CN104086092B - A kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application - Google Patents
A kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application Download PDFInfo
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Abstract
The invention discloses a kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application。Described laminated film has double-decker, and including bottom film and surface layer film, bottom film is the Cu Bi modified2O3Thin film, surface layer film is mesoporous SiO2Thin film；Described preparation method is: be coated with one layer of Cu Bi modified in surface of ordinary glass2O3Thin film, wet film, through super-dry, is placed in Muffle furnace heat treatment, finally coats mesoporous SiO on surface2Thin film, obtains the laminated film of layering through identical processing method。This thin film shows good photocatalytic activity under visible ray or Weak ultraviolet, even at also having Superhydrophilic and thin film water white transparency, stable performance under dark condition。This method use equipment is simple, invest little, environmentally safe；The thin film prepared can be widely applied in the substrate that glass curtain wall, bathroom mirror, vehicle glass, optical instrument parts etc. need self-cleaning fog to process。
Description
Technical field
The invention belongs to technical field of function materials, be specifically related to a kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application。
Background technology
Along with socioeconomic development, problem of environmental pollution is increasingly subject to people's attention, and wherein, the cleaning problems (cleaning such as glass) of various indoor and outdoor construction materials also causes therewith to be paid close attention to widely。Stick to when the pollutant in air on glass of building or automotive glazing, both reduced the transmittance of glass, affect again attractive in appearance。In addition, easily many small water droplets are formed in glass surface condensation during malaria condensation, the light transmission of glass is affected due to the scattering process of these water droplets, bring inconvenience, particularly the overcast and rainy droplet formed on automobile rearview mirror has a strong impact on the sight line of people, there is very big potential safety hazard。The solution appearing as these problems of Superhydrophilic self-cleaning material brings Gospel。
The film material with function on self-cleaning glass surface having been put at present using or researching and developing is mainly with TiO2Or TiO2With other metals, metal-oxide, nonmetal doping complex be main。But TiO2Utilization rate low (Eg=3.2eV) and relatively low quantum efficiency to sunlight, limits its practical application。Therefore, find or design a kind of have visible light-responded novel photocatalyst still be full of challenge。Bi2O3Because of its band gap narrow (about 2.8eV), there is the advantages such as visible light-responded, Lacking oxygen is many, photoresponse is rapid, oxidability is strong, it is believed that be one of the most promising current novel photocatalyst。We are with this promoter compound with it that can effectively catch electronics of Cu ion so that it is light induced electron and hole are efficiently separated, thus significantly improving its photocatalysis efficiency。Additionally, to have the SiO of Superhydrophilic under dark condition2Thin film covers Cu-Bi2O3Film surface, on the one hand due to mesoporous SiO2The Superhydrophilic of thin film makes this thin film have anti-fog performance, has widened its application；On the other hand, due to surface SiO2The existence of thin film makes Cu-Bi2O3The Cu ion of thin film not easily dissociates and causes secondary pollution to environment, and ensure that the life-span of thin film。Therefore, SiO of the present invention2/Cu-Bi2O3Thin film can as a kind of effectively and the self-cleaning antifog material under visible ray can be applied to。
Summary of the invention
It is an object of the invention to provide a kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application。The present invention adopts sol-gel technology, prepares SiO by dip-coating method or spin coating method2/Cu-Bi2O3Thin film。Obtained thin film has good photocatalytic activity and Superhydrophilic, and uniform and stable wear-resisting。
