CN101857381A - Preparation method of polystyrene microsphere template and method for preparing zinc oxide thin film - Google Patents
Preparation method of polystyrene microsphere template and method for preparing zinc oxide thin film Download PDFInfo
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Abstract
The invention belongs to the field of new energy of photoelectric materials, relates to a preparation method of a polystyrene microsphere template and simultaneously relates to a method for preparing an ordered porous zinc oxide thin film by utilizing the preparation method of the polystyrene microsphere template. The method comprises the following steps: firstly preparing polystyrene microsphere suspension, using the polystyrene microsphere suspension to moisten one surface of a substrate A, then placing the substrate A with the upward moistened surface underwater, leading polystyrene microspheres on the substrate A to diffuse on the water surface, being spontaneously assembled into a single-layer polystyrene microsphere thin film under the action of water surface tension, then transferring the single-layer polystyrene microsphere thin film onto a substrate B, and airing the substrate B for forming the polystyrene microsphere template. The method produces the polystyrene microsphere template by utilizing the self-assembly nature of the polystyrene microspheres under the action of the water surface tension, the preparation method is simple, time-saving and material-saving, and the prepared polystyrene microsphere template has the advantages of large area, ordered property and single layer, thereby providing the prior prerequisite for preparing materials with large-area porous ordered structures.
Description
Technical field
The invention belongs to the photoelectric material new energy field, relate to a kind of preparation method of polystyrene microsphere template, relate to a kind of method of utilizing the method for preparing polystyrene microsphere template to prepare ordered porous zinc-oxide film simultaneously.
Background technology
In recent years, microstructure is even owing to having, the convenient controlled very promising dye sensitization solar battery of a class or the light anode construction material of cartridge solar cell as thin as a wafer of becoming of hole dimension for the ordered porous structural material.The porous material of synthetic generally is divided into: poromerics (aperture＜2nm), mesoporous material (aperture is 2-50nm), large pore material (aperture＜1 μ m) and grand hole material (aperture＞1 μ m), wherein the ordered big hole material mainly is that close-packed array structure with mono-dispersion microballoon such as polystyrene microsphere (PS) or silicon dioxide microsphere is as template, pass through the filling transition process of sample presoma in the template sphere gap then, again template is removed at last and obtained the ordered big hole structured material.These ordered big hole materials have broad application prospects at aspects such as battery material, filtration and parting material, support of the catalyst and thermal resistance materials.The ordered big hole structure ZnO film has characteristics such as high visible light transmittance rate, high electron mobility, high IR specific refractory power, high electrochemical stability, nontoxic pollution-free, material source be extensive, therefore, be used widely in industry such as photovoltaic device, liquid-crystal display, transmitter, photochemical catalysis, surface acoustic wave device and technical field.
At present, people mainly utilize centrifugal or method such as gravity settling, vertical deposition, spin coating prepares polystyrene microsphere template, yet preceding two kinds of methods are consuming time and be difficult to prepare single tier templates, although and spin-coating method can be prepared the individual layer polystyrene microsphere template, but area is less, defective is more, thereby order is relatively poor, thereby directly influences the structure and the quality of final ordered big hole material such as ZnO film.
Summary of the invention
The present invention is directed at present centrifugal or settling methods and vertical deposition method are difficult to prepare the individual layer polystyrene microsphere template, and the preparation method that the single tier templates area is little, a difficult problem that order is relatively poor has proposed a kind of polystyrene microsphere template of spin-coating method preparation, this method is simple, can make large-area ordered individual layer polystyrene moulding.
Another object of the present invention is to utilize the preparation method of polystyrene microsphere template to prepare the method for ordered porous zinc-oxide film, finally can prepare the large-area ordered porous zinc bloom film of high quality.
The present invention is by the following technical solutions:
A kind of preparation method of polystyrene microsphere template, the steps include: that a preparation polystyrene microsphere massfraction is that 6-9%, water and ethanol volume ratio are 1: the polystyrene microsphere suspension of 0.9-1.2, with polystyrene microsphere suspension that the one side of substrate A is wetting, with skewed the inserting under water of wetting supine substrate A, the polystyrene microsphere on the substrate A spreads and the spontaneous individual layer polystyrene microsphere film that is assembled under the water surface tension effect at the water surface then; B inserts under the polystyrene microsphere film substrate B is skewed then, on carry substrate B and make the polystyrene microsphere film transfer to substrate B, the substrate B room temperature that is attached with the polystyrene microsphere film is dried the formation polystyrene microsphere template.
