CN1817454A - Production of porous titanium dioxide thin-film - Google Patents
Production of porous titanium dioxide thin-film Download PDFInfo
- Publication number
- CN1817454A CN1817454A CN 200610049154 CN200610049154A CN1817454A CN 1817454 A CN1817454 A CN 1817454A CN 200610049154 CN200610049154 CN 200610049154 CN 200610049154 A CN200610049154 A CN 200610049154A CN 1817454 A CN1817454 A CN 1817454A
- Authority
- CN
- China
- Prior art keywords
- film
- titanium dioxide
- tio
- porous titanium
- dioxide thin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000004408 titanium dioxide Substances 0.000 title claims description 10
- 239000010409 thin film Substances 0.000 title claims description 4
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 229920002678 cellulose Polymers 0.000 claims abstract description 12
- 239000001913 cellulose Substances 0.000 claims abstract description 12
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 27
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000003618 dip coating Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000654 additive Substances 0.000 abstract description 5
- 230000000996 additive effect Effects 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000003980 solgel method Methods 0.000 abstract description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A process for preparing porous TiO2 film from the isobutyl titanate as precursor, ethanediol mether as solvent, and hydroxy cellulose as additive by sol-gel method including immersing and pull-up is disclosed. It has high hydrophilicity and photocatalyzing performance.
Description
Technical field
The present invention relates to a kind of method for preparing porous titanium dioxide thin-film.
Technical background
Broad stopband oxide semiconductor titanium dioxide (TiO
2) because of it has good photoelectric properties and application prospects, receive people's very big concern always.Nano-TiO
2Have functions such as wet quick, air-sensitive and photocatalysis, thereby extensively be used as catalyst, Sensitive Apparatus, photoelectricity and automatically cleaning material.And specific area is the very important factor of the various performances of the applied device of decision, the TiO of preparation loose structure
2Film is one of important channel that increases the film specific area.For example in dye solar cell, for increasing TiO
2The film specific area increases the dyestuff adsorbance, usually with TiO
2Film preparation becomes loose structure.Thereby the TiO of preparation loose structure
2Film increases film TiO
2Specific area, to film TiO
2On device, use and have a great deal of practical meanings.Researchers are once by using different solvents, or different additives and different preparation method prepare porous TiO
2Film improves its specific area.Wherein, with the polyethylene glycol TiO of additive preparation by sol-gal process
2Film has obtained good loose structure, but the reunion effect of polyethylene glycol during for the hydrolysis that prevents TiO 2 particles is desirable not enough.
Summary of the invention
The purpose of this invention is to provide a kind of preparation porous TiO that can prevent effectively that TiO 2 particles from reuniting
2The method of film.
The present invention is to be presoma with the iso-butyl titanate, and EGME is a solvent, is additive with the hydroxylated cellulose, adopts sol-gel method to prepare porous TiO
2Film.Concrete steps are as follows:
1) iso-butyl titanate, EGME 1: 15 in molar ratio～25 is mixed and made into colloidal sol, adds hydroxylated cellulose then, the weight concentration that makes hydroxylated cellulose is regulated colloidal sol pH value 4～6 0.4～1.2%;
2) with the slide be substrate, adopt dip-coating method to prepare film, pull rate 1～2mms
-1, wet film is incubated 30min at least under 500～550 ℃ after 100～550 ℃ of following dryings.
The present invention lifts number of times and speed by change, can regulate TiO
2The thickness of film; The size of coming adjustment hole by the addition that changes hydroxylated cellulose.
Beneficial effect of the present invention is:
Preparation method of the present invention and use equipment are simple, environmentally safe; The poriferous titanium dioxide film that makes has better hydrophily and photocatalysis performance, with the hydroxylated cellulose reunion of additive when effectively having prevented the hydrolysis of TiO 2 particles, and lift number of times by changing dipping, can control the thickness of poriferous titanium dioxide rete.
Description of drawings
Fig. 1 is SEM (SEM) photo of poriferous titanium dioxide film.
The specific embodiment
Further specify the present invention below in conjunction with instantiation.
