CN103553358A - Method for preparing Fe3+/SiO2/TiO2 nano composite film - Google Patents
Method for preparing Fe3+/SiO2/TiO2 nano composite film Download PDFInfo
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- CN103553358A CN103553358A CN201310550268.8A CN201310550268A CN103553358A CN 103553358 A CN103553358 A CN 103553358A CN 201310550268 A CN201310550268 A CN 201310550268A CN 103553358 A CN103553358 A CN 103553358A
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Abstract
The invention discloses a method for preparing a Fe3+/SiO2/TiO2 nano composite film. The method comprises the following steps of preparing Fe3+/TiO2 nano composite sol and SiO2 sol, and fully mixing the two kinds of sol according to a ratio of 90-60 percent to 10-40 percent, thereby obtaining Fe3+/SiO2/TiO2 composite sol; after ageing, coating on a cleaned glass substrate by adopting a dip-coating mode, and putting the Fe3+/SiO2/TiO2 composite sol into a drying oven after coating the finished; putting the Fe3+/SiO2/TiO2 composite sol into a muffle furnace after drying, performing heat treatment at the temperature of 450 DEG C at a temperature rise rate of 1.5 DEG C per minute, keeping the temperature for 2 hours, and annealing, thereby obtaining the Fe3+/SiO2/TiO2 nano composite film which is uniform in surface of the film, stable in crystal form and excellent in hydrophilic performance. The Fe3+/SiO2/TiO2 nano composite film prepared by the method is uniform in surface distribution of the film subjected to heat treatment and is excellent in hydrophilic performance, and a contact angle between the film and water in a darkroom is 0 degree, so that the photocatalytic efficiency and hydrophilic performance of the film are effectively improved.
Description
Technical field
The present invention relates to a kind of preparation method of laminated film, relate in particular to a kind of Fe
3+/ SiO
2/ TiO
2the preparation method of nano compound film.
Background technology
The preparation method of glass with clean plates one or more layers TiO on glass substrate
2film, but the technological difficulties that this technology faces are that film surface can lose photocatalytic activity and wetting ability very soon under the condition of unglazed photograph, thus affecting its self-cleaning function, this has also limited TiO
2the application of film in real life.
In order to solve an above-mentioned difficult problem, both at home and abroad researcher improves TiO by means such as ion doping, semi-conductor are compound
2the photocatalytic activity of film and hydrophilicity thereof, patent CN102162086A has announced a kind of TiO
2/ SiO
2the preparation method of laminated film, it adopts magnetron sputtering method to prepare that sticking power is good, the TiO of film thickness homogeneous
2/ SiO
2laminated film, the photocatalytic activity of this laminated film and wetting ability be purer TiO all
2film increases.Patent CN1424282A has announced titanium dioxide nano-film and the method for making thereof that contains rare earth and silicon-dioxide, the TiO that it makes by sol-gel method
2/ SiO
2photocatalytic activity and the Superhydrophilic of/rare earth laminated film are all significantly improved.Although these methods have improved TiO to a certain extent
2the performance of film, but their photocatalysis efficiency and wetting abilities under visible ray are still undesirable.
Summary of the invention
The present invention seeks to overcome the above-mentioned shortcoming that prior art exists, a kind of Fe is provided
3+/ SiO
2/ TiO
2the preparation method of nano compound film.
For achieving the above object, the technology used in the present invention means are: a kind of Fe
3+/ SiO
2/ TiO
2the preparation method of nano compound film, its concrete steps are as follows:
(1) prepare Fe
3+/ TiO
2nano combined colloidal sol: chemical pure butyl (tetra) titanate is dissolved in dehydrated alcohol, then splashes into a small amount of methyl ethyl diketone, stir 30min under room temperature, form A liquid; Take Fe (NO simultaneously
3)
39H
2o joins in dehydrated alcohol, dissolves, and adds a small amount of deionized water and appropriate PVP, forms B liquid; Under whipped state, B liquid is slowly splashed in A liquid, use dense HNO
3adjust the pH value of solution, continue to stir 3h, after ageing 2-7 days, obtain orange transparent Fe
3+/ TiO
2colloidal sol;
(2) prepare SiO
2colloidal sol: respectively the tetraethoxy of certain mass, dehydrated alcohol mixed and stir 30min, forming C liquid; Meanwhile, by the dehydrated alcohol of certain mass, deionized water, dense HNO
3fully mix, form D liquid; Use magnetic stirring apparatus, under whipped state, D liquid is slowly added drop-wise in C liquid, continue to stir 3h, after ageing 2-7 days, obtain stable SiO
2colloidal sol;
(3) gained colloidal sol in step 1 is fully mixed according to the ratio of 90%-60%:10%-40% with gained colloidal sol in step 2, obtain Fe
3+/ SiO
2/ TiO
2complex sol, ageing is after 2 days, stand-by;
(4) by the Fe obtaining in step 3
3+/ SiO
2/ TiO
2the mode plated film that complex sol adopts dipping to lift on the glass substrate cleaning up, puts it in loft drier dry after plated film is complete;
(5) dried glass substrate in step 4 is put into retort furnace, at 450 ℃ of temperature, heat-treat, temperature rise rate is 1.5 ℃/min, insulation 2h, and annealing, obtains film surface even, stable crystal form, the Fe that hydrophilicity is superpower
3+/ SiO
2/ TiO
2nano compound film.
