | 郑州大学 | Preparation method for iron, cobalt and nitrogen co-doped modified TiO2/SO42-visible light photocatalyst |
| CN103143372B (en) * | 2013-03-20 | 2015-01-21 | 郑州大学 | Preparation method for iron, cobalt and nitrogen co-doped modified TiO2/SO42-visible light photocatalyst |
| CN104852032A (en) * | 2015-03-31 | 2015-08-19 | 浙江大学 | Preparation method of silver-loaded titanium dioxide anode material |
| CN108411309A (en) * | 2018-03-28 | 2018-08-17 | 中国石油大学(北京) | A kind of preparation method of iron oxide composite titanium dioxide thin film light anode for photoproduction cathodic protection |
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