CN104030238A - Preparation method for realizing graphical ZnO nanowire arrays by micro-contact printing - Google Patents
Preparation method for realizing graphical ZnO nanowire arrays by micro-contact printing Download PDFInfo
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- CN104030238A CN104030238A CN201410260626.6A CN201410260626A CN104030238A CN 104030238 A CN104030238 A CN 104030238A CN 201410260626 A CN201410260626 A CN 201410260626A CN 104030238 A CN104030238 A CN 104030238A
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Abstract
The invention discloses a preparation method for micro-sized and graphical ZnO nanowire arrays by adopting two steps of micro-contact printing (MCP) and low-temperature chemical bath deposition (CBD). The preparation method includes: firstly, adopting a sol-gel method to prepare a ZnO seed layer film on conductive glass; transferring TiO2 sol ink to the ZnO seed layer film through elastic polydimethylsiloxane (PDMS) stamps with different graphics to acquire a graphical TiO2 shielding layer film; adopting a chemical bath deposition method to complete select growth of ZnO nanowires in a ZnO seed layer area shielded by the TiO2 film. The preparation method is simple in process, low in cost, large in preparation area and good in repeatability; the three critical techniques in the entire process refer to preparation of the TiO2 sol ink with appropriate viscosity, setting of inkiness of the PDMS stamps and pressure parameter of the printing process and time control of hydrothermal growth of the nanowires.
Description
Technical field
The invention belongs to technical field of micro-nano manufacture, be specifically related to the preparation method that Microcontact printing is realized graphical ZnO nano thread array.
Background technology
In recent years, one-dimensional ZnO nanowires is as a kind of important functional oxide semi-conducting material, because it is at photoelectric device, and near ultraviolet luminescent device, application potential based in EED and self assembled three-dimensional nano-scale systems, has attracted people more and more to pay close attention to.Research about the aspects such as orientation, size and deposition position of ZnO nano-wire is reported widely.For the electronic device of implementation structure, the development of the ZnO nanowire array of microstructure graph has become inevitable, and the realization of micro-structural improves the performance to above device and characteristic development has great importance.
At present, reported that many employing diverse ways realize the graphical of One-Dimensional ZnO nano material, and ZnO nano-wire graphically the most essential is the graphical of ZnO Seed Layer, at present, the patterned method of Seed Layer has comprised: photoetching process, beamwriter lithography method and follow-up Metal Zn depositing operation (magnetron sputtering deposition and optionally corrosion, or metal organic chemical vapor deposition method); Hydrophilic/hydrophobic interaction self assembled monolayer; Self-assembly microspheres monofilm; Ion beam focusing etc.For these above technology, follow-up ZnO nano-wire optionally growth needs superior accommodation, long expend time in, the assisting of harsh preparation condition (high temperature, high pressure) and precious metal catalyst (for example Au, Ag, Pt).
Soft etching method is a technology getting a good chance of at material aspect the micro nano structure processing on a large scale.Prepare patterned strategy relatively with photoetching process or the beamwriter lithography of standard, soft etching method seems and is more suitable for the requirement of those one-step method, large-area graphs.Microcontact printing (MCP) is exactly a kind of of soft etching method, it mainly adopts dimethyl silicone polymer (PDMS) elastomer as seal, mould or a blindage, by contacting closely transition diagram, this elastomer can guarantee tangiblely between PDMS surface and substrate to contact and be easy to discharge and do not damage the micro-structural of formation.
