CN102220596B - Preparation method of nano zinc oxide wire - Google Patents
Preparation method of nano zinc oxide wire Download PDFInfo
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- CN102220596B CN102220596B CN 201110129855 CN201110129855A CN102220596B CN 102220596 B CN102220596 B CN 102220596B CN 201110129855 CN201110129855 CN 201110129855 CN 201110129855 A CN201110129855 A CN 201110129855A CN 102220596 B CN102220596 B CN 102220596B
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- zinc oxide
- oxide nanowire
- electrochemical deposition
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- nucleopore membranes
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 14
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000012528 membrane Substances 0.000 claims abstract description 14
- 238000004070 electrodeposition Methods 0.000 claims abstract description 13
- 239000010931 gold Substances 0.000 claims abstract description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052737 gold Inorganic materials 0.000 claims abstract description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims abstract description 5
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- 238000007747 plating Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 12
- 238000005530 etching Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000004417 polycarbonate Substances 0.000 claims description 8
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 7
- 229920000515 polycarbonate Polymers 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- 229920000728 polyester Polymers 0.000 claims description 5
- 238000007738 vacuum evaporation Methods 0.000 claims description 4
- 239000011263 electroactive material Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910001369 Brass Inorganic materials 0.000 claims description 2
- 239000010951 brass Substances 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 210000004492 nuclear pore Anatomy 0.000 abstract 2
- QRJOYPHTNNOAOJ-UHFFFAOYSA-N copper gold Chemical compound [Cu].[Au] QRJOYPHTNNOAOJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 229960001296 zinc oxide Drugs 0.000 description 14
- 150000002500 ions Chemical class 0.000 description 5
- 229920006267 polyester film Polymers 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 241000784726 Lycaena thetis Species 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009415 formwork Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000009189 diving Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 244000144992 flock Species 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229920006289 polycarbonate film Polymers 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Abstract
The invention discloses a method for preparing a nano zinc oxide wire by using a solid nuclear track technology. The method comprises the steps of taking a penetrating type nuclear pore membrane with the aperture of 100-600 nm as a template, plating a gold layer with the aperture of 110-200 nm on one surface of the nuclear pore membrane, and performing electrochemical deposition on the gold layer to form a copper layer with the thickness of 10-40 microns. Then, using platinum wire as anode and gold copper lining as cathode to electrochemically deposit zinc oxide to produce zinc oxide nanowire, wherein the electrolyte is 0.05-0.2 mol/L KCl and 2-7 mmol/L ZnCl2、3～8mmol/L H2O2The pH value of the mixed solution is 6.5-7.5, the electrolytic voltage is 0.8-1.5V, and the electrochemical deposition time is 1-5 hours. The diameter of the produced zinc oxide nanowire is 100-600 nm, and the length of the zinc oxide nanowire is 5-8 mu m.
Description
Technical field
The invention belongs to the zinc oxide technical field, be specifically related to a kind of method for preparing nano zinc oxide wires with solid state nuclear track technique.
Background technology
The one-D nano zinc oxide wire material has quantum size effect, interfacial effect, quantum confined effect, has at aspects such as power, electricity, light, magnetic the premium properties that other material does not possess.At present, (see document Huang, M.H. Gu prepare the method that nano zinc oxide wires adopts gas-liquid-growth mechanism more; Wu, Y.; Feick, H.; Tran, N.; Weber, E.; Yang, P.Adv.Mater.2001,13,113; And document Kong, Y.C.; Yu, D.P.; Zhang, B.; Fang, W.; Feng, S.Q.Appl.Phys.Lett.2001,78,407.), or chemical Vapor deposition process (is seen document Wu, J.2J.; Liu, S.2C.Adv.Mater.2002,14,215.).Yet sapphire, silicon single crystal mainly with costliness in these methods are solid substrate, need complicated valuable plant and instrument and higher temperature.Document Vayssieres, L.; Keis, K.; Lindquist, S.2E.; Hagfeldt, A.J.Phys.Chem.B 2001,105,3350. in, the simple wet chemical method of the humans such as Vayssieres is prepared height-oriented nano zinc oxide wires in substrate, although this method is simple and easy to do, the diameter of the single rod that generates is approximately 1～2 μ m.Document Govender, K.; Boyle, D.S.; O ' Brien, P.; Binks, D.; West, D.; Coleman, D.Adv.Mater.2002,14,1221. in, the people such as Govender adopt sputter layer of gold film in the conductive glass substrate in advance, the method for then growing in particular solution, prepare height-oriented nano zinc oxide wires in substrate, but the diameter of the single rod that generates is still larger, and mean diameter is about 532nm, has limited the application of nano zinc oxide wires in fields such as nano electron