The diameter of described polystyrene microsphere is 345-375nm; Described substrate A is ITO substrate, FTO substrate, Si substrate or slide glass, and described substrate B is ITO substrate, FTO substrate, Si substrate or slide glass.
When inserting substrate A under water among the described step a, keeping the inclination angle of the substrate A and the water surface is 30-40 °, and the speed that substrate A inserts under water is 5-8cm/min.
Among the described step b substrate B inserted film following time, keeping the inclination angle of the substrate B and the water surface is 30-40 °, on carry substrate B speed be 20-30cm/min.
A kind of method for preparing ordered porous zinc-oxide film, the steps include: that a preparation polystyrene microsphere massfraction is that 6-9%, water and ethanol volume ratio are 1: the polystyrene microsphere suspension of 0.9-1.2, with polystyrene microsphere suspension that the one side of substrate A is wetting, with skewed the inserting under water of wetting supine substrate A, the polystyrene microsphere on the substrate A spreads and the spontaneous individual layer polystyrene microsphere film that is assembled under the water surface tension effect at the water surface then; B inserts under the polystyrene microsphere film substrate B is skewed then, on carry substrate B and make the polystyrene microsphere film transfer to substrate B, the substrate B room temperature that is attached with the polystyrene microsphere film is dried the formation polystyrene microsphere template; C prepares precursor sol, precursor sol is made into by two water zinc acetates, diethanolamine, dehydrated alcohol and water, concrete process for preparation is that two water zinc acetates are added in the dehydrated alcohol, 48-52 ℃ of heated and stirred to solution is emulsus, add diethanolamine then with amount of substances such as two water zinc acetates, treat that solution becomes water white transparency, in clear solution, be incorporated as the water of 2 times of two water zinc acetate amount of substances again, stir and be precursor sol; D floods polystyrene microsphere template in precursor sol, vertically pull out polystyrene microsphere template then and in drying at room temperature, 450-500 ℃ of annealing 2-2.5h removes polystyrene microsphere template then, reduces to room temperature naturally and obtains the ordered porous structural zinc-oxide film.
The volumetric molar concentration of two water zinc acetates is 0.2-0.6mol/L in the described precursor sol.
The diameter of described polystyrene microsphere is 345-375nm; Described substrate A is ITO substrate, FTO substrate, Si substrate or slide glass, and described substrate B is ITO substrate, FTO substrate, Si substrate or slide glass.
When inserting substrate A under water among the described step a, keeping the inclination angle of the substrate A and the water surface is 30-40 °, and the speed that substrate A inserts under water is 5-8cm/min.
Among the described step b substrate B inserted film following time, keeping the inclination angle of the substrate B and the water surface is 30-40 °, on carry substrate B speed be 20-30cm/min.
The speed of pulling out polystyrene microsphere template in the described steps d is 3-6cm/min, and heat-up rate is 1-2 ℃/min.
Utilization of the present invention utilizes polystyrene microsphere self-assembly property under the water surface tension effect to make polystyrene moulding, its principle is that polystyrene microsphere density is slightly less than the density of water, when microballoon is forming crooked concave meniscus between the microballoon after the diffusion on the water surface, at this moment, in order to reduce the surface energy at microballoon/water meter interface, reduce surface energy and realize being self-assembled into large-area ordered polystyrene microsphere film thereby draw close each other gradually at microballoon under the water surface tension effect; Adopting volume ratio is 1: 0.9-1.2 water and ethanol as solution-based at the bottom of, here dehydrated alcohol mainly plays the effect of the vaporator rate of regulating moisture, the density and the polystyrene microsphere density of secondly mixing the back mixed solution with water are more or less the same, and microballoon is suspended in the solvent.This method for preparing template of the present invention is simple, the province's material that saves time, and advantage large-area ordered, individual layer that obtained polystyrene moulding has is for preparation big area porous ordered structural material provides primary prerequisite.The individual layer polystyrene moulding that adopts preceding method to make also passes through suitable concn precursor sol filling template and removes template procedure, thereby can prepare area up to 1-2cm
2The porous ZnO film.
