CN1763263A - Oriented ZnO nanorod or nanowire film and preparation process thereof - Google Patents
Oriented ZnO nanorod or nanowire film and preparation process thereof Download PDFInfo
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- CN1763263A CN1763263A CN 200510086521 CN200510086521A CN1763263A CN 1763263 A CN1763263 A CN 1763263A CN 200510086521 CN200510086521 CN 200510086521 CN 200510086521 A CN200510086521 A CN 200510086521A CN 1763263 A CN1763263 A CN 1763263A
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Abstract
The present invention relates to directional nanometer zinc oxide stick or linear film and its preparation process, and belongs to the field of low-dimensional nanometer film material technology. The present invention adopts hydrothermal deposition process, in which zinc salt solution in molar concentration 1-25 mM and amine surfactant solution are mixed homogeneously and set inside stainless steel reactor with PTFE lining, substrate of glass, polymer, inorganic metal, non-metal or other material and with directional texture ZnO crystal seed is set inside the lining, so as to react at 50-150 deg.c for 1-6 hr. After cooling naturally, directionally grown and high crystallized ZnO nanometer stick array film or nanometer stick of diameter 10-500 nm may be form. The process has low synthesis temperature and easy control, and the grown ZnO film is well directional. The present invention is suitable for industrial production of directional nanometer ZnO stick or film.
Description
Technical field
The invention belongs to the low-dimension nano material film preparation, particularly a kind of crystal seed is induced synthetic zinc oxide nano rod or line film and the technology of preparing thereof of aligning of hydro-thermal sedimentation.
Technical background
Zinc oxide is a kind of important wide bandgap semiconductor functional materials, can band gap be 3.3eV under the room temperature, exciton bind energy has very strong free exciton transition luminescence up to 60meV at ultraviolet band, adds abundant raw materials, low price, nontoxic to environment, be suitable for the epitaxy of film, have broad application prospects at the information photoelectric field, be the GaN that continues in recent years, another in the world research focus after the GaS.Because the ZnO nanostructure of high-sequential growth can be made short-wavelength laser and dye-sensitized nano oxide compound sun power electrode on substrate, becomes the focus of various countries scientist research in recent years.After particularly calendar year 2001 Yang Peidong has found ZnO nano wire photic Ultra-Violet Laser phenomenon at room temperature, promoted the research of the ZnO nano wire (rod) of preparation high quality oriented growth on the solid substrate greatly.And professor Wang Zhonglin has successfully developed ZnO nano belt, nano-rings and has started great disturbance in international nano material circle especially in the recent period.Prepare ZnO nano wire (rod) at present. adopt gas-liquid-solid (VLS) growth mechanism or chemical gaseous phase depositing process etc. to carry out more, yet many sapphire, silicon single crystal with costliness are solid substrate in these methods, need complicated valuable plant and instrument and higher temperature.For the VLS method, temperature required greater than 800 ℃, temperature required greater than 500 ℃ for the CVD method, preparation condition is quite harsh, is unfavorable for mass industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of crystal seed to induce the hydro-thermal sedimentation to synthesize and align zinc oxide nano rod (line) film and preparation method thereof, it is simple that this method has synthetic method, and cost is low, but film formation at low temp is fit to many advantages such as scale operation.
A kind of zinc oxide directional nanometer rod that the present invention proposes or line film and preparation method thereof, adopt the hydro-thermal sedimentation, it is characterized in that: described method is a raw material with zinc solution and amine surfactant soln, to preset ZnO orientation texture crystal seed is deposition substrate, substrate is put in the polytetrafluoroethyllining lining inboard, than under the low reaction temperatures, grows oriented growth on substrate, zinc oxide nano rod arranged in a uniform or linear array film, its technological process is specific as follows:
(1) volumetric molar concentration is 1mM～25mM zinc solution and amine surfactant soln uniform mixing after, put into the teflon-lined stainless steel cauldron;
(2) will preset the glass of ZnO (002) orientation texture crystal seed, high molecular polymer, metal, inorganic non-metallic, the various substrates of conductive glass are put in the polytetrafluoroethyllining lining inboard, and substrate crystal seed face becomes 0～90 ° of angle with the polytetrafluoroethyllining lining bottom surface;
(3) behind 50～150 ℃ of insulation 1～6h, behind the naturally cooling, on substrate, grow into oriented growth, the ZnO nanometer rod of better crystallinity degree or linear array film, the diameter of nanometer rod or line is about 10～500nm.
In above-mentioned preparation method, described zinc salt is a zinc nitrate, zinc chloride, zinc acetate, zinc sulfate, zinc citrate, any in the Zinc Gluconate zinc salt.
In above-mentioned preparation method, described tensio-active agent is hexamethylenetetramine and complex compound thereof, as dihydroxy-benzene-hexamethylenetetramine complex compound, and cyclodextrin-hexamethylenetetramine complex compound.
