CN101306358A - Method for preparing titanic oxide nano-membrane on aluminum base - Google Patents
Method for preparing titanic oxide nano-membrane on aluminum base Download PDFInfo
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- CN101306358A CN101306358A CNA2008100713732A CN200810071373A CN101306358A CN 101306358 A CN101306358 A CN 101306358A CN A2008100713732 A CNA2008100713732 A CN A2008100713732A CN 200810071373 A CN200810071373 A CN 200810071373A CN 101306358 A CN101306358 A CN 101306358A
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Abstract
The invention discloses a method used for preparing a titanium dioxide nanometer film on an aluminum matrix, and relates to a nanometer film. The invention provides a method used for preparing the titanium dioxide nanometer film on the aluminum matrix. Polyethylene glycol is added into complex crystal nanosize titanium dioxide powder to obtain a mixture A, the ratio of the complex crystal nanosize titanium dioxide powder to the polyethylene glycol is equal to 10-4:1, anhydrous ethanol is added in the mixture A, the ratio of the mixture A to the anhydrous ethanol is equal to 1:4-5, and a mixture B is obtained by uniformly mixing; then water is added into the mixture B, the ratio of the mixture B to the water is equal to 1:3-4, and a mixture C is obtained by uniformly mixing; acid is added into the mixture C for adjusting the pH value to be 3-5, and a mixture D is obtained by uniformly mixing; the mixture D is uniformly dispersed under ultrasonic to obtain titania sol; after the surface is processed by acid or alkali, the aluminum matrix is washed and dried for later use; the pretreated aluminum matrix is dipped and coated with a film in the titania sol, the pore solution is spin-dried after the film is taken out, and finally the titanium dioxide nanometer film is prepared on the aluminum matrix by calcining after drying.
Description
Technical field
The present invention relates to a kind of nanometer film, especially relate to a kind of on aluminium base titanium dioxide (the TiO of preparation photocatalytic degradation effect
2) method of nanometer film.
Background technology
Nano titanium oxide has higher photocatalysis usefulness, the volatile organic matter pollutant (VOCs) of can effectively degrading, also have function ([1] SaxenaA such as sterilization, sterilization, deodorizing, Sahai Y.Modeling of Fluid Flow and Heat Transfer inTwin 2 Roll Casting of Aluminum Alloys[J] .The Japan Institute of Metals, 2002,43 (2): 206-213; [2] Haga T, Suzuki S.A High Speed Twin Roll Caster for Aluminum Alloy Strip[J] .Journal ofMaterials Processing Technology, 2001,113:291-2).Loading nano-titania film light catalysis technique has overcome the difficult shortcoming that reclaims of powder titanium deoxide catalyst, has stronger practicality, therefore become focus ([3] Bahnemann D W of photocatalysis research, Kholuiskaya S N, Dillert R, et al.Pho 2 todestruction of dichloroacetic acidcatalysis B:Environmental, 2002, (36): 161-169; [4] Hoffmann M F, Martin S T, Choi W, et al.Environmental application of semiconductor photocatalysis[J] .Chemical Review, 1995, (95): 69-96), especially aspect the airborne volatile organic matter of degraded special advantages ([5] Geula Dagan, MichaTomkiewicz.Praparation and characterization of TiO are being arranged
2Aerogels for use as photocatalysts[J] .Journalof Non-Crystalline Solids, 1994,175 (2-3): 294-302), have stronger practicality.The nanometer film catalysis material that is used for air cleaning at present is many with stainless steel cloth or ceramic honey comb ([6] Furman P, Gluszek J, Masalski J.Titaniumdioxide film obtained using the MOVCD method on 316L steel[J] .Journal of Materials ScienceLetters, 1997,16 (6): 471-472; [7] Natarajan C, Nogami G.Catholic electrodeposition ofnanocrystallyine titanium dioxide thin films[J] .Journal of the Electrochemical Society, 1996,143 (5): 1547-1550; [8] Sopyan I, Watanabe M, Mursawa S, et al.A film-type photocatalystincorporating highly active TiO
2Powder and fluroresin binder photocatalytic activity and long-termstability[J] .Joural of Electoanalytical Chemistry, 1996,415:183-186; [9] Zhu Yongfa, Li Wei, what Yu, still quiet. the online TiO of stainless steel metal wire
2The research of nano-film photocatalyst [J]; SCI; 2003; 3 (24): 465-468) as the load section bar; and on the film technique; industrial production adopts Sol-gel method ([5] GeulaDagan, Micha Tomkiewicz.Praparation and characterization of TiO usually
2Aerogels for use asphotocatalysts[J] .Journal of Non-Crystalline Solids, 1994,175 (2-3): 294-302).In recent years, the aluminium honeycomb section bar is extensive use of, and premium properties such as that its material has is in light weight, low-cost, high-specific surface area and low vapour lock have the good potential quality of alternative stainless steel cloth or ceramic honey comb.But because required calcining heat is higher during Sol-gel method film forming, cost height not only, and make the distortion of aluminium honeycomb section bar easily, limited the application of aluminium honeycomb section bar on photocatalysis membrana.Publication number is the formation method of filming that the Chinese patent application of CN1729062 discloses a kind of aluminium base, comprising: coating contains the operation that has the Thermocurable of luminescent material mylar that light powder base coating and roasting are arranged on the aluminium base surface; Then, coated heat solidifies based acrylic resin transparent powder paint and roasting, is formed with the light multilayer film.But do not relate to nanometer film with photocatalytic degradation effect.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing titanic oxide nano-membrane on aluminium base.