Few about utilizing the method for Microcontact printing to prepare the report of patterned ZnO nanowire array, the people such as Kang [HW Kang, J Yeo, JO Hwang, J.Phys.Chem.C, 2011,115,11435] utilize ZnO quantum dot and elasticity PDMS for seed layer materials and seal, on ITO electro-conductive glass directly impression to prepare minimum unit be the square seed tunic of 30 μ m*30 μ m, then adopt Hydrothermal Growth ZnO nano-wire.The people such as Lee [J-H Lee, M-H Hon, Y-W Chung, J.Am.Ceram.Soc., 2009,92,2192] utilize elasticity PDMS for seal at ZnO seed thin film surface self-organization octadecyl trichlorosilane alkane (OTS) monolayer as blocking masterplate, to have prepared width be 20 μ m bar shaped ZnO seed tunics, then adopt Hydrothermal Growth ZnO nano-wire.From the result of research, because the quantum dot skewness directly impressing, so the serious inclination growth of the most of generation of ZnO nano-wire.The method that adopts OTS monolayer to block need to be dry environment, individual layer be also difficult to assembling, and in the region of blocking, also have the growth of nano wire.Above two kinds of common deficiencies of method are that patterned minimum unit area is still very large.How to use above preparation method's thought and overcome its deficiency, in the environment without any protection, utilize Microcontact printing to realize minimum unit and be less than 5 μ m, and the ZnO nanowire array of favorable orientation is one and has problem to be solved.
Summary of the invention
The object of the invention is to prepare graphical ZnO nano thread array for Physicals such as photoetching process, ion beam focusing etchings and need sophisticated equipment, high time-consuming, exacting terms, precious metal catalyst, for Microcontact printing legal system, for OTS monolayer and the brilliant graphical problem that Seed Layer growing ZnO nano-wire is of poor quality, pattern dimension is large of ZnO nano, provide a kind of Microcontact printing to realize the preparation method of graphical ZnO nano thread array.
To achieve the above object, the technical solution used in the present invention is: the 1) preparation of ZnO Seed Layer film:
Adopt the ethanolic solution of solution chemical method preparation 5mmol/L zinc acetate as precursor solution, take ITO electro-conductive glass as substrate, first utilize sol evenning machine to prepare zinc acetate colloid film at rotary speed and rotational time under for 2000rmp and 30s, then in the Muffle furnace of 300 ℃, Thin-film anneal 0.5-1h is obtained to ZnO Seed Layer;
2) TiO
2the preparation of colloidal sol ink: by volume to get the butyl titanate of 4 parts be that titanium source, the EGME of 16 parts are that the stickiness that solvent adds after evenly the diethanol amine of 2.5-3 part to adjust colloidal sol ink again obtains TiO to umber
2colloidal sol ink;
3) preparation of graphical ZnO Seed Layer: utilize spin-coating method spin coating TiO on slide
2colloidal sol ink; Then utilize micro-contact cladding process by TiO
2colloidal sol ink is transferred to PDMS seal surface from slide surface; And then utilize Microcontact printing method by TiO
2colloidal sol ink is transferred to ZnO Seed Layer film surface from PDMS seal; Last patterned ZnO/TiO
2film obtains graphical ZnO Seed Layer through Overheating Treatment;
4) graphical ZnO nano thread array is synthetic: the Zn (NO that the NaOH that employing immersion method is 0.8mol/L in concentration and concentration are 0.04mol/L
3)
2, or the concentration hexamethylenetetramine that is 0.05mol/L and the concentration Zn (NO that is 0.05mol/L
3)
2water solution system in selective growth ZnO nano-wire.
Described step 1) utilize sol evenning machine rotary speed and rotational time for 2000rmp and 30s under spin coating 5 times continuously, then wet film is put into Muffle furnace, with 3 ℃/min speed, from room temperature, be raised to 300 ℃ and at this annealing temperature 0.5-1h.
Described step 3) preparation of graphical ZnO Seed Layer: first will be of a size of 0.25cm
2elasticity PDMS seal ultrasonic cleaning 20min in absolute ethyl alcohol, and dry up with nitrogen; Then take clean slide as substrate, adopt 3000rmp, 1 TiO of 30s rotating technics spin coating
2colloidal sol ink, and immediately at 100-150g/cm
2pressure under by PDMS seal film close contact therewith, after 1min, PDMS seal is peeled off lightly; And then will be covered with TiO
2the PDMS seal of colloidal sol is at 50-90g/cm
2vertical pressure under with ZnO seed layer substrate surface close contact, after 2-3min, PDMS seal is peeled off; Finally, after patterned wet film substrate horizontal positioned 30min, put it in stove and be warmed up to 400 ℃ with 3 ℃/min speed, and at this annealing temperature 0.5h, make patterned ZnO Seed Layer.