Polystyrene microsphere template as above-mentioned the inventive method preparation also can be used for the large-area ordered SnO of individual layer
2The preparation of porous membrane, CuO hemispherical Shell film and other metals or sull.
Description of drawings
Fig. 1 is the orderly polystyrene moulding SEM figure of the individual layer of preparation among the embodiment 1 (6000 times of magnifications);
Fig. 2 is the orderly polystyrene moulding low power of the individual layer SPM figure of preparation among the embodiment 1;
Fig. 3 is the orderly polystyrene moulding high power of the individual layer SPM figure of preparation among the embodiment 1;
Fig. 4 is the orderly polystyrene moulding ball of the individual layer size measuring SPM figure of preparation among the embodiment 1;
Fig. 5 is the orderly polystyrene moulding UV-vis of the individual layer transmitted light spectrogram of preparation among the embodiment 1;
The ordered porous ZnO film SEM figure (magnification 10000 times) of Fig. 6 for obtaining among the embodiment 2;
Fig. 7 is the individual layer ordered porous structural ZnO film low power SPM figure of preparation among the embodiment 2;
Fig. 8 is the individual layer ordered porous structural ZnO film high power SPM figure of preparation among the embodiment 2;
Fig. 9 is the individual layer ordered porous structural ZnO film film thickness test SPM figure of preparation among the embodiment 2;
Figure 10 is the individual layer ordered porous structural ZnO film XRD figure of preparation among the embodiment 2;
Figure 11 is the individual layer ordered porous structural ZnO film UV-vis transmitted light spectrogram of preparation among the embodiment 2;
The ordered porous ZnO film SEM figure (magnification 10000 times) of Figure 12 for obtaining among the embodiment 4;
The ordered porous ZnO film SEM figure (magnification 10000 times) of Figure 13 for obtaining among the embodiment 6.
Embodiment
At first prepare the polystyrene microsphere massfraction and be 8%, water and ethanol volume ratio are 1: 1 polystyrene microsphere suspension, the diameter of polystyrene microsphere is 345-375nm, and (one side of 1cm * 2cm) is evenly wetting with clean quiet slide glass with polystyrene microsphere suspension; Secondly will wetting supine slide glass one end contact with the water surface in the culture dish and go deep into downwards below the water surface with the speed of 5cm/min with 30 ° of inclination angles, the polystyrene microsphere on the slide glass spread on the water surface rapidly and came this moment, and the while is assembled into large-area ordered single thin film the spontaneous under the water surface tension effect at the interface of air and water; Afterwards, the ITO substrate of cleaning is inserted with 30 ° inclination angle carry film transfer to the ITO substrate on the speed with 20cm/min then below the single thin film; At last ITO substrate room temperature is dried, finally form the polystyrene microsphere template of high-sequential, characterization result is seen Fig. 1,2,3,4,5.It is regular in order wherein to observe the polystyrene microsphere template big area of 1 preparation of embodiment as can be seen by Fig. 1 SEM; It is adjacent with six other balls to observe each polystyrene microsphere by Fig. 2,3SPM microcell, forms close-packed structure, and it is 360nm that Fig. 4 records the microballoon mean diameter; Transmission paddy has appearred in the transmitted spectrum of Fig. 5 near 416nm, say also that from the side the polystyrene microsphere template of this embodiment preparation is regular in order.
At first, with the two water zinc acetate (CH of 0.04mol
6O
4Zn2H
2O) join the dehydrated alcohol (CH of 200ml
3CH
2OH) in, and 50 ℃ of heating follow magnetic agitation to treat that solution is emulsus, dropwise drip 0.04mol diethanolamine (C then
4H
11NO
2), treat that milk sap is water white transparency, drip three distilled water of 0.08mol again, stir 2h and get the precursor sol that volumetric molar concentration is 0.2mol/L; At last, the polystyrene microsphere template that embodiment 1 is made floods in precursor sol, slowly vertically pull out and drying at room temperature 30min with the speed of 4cm/min then, at last its 450 ℃ of annealing 2h in the controlled box-type furnace of temperature rise rate are removed template, finally obtain ordered porous ZnO film, characterization result is seen accompanying drawing 6,7,8,9,10,11.Fig. 6,7,8 as can be seen, ZnO film forms regular ordered porous structural.