The present invention includes following steps:
1) preparation TiO 2 sol: in the mixed crystal type nanometer titanium dioxide powder, add polyethylene glycol, get mixture A, press mass ratio, mixed crystal type nanometer titanium dioxide powder: polyethylene glycol=(10～4): 1, in mixture A, add absolute ethyl alcohol, press mass ratio, mixture A: absolute ethyl alcohol=1: (4～5), stirring and evenly mixing get mixture B; In mixture B, add entry then, press mass ratio, mixture B: water=1: (3～4), stirring and evenly mixing gets mixture C; Adding acid for adjusting pH value in mixture C is 3～5, and stirring and evenly mixing gets mixture D; Mixture D is placed under the supersonic generator, be uniformly dispersed, get TiO 2 sol;
2) carrier preliminary treatment: after soda acid was handled, washing is also dried, and was stand-by with aluminium base carrier surface;
3) carrier plated film: pretreated aluminium base carrier is flooded plated film in TiO 2 sol, take out the solution in the back drying hole, the calcining of dry back has promptly prepared titanic oxide nano-membrane on aluminium base.
In the step 1, by mass percentage, preferably the nanometer anatase titania powder accounts for 80%～60% in the described mixed crystal type nanometer titanium dioxide powder, and the rutile type nano titanic oxide powder accounts for 20%～40%; Described polyethylene glycol preferably molecular weight is 6000 polyethylene glycol (PEG6000); The most handy magnetic stirrer of described stirring, mixing time be 10min at least preferably, mixes guaranteeing; The time that described ultrasonic wave disperses is 15min at least preferably, mixes guaranteeing; Describedly in mixture C, add acid for adjusting pH value preferably to adopt concentration of volume percent be that 10% salpeter solution is regulated, press mass ratio, mixture C: salpeter solution=1: 0.01.
In the step 2, the temperature of described oven dry is preferably 80～100 ℃.
In the step 3, the time of described dipping plated film is preferably each 1min; Described pretreated aluminium base carrier is flooded plated film in TiO 2 sol, take out the solution that the back dries in the hole and preferably repeat 5～8 times; The temperature of described calcining is preferably 250～350 ℃, and the time of calcining is preferably 1h.
With the sol-gel method of routine relatively, the present invention can aluminium base (for example: thin aluminium monolith substrate) the immobilized mixed crystal type nanometer TiO of surface-stable
2Powder has improved the stability of its batch process significantly.Calcining heat in the preparation process of the present invention obviously descends than the calcining heat of sol-gel method.The sol-gel method generates the needed calcining heat of nano titanium oxide and is generally more than 400～450 ℃.The present invention directly uses the nano titanium oxide powder of moulding, does not therefore need high-temperature calcination to form nano particle, and used temperature only is 250～350 ℃, mainly is the carbonization that helps the template agent.Make thin aluminium honeycomb section bar distortion easily owing to be higher than 400 ℃ temperature, therefore, one of great advantage of the present invention is can utilize to apply on thin aluminium honeycomb section bar under the temperature that is lower than 350 ℃ and fixing titanium dioxide nanoparticle and indeformable.Two of advantage of the present invention be energy-conservation, save equipment cost, and easy control of process conditions, this is because high-temperature service cost height not only, and energy consumption is big, the temperature range that the present invention adopts is lower, to saving cost and the control process conditions are all very favourable.Because the present invention is applicable on the aluminium base honeycomb section bar, aluminium base honeycomb section bar light weight is inexpensive, and specific area is big, photocatalytic degradation efficient height.The present invention has identical degradation property with the common producible steel substrate photocatalytic degradation film of sol-gel method of routine.The results showed that the present invention also is applicable to novel exotic materials such as ceramic base material, thereby be with a wide range of applications.
