CN102219557B - Preparation method of patterned zinc oxide film - Google Patents
Preparation method of patterned zinc oxide film Download PDFInfo
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- CN102219557B CN102219557B CN201110095122A CN201110095122A CN102219557B CN 102219557 B CN102219557 B CN 102219557B CN 201110095122 A CN201110095122 A CN 201110095122A CN 201110095122 A CN201110095122 A CN 201110095122A CN 102219557 B CN102219557 B CN 102219557B
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Abstract
The invention belongs to the technical field of nanoprocessing and in particular relates to a method for preparing a patterned zinc oxide nanofilm by a nanoimprint technology. The method mainly comprises the following steps of: preparing a colloidal ball template; preparing a polydimethylsiloxane negative type structure soft template; preparing zinc oxide precursor sol; and preparing the patterned zinc oxide film by the nanoimprint technology. In the method, the templates required by nanoimprint are assembled by a self-assembling technology; the zinc oxide precursor sol serves as a barrier layer; and nanoimprint process parameters are controlled, so that the sol is converted into gel in the impressing process and the patterned zinc oxide film is directly impressed without subsequent etching process. The method is high in repeatability. By the method, the patterned oxide films can be prepared on a large scale and under the conditions of high efficiency and low price.
Description
Technical field
The invention belongs to technical field of nano-processing, be specifically related to a kind of method of utilizing nanometer embossing to prepare the patterning zinc oxide nano film.
Background technology
Zinc oxide (ZnO) is a kind of novel broad stopband direct band gap II-VI family semi-conducting material; Energy gap under the room temperature is 3.37 eV; Exciton bind energy is widely used in short-wavelength light electric devices such as development high efficient LED (LED), ultraviolet detector up to 60 meV.In solar battery process, the patterning nano-ZnO thin film can improve the light transmission rate of visible region, and can improve its conductivity through mixing, and is the excellent structural material as window layer of solar battery and top electrode.Technology such as traditional ZnO film preparation method such as magnetron sputtering can only be made the film of planar structure; And the cost-effective rate of preparation nano-patterning structures such as traditional nanometer micro-processing technology such as photoetching, electron beam lithography EBL, ion beam etching IBL is low, can not be on a large scale, high efficiency, prepare the film of nano-patterning at low cost.
Nanometer embossing was at first proposed by professor chou of Princeton University in nineteen ninety-five; The template that its utilization has a figure utilize mechanical force with design transfer to polymer latex; With other photoetching techniques such as EBL; IBL etc. compare, and nano impression is the figure transfer technology of a kind of high yield, cheapness, and resolution is also high can be reached below 10 nm.Fields such as microelectronic component, biological detection, precision optics have been widely used in through ten years development.
The employed template resolution of nano impression has determined the resolution of pattern on the polymer, and the acquisition of high-quality template still is a more formidable problem.Template construct method the most commonly used at present is the ion etching of e-beam direct-writing exposure association reaction, and is with high costs, inefficiency.More importantly be, nanometer embossing mainly is that die plate pattern is transferred on the thin polymer film, also need utilize subsequent techniques such as etching, vapor deposition to realize the patterning to other metals, semi-conducting material, and process is complicated.
Summary of the invention
The object of the present invention is to provide the preparation method of the high patterning zinc-oxide film of a kind of repeatability.
