CN103553358B - A kind of Fe 3+/ SiO 2/ TiO 2the preparation method of nano compound film - Google Patents
A kind of Fe 3+/ SiO 2/ TiO 2the preparation method of nano compound film Download PDFInfo
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- CN103553358B CN103553358B CN201310550268.8A CN201310550268A CN103553358B CN 103553358 B CN103553358 B CN 103553358B CN 201310550268 A CN201310550268 A CN 201310550268A CN 103553358 B CN103553358 B CN 103553358B
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Abstract
The invention discloses a kind of Fe
3+/ SiO
2/ TiO
2the preparation method of nano compound film, by preparation Fe
3+/ TiO
2nanocomposite sol and SiO
2colloidal sol, and gained colloidal sol is fully mixed according to 90%-60%:10%-40%, obtain Fe
3+/ SiO
2/ TiO
2complex sol, after ageing, the glass substrate cleaned up adopts the mode plated film of Best-Effort request, puts into loft drier after plated film is complete, after drying, put into retort furnace, heat-treat at 450 DEG C of temperature, temperature rise rate is 1.5 DEG C/min, and insulation 2h annealing, obtains film surface even, stable crystal form, the Fe that hydrophilicity is superpower
3+/ SiO
2/ TiO
2nano compound film.Adopt Fe prepared by present method
3+/ SiO
2/ TiO
2nano compound film, film surface is evenly distributed after heat treatment, wetting ability is excellent, and in darkroom, film and water contact angle reach 0 degree, thus the effectively photocatalysis efficiency of raising film and hydrophilicity.
Description
Technical field
The present invention relates to a kind of preparation method of laminated film, particularly relate 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 a 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 affect its self-cleaning function, which also limits TiO
2the application of film in real life.
In order to solve an above-mentioned difficult problem, domestic and international researcher improves TiO by the means such as ion doping, semiconductors coupling
2the photocatalytic activity of film and hydrophilicity thereof, patent CN102162086A discloses a kind of TiO
2/ SiO
2the preparation method of laminated film, its adopted magnetron sputtering method to prepare sticking power is good, film thickness is homogeneous TiO
2/ SiO
2laminated film, all purer TiO of the photocatalytic activity of this laminated film and wetting ability
2film increases.Patent CN1424282A discloses titanium dioxide nano-film containing rare earth and silicon-dioxide and method for making thereof, and it is by the obtained TiO of sol-gel method
2/ SiO
2photocatalytic activity and the Superhydrophilic of/rare earth laminated film are all significantly improved.Although these methods improve TiO to a certain extent
2the performance of film, but their photocatalysis efficiencies under visible light and wetting ability still undesirable.
Summary of the invention
The present invention seeks to the above-mentioned shortcoming overcoming prior art existence, 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) Fe is prepared
3+/ TiO
2nanocomposite sol: chemical pure butyl (tetra) titanate is dissolved in dehydrated alcohol, then instill a small amount of methyl ethyl diketone, stirred at ambient temperature 30min, 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 instilled in A liquid, use dense HNO
3adjust the pH value of solution, continue to stir after 3h, ageing 2-7 days, obtain orange transparent Fe
3+/ TiO
2colloidal sol;
(2) SiO is prepared
2colloidal sol: the tetraethoxy of certain mass, dehydrated alcohol are mixed and stir 30min respectively, forms C liquid; Meanwhile, by the dehydrated alcohol of certain mass, deionized water, dense HNO
3abundant mixing, forms D liquid; Use magnetic stirring apparatus, under whipped state, D liquid is slowly added drop-wise in C liquid, continue to stir after 3h, ageing 2-7 days, obtain stable SiO
2colloidal sol;
(3) gained colloidal sol in step one 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) Fe will obtained in step 3
3+/ SiO
2/ TiO
2complex sol adopts the mode plated film of Best-Effort request on the glass substrate cleaned up, and puts it in loft drier dry after plated film is complete;
(5) glass substrate dried in step 4 is put into retort furnace, heat-treat at 450 DEG C of temperature, temperature rise rate is 1.5 DEG C/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 one, be dissolved in the dehydrated alcohol of 31.6g by 19.32g butyl (tetra) titanate, and add the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains solution A; Next takes 0.12gFe (NO
3)
39H
2in the dehydrated alcohol that O and 0.01gPVP is dissolved in 15.8g and 2g deionized water, mix to obtain B solution; Under vigorous stirring, B solution is slowly instilled in solution A, and use dense HNO
3adjust solution ph to be 3, continue to stir 3h.
Further, in described step 2, by 9.34g tetraethoxy, 31.6g dehydrated alcohol mixing also magnetic agitation 30min, obtain C solution; Simultaneously by dense for 0.7g HNO
3be added in 15.8g dehydrated alcohol with 2g deionized water, mixing, obtains solution D; Under the violent stirring of magnetic stirring apparatus, solution D is slowly added drop-wise in C solution, continues to stir 2h.