At first prepare the polystyrene microsphere massfraction and be 6%, water and ethanol volume ratio are 1: 1.2 polystyrene microsphere suspension, the diameter of polystyrene microsphere is 345-375nm, and (one side of 1cm * 2cm) is evenly wetting with clean quiet Si substrate with polystyrene microsphere suspension; Secondly will wetting supine Si substrate one end contact with the water surface in the culture dish and go deep into downwards below the water surface with the speed of 6cm/min with 35 ° of inclination angles, polystyrene microsphere on this moment Si substrate spread on the water surface rapidly and comes, and the while is assembled into large-area ordered single thin film the spontaneous under the water surface tension effect at the interface of air and water; Afterwards, the slide glass of cleaning is inserted with 35 ° inclination angle carry film transfer to slide glass on the speed with 25cm/min then below the single thin film; At last the slide glass room temperature is dried, finally form the polystyrene microsphere template of high-sequential.
At first, with the two water zinc acetate (CH of 0.08mol
6O
4Zn2H
2O) join the dehydrated alcohol (CH of 200ml
3CH
2OH) in, and 48 ℃ of heating follow magnetic agitation to treat that solution is emulsus, dropwise drip 0.08mol diethanolamine (C then
4H
11NO
2), treat that milk sap is water white transparency, drip three distilled water of 0.16mol again, it is 0.4mol/L ZnO precursor sol that stirring 2h gets volumetric molar concentration; At last, the polystyrene microsphere template that embodiment 3 is made floods in precursor sol, slowly vertically pull out and drying at room temperature 40min with the speed of 3cm/min then, at last its 480 ℃ of annealing 2.3h in the controlled box-type furnace of temperature rise rate are removed template, finally obtain ordered porous ZnO film.ZnO film forms regular ordered porous structural as seen from Figure 12, and structure is tight.
Embodiment 5
At first prepare the polystyrene microsphere massfraction and be 9%, water and ethanol volume ratio are 1: 0.9 polystyrene microsphere suspension, the diameter of polystyrene microsphere is 345-375nm, and (one side of 1cm * 2cm) is evenly wetting with clean quiet ITO substrate with polystyrene microsphere suspension; Secondly will wetting supine ITO substrate one end contact with the water surface in the culture dish and go deep into downwards below the water surface with the speed of 8cm/min with 40 ° of inclination angles, polystyrene microsphere on this moment ITO substrate spread on the water surface rapidly and comes, and the while is assembled into large-area ordered single thin film the spontaneous under the water surface tension effect at the interface of air and water; Afterwards, the Si substrate of cleaning is inserted with 40 ° inclination angle carry film transfer to the Si substrate on the speed with 30cm/min then below the single thin film; At last Si substrate room temperature is dried, finally form the polystyrene microsphere template of high-sequential.
Embodiment 6
Two water zinc acetate (CH with 0.12mol
6O
4Zn2H
2O) join the dehydrated alcohol (CH of 200ml
3CH
2OH) in, and 52 ℃ of heating follow magnetic agitation to treat that solution is emulsus, dropwise drip 0.12mol diethanolamine (C then
4H
11NO
2), treat that milk sap is water white transparency, drip three distilled water of 0.24mol again, it is 0.6mol/L ZnO precursor sol that stirring 2h gets volumetric molar concentration; At last, the polystyrene microsphere template that embodiment 5 is made floods in precursor sol, slowly vertically pull out and drying at room temperature 50min with the speed of 6cm/min then, at last its 500 ℃ of annealing 2.5h in the controlled box-type furnace of temperature rise rate are removed template, finally obtain ordered porous ZnO film.Find out that by Figure 13 ZnO film forms regular ordered porous structural.
Laboratory apparatus of the present invention, SEM: the JSM-5600 scanning electron microscope that adopts Japanese JEOL company; SPM: the SPA400 that adopts NSK (S II); XRD: the X ' PertPro MPD diffractometer (Cu target K α) that adopts Dutch Philips company; UV-vis transmitted spectrum: the rHE λ IOS that adopts Britain UNICAM company.