The present invention adopts following technical scheme:
The preparation method of patterning zinc-oxide film may further comprise the steps:
(1) preparation colloidal spheres template: polystyrene spheres suspension is splashed in the deionized water; The self assembly of gas-liquid interface place forms one deck polystyrene film; Then polystyrene film is transferred in the substrate; The dry colloidal spheres template that gets, dry purpose are to remove unnecessary solvent to strengthen the tackness of polystyrene film and substrate;
(2) preparation dimethyl silicone polymer minus structure soft template:, vacuumize and slough bubble with dimethyl silicone polymer and curing agent mixing; With octadecyl trichlorosilane solution the colloidal spheres template is soaked 10-30s; During with the dimethyl silicone polymer template demoulding avoiding solidifying and the colloidal spheres template stick together; Mixture with dimethyl silicone polymer and curing agent is cast on the colloidal spheres template then; Heating in vacuum is solidified, and the dimethyl silicone polymer layer is taken off obtaining dimethyl silicone polymer minus structure soft template from the colloidal spheres template;
(3) preparation zinc oxide precursor colloidal sol: zinc nitrate, zinc chloride or zinc sulfate are dissolved in the solvent; Adding gets water white zinc oxide precursor colloidal sol as the polyacrylic acid mixing that increases steady agent and chelating agent, and zinc oxide precursor colloidal sol is spun to silicon chip surface;
(4) preparation patterning zinc-oxide film: adopt nanometer embossing that dimethyl silicone polymer minus structure soft template is stamped on the zinc oxide precursor colloidal sol that is spin-coated on the silicon chip as seal, promptly get the patterning zinc-oxide film.
The detailed process of said step (1) is: use glue head dropper to draw the polystyrene spheres hanging drop to slide; Then slide one end is contacted with the deionized water water surface with inclination angle 20-30 ° and slowly go deep into water surface below; PS suspension on the slide spreads on the water surface rapidly and comes at this moment, is self-assembled into the individual layer polystyrene film at the gas-liquid interface place simultaneously; Insert PS single thin film below with the direction that is parallel to liquid level substrate then and move slowly polystyrene film is transferred in the substrate, 80-120 ℃ of dry colloidal spheres template.
In the said step (1) during the polystyrene spheres suspension preparation with polystyrene spheres water-soluble with ethanol mixed solvent in; The mass percent of polystyrene spheres is 1-5% in the polystyrene spheres suspension; The mass ratio of water and ethanol is 1:1-3; The sphere diameter of polystyrene spheres is 100-500nm, and substrate is silicon chip or quartz.
The mass ratio of dimethyl silicone polymer and curing agent is 5-10:1 in the said step (2), and the mass concentration of octadecyl trichlorosilane solution is 0.1-1%, and the temperature of heating in vacuum is 80-120 ℃, and vacuum degree is 10
-3-10
-4Pa, the time is 30-60 min.
Solvent is deionized water, diethanol amine and two kinds of equal-volumes in the EGME compare mixed solution in the said step (3); Polyacrylic acid is 1:1-2 with the amount of substance ratio of zinc ion; Speed during spin coating is 1000-5000 rpm, and thickness is approximately 50-150 nm.
The condition of nano impression is in the said step (4): temperature 100-150 ℃, and pressure 5-30 * 10
5Pa, retention time 10-30 min, chilling temperature are 50-80 ℃.
The present invention selects for use polyacrylic acid as steady agent of increasing of zinc oxide precursor colloidal sol and chelating agent, and this is that the Tg vitrification point is 102 ℃ because polyacrylic acid PAA is the polymerizing acrylic acid thing; It is a kind of water-soluble polymer; Contain a large amount of carboxyls in the PAA molecule, can react, also can dewater, degraded and complex reaction with alkali, alcohol, amine; Can make thickener, dispersant, flocculant, adhesive and film forming agent etc.; PAA is soluble in water and can form stable compound with metal ion, metal ion is evenly disperseed, in the colloidal sol precursor in the hot padding process; When heating temperature is higher than the vitrification point of PAA PAA be converted into solid-state, the micro-nano structure after can effectively keeping impressing.
The present invention utilizes the self-assembling technique assemble nanometer to impress required template; As the barrier layer, the technological parameter of control nano impression makes colloidal sol in moulding process, be converted into gel with zinc oxide precursor colloidal sol; Need not subsequent etching technology, directly impress out the zinc-oxide film of patterning.The inventive method is repeatable high, can be on a large scale, high efficiency, cheap preparation patterning zinc-oxide film.