The object of the invention is achieved through the following technical solutions:
A kind of Superhydrophilic self-cleaning antifog laminated film, described laminated film has double-decker, and including bottom film and surface layer film, bottom film is the Cu Bi modified2O3Thin film, surface layer film is mesoporous SiO2Thin film；In bottom film, the mol ratio of Cu and Bi is n (Cu): n (Bi)=3%～7%。
The preparation method of a kind of Superhydrophilic self-cleaning antifog laminated film, comprises the following steps:
(1) prepare Cu and modify Bi2O3Thin film (Cu-Bi2O3)；
(1.1) by 5-7.5g five nitric hydrate bismuth (Bi (NO3)3·5H2O) it is dissolved in 4.2-6.3mLHNO3In, it is subsequently added into 2-3g citric acid, 4-6mL triton x-100 (OP), 2-3mL polyethylene glycol 200 and 10-15mL acetone, after stirring 5-6h, adds copper sulfate pentahydrate (CuSO4·5H2O), it is stirred for 2-3h afterwards and namely obtains Cu-Bi2O3Colloidal sol；
(1.2) ordinary glass substrate is cleaned post-drying, ordinary glass substrate is cleaned post-drying, by step (1.1) described Cu-Bi2O3Colloidal sol, with film forming on glass substrate after cleaning of dip-coating method or spin coating method, is dried in electric heating constant-temperature blowing drying box and is obtained precursor film a；；
(1.3) precursor film a is calcined 4～5h at 450～550 DEG C of blowing airs, obtain Cu-Bi2O3Thin film;
(2) SiO is prepared2/Cu-Bi2O3Hierarchical composite thin film；
(2.1) tetraethyl orthosilicate (TEOS) is dissolved in dehydrated alcohol (EtOH), is added dropwise to polyoxyethylene (4) ether lauryl alcohol (Brij subsequentlyR30) with in the mixed liquor of hydrochloric acid, obtain the mixed liquor of reactant, then stirring obtain sol-gel precursor in heat collecting type constant-temperature heating magnetic stirring apparatus, i.e. SiO2Colloidal sol。
(2.2) adopt dip-coating method or spin coating method with step (2.1) described SiO2Colloidal sol is being coated with Cu-Bi2O3Plated film on the simple glass of thin film, dries in electric heating constant-temperature blowing drying box and obtains precursor film b；
(2.3) precursor film b is calcined 4～5h at 450～550 DEG C of blowing airs, obtain SiO2/Cu-Bi2O3Hierarchical composite thin film, i.e. a kind of Superhydrophilic self-cleaning antifog laminated film。
In said method, the stirring described in step (1.1), at 25～35 DEG C, is stirred with the stir speed (S.S.) of 15～25r/min。
In said method, it is n (Cu): n (Bi)=3%～7% that the described copper sulfate pentahydrate addition of step (1.1) meets mol ratio。
In said method, the drying described in step (1.2) is dry 20-40min at 80～100 DEG C。
In said method, the whipping temp of step (2.1) described stirring is 25～35 DEG C, and rotating speed is 15～25r/min。
In said method, the mol ratio of the reactant described in step (2.1) is tetraethyl orthosilicate: BrijR30: hydrochloric acid: dehydrated alcohol=8～32:0.9:1:50～100。
Gained Superhydrophilic self-cleaning antifog laminated film of the present invention is applied in self-cleaning antifog material。
Compared with prior art, the present invention has the advantage that
The technological process of the present invention is simple, operates fast and convenient, invests little, the SiO of gained2/Cu-Bi2O3Thin film is (1mw/cm under visible ray or low light condition2) namely show good photocatalytic activity, all can show good Superhydrophilic having, under non-illuminated conditions, and there is persistency；The thin film the prepared average transmittance in visible region is more than 90%；This thin film can as a kind of self-cleaning antifog material for needing the substrate of cleaning or antifog process。
Accompanying drawing explanation
Fig. 1 is the transmitance figure that surface scribbles the glass of thin film prepared by the present invention；
Fig. 2 a is Cu-Bi2O3The water contact angle photo of thin film, Fig. 2 b is SiO2/Cu-Bi2O3The water contact angle photo of thin film；
Fig. 3 is the SiO that surface scribbles prepared by the present invention2/Cu-Bi2O3The infrared spectrogram that the glass surface oleic acid of thin film changed with the UV Light time；