Further, in described step 1,19.32g butyl (tetra) titanate is dissolved in the dehydrated alcohol of 31.6g, and adds the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains A solution; Next takes 0.12gFe (NO
3)
39H
2o and 0.01gPVP are dissolved in the dehydrated alcohol and 2g deionized water of 15.8g, mix to obtain B solution; Under violent stirring, B solution is slowly splashed in A solution, and use dense HNO
3adjusting pH is 3, continues to stir 3h.
Further, in described step 2,9.34g tetraethoxy, 31.6g dehydrated alcohol are mixed and magnetic agitation 30min, obtain C solution; Simultaneously by the dense HNO of 0.7g
3be added in 15.8g dehydrated alcohol with 2g deionized water, mix, obtain D solution; Under the violent stirring of magnetic stirring apparatus, D solution is slowly added drop-wise in C solution, continue to stir 2h.
Further, in described step 4, the rate of pulling is 90mm/min, and soak time is 1min, and the loft drier of putting into 80 ℃ after plated film is complete is dry.
The invention has the beneficial effects as follows: the Fe that adopts present method to prepare
3+/ SiO
2/ TiO
2nano compound film, even in thermal treatment rear film surface arrangement, wetting ability is excellent, in darkroom, film and water contact angle reach 0 degree, thereby effectively improve photocatalysis efficiency and the hydrophilicity of film.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the contact angle photo of the nano compound film prepared of the present invention after indoor storage 24h.
Embodiment
embodiment 1
19.32g butyl (tetra) titanate is dissolved in the dehydrated alcohol of 31.6g, and adds the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains A solution; Next takes 0.12gFe (NO
3)
39H
2o and 0.01gPVP are dissolved in the dehydrated alcohol and 2g deionized water of 15.8g, mix to obtain B solution.Under violent stirring, B solution is slowly splashed in A solution, and use dense HNO
3adjusting pH is 3, continues to stir 3h, just obtains stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 2 days is standby.
9.34g tetraethoxy, 31.6g dehydrated alcohol are mixed and magnetic agitation 30min, obtain C solution; Simultaneously by the dense HNO of 0.7g
3be added in 15.8g dehydrated alcohol with 2g deionized water, mix, obtain D solution.Under the violent stirring of magnetic stirring apparatus, D solution is slowly added drop-wise in C solution, continue to stir 2h, obtain SiO
2colloidal sol, ageing 2 days.
By ratio of component 90%Fe
3+/ TiO
2colloidal sol and 10%SiO
2colloidal sol mixes, and ageing, after 2 days, obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The mode of utilizing dipping to lift on the slide glass cleaning up is prepared nano-TiO
2film, the rate of pulling is 90mm/min, soak time is 1min, has plated in the loft drier that puts it into 80 ℃ after film dry.Then, will be coated with Fe
3+/ SiO
2/ TiO
2the slide glass of laminated film is put into the retort furnace insulation 2h that is slowly warming up to 450 ℃ of temperature with the speed of 1.5 ℃/min, and naturally cooling, obtains Fe
3+/ SiO
2/ TiO
2film.
embodiment 2
19.32g butyl (tetra) titanate is dissolved in the dehydrated alcohol of 31.6g, and adds the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains A solution; Next takes 0.12gFe (NO
3)
39H
2o and 0.01gPVP are dissolved in the dehydrated alcohol and 2g deionized water of 15.8g, mix to obtain B solution.Under violent stirring, B solution is slowly splashed in A solution, and use dense HNO
3adjusting pH is 3, continues to stir 3h, just obtains stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 7 days is standby.
9.34g tetraethoxy, 31.6g dehydrated alcohol are mixed and magnetic agitation 30min, obtain C solution; Simultaneously by the dense HNO of 0.7g
3be added in 15.8g dehydrated alcohol with 2g deionized water, mix, obtain D solution.Under the violent stirring of magnetic stirring apparatus, D solution is slowly added drop-wise in C solution, continue to stir 2h, obtain SiO
2colloidal sol, ageing 7 days.