Claims (10)
1. the preparation method of a polystyrene microsphere template, the steps include: that a preparation polystyrene microsphere massfraction is that 6-9%, water and ethanol volume ratio are 1: the polystyrene microsphere suspension of 0.9-1.2, with polystyrene microsphere suspension that the one side of substrate A is wetting, with skewed the inserting under water of wetting supine substrate A, the polystyrene microsphere on the substrate A spreads and the spontaneous individual layer polystyrene microsphere film that is assembled under the water surface tension effect at the water surface then; B inserts under the polystyrene microsphere film substrate B is skewed then, on carry substrate B and make the polystyrene microsphere film transfer to substrate B, the substrate B room temperature that is attached with the polystyrene microsphere film is dried the formation polystyrene microsphere template.
2. the preparation method of polystyrene microsphere template as claimed in claim 1, it is characterized in that: the diameter of described polystyrene microsphere is 345-375nm; Described substrate A is ITO substrate, FTO substrate, Si substrate or slide glass, and described substrate B is ITO substrate, FTO substrate, Si substrate or slide glass.
3. the preparation method of polystyrene microsphere template as claimed in claim 1 or 2 is characterized in that: when inserting substrate A under water among the described step a, keeping the inclination angle of the substrate A and the water surface is 30-40 °, and the speed that substrate A inserts under water is 5-8cm/min.
4. the preparation method of polystyrene microsphere template as claimed in claim 3 is characterized in that: among the described step b substrate B inserted film following time, keeping the inclination angle of the substrate B and the water surface is 30-40 °, on carry substrate B speed be 20-30cm/min.
5. method for preparing ordered porous zinc-oxide film, the steps include: that a preparation polystyrene microsphere massfraction is that 6-9%, water and ethanol volume ratio are 1: the polystyrene microsphere suspension of 0.9-1.2, with polystyrene microsphere suspension that the one side of substrate A is wetting, with skewed the inserting under water of wetting supine substrate A, the polystyrene microsphere on the substrate A spreads and the spontaneous individual layer polystyrene microsphere film that is assembled under the water surface tension effect at the water surface then; B inserts under the polystyrene microsphere film substrate B is skewed then, on carry substrate B and make the polystyrene microsphere film transfer to substrate B, the substrate B room temperature that is attached with the polystyrene microsphere film is dried the formation polystyrene microsphere template; C prepares precursor sol, precursor sol is made into by two water zinc acetates, diethanolamine, dehydrated alcohol and water, concrete process for preparation is that two water zinc acetates are added in the dehydrated alcohol, 48-52 ℃ of heated and stirred to solution is emulsus, add diethanolamine then with amount of substances such as two water zinc acetates, treat that solution becomes water white transparency, in clear solution, be incorporated as the water of 2 times of two water zinc acetate amount of substances again, stir and be precursor sol; D floods polystyrene microsphere template in precursor sol, vertically pull out polystyrene microsphere template then and in drying at room temperature, 450-500 ℃ of annealing 2-2.5h removes polystyrene microsphere template then, reduces to room temperature naturally and obtains the ordered porous structural zinc-oxide film.
6. prepare the method for ordered porous zinc-oxide film as the preparation method who utilizes claim 5 polystyrene microsphere template, it is characterized in that: the volumetric molar concentration of two water zinc acetates is 0.2-0.6mol/L in the described precursor sol.
7. prepare the method for ordered porous zinc-oxide film as the preparation method who utilizes claim 5 or 6 polystyrene microsphere templates, it is characterized in that: the diameter of described polystyrene microsphere is 345-375nm; Described substrate A is ITO substrate, FTO substrate, Si substrate or slide glass, and described substrate B is ITO substrate, FTO substrate, Si substrate or slide glass.
8. the method for preparing ordered porous zinc-oxide film as the preparation method who utilizes claim 7 polystyrene microsphere template, it is characterized in that: when inserting substrate A under water among the described step a, keeping the inclination angle of the substrate A and the water surface is 30-40 °, and the speed that substrate A inserts under water is 5-8cm/min.
9. the method for preparing ordered porous zinc-oxide film as the preparation method who utilizes claim 8 polystyrene microsphere template, it is characterized in that: among the described step b substrate B inserted film following time, keeping the inclination angle of the substrate B and the water surface is 30-40 °, on carry substrate B speed be 20-30cm/min.
10. prepare the method for ordered porous zinc-oxide film as the preparation method who utilizes claim 9 polystyrene microsphere template, it is characterized in that: the speed of pulling out polystyrene microsphere template in the described steps d is 3-6cm/min, and heat-up rate is 1-2 ℃/min.
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