Description of drawings
Fig. 1 utilizes nano impression and sol-gel technique to prepare the flow chart of patterning zinc-oxide film with the colloidal spheres template as template in being;
Fig. 2 is the surface topography map of the colloidal spheres template of embodiment 2 original sizes 300 nm;
Fig. 3 is the surface topography map of the dimethyl silicone polymer minus structure soft template of embodiment 2 original sizes 300 nm;
Fig. 4 is the surface topography map of the colloidal spheres template of embodiment 3 original sizes 500 nm;
Fig. 5 is the surface topography map of the dimethyl silicone polymer minus structure soft template of embodiment 3 original sizes 500 nm;
Fig. 6 is the surface topography map of embodiment 2 patterning zinc-oxide films;
Fig. 7 is the 3 dimensional drawing of embodiment 2 patterning zinc-oxide films.
Embodiment
The preparation method of patterning zinc-oxide film may further comprise the steps:
(1) preparation colloidal spheres template
The preparation of a, polystyrene spheres suspension, with polystyrene spheres water-soluble with ethanol mixed solvent in, the mass percent of polystyrene spheres is 1% in the polystyrene spheres suspension, the mass ratio of water and ethanol is 1:1, the sphere diameter of polystyrene spheres is 100nm;
B, use glue head dropper are drawn the polystyrene spheres hanging drop to slide; Then slide one end is contacted with the deionized water water surface with 20 ° at inclination angle and slowly go deep into water surface below; PS suspension on the slide spreads on the water surface rapidly and comes at this moment, is self-assembled into the individual layer polystyrene film at the gas-liquid interface place simultaneously; Insert PS single thin film below with the direction that is parallel to liquid level quartz substrate then and move slowly polystyrene film is transferred in the substrate; 90 ℃ of dry colloidal spheres templates that get, dry purpose are to remove unnecessary solvent to strengthen the tackness of polystyrene film and substrate;
(2) preparation dimethyl silicone polymer minus structure soft template
With dimethyl silicone polymer and curing agent mixing, the mass ratio of dimethyl silicone polymer and curing agent is 5:1, vacuumizes and sloughs bubble; Using mass concentration is that 0.1% octadecyl trichlorosilane solution soaks 10s to the colloidal spheres template; During with the dimethyl silicone polymer template demoulding avoiding solidifying and the colloidal spheres template stick together, the mixture with dimethyl silicone polymer and curing agent is cast on the colloidal spheres template then, heating in vacuum is solidified; The temperature of heating in vacuum is 80 ℃, and vacuum degree is 10
-3Pa, the time is 30min, the dimethyl silicone polymer layer is taken off obtaining dimethyl silicone polymer minus structure soft template from the colloidal spheres template;
(3) preparation zinc oxide precursor colloidal sol
Zinc nitrate is dissolved in the solvent; Solvent be deionized water with the equal-volume of diethanol amine than mixed solution, add as the polyacrylic acid mixing that increases steady agent and chelating agent and get water white zinc oxide precursor colloidal sol, zinc ion concentration is 10mM in the colloidal sol; Polyacrylic acid is 1:1 with the amount of substance ratio of zinc ion; Zinc oxide precursor colloidal sol is spun to silicon chip surface, and the speed during spin coating is 1000 rpm, and thickness is approximately 50nm;
(4) preparation patterning zinc-oxide film
Adopt nanometer embossing that dimethyl silicone polymer minus structure soft template is stamped on the zinc oxide precursor colloidal sol that is spin-coated on the silicon chip as seal, the condition of nano impression is: 100 ℃ of temperature, pressure 5 * 10
5Pa, retention time 10min, chilling temperature are 50 ℃, promptly get the patterning zinc-oxide film.