By ratio of component 80% Fe
3+/ TiO
2colloidal sol and 20%SiO
2colloidal sol mixes, and ageing, after 2 days, obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The mode of utilizing dipping to lift on the slide glass cleaning up is prepared nano-TiO
2film, the rate of pulling is 90mm/min, soak time is 1min, has plated in the loft drier that puts it into 80 ℃ after film dry.Then, will be coated with Fe
3+/ SiO
2/ TiO
2the slide glass of laminated film is put into the retort furnace insulation 2h that is slowly warming up to 450 ℃ of temperature with the speed of 1.5 ℃/min, and naturally cooling, obtains Fe
3+/ SiO
2/ TiO
2film.
embodiment 3
19.32g butyl (tetra) titanate is dissolved in the dehydrated alcohol of 31.6g, and adds the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains A solution; Next takes 0.12gFe (NO
3)
39H
2o and 0.01gPVP are dissolved in the dehydrated alcohol and 2g deionized water of 15.8g, mix to obtain B solution.Under violent stirring, B solution is slowly splashed in A solution, and use dense HNO
3adjusting pH is 3, continues to stir 3h, just obtains stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 4 days is standby.
9.34g tetraethoxy, 31.6g dehydrated alcohol are mixed and magnetic agitation 30min, obtain C solution; Simultaneously by the dense HNO of 0.7g
3be added in 15.8g dehydrated alcohol with 2g deionized water, mix, obtain D solution.Under the violent stirring of magnetic stirring apparatus, D solution is slowly added drop-wise in C solution, continue to stir 2h, obtain SiO
2colloidal sol, ageing 4 days.
By ratio of component 70% Fe
3+/ TiO
2colloidal sol and 30%SiO
2colloidal sol mixes, and ageing, after 2 days, obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The mode of utilizing dipping to lift on the slide glass cleaning up is prepared nano-TiO
2film, the rate of pulling is 90mm/min, soak time is 1min, has plated in the loft drier that puts it into 80 ℃ after film dry.Then, will be coated with Fe
3+/ SiO
2/ TiO
2the slide glass of laminated film is put into the retort furnace insulation 2h that is slowly warming up to 450 ℃ of temperature with the speed of 1.5 ℃/min, and naturally cooling, obtains Fe
3+/ SiO
2/ TiO
2film.
embodiment 4
19.32g butyl (tetra) titanate is dissolved in the dehydrated alcohol of 31.6g, and adds the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains A solution; Next takes 0.12gFe (NO
3)
39H
2o and 0.01gPVP are dissolved in the dehydrated alcohol and 2g deionized water of 15.8g, mix to obtain B solution.Under violent stirring, B solution is slowly splashed in A solution, and use dense HNO
3adjusting pH is 3, continues to stir 3h, just obtains stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 2～7 days is standby.
9.34g tetraethoxy, 31.6g dehydrated alcohol are mixed and magnetic agitation 30min, obtain C solution; Simultaneously by the dense HNO of 0.7g
3be added in 15.8g dehydrated alcohol with 2g deionized water, mix, obtain D solution.Under the violent stirring of magnetic stirring apparatus, D solution is slowly added drop-wise in C solution, continue to stir 2h, obtain SiO
2colloidal sol, ageing 2～7 days.
By ratio of component 60% Fe
3+/ TiO
2colloidal sol and 40%SiO
2colloidal sol mixes, and ageing, after 2 days, obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The mode of utilizing dipping to lift on the slide glass cleaning up is prepared nano-TiO
2film, the rate of pulling is 90mm/min, soak time is 1min, has plated in the loft drier that puts it into 80 ℃ after film dry.Then, will be coated with Fe
3+/ SiO
2/ TiO
2the slide glass of laminated film is put into the retort furnace insulation 2h that is slowly warming up to 450 ℃ of temperature with the speed of 1.5 ℃/min, and naturally cooling, obtains Fe
3+/ SiO
2/ TiO
2film.
In order to strengthen TiO
2performance under the visible ray of film, first the present invention passes through at TiO
2in colloidal sol, mix Fe
3+improve TiO
2the photocatalytic activity of film.Pass through Fe
3+effectively mix, can reduce TiO
2energy gap, make energy of absorption edge red shift, thereby improve the utilization ratio of film to visible ray, the effectively photocatalysis efficiency of enhanced film.Meanwhile, Fe
3+with Ti
4+ionic radius is very approaching, Fe
3+after doping, in heat treated process, easily replace the Ti on crystallographic site
4+or directly enter interstitial void, thereby doped F e
3+do not affect TiO
2be uniformly distributed.In addition, in order to strengthen TiO
2the wetting ability of film, the Fe making
3+/ TiO
2continue composite S iO
2, be because SiO
2a kind of water-storage material, appropriate SiO
2compoundly can effectively extend Fe
3+/ TiO
2the hydrophilic time length of film.Therefore, the present invention is by effective Fe
3+mix and SiO
2compound, thus TiO effectively improved
2the photocatalysis efficiency of film and hydrophilicity.