Fig. 4 is the Bi that surface scribbles prepared by the present invention2O3、Cu-Bi2O3、SiO2/Cu-Bi2O3The clearance of methyl orange is compared by thin film after visible ray light irradiates 5h。
Detailed description of the invention
Embodiment 1
The present invention adopts sol-gel technology。By 5g five nitric hydrate bismuth (Bi (NO3)3·5H2O) it is dissolved in 4.2mLHNO3In, it is subsequently added into 2g citric acid, 4mL triton x-100 (OP), 2mL polyethylene glycol 200 and 10mL acetone, after stirring 5h, adds copper sulfate pentahydrate (CuSO4·5H2O), it is stirred for (wherein mixing speed is 25r/min, and temperature is 30 DEG C) 3h afterwards and namely obtains the Cu-Bi that mol ratio is n (Cu): n (Bi)=5%2O3Colloidal sol；Tetraethyl orthosilicate (TEOS) is dissolved in dehydrated alcohol (EtOH), is added dropwise to polyoxyethylene (4) ether lauryl alcohol (Brij subsequentlyR30) with in the mixed liquor of hydrochloric acid, obtain the mixed liquor of reactant, then in heat collecting type constant-temperature heating magnetic stirring apparatus, stir (wherein mixing speed is 20r/min, and temperature is 30 DEG C) obtain SiO2Colloidal sol, wherein tetraethyl orthosilicate: BrijR30: hydrochloric acid: dehydrated alcohol=8:0.9:1:50 (mol ratio)。Dip-coating method (wherein pull rate is 0.5mm/s, and dip time is 30s) is adopted to make the Cu-Bi of n (Cu): n (Bi)=5% that prepare2O3Colloidal sol is uniformly distributed on common glass substrates, and the common glass substrates scribbling colloidal sol is dried in electric heating constant-temperature blowing drying box, the inherent 450 DEG C of blowing airs calcining 5h of Muffle furnace that is placed on obtain 5%Cu-Bi2O3Thin film, is again with, after taking out cooling, the SiO that dip-coating method (wherein pull rate is 1.5mm/s, and dip time is 60s) makes to prepare2Colloidal sol is evenly distributed on above-mentioned film surface, dries in electric heating constant-temperature blowing drying box, the inherent 450 DEG C of blowing airs calcining 5h of Muffle furnace that is placed on obtain SiO2/Cu-Bi2O3Thin film。
Embodiment 2
The present invention adopts sol-gel technology。By 6g five nitric hydrate bismuth (Bi (NO3)3·5H2O) it is dissolved in 5.5mLHNO3In, it is subsequently added into 2.5g citric acid, 5mL triton x-100 (OP), 2.5mL polyethylene glycol 200 and 13mL acetone, after stirring 5.5h, adds copper sulfate pentahydrate (CuSO4·5H2O), it is stirred for (wherein mixing speed is 20r/min, and temperature is 35 DEG C) 2.5h afterwards and namely obtains the Cu-Bi that mol ratio is n (Cu): n (Bi)=3%2O3Colloidal sol；Tetraethyl orthosilicate (TEOS) is dissolved in dehydrated alcohol (EtOH), is added dropwise to polyoxyethylene (4) ether lauryl alcohol (Brij subsequentlyR30) with in the mixed liquor of hydrochloric acid, obtain the mixed liquor of reactant, then in heat collecting type constant-temperature heating magnetic stirring apparatus, stir (wherein mixing speed is 25r/min, and temperature is 35 DEG C) obtain SiO2Colloidal sol, wherein tetraethyl orthosilicate: BrijR30: hydrochloric acid: dehydrated alcohol=24:0.9:1:75(mol ratio)。Dip-coating method (wherein pull rate is 1mm/s, and dip time is 45s) is adopted to make the 3%Cu-Bi prepared2O3Colloidal sol is uniformly distributed on common glass substrates, and the common glass substrates scribbling colloidal sol is dried in electric heating constant-temperature blowing drying box, the inherent 550 DEG C of blowing airs calcining 4h of Muffle furnace that is placed on obtain 3%Cu-Bi2O3Thin film, is again with, after taking out cooling, the SiO that spin coating method (wherein spin speed is 4000r/min, and spin coating time is 60s) makes to prepare2Colloidal sol is evenly distributed on above-mentioned film surface, and the common glass substrates scribbling colloidal sol is dried in electric heating constant-temperature blowing drying box, the inherent 550 DEG C of blowing airs calcining 4h of Muffle furnace that is placed on obtain SiO2/Cu-Bi2O3Thin film。
Embodiment 3