The preparation method of patterning zinc-oxide film may further comprise the steps:
(1) preparation colloidal spheres template
The preparation of a, polystyrene spheres suspension, with polystyrene spheres water-soluble with ethanol mixed solvent in, the mass percent of polystyrene spheres is 3% in the polystyrene spheres suspension, the mass ratio of water and ethanol is 1:2, the sphere diameter of polystyrene spheres is 300nm;
B, use glue head dropper are drawn the polystyrene spheres hanging drop to slide; Then slide one end is contacted with the deionized water water surface with 25 ° at inclination angle and slowly go deep into water surface below; PS suspension on the slide spreads on the water surface rapidly and comes at this moment, is self-assembled into the individual layer polystyrene film at the gas-liquid interface place simultaneously; Then with inserting below the PS single thin film with the direction that is parallel to liquid level at the bottom of the silicon wafer-based and moving slowly polystyrene film is transferred in the substrate; 80 ℃ of dry colloidal spheres templates that get, dry purpose are to remove unnecessary solvent to strengthen the tackness of polystyrene film and substrate; The surface topography map of colloidal spheres template is as shown in Figure 2; Fig. 2 finds out that the individual layer PS colloidal state ball that adopts the rete transfer method to obtain arranges with hexagonal tight structure (hcp); Strict the colloidal state bulb diameter is 306 nm by same planar alignment, and adjacent two ball center distance is respectively 368 nm; Smooth surface, at interval evenly;
(2) preparation dimethyl silicone polymer minus structure soft template
With dimethyl silicone polymer and curing agent mixing, the mass ratio of dimethyl silicone polymer and curing agent is 8:1, vacuumizes and sloughs bubble; Using mass concentration is that 0.5% octadecyl trichlorosilane solution soaks 20s to the colloidal spheres template; During with the dimethyl silicone polymer template demoulding avoiding solidifying and the colloidal spheres template stick together, the mixture with dimethyl silicone polymer and curing agent is cast on the colloidal spheres template then, heating in vacuum is solidified; The temperature of heating in vacuum is 100 ℃, and vacuum degree is 10
-3Pa, the time is 45min, the dimethyl silicone polymer layer is taken off obtaining dimethyl silicone polymer minus structure soft template from the colloidal spheres template; The surface topography map of dimethyl silicone polymer minus structure soft template is as shown in Figure 3; Fig. 3 finds out that dimethyl silicone polymer minus structure soft template surface is made up of the hole of hexagonal solid matter; Adjacent two hole centre distances are 335 nm, and the hole degree of depth is 70 nm, because dimethyl silicone polymer is an organic polymer; When characterization is placed sample, can make the surface that certain elastic deformation is arranged, cause hole size shown in the figure that some differences and distortion are arranged;
(3) preparation zinc oxide precursor colloidal sol
Zinc sulfate is dissolved in the solvent; Solvent be deionized water with the EGME equal-volume than mixed solution, add as the polyacrylic acid mixing that increases steady agent and chelating agent and get water white zinc oxide precursor colloidal sol, zinc ion concentration is 60 mM in the colloidal sol; Polyacrylic acid is 1:1.5 with the amount of substance ratio of zinc ion; Zinc oxide precursor colloidal sol is spun to silicon chip surface, and the speed during spin coating is 3000 rpm, and thickness is approximately 100nm;
(4) preparation patterning zinc-oxide film
Adopt nanometer embossing that dimethyl silicone polymer minus structure soft template is stamped on the zinc oxide precursor colloidal sol that is spin-coated on the silicon chip as seal, the condition of nano impression is: 130 ℃ of temperature, pressure 20 * 10
5Pa, retention times 20 min, chilling temperature are 65 ℃, promptly get the patterning zinc-oxide film.The surface topography map of patterning zinc-oxide film is as shown in Figure 6, and 3 dimensional drawing is as shown in Figure 7, and Fig. 6,7 finds out that patterning zinc-oxide film array structure diameter is approximately 277 nm; Highly be 50 nm; Vertical height ratio is big, and pattern edge is level and smooth, the more complete pattern that has duplicated the PDMS template.