The mechanism of action of the present invention is summarized as follows:
Mixed crystal type nanometer titanium dioxide is light-catalysed main body, and PEG6000 is as pore creating material and template agent, and absolute ethyl alcohol and water are solvent.The present invention utilizes the agent of PEG template that nano titanium oxide is fixed on the aluminium base, increases the surface area of template agent by calcining.Main photocatalytic degradation mechanism is to utilize ultraviolet lighting to impel mixed crystal type nanometer titanium dioxide to inspire the electron hole, thereby produces extremely strong oxidability, degradation of organic substances.
The specific embodiment
Embodiment 1
1) preparation TiO 2 sol: take by weighing P25 (trade name of German Degussa company product, commercial) mixed crystal type nanometer titanium dioxide powder (anatase titanium dioxide accounts for 80%, and rutile-type accounts for 20%) 50g, add molecular weight and be 6000 polyethylene glycol 5g, mixture A.In mixture A, add absolute ethyl alcohol 250g, stir be mixed mixture B, in mixture B, slowly add distilled water 700g then, stir 15min be mixed mixture C.In mixture C, add 10% dilute nitric acid solution 7.0g, stir 15min be mixed mixture D.Mixture D is placed under the supersonic generator, disperse about 30min, become TiO 2 sol.
2) carrier preliminary treatment: get the aluminium base carrier of honeycomb, rinse well repeatedly with distilled water after adopting diluted acid, diluted alkaline respectively to wash 5min on the surface, 90～100 ℃ of oven dry down, stand-by.
3) carrier plated film: the aluminium base carrier of pretreated honeycomb is flooded 1min in TiO 2 sol, slowly from TiO 2 sol, lift out the aluminium base carrier of honeycomb then, dry the solution in the hole, 5 times so repeatedly, after the drying carrier is calcined 1h in 250 ℃.
Through Raman spectroscopy, the aluminium base photocatalytic degradation film of the honeycomb of producing still keeps original rutile-type and anatase titanium dioxide mixed crystal ratio.Measuring its catalytic degradation formaldehyde ability by correlation technique is more than 75%.
Embodiment 2
1) preparation TiO 2 sol: take by weighing P25 (trade name of German Degussa company product, commercial) mixed crystal type nanometer titanium dioxide powder 50g, add molecular weight and be 6000 polyethylene glycol 8g, mixture A.In mixture A, add absolute ethyl alcohol 220g, stir be mixed mixture B, in mixture B, slowly add distilled water 650g then, stir 15min be mixed mixture C.In mixture C, add 10% dilute nitric acid solution 6.50g and regulate acidity, stir 15min be mixed mixture D.Mixture D is placed under the supersonic generator, disperse about 30min, become TiO 2 sol.
2) carrier preliminary treatment: get the aluminium base carrier of honeycomb, rinse well repeatedly with distilled water after adopting diluted acid, diluted alkaline respectively to wash 5min on the surface, 80～90 ℃ of oven dry down, stand-by.
3) carrier plated film: the aluminium base carrier of pretreated honeycomb is flooded 1min in TiO 2 sol, slowly from TiO 2 sol, lift out the aluminium base carrier of honeycomb then, dry the solution in the hole, 7 times so repeatedly, after the drying carrier is calcined 1h in 350 ℃.
After measured, the aluminium base photocatalytic degradation film of the honeycomb of producing still keeps original rutile-type of P25 and anatase titanium dioxide mixed crystal ratio.Measuring its catalytic degradation formaldehyde ability by correlation technique is more than 86%.
Embodiment 3
1) preparation TiO 2 sol: with embodiment 2.
2) carrier preliminary treatment: get honeycomb ceramic carrier, rinse well repeatedly with distilled water after adopting diluted alkaline washing 2min on the surface, 90～95 ℃ of oven dry down, stand-by.
3) carrier plated film: with embodiment 2.