Further, in described step 4, the rate of pulling is 90mm/min, and soak time is 1min, and the loft drier putting into 80 DEG C after plated film is complete is dry.
The invention has the beneficial effects as follows: adopt Fe prepared by present method
3+/ SiO
2/ TiO
2nano compound film, film surface is evenly distributed after heat treatment, wetting ability is excellent, and in darkroom, film and water contact angle reach 0 degree, thus the effectively photocatalysis efficiency of raising film and hydrophilicity.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the contact angle photo of nano compound film after indoor storage 24h prepared by the present invention.
Embodiment
embodiment 1
Be dissolved in the dehydrated alcohol of 31.6g by 19.32g butyl (tetra) titanate, and add the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains solution A; Next takes 0.12gFe (NO
3)
39H
2in the dehydrated alcohol that O and 0.01gPVP is dissolved in 15.8g and 2g deionized water, mix to obtain B solution.Under vigorous stirring, B solution is slowly instilled in solution A, and use dense HNO
3adjust solution ph to be 3, continue to stir 3h, just obtain stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 2 days is for subsequent use.
By 9.34g tetraethoxy, 31.6g dehydrated alcohol mixing also magnetic agitation 30min, obtain C solution; Simultaneously by dense for 0.7g HNO
3be added in 15.8g dehydrated alcohol with 2g deionized water, mixing, obtains solution D.Under the violent stirring of magnetic stirring apparatus, solution D is slowly added drop-wise in C solution, continues 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, namely obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The slide glass cleaned up utilize the mode of Best-Effort request prepare nano-TiO
2film, the rate of pulling is 90mm/min, and soak time is 1min, puts it in the loft drier of 80 DEG C dry after having plated film.Then, Fe will be coated with
3+/ SiO
2/ TiO
2the retort furnace inside holding 2h being slowly warming up to 450 DEG C of temperature with the speed of 1.5 DEG C/min put into by the slide glass of laminated film, and naturally cooling, namely obtains Fe
3+/ SiO
2/ TiO
2film.
embodiment 2
Be dissolved in the dehydrated alcohol of 31.6g by 19.32g butyl (tetra) titanate, and add the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains solution A; Next takes 0.12gFe (NO
3)
39H
2in the dehydrated alcohol that O and 0.01gPVP is dissolved in 15.8g and 2g deionized water, mix to obtain B solution.Under vigorous stirring, B solution is slowly instilled in solution A, and use dense HNO
3adjust solution ph to be 3, continue to stir 3h, just obtain stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 7 days is for subsequent use.
By 9.34g tetraethoxy, 31.6g dehydrated alcohol mixing also magnetic agitation 30min, obtain C solution; Simultaneously by dense for 0.7g HNO
3be added in 15.8g dehydrated alcohol with 2g deionized water, mixing, obtains solution D.Under the violent stirring of magnetic stirring apparatus, solution D is slowly added drop-wise in C solution, continues 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, namely obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The slide glass cleaned up utilize the mode of Best-Effort request prepare nano-TiO
2film, the rate of pulling is 90mm/min, and soak time is 1min, puts it in the loft drier of 80 DEG C dry after having plated film.Then, Fe will be coated with
3+/ SiO
2/ TiO
2the retort furnace inside holding 2h being slowly warming up to 450 DEG C of temperature with the speed of 1.5 DEG C/min put into by the slide glass of laminated film, and naturally cooling, namely obtains Fe
3+/ SiO
2/ TiO
2film.
embodiment 3
Be dissolved in the dehydrated alcohol of 31.6g by 19.32g butyl (tetra) titanate, and add the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains solution A; Next takes 0.12gFe (NO
3)
39H
2in the dehydrated alcohol that O and 0.01gPVP is dissolved in 15.8g and 2g deionized water, mix to obtain B solution.Under vigorous stirring, B solution is slowly instilled in solution A, and use dense HNO
3adjust solution ph to be 3, continue to stir 3h, just obtain stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 4 days is for subsequent use.
By 9.34g tetraethoxy, 31.6g dehydrated alcohol mixing also magnetic agitation 30min, obtain C solution; Simultaneously by dense for 0.7g HNO
3be added in 15.8g dehydrated alcohol with 2g deionized water, mixing, obtains solution D.Under the violent stirring of magnetic stirring apparatus, solution D is slowly added drop-wise in C solution, continues 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, namely obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The slide glass cleaned up utilize the mode of Best-Effort request prepare nano-TiO
2film, the rate of pulling is 90mm/min, and soak time is 1min, puts it in the loft drier of 80 DEG C dry after having plated film.Then, Fe will be coated with
3+/ SiO
2/ TiO
2the retort furnace inside holding 2h being slowly warming up to 450 DEG C of temperature with the speed of 1.5 DEG C/min put into by the slide glass of laminated film, and naturally cooling, namely obtains Fe
3+/ SiO
2/ TiO
2film.
embodiment 4
Be dissolved in the dehydrated alcohol of 31.6g by 19.32g butyl (tetra) titanate, and add the methyl ethyl diketone of 3g, room temperature lower magnetic force stirs 30min, obtains solution A; Next takes 0.12gFe (NO
3)
39H
2in the dehydrated alcohol that O and 0.01gPVP is dissolved in 15.8g and 2g deionized water, mix to obtain B solution.Under vigorous stirring, B solution is slowly instilled in solution A, and use dense HNO
3adjust solution ph to be 3, continue to stir 3h, just obtain stable orange Fe
3+/ TiO
2colloidal sol.Obtained colloidal sol ageing 2 ~ 7 days is for subsequent use.