The preparation method of patterning zinc-oxide film may further comprise the steps:
(1) preparation colloidal spheres template
The preparation of a, polystyrene spheres suspension, with polystyrene spheres water-soluble with ethanol mixed solvent in, the mass percent of polystyrene spheres is 5% in the polystyrene spheres suspension, the mass ratio of water and ethanol is 1:3, the sphere diameter of polystyrene spheres is 500nm;
B, use glue head dropper are drawn the polystyrene spheres hanging drop to slide; Then slide one end is contacted with the deionized water water surface with 30 ° at inclination angle and slowly go deep into water surface below; PS suspension on the slide spreads on the water surface rapidly and comes at this moment, is self-assembled into the individual layer polystyrene film at the gas-liquid interface place simultaneously; Insert PS single thin film below with the direction that is parallel to liquid level quartz substrate then and move slowly polystyrene film is transferred in the substrate; 120 ℃ of dry colloidal spheres templates that get, dry purpose are to remove unnecessary solvent to strengthen the tackness of polystyrene film and substrate; The surface topography map of colloidal spheres template is as shown in Figure 4, and Fig. 4 finds out that the colloidal state bulb diameter is 517 nm, and adjacent two ball center distance is respectively 551 nm, smooth surface, at interval evenly;
(2) preparation dimethyl silicone polymer minus structure soft template
With dimethyl silicone polymer and curing agent mixing, the mass ratio of dimethyl silicone polymer and curing agent is 10:1, vacuumizes and sloughs bubble; Using mass concentration is that 1% octadecyl trichlorosilane solution soaks 30s to the colloidal spheres template; During with the dimethyl silicone polymer template demoulding avoiding solidifying and the colloidal spheres template stick together, the mixture with dimethyl silicone polymer and curing agent is cast on the colloidal spheres template then, heating in vacuum is solidified; The temperature of heating in vacuum is 120 ℃, and vacuum degree is 10
-4Pa, the time is 60 min, the dimethyl silicone polymer layer is taken off obtaining dimethyl silicone polymer minus structure soft template from the colloidal spheres template; The surface topography map of dimethyl silicone polymer minus structure soft template is as shown in Figure 5, and Fig. 5 finds out that dimethyl silicone polymer minus structure soft template surface is made up of the hole of hexagonal solid matter, and adjacent two hole centre distances are 552 nm, and the hole degree of depth is 150 nm;
(3) preparation zinc oxide precursor colloidal sol
Zinc chloride is dissolved in the solvent; Solvent be diethanol amine with the EGME equal-volume than mixed solution, add as the polyacrylic acid mixing that increases steady agent and chelating agent and get water white zinc oxide precursor colloidal sol, zinc ion concentration is 100 mM in the colloidal sol; Polyacrylic acid is 1:2 with the amount of substance ratio of zinc ion; Zinc oxide precursor colloidal sol is spun to silicon chip surface, and the speed during spin coating is 5000 rpm, and thickness is approximately 150 nm;
(4) preparation patterning zinc-oxide film
Adopt nanometer embossing that dimethyl silicone polymer minus structure soft template is stamped on the zinc oxide precursor colloidal sol that is spin-coated on the silicon chip as seal, the condition of nano impression is: 150 ℃ of temperature, pressure 30 * 10
5Pa, retention times 30 min, chilling temperature are 80 ℃, promptly get the patterning zinc-oxide film.
Claims (6)
1. the preparation method of patterning zinc-oxide film is characterized in that: may further comprise the steps:
(1) preparation colloidal spheres template: polystyrene spheres suspension is splashed in the deionized water, and the self assembly of gas-liquid interface place forms one deck polystyrene film, then polystyrene film is transferred in the substrate, the dry colloidal spheres template that gets;
(2) preparation dimethyl silicone polymer minus structure soft template:, vacuumize and slough bubble with dimethyl silicone polymer and curing agent mixing; With octadecyl trichlorosilane solution the colloidal spheres template is soaked 10-30s; Mixture with dimethyl silicone polymer and curing agent is cast on the colloidal spheres template then; Heating in vacuum is solidified, and the dimethyl silicone polymer layer is taken off obtaining dimethyl silicone polymer minus structure soft template from the colloidal spheres template;
(3) preparation zinc oxide precursor colloidal sol: zinc nitrate, zinc chloride or zinc sulfate are dissolved in the solvent, add the polyacrylic acid mixing and get zinc oxide precursor colloidal sol, zinc oxide precursor colloidal sol is spun to silicon chip surface;
(4) preparation patterning zinc-oxide film: adopt nanometer embossing that dimethyl silicone polymer minus structure soft template is stamped on the zinc oxide precursor colloidal sol that is spin-coated on the silicon chip as seal, promptly get the patterning zinc-oxide film.