The present embodiment is only with the explanation of this apparatus function of opposing, and or not as the restriction to this device, the simple replacement that those skilled in the art carry out according to this apparatus structure, is not included within the scope of the rights protection of this patent.
Claims (4)
1. a Fe
3+/ SiO
2/ TiO
2the preparation method of nano compound film, its concrete steps are as follows:
(1) prepare Fe
3+/ TiO
2nano combined colloidal sol: chemical pure butyl (tetra) titanate is dissolved in dehydrated alcohol, then splashes into a small amount of methyl ethyl diketone, stir 30min under room temperature, form A liquid; Take Fe (NO simultaneously
3)
39H
2o joins in dehydrated alcohol, dissolves, and adds a small amount of deionized water and appropriate PVP, forms B liquid; Under whipped state, B liquid is slowly splashed in A liquid, use dense HNO
3adjust the pH value of solution, continue to stir 3h, after ageing 2-7 days, obtain orange transparent Fe
3+/ TiO
2colloidal sol;
(2) prepare SiO
2colloidal sol: respectively the tetraethoxy of certain mass, dehydrated alcohol mixed and stir 30min, forming C liquid; Meanwhile, by the dehydrated alcohol of certain mass, deionized water, dense HNO
3fully mix, form D liquid; Use magnetic stirring apparatus, under whipped state, D liquid is slowly added drop-wise in C liquid, continue to stir 3h, after ageing 2-7 days, obtain stable SiO
2colloidal sol;
(3) gained colloidal sol in step 1 is fully mixed according to the ratio of 90%-60%:10%-40% with gained colloidal sol in step 2, obtain Fe
3+/ SiO
2/ TiO
2complex sol, ageing is after 2 days, stand-by;
(4) by the Fe obtaining in step 3
3+/ SiO
2/ TiO
2the mode plated film that complex sol adopts dipping to lift on the glass substrate cleaning up, puts it in loft drier dry after plated film is complete;
(5) dried glass substrate in step 4 is put into retort furnace, at 450 ℃ of temperature, heat-treat, temperature rise rate is 1.5 ℃/min, insulation 2h, and annealing, obtains film surface even, stable crystal form, the Fe that hydrophilicity is superpower
3+/ SiO
2/ TiO
2nano compound film.
2. Fe according to claim 1
3+/ SiO
2/ TiO
2the preparation method of nano compound film, is characterized in that: in described step 1,19.32g butyl (tetra) titanate is dissolved in the dehydrated alcohol of 31.6g, and adds the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains A solution; Next takes 0.12gFe (NO
3)
39H
2o and 0.01gPVP are dissolved in the dehydrated alcohol and 2g deionized water of 15.8g, mix to obtain B solution; Under violent stirring, B solution is slowly splashed in A solution, and use dense HNO
3adjusting pH is 3, continues to stir 3h.
3. Fe according to claim 1
3+/ SiO
2/ TiO
2the preparation method of nano compound film, is characterized in that: in described step 2,9.34g tetraethoxy, 31.6g dehydrated alcohol are mixed and magnetic agitation 30min, obtain C solution; Simultaneously by the dense HNO of 0.7g
3be added in 15.8g dehydrated alcohol with 2g deionized water, mix, obtain D solution; Under the violent stirring of magnetic stirring apparatus, D solution is slowly added drop-wise in C solution, continue to stir 2h.
4. Fe according to claim 1
3+/ SiO
2/ TiO
2the preparation method of nano compound film, is characterized in that: in described step 4, the rate of pulling is 90mm/min, and soak time is 1min, and the loft drier of putting into 80 ℃ after plated film is complete is dry.
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Cited By (2)
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| CN108147677A (en) * | 2017-12-06 | 2018-06-12 | 吕莉 | A kind of preparation method of high efficiency photocatalysis glass with clean |
| CN113426434A (en) * | 2021-06-24 | 2021-09-24 | 蚌埠学院 | SnO (stannic oxide)2/Ag2(1-x)NixFe2O4Preparation method of composite film material |
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| CN113426434A (en) * | 2021-06-24 | 2021-09-24 | 蚌埠学院 | SnO (stannic oxide)2/Ag2(1-x)NixFe2O4Preparation method of composite film material |
| CN113426434B (en) * | 2021-06-24 | 2022-03-18 | 蚌埠学院 | SnO (stannic oxide)2/Ag2(1-x)NixFe2O4Preparation method of composite film material |
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