The present invention adopts sol-gel technology。By 7.5g five nitric hydrate bismuth (Bi (NO3)3·5H2O) it is dissolved in 6.3mLHNO3In, it is subsequently added into 3g citric acid, 6mL triton x-100 (OP), 3mL polyethylene glycol 200 and 15mL acetone, after stirring 6h, adds copper sulfate pentahydrate (CuSO4·5H2O), it is stirred for (wherein mixing speed is 15r/min, and temperature is 25 DEG C) 2h afterwards and namely obtains the Cu-Bi that mol ratio is n (Cu): n (Bi)=7%2O3Colloidal sol；Tetraethyl orthosilicate (TEOS) is dissolved in dehydrated alcohol (EtOH), is added dropwise to polyoxyethylene (4) ether lauryl alcohol (Brij subsequentlyR30) with in the mixed liquor of hydrochloric acid, obtain the mixed liquor of reactant, then in heat collecting type constant-temperature heating magnetic stirring apparatus, stir (wherein mixing speed is 15r/min, and temperature is 25 DEG C) obtain SiO2Colloidal sol, wherein tetraethyl orthosilicate: BrijR30: hydrochloric acid: dehydrated alcohol=32:0.9:1:100(mol ratio)。Spin coating method (wherein spin speed is 6000r/min, and spin coating time is 40s) is adopted to make the 7%Cu-Bi prepared2O3Colloidal sol is uniformly distributed on common glass substrates, and the common glass substrates scribbling colloidal sol is dried in electric heating constant-temperature blowing drying box, the inherent 500 DEG C of blowing airs calcining 5h of Muffle furnace that is placed on obtain 7%Cu-Bi2O3Thin film, is again with, after taking out cooling, the SiO that dip-coating method (wherein pull rate is 1mm/s, and dip time is 30s) makes to prepare2Colloidal sol is evenly distributed on above-mentioned film surface, dries in electric heating constant-temperature blowing drying box, the inherent 500 DEG C of blowing airs calcining 5h of Muffle furnace that is placed on obtain SiO2/Cu-Bi2O3Thin film。
Embodiment 4
Thin film obtained by the present invention all shows the good transparency。Test surface with uv-visible absorption spectra instrument (UV-vis) and scribble the transmitance of the glass substrate of thin film prepared by embodiment 1 in the present invention。Test result is shown in Fig. 1。Show that surface scribbles SiO2/Cu-Bi2O3The glass substrate of thin film has the good transparency at visible ray place, in visible region absorbance more than 75%。
Embodiment 5
Hydrophilicity analysis: adopt measurement water droplet contact angle on material to characterize surface and scribble SiO2/Cu-Bi2O3Thin film or Cu-Bi2O3The Superhydrophilic of film glass。Drip and scribble Cu-Bi on the surface of embodiment 1 preparation2O3On the glass of thin film, it can be observed that the water contact angle of film surface is about 39.2 ° (as shown in Figure 2 a)；And drip and scribble SiO on the surface of embodiment 1 preparation2/Cu-Bi2O3On the glass of thin film, its water contact angle is about 0 °, and (as shown in Figure 2 b) film exhibits goes out Superhydrophilic。
Embodiment 6
Self-cleaning is analyzed: by the SiO prepared by the stearic acid Experimental Characterization embodiment 1 on degradable film surface under irradiation under ultraviolet ray2/Cu-Bi2O3The self-cleaning of thin film。Surface is scribbled SiO2/Cu-Bi2O3On the glass drop of thin film, stearic methanol solution drying and processing is placed under ultraviolet light (1mw/cm2), infrared spectrogram that glass surface stearic acid changed with the UV Light time fig. 3, it is shown that when, after illumination 90min, stearic acid C-H stretching vibration absworption peak is wholly absent, illustrate stearic acid under irradiation under ultraviolet ray by SiO2/Cu-Bi2O3Film degradation, i.e. SiO2/Cu-Bi2O3Thin film has self-cleaning performance。
Embodiment 7
Photocatalytic activity is analyzed: employing methyl orange is model pollutant, compares surface and scribbles the photocatalytic activity of different thin film。Photocatalytic degradation reaction carries out in homemade photocatalytic reaction device, and thin film light-receiving area is 12.5cm2；Light source is 500W halogen tungsten lamp；Light intensity is 1mw/cm2；The initial concentration of methyl orange is 5mg/L；Halfhour dark adsorption reaction is first carried out before opening halogen tungsten lamp；By measuring the solution absorbance at 464nm wavelength place the clearance of combined standard curve calculating methyl orange: D=(C0-C)/C0× 100%, C0For the initial concentration of methyl orange, C is the concentration of t methyl orange。Test result indicate that, surface scribbles SiO2/Cu-Bi2O3The methyl orange of about 70% removed by the glass of thin film in 5h, is about pure Bi2O3About 2 times (Fig. 4) of thin film, show good photocatalytic activity。