Because the present invention adopts the hydro-thermal low temperature deposition method, products therefrom has fine crystallinity, synthetic zinc oxide nano rod (line) film, directional property is good, the degree of crystallinity height, nanometer rod (line) size is even, and zinc oxide nano rod (line) array film of diameter range between 10～500nm can both be synthesized.The glass of ZnO (002) orientation texture crystal seed is preset in employing, high molecular polymer, and metal, inorganic non-metallic, conductive glass etc. are deposition substrate, obtain good ZnO nanometer rod (line) film of all even directional property in surface.This preparation method is at synthetic zinc oxide nano rod (line) film that aligns of low temperature in addition, and required equipment is simple, and cost is low, is suitable for zinc oxide nano rod (line) film that scale operation aligns.
Description of drawings
Figure 1 shows that the experimental installation structural representation.
Fig. 2 is the SEM figure of resultant zinc oxide directional nanometer rod (line) film among the embodiment 1.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
Fig. 1 is the experimental installation structural representation, for crystal seed of the present invention is induced the synthetic experimental installation that aligns zinc oxide nano rod (line) film of hydro-thermal sedimentation, it is heating source with the air dry oven, the teflon-lined stainless steel cauldron is a reaction vessel, with zinc nitrate, zinc chloride, zinc acetate, zinc sulfate, zinc citrate, zinc salt such as Zinc Gluconate and amine tensio-active agent are experimental raw, under lower hydrothermal temperature, in the glass that presets ZnO (002) orientation texture crystal seed, high molecular polymer, metal, inorganic non-metallic, grow evenly good ZnO nanometer rod (line) film of directional property of surface on the substrates such as conductive glass, deposition substrate crystal seed face becomes 0～90 ° of angle with the polytetrafluoroethyllining lining bottom surface.
Embodiment 1:
After volumetric molar concentration is the zinc nitrate solution of 1mM and hexamethylenetetramine solution uniform mixing that volumetric molar concentration is 2mM, put into the teflon-lined stainless steel cauldron, the silicon chip substrate that will preset ZnO (002) orientation texture crystal seed simultaneously is put in the polytetrafluoroethyllining lining inboard, deposition substrate crystal seed face and polytetrafluoroethyllining lining bottom surface are at an angle of 90, behind 60 ℃ of insulation 1h, behind the naturally cooling, on substrate, grow into oriented growth at last, ZnO nanometer rod (line) array film of better crystallinity degree, the diameter of nanometer rod (line) is about 10～30nm.
Embodiment 2:
After volumetric molar concentration is the zinc acetate solution of 6mM and hexamethylenetetramine solution uniform mixing that volumetric molar concentration is 5mM, put into the teflon-lined stainless steel cauldron, the plastic that will preset ZnO (002) orientation texture crystal seed simultaneously is put in the polytetrafluoroethyllining lining inboard, deposition substrate crystal seed face becomes 70 ° of angles with the polytetrafluoroethyllining lining bottom surface, behind 70 ℃ of insulation 2h, behind the naturally cooling, on substrate, grow into oriented growth at last, ZnO nanometer rod (line) array film of better crystallinity degree, the diameter of nanometer rod (line) is about 40～60nm.
Embodiment 3:
After volumetric molar concentration is the zinc citrate solution of 10mM and cyclodextrin-hexamethylenetetramine solution uniform mixing that volumetric molar concentration is 10mM, put into the teflon-lined stainless steel cauldron, the glass substrate that will preset ZnO (002) orientation texture crystal seed simultaneously is put in the polytetrafluoroethyllining lining inboard, deposition substrate crystal seed face becomes 50 ° of angles with the polytetrafluoroethyllining lining bottom surface, behind 90 ℃ of insulation 2h, behind the naturally cooling, on substrate, grow into oriented growth at last, ZnO nanometer rod (line) array film of better crystallinity degree, the diameter of nanometer rod (line) is about 50～80nm.
Embodiment 4:
After volumetric molar concentration is the liquor zinci chloridi of 17mM and cyclodextrin-hexamethylenetetramine solution uniform mixing that volumetric molar concentration is 25mM, put into the teflon-lined stainless steel cauldron, the nickel sheet substrate that will preset ZnO (002) orientation texture crystal seed simultaneously is put in the polytetrafluoroethyllining lining inboard, deposition substrate crystal seed face becomes 30 ° of angles with the polytetrafluoroethyllining lining bottom surface, behind 120 ℃ of insulation 4h, behind the naturally cooling, on substrate, grow into oriented growth at last, ZnO nanometer rod (line) array film of better crystallinity degree, the diameter of nanometer rod (line) is about 100～140nm.
