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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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002073 nanorod Substances 0.000 title claims description 10
- 239000002070 nanowire Substances 0.000 title description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000011787 zinc oxide Substances 0.000 claims abstract description 44
- 239000000758 substrate Substances 0.000 claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 150000003751 zinc Chemical class 0.000 claims abstract description 4
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 9
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical group C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical group [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- WHMDKBIGKVEYHS-IYEMJOQQSA-L Zinc gluconate Chemical compound [Zn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O WHMDKBIGKVEYHS-IYEMJOQQSA-L 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 4
- WGIWBXUNRXCYRA-UHFFFAOYSA-H trizinc;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WGIWBXUNRXCYRA-UHFFFAOYSA-H 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- 239000011746 zinc citrate Substances 0.000 claims description 4
- 235000006076 zinc citrate Nutrition 0.000 claims description 4
- 229940068475 zinc citrate Drugs 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229960000314 zinc acetate Drugs 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- 229960001939 zinc chloride Drugs 0.000 claims description 3
- 239000011670 zinc gluconate Substances 0.000 claims description 3
- 235000011478 zinc gluconate Nutrition 0.000 claims description 3
- 229960000306 zinc gluconate Drugs 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 2
- 238000005137 deposition process Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229910052755 nonmetal Inorganic materials 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000000151 deposition Methods 0.000 description 10
- 238000009434 installation Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002063 nanoring Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
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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| CN 200510086521 CN1763263A (en) | 2005-09-27 | 2005-09-27 | Oriented ZnO nanorod or nanowire film and preparation process thereof |
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| CN 200510086521 CN1763263A (en) | 2005-09-27 | 2005-09-27 | Oriented ZnO nanorod or nanowire film and preparation process thereof |
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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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