Described step 4) graphical ZnO nano thread is synthetic: the Zn (NO that first compound concentration is 0.08mol/L respectively under magnetic agitation
3)
2naOH aqueous solution 50ml with 1.8mol/L; Then by the Zn (NO stirring
3)
2solution is poured NaOH solution lentamente into, continues to stir 1h; Then patterned ZnO Seed Layer film front is tiltedly inserted in growth solution down, and the 10-20min that grows in the hydro-thermal of 80 ℃; Finally take out the nano wire film of having grown and rinse well by deionized water, and dry at the Muffle furnace of 100 ℃.
The present invention adopts sol-gel process making ZnO Seed Layer film, adopts Microcontact printing to prepare patterned TiO on the surface of ZnO Seed Layer film
2barrier bed, adopts the hydro-thermal method ZnO nano-wire of optionally having grown, and has prepared the ZnO nanowire array of the periodic micro structure of structural integrity.Graphical ZnO nano thread array preparation of the present invention has the following advantages: the first, do not need superior accommodation, complicated technique and exacting terms; The second, technique is carried out without any need for protection in air, the regular perfection of graphical ZnO nano thread array of preparation, and clear patterns, unit size is less.This preparation method is applicable to minute manufacturing electronic device and novel solar battery application.
Accompanying drawing explanation
Fig. 1 is the TiO of the different pattern prepared of Microcontact printing
2film: (a) square column: hem width 5 μ m, limit spacing 3 μ m, the degree of depth 4 μ m; (b) cylinder: diameter 5 μ m, centre-to-centre spacing 8 μ m, the degree of depth 4 μ m; (c) cylinder: diameter 3 μ m, centre-to-centre spacing 5 μ m, the degree of depth 2 μ m
Fig. 2 is different proportionings (too sour four butyl esters: EGME: the graphical TiO that diethanol amine) prepared by ink
2film: (a) 4:16:2, (b) 4:16:2.25, (c) 4:16:2.5, (d) 4:16:3 (ml)
Fig. 3 is graphical TiO prepared by different pressures
2film: (a) 50g/0.25cm
2, (b) 90g/0.25cm
2, (c) 130g/0.25cm
2, (d) 180g/0.25cm
2
Fig. 4 is synthetic graphical ZnO nano thread array of different water-bath time.
The specific embodiment:
Below in conjunction with example, the present invention is further elaborated, rather than will limit the invention with this.
Embodiment:
The preparation of ZnO Seed Layer film: first prepare the ethanolic solution of 5mmol/L zinc acetate, take ITO electro-conductive glass as substrate, adopt 2000rmp, the continuous spin coating of 30s rotating technics 5 times; Follow 300 ℃ of heat treatment 20min (repeating 2 times from being spun to heat treatment) in Muffle furnace; Finally put it in stove and be warmed up to 300 ℃ with 3 ℃/min speed, and at this annealing temperature 0.5-1h, make ZnO Seed Layer.
TiO
2the preparation of colloidal sol ink: first under magnetic agitation, the butyl titanate of 4ml is dropwise added in the EGME of 16ml, stir; Then 2.5ml diethanol amine is dropwise added, magnetic agitation is to mixing for a long time.