By 9.34g tetraethoxy, 31.6g dehydrated alcohol mixing also magnetic agitation 30min, obtain C solution; Simultaneously by dense for 0.7g HNO
3be added in 15.8g dehydrated alcohol with 2g deionized water, mixing, obtains solution D.Under the violent stirring of magnetic stirring apparatus, solution D is slowly added drop-wise in C solution, continues 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, namely obtains highly stable Fe
3+/ SiO
2/ TiO
2complex sol.
The slide glass cleaned up utilize the mode of Best-Effort request prepare nano-TiO
2film, the rate of pulling is 90mm/min, and soak time is 1min, puts it in the loft drier of 80 DEG C dry after having plated film.Then, Fe will be coated with
3+/ SiO
2/ TiO
2the retort furnace inside holding 2h being slowly warming up to 450 DEG C of temperature with the speed of 1.5 DEG C/min put into by the slide glass of laminated film, and naturally cooling, namely 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
2fe is mixed in colloidal sol
3+improve TiO
2the photocatalytic activity of film.Pass through Fe
3+effectively mix, can TiO be reduced
2energy gap, make energy of absorption edge red shift, thus improve film to the utilization ratio of visible ray, the photocatalysis efficiency of effective enhanced film.Meanwhile, Fe
3+with Ti
4+ionic radius is very close, Fe
3+in heat treated process, the Ti on crystallographic site is easily replaced after doping
4+or directly enter interstitial void, thus doped F e
3+do not affect TiO
2be uniformly distributed.In addition, in order to strengthen TiO
2the wetting ability of film, at obtained Fe
3+/ TiO
2continue composite S iO
2, be because SiO
2a kind of water-storage material, appropriate SiO
2compound effectively can extend Fe
3+/ TiO
2the hydrophilic time length of film.Therefore, the present invention is by effective Fe
3+mix and SiO
2compound, thus effectively improve TiO
2the photocatalysis efficiency of film and hydrophilicity.
The present embodiment is only used as the explanation to this apparatus function, and not as the restriction to this device, the simple replacement that those skilled in the art carry out according to this apparatus structure, is 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) Fe is prepared
3+/ TiO
2nanocomposite sol: chemical pure butyl (tetra) titanate is dissolved in dehydrated alcohol, then instill a small amount of methyl ethyl diketone, stirred at ambient temperature 30min, 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 instilled in A liquid, use dense HNO
3adjust the pH value of solution, continue to stir after 3h, ageing 2-7 days, obtain orange transparent Fe
3+/ TiO
2colloidal sol;
(2) SiO is prepared
2colloidal sol: the tetraethoxy of certain mass, dehydrated alcohol are mixed and stir 30min respectively, forms C liquid; Meanwhile, by the dehydrated alcohol of certain mass, deionized water, dense HNO
3abundant mixing, forms D liquid; Use magnetic stirring apparatus, under whipped state, D liquid is slowly added drop-wise in C liquid, continue to stir after 3h, ageing 2-7 days, obtain stable SiO
2colloidal sol;
(3) gained colloidal sol in step one 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) Fe will obtained in step 3
3+/ SiO
2/ TiO
2complex sol adopts the mode plated film of Best-Effort request on the glass substrate cleaned up, and puts it in loft drier dry after plated film is complete;
(5) glass substrate dried in step 4 is put into retort furnace, heat-treat at 450 DEG C of temperature, temperature rise rate is 1.5 DEG C/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 one, is dissolved in the dehydrated alcohol of 31.6g by 19.32g butyl (tetra) titanate, and adds the methyl ethyl diketone of 3g, and room temperature lower magnetic force stirs 30min, obtains solution A; Next takes 0.12gFe (NO
3)
39H
2in the dehydrated alcohol that O and 0.01gPVP is dissolved in 15.8g and 2g deionized water, mix to obtain B solution; Under vigorous stirring, B solution is slowly instilled in solution A, and use dense HNO
3adjust solution ph to be 3, continue 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, by 9.34g tetraethoxy, 31.6g dehydrated alcohol mixing also magnetic agitation 30min, obtains C solution; Simultaneously by dense for 0.7g HNO
3be added in 15.8g dehydrated alcohol with 2g deionized water, mixing, obtains solution D; Under the violent stirring of magnetic stirring apparatus, solution D is slowly added drop-wise in C solution, continues 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 putting into 80 DEG C after plated film is complete is dry.
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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 |
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