Above example is only the condition restriction in order to technical scheme and non-critical to be described, those skilled in the art is to be understood that, it is possible in the spirit and scope not necessarily departing from claims invention defined, to it, its details or form are made various change。
Claims (7)
1. a Superhydrophilic self-cleaning antifog laminated film, it is characterised in that described laminated film has double-decker, including bottom film and surface layer film, bottom film is the Cu Bi modified2O3Thin film, surface layer film is mesoporous SiO2Thin film；In bottom film, the mol ratio of Cu and Bi is n (Cu): n (Bi)=3%～7%；
The preparation method of described laminated film, comprises the following steps:
(1) prepare Cu and modify Bi2O3Thin film；
(1.1) by 5-7.5g five nitric hydrate bismuth (Bi (NO3)3·5H2O) it is dissolved in 4.2-6.3mLHNO3In, it is subsequently added into 2-3g citric acid, 4-6mL triton x-100,2-3mL polyethylene glycol 200 and 10-15mL acetone, after stirring 5-6h, adds copper sulfate pentahydrate (CuSO4·5H2O), it is stirred for 2-3h afterwards and namely obtains Cu-Bi2O3Colloidal sol；
(1.2) ordinary glass substrate is cleaned post-drying, by step (1.1) described Cu-Bi2O3Colloidal sol, with film forming in ordinary glass substrate after cleaning of dip-coating method or spin coating method, is dried in electric heating constant-temperature blowing drying box and is obtained precursor film a；
(1.3) precursor film a is calcined 4～5h at 450～550 DEG C of blowing airs, obtain Cu-Bi2O3Thin film;
(2) SiO is prepared2/Cu-Bi2O3Hierarchical composite thin film；
(2.1) tetraethyl orthosilicate (TEOS) is dissolved in dehydrated alcohol (EtOH), it is added dropwise in the mixed liquor of polyoxyethylene (4) ether lauryl alcohol and hydrochloric acid subsequently, obtain the mixed liquor of reactant, in heat collecting type constant-temperature heating magnetic stirring apparatus, stirring obtains sol-gel precursor again, i.e. SiO2Colloidal sol；
(2.2) adopt dip-coating method or spin coating method with step (2.1) described SiO2Colloidal sol is being coated with Cu-Bi2O3Plated film on the simple glass of thin film, dries in electric heating constant-temperature blowing drying box and obtains precursor film b；
(2.3) precursor film b is calcined 4～5h at 450～550 DEG C of blowing airs, obtain SiO2/Cu-Bi2O3Hierarchical composite thin film, i.e. a kind of Superhydrophilic self-cleaning antifog laminated film。
2. Superhydrophilic self-cleaning antifog laminated film according to claim 1, it is characterised in that the stirring described in step (1.1), at 25～35 DEG C, is stirred with the stir speed (S.S.) of 15～25r/min。
3. Superhydrophilic self-cleaning antifog laminated film according to claim 1, it is characterised in that it is n (Cu): n (Bi)=3%～7% that the described copper sulfate pentahydrate addition of step (1.1) meets mol ratio。
4. Superhydrophilic self-cleaning antifog laminated film according to claim 1, it is characterised in that the drying described in step (1.2) is dry 20-40min at 80～100 DEG C。
5. Superhydrophilic self-cleaning antifog laminated film according to claim 1, it is characterised in that the whipping temp of step (2.1) described stirring is 25～35 DEG C, and rotating speed is 15～25r/min。
6. Superhydrophilic self-cleaning antifog laminated film according to claim 1, it is characterised in that the mol ratio of the reactant described in step (2.1) is tetraethyl orthosilicate: polyoxyethylene (4) ether lauryl alcohol: hydrochloric acid: dehydrated alcohol=8～32:0.9:1:50～100。
7. described in claim 1, Superhydrophilic self-cleaning antifog laminated film is applied in self-cleaning antifog material。
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| CN109437580B (en) * | 2018-11-20 | 2021-11-02 | 萍乡亨厚新材科技有限公司 | Hydrophilic antifogging and waterproof bead glass coating agent and coating method |
| CN111620562A (en) * | 2020-06-01 | 2020-09-04 | 九牧厨卫股份有限公司 | Antifouling glaze and antifouling ceramic with higher water contact angle and preparation method thereof |
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