The preparation of graphical ZnO Seed Layer: first will be of a size of 0.25cm
2elasticity PDMS seal ultrasonic cleaning 20min in absolute ethyl alcohol, and dry up with nitrogen; Then take clean slide as substrate, adopt 3000rmp, 1 TiO of 30s rotating technics spin coating
2colloidal sol ink, and immediately under the pressure of 130g by PDMS seal film close contact therewith, after 1min, PDMS seal is peeled off lightly; And then will be covered with TiO
2the PDMS seal of colloidal sol under the vertical pressure of 90g with ZnO seed layer substrate surface close contact, after 2-3min, PDMS seal is peeled off lightly; Finally, after patterned wet film substrate horizontal positioned 30min, put it in stove and be warmed up to 400 ℃ with 3 ℃/min speed, and at this annealing temperature 0.5h, make patterned ZnO Seed Layer.
Graphical ZnO nano thread synthetic: first compound concentration is respectively the Zn (NO of 0.08mol/L under magnetic agitation
3)
2naOH aqueous solution 50ml with 1.8mol/L; Then by the Zn (NO stirring
3)
2solution is poured NaOH solution lentamente into, continues to stir 1h; Then patterned ZnO Seed Layer film front is tiltedly inserted in growth solution down, and the 10-20min that grows in the hydro-thermal of 80 ℃; Finally take out the nano wire film of having grown and rinse well by deionized water, and dry at the Muffle furnace of 100 ℃.
Claims (4)
1. Microcontact printing is realized the preparation method of graphical ZnO nano thread array, it is characterized in that:
1) preparation of ZnO Seed Layer film:
Adopt the ethanolic solution of solution chemical method preparation 5mmol/L zinc acetate as precursor solution, take ITO electro-conductive glass as substrate, first utilize sol evenning machine to prepare zinc acetate colloid film at rotary speed and rotational time under for 2000rmp and 30s, then in the Muffle furnace of 300 ℃, Thin-film anneal 0.5-1h is obtained to ZnO Seed Layer;
2) TiO
2the preparation of colloidal sol ink: by volume to get the butyl titanate of 4 parts be that titanium source, the EGME of 16 parts are that the stickiness that solvent adds after evenly the diethanol amine of 2.5-3 part to adjust colloidal sol ink again obtains TiO to umber
2colloidal sol ink;
3) preparation of graphical ZnO Seed Layer: utilize spin-coating method spin coating TiO on slide
2colloidal sol ink; Then utilize micro-contact cladding process by TiO
2colloidal sol ink is transferred to PDMS seal surface from slide surface; And then utilize Microcontact printing method by TiO
2colloidal sol ink is transferred to ZnO Seed Layer film surface from PDMS seal; Last patterned ZnO/TiO
2film obtains graphical ZnO Seed Layer through Overheating Treatment;
4) graphical ZnO nano thread array is synthetic: the Zn (NO that the NaOH that employing immersion method is 0.8mol/L in concentration and concentration are 0.04mol/L
3)
2, or the concentration hexamethylenetetramine that is 0.05mol/L and the concentration Zn (NO that is 0.05mol/L
3)
2water solution system in selective growth ZnO nano-wire.
2. Microcontact printing according to claim 1 is realized the preparation method of graphical ZnO nano thread array, it is characterized in that: described step 1) utilize sol evenning machine rotary speed and rotational time for 2000rmp and 30s under spin coating 5 times continuously, then wet film is put into Muffle furnace, with 3 ℃/min speed, from room temperature, be raised to 300 ℃ and at this annealing temperature 0.5-1h.
3. Microcontact printing according to claim 1 is realized the preparation method of graphical ZnO nano thread array, it is characterized in that: the described step 3) preparation of graphical ZnO Seed Layer: first will be of a size of 0.25cm
2elasticity PDMS seal ultrasonic cleaning 20min in absolute ethyl alcohol, and dry up with nitrogen; Then take clean slide as substrate, adopt 3000rmp, 1 TiO of 30s rotating technics spin coating
2colloidal sol ink, and immediately at 100-150g/cm
2pressure under by PDMS seal film close contact therewith, after 1min, PDMS seal is peeled off lightly; And then will be covered with TiO
2the PDMS seal of colloidal sol is at 50-90g/cm
2vertical pressure under with ZnO seed layer substrate surface close contact, after 2-3min, PDMS seal is peeled off; Finally, after patterned wet film substrate horizontal positioned 30min, put it in stove and be warmed up to 400 ℃ with 3 ℃/min speed, and at this annealing temperature 0.5h, make patterned ZnO Seed Layer.