Embodiment 1
1) be that 1: 20 iso-butyl titanate and EGME fully is mixed and made into colloidal sol by stirring with mol ratio, add hydroxylated cellulose, the weight concentration that makes hydroxylated cellulose adds HNO 0.6%
3, regulate colloidal sol pH value 4.3;
2) making substrate with clean simple glass slide adopts dip-coating method to prepare film, pull rate 2mms
-1, wet film repeats above operation 5 times behind dry 3min under 100 ℃, at last the sample that obtains is put into Muffle furnace and be incubated 30min under 550 ℃ of conditions.
The SEM of prepared titanium dioxide film (SEM) photo as shown in Figure 1, as seen from the figure, this film has loose structure.
Embodiment 2
1) be that 1: 25 iso-butyl titanate and EGME fully is mixed and made into colloidal sol by stirring with mol ratio, add hydroxylated cellulose, the weight concentration that makes hydroxylated cellulose adds HCl 1.0%, regulates colloidal sol pH value 5.6;
2) making substrate with clean simple glass slide adopts dip-coating method to prepare film, pull rate 1.5mms
-1, wet film repeats above operation 5 times behind dry 3min under 150 ℃, at last the sample that obtains is put into Muffle furnace and be incubated 45min under 550 ℃ of conditions.
Experiment shows, poriferous titanium dioxide film of the present invention has good Superhydrophilic and photocatalysis performance, deionized water at the contact angle on this porous membrane surface less than 10 °, this porous membrane is put into methyl orange solution, behind UV-irradiation, methyl orange solution fades rapidly, and what color took off when shining under ultraviolet light than no film is faster.This poriferous titanium dioxide film is having wide prospect aspect device application and the automatically cleaning.
Claims (1)
1. method for preparing porous titanium dioxide thin-film is characterized in that may further comprise the steps:
1) iso-butyl titanate, EGME 1: 15 in molar ratio～25 is mixed and made into colloidal sol, adds hydroxylated cellulose then, the weight concentration that makes hydroxylated cellulose is regulated colloidal sol pH value 4～6 0.4～1.2%;
2) with the slide be substrate, adopt dip-coating method to prepare film, pull rate 1～2mms
-1, wet film is incubated 30min at least under 500～550 ℃ after 100～550 ℃ of following dryings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610049154 CN1817454A (en) | 2006-01-18 | 2006-01-18 | Production of porous titanium dioxide thin-film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610049154 CN1817454A (en) | 2006-01-18 | 2006-01-18 | Production of porous titanium dioxide thin-film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1817454A true CN1817454A (en) | 2006-08-16 |
Family
ID=36917776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610049154 Pending CN1817454A (en) | 2006-01-18 | 2006-01-18 | Production of porous titanium dioxide thin-film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1817454A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104596994A (en) * | 2014-12-15 | 2015-05-06 | 浙江大学 | Europium-doped titanium dioxide/graphene oxide composite film and preparation method thereof |
| CN105350068A (en) * | 2015-10-29 | 2016-02-24 | 上海师范大学 | Preparation method of porous monocrystalline TiO2 thin film |
| CN105727918A (en) * | 2016-02-02 | 2016-07-06 | 四川大学 | Method for preparing highly-porous titanium dioxide film photocatalyst |
-
2006
- 2006-01-18 CN CN 200610049154 patent/CN1817454A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104596994A (en) * | 2014-12-15 | 2015-05-06 | 浙江大学 | Europium-doped titanium dioxide/graphene oxide composite film and preparation method thereof |
| CN104596994B (en) * | 2014-12-15 | 2017-05-03 | 浙江大学 | Europium-doped titanium dioxide/graphene oxide composite film and preparation method thereof |
| CN105350068A (en) * | 2015-10-29 | 2016-02-24 | 上海师范大学 | Preparation method of porous monocrystalline TiO2 thin film |
| CN105727918A (en) * | 2016-02-02 | 2016-07-06 | 四川大学 | Method for preparing highly-porous titanium dioxide film photocatalyst |
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| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |