CN104086092A - Super-hydrophilic self-cleaning antifogging composite film, and preparation method and application thereof - Google Patents

Super-hydrophilic self-cleaning antifogging composite film, and preparation method and application thereof Download PDF

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CN104086092A
CN104086092A CN201410304219.0A CN201410304219A CN104086092A CN 104086092 A CN104086092 A CN 104086092A CN 201410304219 A CN201410304219 A CN 201410304219A CN 104086092 A CN104086092 A CN 104086092A
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film
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cleaning
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sio
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CN104086092B (en
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胡芸
单文杰
韦朝海
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South China University of Technology SCUT
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Abstract

The invention discloses a super-hydrophilic self-cleaning antifogging composite film, and a preparation method and application thereof. The composite film has a two-layer structure and comprises a bottom film and a surface film, wherein the bottom film is a Cu-modified Bi2O3 film, and the surface film is a mesoporous SiO2 film. The preparation method comprises the following steps: coating a Cu-modified Bi2O3 film on the surface of common glass, drying the wet film, carrying out heat treatment in a muffle furnace, coating a mesoporous SiO2 film on the surface, and carrying the same treatment process to obtain the laminated composite film. The film has favorable photocatalytic activity under visible light or weak ultraviolet light, has super-hydrophilicity even under dark conditions, is colorless and transparent and has stable performance. The method has the advantages of simple equipment, low investment and no environment pollution; and the prepared film can be widely used on glass curtain walls, bathroom mirrors, automobile glass, optical instrument components and other substrates in need of self-cleaning antifogging treatment.

Description

A kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application
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 more and more subject to people's attention, and wherein, the cleaning problems of various indoor and outdoor material of construction (as cleaning of glass) has also caused widely thereupon and paid close attention to.When airborne contamination adhesion is on glass of building or automotive glazing, both reduced the transparence of glass, affect again attractive in appearance.In addition, during malaria condensation, easily in glass surface condensation, form many small water droplets, because the scattering process of these water droplets affects the light transmission of glass, to people, make troubles, particularly the overcast and rainy droplet forming on automobile rearview mirror has a strong impact on people's sight line, exists very large potential safety hazard.The solution that appears as these problems of Superhydrophilic self-cleaning material has brought Gospel.
The film material with function on the self-cleaning glass surface of having come into operation at present or having researched and developed is mainly with TiO 2or TiO 2with the mixture of other metals, metal oxide, nonmetal doping be main.Yet TiO 2low (the Eg=3.2 eV) of utilization ratio and lower quantum yield to sunlight, limited its practical application.Therefore, find or design and a kind ofly there is visible light-responded novel photocatalyst and be still full of challenge.Bi 2o 3because of its band gap narrow (approximately 2.8 eV), there is the advantages such as visible light-responded, oxygen room is many, photoresponse is rapid, oxidation capacity is strong, be considered at present one of the most promising novel photocatalyst.We are compound with it with the promotor of this effectively trapped electron of Cu ion, its light induced electron and hole are obtained effective separated, thereby significantly improve its photocatalysis efficiency.In addition, to there is the SiO of Superhydrophilic under dark condition 2film covers Cu-Bi 2o 3film surface, on the one hand due to mesoporous SiO 2the Superhydrophilic of film makes this film have anti-fog performance, has widened its Application Areas; On the other hand, due to surperficial SiO 2the existence of film makes Cu-Bi 2o 3the Cu ion of film is difficult for dissociating to environment and causes secondary pollution, and has guaranteed the life-span of film.Therefore, SiO of the present invention 2/ Cu-Bi 2o 3film can be used as a kind of effectively and can be applied to the self-cleaning antifog material under visible ray.
Summary of the invention
The object of the present invention is to provide a kind of Superhydrophilic self-cleaning antifog laminated film and preparation method thereof and application.The present invention adopts sol-gel technology, by dip-coating method or spin coating method, prepares SiO 2/ Cu-Bi 2o 3film.Prepared 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 Superhydrophilic self-cleaning antifog laminated film, described laminated film has bilayer structure, comprises bottom film and surface layer film, and bottom film is the Bi that Cu modifies 2o 3film, surface layer film is mesoporous SiO 2film; In bottom film, the mol ratio of Cu and Bi is n (Cu): n (Bi)=3%～7%.
A preparation method for Superhydrophilic self-cleaning antifog laminated film, comprises the following steps:
(1) prepare Cu and modify Bi 2o 3film (Cu-Bi 2o 3);
(1.1) by 5-7.5 g five nitric hydrate bismuth (Bi (NO 3) 35H 2o) be dissolved in 4.2-6.3 mL HNO 3in, then add 2-3 g citric acid, 4-6 mL triton x-100 (OP), 2-3 mL Macrogol 200 and 10-15 mL acetone, after stirring 5-6 h, add Salzburg vitriol (CuSO 45H 2o), stir again afterwards 2-3 h and obtain Cu-Bi 2o 3colloidal sol;
(1.2) ordinary glass substrate is cleaned to post-drying, ordinary glass substrate is cleaned to post-drying, by the described Cu-Bi of step (1.1) 2o 3colloidal sol is film forming on the glass substrate after cleaning with dip-coating method or spin coating method, in electric heating constant-temperature blowing drying box, dries and obtains precursor film a; ;
(1.3) precursor film a is calcined to 4～5 h at 450～550 ℃ of blowing airs, obtain Cu-Bi 2o 3film;
(2) prepare SiO 2/ Cu-Bi 2o 3hierarchical composite film;
(2.1) tetraethoxy (TEOS) is dissolved in dehydrated alcohol (EtOH), dropwise joins subsequently polyoxyethylene (4) ether lauryl alcohol (Brij r30) with the mixed solution of hydrochloric acid in, obtain the mixed solution of reactant, then stir and obtain sol-gel presoma, i.e. SiO in heat collecting type constant-temperature heating magnetic stirring apparatus 2colloidal sol.
(2.2) adopt dip-coating method or spin coating method with the described SiO of step (2.1) 2colloidal sol is being coated with Cu-Bi 2o 3plated film on the simple glass of film is dried and is obtained precursor film b in electric heating constant-temperature blowing drying box;
(2.3) precursor film b is calcined to 4～5 h at 450～550 ℃ of blowing airs, obtain SiO 2/ Cu-Bi 2o 3hierarchical composite film, i.e. a kind of Superhydrophilic self-cleaning antifog laminated film.
In aforesaid method, what step (1.1) was described is stirred in 25～35 ℃, with the stir speed (S.S.) stirring of 15～25 r/min.
In aforesaid method, it is n (Cu): n (Bi)=3%～7% that the described Salzburg vitriol add-on of step (1.1) meets mol ratio.
In aforesaid method, the described oven dry of step (1.2) is dry 20-40 min at 80～100 ℃.
In aforesaid method, the whipping temp of the described stirring of step (2.1) is 25～35 ℃, and rotating speed is 15～25 r/min.
In aforesaid method, the mol ratio of the reactant that step (2.1) is described is tetraethoxy: Brij r30: 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 following advantage:
Technical process of the present invention is simple, operate fast and convenient, invest little, the SiO of gained 2/ Cu-Bi 2o 3film is (1mw/cm under visible ray or low light condition 2) show good photocatalytic activity, having, without all showing good Superhydrophilic under illumination condition, and there is persistence; The average transmittance of the film making in visible region is more than 90 %; This film can be used as the matrix of a kind of self-cleaning antifog material or antifog processing clean for needs.
Accompanying drawing explanation
Fig. 1 is the surperficial transmitance figure that scribbles the glass of the prepared film of the present invention;
Fig. 2 a is Cu-Bi 2o 3the water contact angle photo of film, Fig. 2 b is SiO 2/ Cu-Bi 2o 3the water contact angle photo of film;
Fig. 3 is that surface scribbles SiO prepared by the present invention 2/ Cu-Bi 2o 3the infrared spectrogram that the glass surface oleic acid of film changed with the UV Light time;
Fig. 4 is that surface scribbles Bi prepared by the present invention 2o 3, Cu-Bi 2o 3, SiO 2/ Cu-Bi 2o 3film is the clearance comparison to tropeolin-D after visible ray rayed 5 h.
Embodiment
Embodiment 1
The present invention adopts sol-gel technology.By 5g five nitric hydrate bismuth (Bi (NO 3) 35H 2o) be dissolved in 4.2 mL HNO 3in, then add 2 g citric acids, 4 mL triton x-100s (OP), 2mL Macrogol 200 and 10 mL acetone, after stirring 5 h, add Salzburg vitriol (CuSO 45H 2o), stir again afterwards (wherein stirring velocity is 25 r/min, and temperature is 30 ℃) 3 h and obtain the Cu-Bi that mol ratio is n (Cu): n (Bi)=5% 2o 3colloidal sol; Tetraethoxy (TEOS) is dissolved in dehydrated alcohol (EtOH), dropwise joins subsequently polyoxyethylene (4) ether lauryl alcohol (Brij r30) with the mixed solution of hydrochloric acid in, obtain the mixed solution of reactant, then in heat collecting type constant-temperature heating magnetic stirring apparatus, stir (wherein stirring velocity is 20 r/min, and temperature is 30 ℃) and obtain SiO 2colloidal sol, wherein tetraethoxy: Brij r30: hydrochloric acid: dehydrated alcohol=8: 0.9: 1: 50 (mol ratio).Adopt dip-coating method (wherein pull rate is 0.5 mm/s, and dipping time is 30 s) to make the n (Cu) making: the Cu-Bi of n (Bi)=5% 2o 3colloidal sol is evenly distributed in common glass substrates, and the common glass substrates that scribbles colloidal sol is dried in electric heating constant-temperature blowing drying box, is placed in afterwards the inherent 450 ℃ of blowing airs of retort furnace and calcines 5 h and obtain 5%Cu-Bi 2o 3film, takes out after cooling and again adopts dip-coating method (wherein pull rate is 1.5 mm/s, and dipping time is 60 s) to make the SiO making 2colloidal sol is evenly distributed on above-mentioned film surface, in electric heating constant-temperature blowing drying box, dries, and is placed in afterwards the inherent 450 ℃ of blowing airs of retort furnace and calcines 5 h and obtain SiO 2/ Cu-Bi 2o 3film.
Embodiment 2
The present invention adopts sol-gel technology.By 6g five nitric hydrate bismuth (Bi (NO 3) 35H 2o) be dissolved in 5.5 mL HNO 3in, then add 2.5 g citric acids, 5 mL triton x-100s (OP), 2.5 mL Macrogol 200s and 13 mL acetone, after stirring 5.5 h, add Salzburg vitriol (CuSO 45H 2o), stir again afterwards (wherein stirring velocity is 20 r/min, and temperature is 35 ℃) 2.5 h and obtain the Cu-Bi that mol ratio is n (Cu): n (Bi)=3% 2o 3colloidal sol; Tetraethoxy (TEOS) is dissolved in dehydrated alcohol (EtOH), dropwise joins subsequently polyoxyethylene (4) ether lauryl alcohol (Brij r30) with the mixed solution of hydrochloric acid in, obtain the mixed solution of reactant, then in heat collecting type constant-temperature heating magnetic stirring apparatus, stir (wherein stirring velocity is 25 r/min, and temperature is 35 ℃) and obtain SiO 2colloidal sol, wherein tetraethoxy: Brij r30: hydrochloric acid: dehydrated alcohol=24: 0.9: 1: 75(mol ratio).Adopt dip-coating method (wherein pull rate is 1 mm/s, and dipping time is 45 s) to make the 3%Cu-Bi making 2o 3colloidal sol is evenly distributed in common glass substrates, and the common glass substrates that scribbles colloidal sol is dried in electric heating constant-temperature blowing drying box, is placed in afterwards the inherent 550 ℃ of blowing airs calcining of retort furnace 4h and obtains 3%Cu-Bi 2o 3film, takes out after cooling and again adopts spin coating method (wherein spin speed is 4000 r/min, and the even glue time is 60 s) to make the SiO making 2colloidal sol is evenly distributed on above-mentioned film surface, and the common glass substrates that scribbles colloidal sol is dried in electric heating constant-temperature blowing drying box, is placed in afterwards the inherent 550 ℃ of blowing airs calcining of retort furnace 4h and obtains SiO 2/ Cu-Bi 2o 3film.
Embodiment 3
The present invention adopts sol-gel technology.By 7.5g five nitric hydrate bismuth (Bi (NO 3) 35H 2o) be dissolved in 6.3 mL HNO 3in, then add 3 g citric acids, 6 mL triton x-100s (OP), 3 mL Macrogol 200s and 15 mL acetone, after stirring 6 h, add Salzburg vitriol (CuSO 45H 2o), stir again afterwards (wherein stirring velocity is 15 r/min, and temperature is 25 ℃) 2 h and obtain the Cu-Bi that mol ratio is n (Cu): n (Bi)=7% 2o 3colloidal sol; Tetraethoxy (TEOS) is dissolved in dehydrated alcohol (EtOH), dropwise joins subsequently polyoxyethylene (4) ether lauryl alcohol (Brij r30) with the mixed solution of hydrochloric acid in, obtain the mixed solution of reactant, then in heat collecting type constant-temperature heating magnetic stirring apparatus, stir (wherein stirring velocity is 15 r/min, and temperature is 25 ℃) and obtain SiO 2colloidal sol, wherein tetraethoxy: Brij r30: hydrochloric acid: dehydrated alcohol=32: 0.9: 1: 100(mol ratio).Adopt spin coating method (wherein spin speed is 6000 r/min, and the even glue time is 40 s) to make the 7%Cu-Bi making 2o 3colloidal sol is evenly distributed in common glass substrates, and the common glass substrates that scribbles colloidal sol is dried in electric heating constant-temperature blowing drying box, is placed in afterwards the inherent 500 ℃ of blowing airs of retort furnace and calcines 5 h and obtain 7%Cu-Bi 2o 3film, takes out after cooling and again adopts dip-coating method (wherein pull rate is 1 mm/s, and dipping time is 30 s) to make the SiO making 2colloidal sol is evenly distributed on above-mentioned film surface, in electric heating constant-temperature blowing drying box, dries, and is placed in afterwards the inherent 500 ℃ of blowing airs of retort furnace and calcines 5 h and obtain SiO 2/ Cu-Bi 2o 3film.
Embodiment 4
The prepared film of the present invention all shows the good transparency.With uv-visible absorption spectra instrument (UV-vis), tested the surperficial transmitance that scribbles the glass substrate of embodiment 1 prepared film in the present invention.Test result is shown in Fig. 1.Shown that surface scribbles SiO 2/ Cu-Bi 2o 3the glass substrate of film has the good transparency at visible ray place, in visible region transmissivity more than 75%.
Embodiment 5
Hydrophilicity analysis: adopt the contact angle of measurement water droplet on material to come characterization of surfaces to scribble SiO 2/ Cu-Bi 2o 3film or Cu-Bi 2o 3the Superhydrophilic of film glass.Drip and scribble Cu-Bi on the surface of embodiment 1 preparation 2o 3film on glass, the water contact angle that can observe film surface is about 39.2 ° (as shown in Figure 2 a); And drip, on the surface of embodiment 1 preparation, scribble SiO 2/ Cu-Bi 2o 3film on glass, its water contact angle is about 0 °, and (as shown in Figure 2 b) film shows Superhydrophilic.
Embodiment 6
Self-cleaning is analyzed: by the prepared SiO of the stearic acid Experimental Characterization embodiment 1 on degradable film surface under UV-irradiation 2/ Cu-Bi 2o 3the self-cleaning of film.Surface is scribbled to SiO 2/ Cu-Bi 2o 3on the glass drop of film, stearic methanol solution drying and processing is placed on (1 mw/cm under UV-light 2), the infrared spectrogram that glass surface stearic acid changed with the UV Light time as shown in Figure 3, can find out, after illumination 90 min, the completely dissolve of stearic acid C-H stretching vibration absorption peak, illustrate stearic acid under UV-irradiation by SiO 2/ Cu-Bi 2o 3film degradation, i.e. SiO 2/ Cu-Bi 2o 3film has self-cleaning performance.
Embodiment 7
Photocatalytic activity is analyzed: employing tropeolin-D is model pollutant, has compared the surperficial photocatalytic activity that scribbles different films.Photocatalytic degradation reaction is carried out in homemade photocatalytic reaction device, and film light-receiving area is 12.5 cm 2; Light source is 500 W halogen tungsten lamps; Light intensity is 1 mw/cm 2; The starting point concentration of tropeolin-D is 5 mg/L; Before opening halogen tungsten lamp, first carry out halfhour dark absorption reaction; By measuring solution at the absorbance at 464 nm wavelength places the clearance of combined standard curve calculation tropeolin-D: D=(C 0-C)/C 0* 100%, C 0for the starting point concentration of tropeolin-D, C is the t concentration of tropeolin-D constantly.Experimental result shows, surface scribbles SiO 2/ Cu-Bi 2o 3the glass of film is removed the tropeolin-D of 70% left and right in 5 h, is about pure Bi 2o 32 times of left and right (Fig. 4) of film, show good photocatalytic activity.
Above embodiment illustrates technical scheme of the present invention but not strict condition restriction, the ordinary person of this area should be appreciated that and can to its details or form, to it, make various variations not departing from the spirit and scope of the present invention that claims limit.

Claims (8)

1. a Superhydrophilic self-cleaning antifog laminated film, is characterized in that, described laminated film has bilayer structure, comprises bottom film and surface layer film, and bottom film is the Bi that Cu modifies 2o 3film, surface layer film is mesoporous SiO 2film; In bottom film, the mol ratio of Cu and Bi is n (Cu): n (Bi)=3%～7%.
2. the preparation method of Superhydrophilic self-cleaning antifog laminated film claimed in claim 1, is characterized in that, comprises the following steps:
(1) prepare Cu and modify Bi 2o 3film (Cu-Bi 2o 3);
(1.1) by 5-7.5 g five nitric hydrate bismuth (Bi (NO 3) 35H 2o) be dissolved in 4.2-6.3 mL HNO 3in, then add 2-3 g citric acid, 4-6 mL triton x-100 (OP), 2-3 mL Macrogol 200 and 10-15 mL acetone, after stirring 5-6 h, add Salzburg vitriol (CuSO 45H 2o), stir again afterwards 2-3 h and obtain Cu-Bi 2o 3colloidal sol;
(1.2) ordinary glass substrate is cleaned to post-drying, by the described Cu-Bi of step (1.1) 2o 3colloidal sol is film forming in the ordinary glass substrate after cleaning with dip-coating method or spin coating method, in electric heating constant-temperature blowing drying box, dries and obtains precursor film a;
(1.3) precursor film a is calcined to 4～5 h at 450～550 ℃ of blowing airs, obtain Cu-Bi 2o 3film;
(2) prepare SiO 2/ Cu-Bi 2o 3hierarchical composite film;
(2.1) tetraethoxy (TEOS) is dissolved in dehydrated alcohol (EtOH), dropwise joins subsequently polyoxyethylene (4) ether lauryl alcohol (Brij r30) with the mixed solution of hydrochloric acid in, obtain the mixed solution of reactant, then stir and obtain sol-gel presoma, i.e. SiO in heat collecting type constant-temperature heating magnetic stirring apparatus 2colloidal sol;
(2.2) adopt dip-coating method or spin coating method with the described SiO of step (2.1) 2colloidal sol is being coated with Cu-Bi 2o 3plated film on the simple glass of film is dried and is obtained precursor film b in electric heating constant-temperature blowing drying box;
(2.3) precursor film b is calcined to 4～5 h at 450～550 ℃ of blowing airs, obtain SiO 2/ Cu-Bi 2o 3hierarchical composite film, i.e. a kind of Superhydrophilic self-cleaning antifog laminated film.
3. the preparation method of Superhydrophilic self-cleaning antifog laminated film according to claim 2, is characterized in that, what step (1.1) was described is stirred in 25～35 ℃, with the stir speed (S.S.) stirring of 15～25 r/min.
4. the preparation method of Superhydrophilic self-cleaning antifog laminated film according to claim 2, is characterized in that, it is n (Cu): n (Bi)=3%～7% that the described Salzburg vitriol add-on of step (1.1) meets mol ratio.
5. the preparation method of Superhydrophilic self-cleaning antifog laminated film according to claim 2, is characterized in that, the described oven dry of step (1.2) is dry 20-40 min at 80～100 ℃.
6. the preparation method of Superhydrophilic self-cleaning antifog laminated film according to claim 2, is characterized in that, the whipping temp of the described stirring of step (2.1) is 25～35 ℃, and rotating speed is 15～25 r/min.
7. the preparation method of Superhydrophilic self-cleaning antifog laminated film according to claim 2, is characterized in that, the mol ratio of the reactant that step (2.1) is described is tetraethoxy: Brij r30: hydrochloric acid: dehydrated alcohol=8～32: 0.9: 1: 50～100.
8. described in claim 1, Superhydrophilic self-cleaning antifog laminated film is applied in self-cleaning antifog material.
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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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