4. Microcontact printing according to claim 1 is realized the preparation method of graphical ZnO nano thread array, it is characterized in that: described step 4) graphical ZnO nano thread is synthetic: the Zn (NO that first compound concentration is 0.08mol/L respectively under magnetic agitation
3)
2naOH aqueous solution 50ml with 1.8mol/L; Then by the Zn (NO stirring
3)
2solution is poured NaOH solution lentamente into, continues to stir 1h; Then patterned ZnO Seed Layer film front is tiltedly inserted in growth solution down, and the 10-20min that grows in the hydro-thermal of 80 ℃; Finally take out the nano wire film of having grown and rinse well by deionized water, and dry at the Muffle furnace of 100 ℃.
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| CN105253852A (en) * | 2015-09-02 | 2016-01-20 | 西安建筑科技大学 | Manufacturing method of template of micro-nano composite structure |
| CN106527044A (en) * | 2016-12-02 | 2017-03-22 | 江南大学 | Method for preparing zinc oxide pattern without residual layer by using room-temperature transfer imprinting technology |
| CN107856427A (en) * | 2017-11-24 | 2018-03-30 | 华中科技大学 | A kind of ultrasonic vibration assistant metal coin chapter impressing building mortion and method |
| CN112271248A (en) * | 2020-10-26 | 2021-01-26 | 中国科学院微电子研究所 | Pressure sensor structure based on oxide nanowires and preparation method thereof |
| CN112271250A (en) * | 2020-10-26 | 2021-01-26 | 中国科学院微电子研究所 | Pressure sensor based on zinc oxide nanowire and preparation method thereof |
| CN112774255A (en) * | 2019-11-08 | 2021-05-11 | 迈迪生物科技有限公司 | Super-hydrophobic oil-water separation membrane with self-cleaning characteristic and preparation and application thereof |
| CN113937243A (en) * | 2021-08-26 | 2022-01-14 | 福州大学 | Preparation method of high PPI quantum dot array based on hydrophilic and hydrophobic treatment of substrate surface |
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| CN105253852A (en) * | 2015-09-02 | 2016-01-20 | 西安建筑科技大学 | Manufacturing method of template of micro-nano composite structure |
| CN106527044A (en) * | 2016-12-02 | 2017-03-22 | 江南大学 | Method for preparing zinc oxide pattern without residual layer by using room-temperature transfer imprinting technology |
| CN107856427A (en) * | 2017-11-24 | 2018-03-30 | 华中科技大学 | A kind of ultrasonic vibration assistant metal coin chapter impressing building mortion and method |
| CN112774255A (en) * | 2019-11-08 | 2021-05-11 | 迈迪生物科技有限公司 | Super-hydrophobic oil-water separation membrane with self-cleaning characteristic and preparation and application thereof |
| CN112271248A (en) * | 2020-10-26 | 2021-01-26 | 中国科学院微电子研究所 | Pressure sensor structure based on oxide nanowires and preparation method thereof |
| CN112271250A (en) * | 2020-10-26 | 2021-01-26 | 中国科学院微电子研究所 | Pressure sensor based on zinc oxide nanowire and preparation method thereof |
| CN113937243A (en) * | 2021-08-26 | 2022-01-14 | 福州大学 | Preparation method of high PPI quantum dot array based on hydrophilic and hydrophobic treatment of substrate surface |
| CN113937243B (en) * | 2021-08-26 | 2024-01-30 | 福州大学 | Preparation method of high PPI quantum dot array based on substrate surface hydrophilic and hydrophobic treatment |
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