After measured, the ceramic honey comb photocatalytic degradation film of producing still keeps original rutile-type of P25 and anatase titanium dioxide mixed crystal ratio.Measuring its catalytic degradation formaldehyde ability by correlation technique is more than 70%.
Claims (10)
1. prepare the method for titanic oxide nano-membrane on aluminium base, it is characterized in that may further comprise the steps:
1) preparation TiO 2 sol: in the mixed crystal type nanometer titanium dioxide powder, add polyethylene glycol, get mixture A, press mass ratio, mixed crystal type nanometer titanium dioxide powder: polyethylene glycol=10～4: 1, in mixture A, add absolute ethyl alcohol, press mass ratio, mixture A: absolute ethyl alcohol=1: 4～5, stirring and evenly mixing get mixture B; In mixture B, add entry then, press mass ratio, mixture B: water=1: 3～4, stirring and evenly mixing gets mixture C; Adding acid for adjusting pH value in mixture C is 3～5, and stirring and evenly mixing gets mixture D; Mixture D is placed under the supersonic generator, be uniformly dispersed, get TiO 2 sol;
2) carrier preliminary treatment: after soda acid was handled, washing is also dried, and was stand-by with aluminium base carrier surface;
3) carrier plated film: pretreated aluminium base carrier is flooded plated film in TiO 2 sol, take out the solution in the back drying hole, the calcining of dry back has promptly prepared titanic oxide nano-membrane on aluminium base.
2. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1, it is characterized in that in step 1, in the described mixed crystal type nanometer titanium dioxide powder by mass percentage, the nanometer anatase titania powder accounts for 80%～60%, and the rutile type nano titanic oxide powder accounts for 20%～40%.
3. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 1 described polyethylene glycol is that molecular weight is 6000 polyethylene glycol.
4. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 1 described stirring is to use magnetic stirrer, and mixing time is 10min at least.
5. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 1 time that described ultrasonic wave disperses is 15min at least.
6. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 1, and the described acid for adjusting pH value that adds in mixture C is that to adopt concentration of volume percent be that 10% salpeter solution is regulated.
7. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 6 is characterized in that pressing mass ratio in step 1, mixture C: salpeter solution=1: 0.01.
8. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 2 temperature of described oven dry is 80～100 ℃.
9. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 3 time of described dipping plated film is each 1min; Described pretreated aluminium base carrier is flooded plated film in TiO 2 sol, take out the solution that the back dries in the hole and repeat 5～8 times.
10. the method for preparing titanic oxide nano-membrane on aluminium base as claimed in claim 1 is characterized in that in step 3 temperature of described calcining is 250～350 ℃, and the time of calcining is 1h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899654A (en) * | 2010-07-09 | 2010-12-01 | 浙江大学 | Method for preparing bioactive spherical titanium dioxide nanometer points on surface of medical metal |
| CN102180705A (en) * | 2011-02-28 | 2011-09-14 | 武汉大方机电有限公司 | Preparation method for titanium dioxide thin layer loaded on surface of inorganic ceramic matrix |
| WO2014198163A1 (en) * | 2013-06-13 | 2014-12-18 | 南京大学 | Preparation method for metallic oxide spherical cascade structure |
| CN113842709A (en) * | 2021-07-17 | 2021-12-28 | 北京工业大学 | Preparation method of multifunctional pollution-removing metal filter screen loaded with titanium dioxide |
-
2008
- 2008-07-09 CN CNA2008100713732A patent/CN101306358A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899654A (en) * | 2010-07-09 | 2010-12-01 | 浙江大学 | Method for preparing bioactive spherical titanium dioxide nanometer points on surface of medical metal |
| CN102180705A (en) * | 2011-02-28 | 2011-09-14 | 武汉大方机电有限公司 | Preparation method for titanium dioxide thin layer loaded on surface of inorganic ceramic matrix |
| CN102180705B (en) * | 2011-02-28 | 2013-04-10 | 武汉大方机电有限公司 | Preparation method for titanium dioxide thin layer loaded on surface of inorganic ceramic matrix |
| WO2014198163A1 (en) * | 2013-06-13 | 2014-12-18 | 南京大学 | Preparation method for metallic oxide spherical cascade structure |
| CN113842709A (en) * | 2021-07-17 | 2021-12-28 | 北京工业大学 | Preparation method of multifunctional pollution-removing metal filter screen loaded with titanium dioxide |
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Open date: 20081119 |