Embodiment 5:
After volumetric molar concentration is the gluconic acid zinc solution of 21mM and dihydroxy-benzene-hexamethylenetetramine solution uniform mixing that volumetric molar concentration is 16mM, put into the teflon-lined stainless steel cauldron, the Conducting Glass that will preset ZnO (002) orientation texture crystal seed simultaneously is put in the polytetrafluoroethyllining lining inboard, deposition substrate crystal seed face becomes 20 ° of angles with the polytetrafluoroethyllining lining bottom surface, behind 150 ℃ of insulation 3h, behind the naturally cooling, on substrate, grow into oriented growth at last, ZnO nanometer rod (line) array film of better crystallinity degree, the diameter of nanometer rod (line) is about 200～500nm.
Claims (3)
1, a kind of zinc oxide directional nanometer rod or line film and preparation method thereof, adopt the hydro-thermal sedimentation, it is characterized in that: described method is a raw material with zinc solution and amine surfactant soln, to preset ZnO orientation texture crystal seed is deposition substrate, substrate is put in the polytetrafluoroethyllining lining inboard, than under the low reaction temperatures, grows oriented growth on substrate, zinc oxide nano rod arranged in a uniform or linear array film, its technological process is specific as follows:
(1) volumetric molar concentration is 1mM～25mM zinc solution and amine surfactant soln uniform mixing after, put into the teflon-lined stainless steel cauldron;
(2) will preset the glass of ZnO (002) orientation texture crystal seed, high molecular polymer, metal, inorganic non-metallic, the various substrates of conductive glass are put in the polytetrafluoroethyllining lining inboard, and substrate crystal seed face becomes 0～90 ° of angle with the polytetrafluoroethyllining lining bottom surface;
(3) behind 50～150 ℃ of insulation 1～6h, behind the naturally cooling, on substrate, grow into oriented growth, the ZnO nanometer rod of better crystallinity degree or linear array film, the diameter of nanometer rod or line is about 10～500nm.
2, preparation method according to claim 1 is characterized in that: described zinc salt is a zinc nitrate, zinc chloride, zinc acetate, zinc sulfate, zinc citrate, any in the Zinc Gluconate zinc salt.
3, preparation method according to claim 1 is characterized in that: described tensio-active agent is hexamethylenetetramine and complex compound thereof, as dihydroxy-benzene-hexamethylenetetramine complex compound, and cyclodextrin-hexamethylenetetramine complex compound.
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| US7402506B2 (en) * | 2005-06-16 | 2008-07-22 | Eastman Kodak Company | Methods of making thin film transistors comprising zinc-oxide-based semiconductor materials and transistors made thereby |
| CN100582012C (en) * | 2006-09-26 | 2010-01-20 | 中国科学院上海硅酸盐研究所 | Nano porous zinc oxide thin film with high C-axis orientation and preparation method thereof |
| CN101863451A (en) * | 2010-04-20 | 2010-10-20 | 上海大学 | Method for preparing zinc oxide in three-dimensional nanostructure with cryogenic fluid method |
| CN101481134B (en) * | 2008-01-11 | 2010-12-08 | 南京理工大学 | Process for preparing zinc oxide nano film |
| CN101319372B (en) * | 2008-06-03 | 2011-12-14 | 中山大学 | Method for low temperature controllable preparation of zinc oxide nano line and application thereof |
| CN101798105B (en) * | 2009-11-13 | 2012-01-11 | 襄樊学院 | Preparation technology for growing ZnO nanorod arrays on ITO PET film |
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| CN102491405A (en) * | 2011-11-18 | 2012-06-13 | 华东理工大学 | Composite nano-zinc oxide material and its preparation method |
| CN101236208B (en) * | 2007-02-01 | 2012-07-04 | 四川大学 | Method for identifying blood albumen by chemically modified zinc oxide nanometer rod array film |
| CN101358973B (en) * | 2007-08-02 | 2012-07-04 | 四川大学 | Hepatocarcinoma early diagnosis kit based on ZnO nano-bar array |
| CN101845672B (en) * | 2009-03-28 | 2012-09-26 | 中国科学院合肥物质科学研究院 | Zinc oxide nanocone array with controllable sharpness and preparation method thereof |
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| CN102923757A (en) * | 2012-11-15 | 2013-02-13 | 中国科学院深圳先进技术研究院 | Method for preparing ZnO Nano-rods |
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| CN105883900A (en) * | 2014-12-29 | 2016-08-24 | 神华集团有限责任公司 | Method for controlling density and optical band gap of zinc oxide nanorod array |
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| CN106882834A (en) * | 2017-04-01 | 2017-06-23 | 景德镇陶瓷大学 | A kind of original position prepares the method and its obtained film of ZnO nano-rod array film |
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| US7402506B2 (en) * | 2005-06-16 | 2008-07-22 | Eastman Kodak Company | Methods of making thin film transistors comprising zinc-oxide-based semiconductor materials and transistors made thereby |
| CN100582012C (en) * | 2006-09-26 | 2010-01-20 | 中国科学院上海硅酸盐研究所 | Nano porous zinc oxide thin film with high C-axis orientation and preparation method thereof |
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