2. the preparation method of patterning zinc-oxide film as claimed in claim 1; It is characterized in that: the detailed process of said step (1) is: use glue head dropper to draw the polystyrene spheres hanging drop to slide; Then slide one end is contacted with the deionized water water surface with inclination angle 20-30 ° and slowly go deep into water surface below, the gas-liquid interface place is self-assembled into the individual layer polystyrene film; Insert PS single thin film below with the direction that is parallel to liquid level substrate then and move slowly polystyrene film is transferred in the substrate, 80-120 ℃ of dry colloidal spheres template.
3. according to claim 1 or claim 2 the preparation method of patterning zinc-oxide film; It is characterized in that: in the said step (1) during the polystyrene spheres suspension preparation with polystyrene spheres water-soluble with ethanol mixed solvent in; The mass percent of polystyrene spheres is 1-5% in the polystyrene spheres suspension; The mass ratio of water and ethanol is 1: 1-3, the sphere diameter of polystyrene spheres are 100-500nm, and substrate is silicon chip or quartz.
4. according to claim 1 or claim 2 the preparation method of patterning zinc-oxide film; It is characterized in that: the mass ratio of dimethyl silicone polymer and curing agent is 5-10 in the said step (2): 1; The mass concentration of octadecyl trichlorosilane solution is 0.1-1%; The temperature of heating in vacuum is 80-120 ℃, and vacuum degree is 10
-3-10
-4Pa, the time is 30-60min.
5. according to claim 1 or claim 2 the preparation method of patterning zinc-oxide film; It is characterized in that: solvent is deionized water, diethanol amine and two kinds of equal-volumes in the EGME compare mixed solution in the said step (3); Polyacrylic acid is 1 with the amount of substance ratio of zinc ion: 1-2; Zinc ion concentration is 10-100mM in the zinc oxide precursor colloidal sol, and the speed during spin coating is 1000-5000rpm, and thickness is 50-150nm.
6. according to claim 1 or claim 2 the preparation method of patterning zinc-oxide film, it is characterized in that: the condition of nano impression is in the said step (4): temperature 100-150 ℃, pressure 5-30 * 10
5Pa, retention time 10-30min, chilling temperature are 50-80 ℃.
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| TWI610804B (en) * | 2016-05-23 | 2018-01-11 | 國立成功大學 | Energy-saving Glass and Method of Manufacturing the Same |
| CN108249773B (en) * | 2018-03-20 | 2021-05-25 | 常州大学 | Preparation method of glass surface antireflection coating |
| CN110911051A (en) * | 2019-11-13 | 2020-03-24 | Tcl华星光电技术有限公司 | Flexible conductive wire manufacturing method, flexible conductive wire and display device |
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| CN1837965A (en) * | 2006-02-24 | 2006-09-27 | 浙江大学 | Method for drawing sub-micron ultraviolet luminous pattern on zinc oxide film |
| CN101058867A (en) * | 2006-04-17 | 2007-10-24 | Imra美国公司 | P-type semiconductor zinc oxide films, process for preparation thereof, and pulsed laser deposition method using transparent substrates |
| CN101186447A (en) * | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | Method for preparing zinc oxide self-assembly particle film |
| CN101857381A (en) * | 2010-05-31 | 2010-10-13 | 河南大学 | Preparation method of polystyrene microsphere template and method for preparing zinc oxide thin film |
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| US20070158661A1 (en) * | 2006-01-12 | 2007-07-12 | Rutgers, The State University Of New Jersey | ZnO nanostructure-based light emitting device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837965A (en) * | 2006-02-24 | 2006-09-27 | 浙江大学 | Method for drawing sub-micron ultraviolet luminous pattern on zinc oxide film |
| CN101058867A (en) * | 2006-04-17 | 2007-10-24 | Imra美国公司 | P-type semiconductor zinc oxide films, process for preparation thereof, and pulsed laser deposition method using transparent substrates |
| CN101186447A (en) * | 2007-12-14 | 2008-05-28 | 北京航空航天大学 | Method for preparing zinc oxide self-assembly particle film |
| CN101857381A (en) * | 2010-05-31 | 2010-10-13 | 河南大学 | Preparation method of polystyrene microsphere template and method for preparing zinc oxide thin film |
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