devices.Document Guo Min, Diao Peng, Cai Shengming, the chemistry journal, 2003,61 (8), in 1165, the people such as Guo Min have improved the method for Vayssieres, and preparation nano zine oxide film of nanoparticles, then successfully prepare with the method for low-temperature hydrothermal the nano zine oxide linear array that mean diameter is 150nm in the ITO substrate.Take porous material as template the work of the long-pending preparation of inner hole deposition zinc oxide nanowire start from Possin (see document Possin, E.Rev.Sci.Instrum., 1970,41:772), template commonly used has alumina formwork (to see document Qingtao Wang; Guanzhong Wang; Bo Xu, Materials Letters 59 (2005) 1378; And document Wang, X.W.; Fei, G.T.; Wu, B.; Chen, L.; Chu, Z.Q.Phys.Lett.A, 2006,359:220), the porous silicon template (is seen document Chang, C.C.; Chang, C.S.Jpn.J.Appl.Phys., 2004,43:8360), heavy ion template (see document Y.Leprince-Wang, A.Yacoubi-Ouslim, G.Y.Wang, Microelectronics Journal 36 (2005) 625).Wherein alumina formwork has nano aperture little (10nm), density large (10
12/ cm
2), resistant to elevated temperatures characteristics and being widely used, but after with acid or alkali removal alumina formwork, nano wire will flock together, and its order is destroyed.Therefore due to the existence of aluminum oxide, limited to a great extent its actual application prospect.And the heavy ion template as polycarbonate (PC), polyester (PET) etc., relatively has lot of advantages with other templates, can realize the selection of and orientation big or small to Track density by controlling the irradiate ion parameter.For example, the irradiation dose of controlling heavy ion on accelerator can be realized aperture density 10
6-10
9/ cm
2, pore size and shape can be by controlling etching reagent composition, etch temperature, etching period and track etching speed Vt and whole etch-rate V
bRatio (Vt/V
b) regulate.Wherein the people such as Y.Leprince of France are 30nm, 60nm in the aperture of polycarbonate surface, in 100nm and 150nm nuclear track hole, electrochemical deposition has prepared zinc oxide nanowire, but their the zinc-oxide nano line length of preparation is only 1.5 μ m, and is not the array of ordered arrangement.
Summary of the invention
(1) goal of the invention
For at present take porous material as template, in the long-pending existing defective of method for preparing zinc oxide nanowire of inner hole deposition, the present invention aims to provide a kind of take porous material as template, the preparation method of the zinc oxide nanowire of long, the ordered arrangement of electrochemical deposition length in the hole.
(2) technical scheme
For achieving the above object, the invention provides following technical scheme:
A kind of zinc oxide nanowire preparation method, penetrating type nucleopore membranes take the aperture as 100～600nm is template, first at the gold layer of the one side plating 110～200nm of nucleopore membranes, then on the gold layer the thick copper layer of electrochemical deposition one deck 10-40 μ m, do support substrates material and cathode electroactive material; Then make anode with platinum filament, make negative electrode with golden brass, electrochemical deposition zinc oxide generates zinc oxide nanowire, and wherein electrolytic solution is 0.05～0.2mol/LKCl, 2～7mmol/L ZnCl
2, 3～8mmol/L H
2O
2Mixing solutions, the pH value is 6.5～7.5, electrolysis voltage is 0.8～1.5V, the electrochemical deposition time is 1～5 hour.
Described nucleopore membranes is selected polycarbonate or polyester material.
The technique that Gold plated Layer adopts on nucleopore membranes is the method for vacuum-evaporation.
(3) invention effect
After the zinc oxide nanowire preparation is completed, adopt methylene dichloride (CH
2Cl
2) solution dissolving nucleopore membranes, zinc oxide nanowire just stands upright on golden copper substrate.Electronic scanning Electronic Speculum Image Display, standing is the conical zinc oxide nano-wire array of ordered arrangement on golden copper substrate, and diameter is 100～600nm, and length is 5～8 μ m, and the zinc oxide nanowire of this size can satisfy the industrial application requirement.
Embodiment
Below in conjunction with embodiment, the technical scheme of invention is further elaborated.
The energy that utilizes China Atomic Energy Science Research Institute's HI-13 tandem accelerator to provide is strong for 20nA's for 80MeV, stream
32Polycarbonate membrane or polyester film that S ion irradiation 20 μ m are thick, irradiation density are 10
8-10
9Individual/cm
2Irradiated sample is placed in the dry environment of cleaning and places for some time, after alcohol wash,, make in the track of diving photooxydation occurs with each irradiation sensitization of two surfaces of sample 1 hour with the UV-light of 360nm wavelength, the track hole is deepened or is widened, and improves the etch-rate Vt of track.Carry out at last etching in thermostatic bath, etching condition is: NaOH solution, concentration is 6mol/L-7mol/L, temperature is 55 ℃-65 ℃, etching period is 6min-18min, obtaining the aperture is the template with penetrating type nuclear track hole of 100nm-600nm, and the aperture that the present embodiment uses is 400nm-500nm.
Adopt the method for vacuum-evaporation, polycarbonate membrane after etching or the one side of polyester film first the method plating one deck 110～200nm with vacuum-evaporation are thick, the Au layer of preferred 180nm, again on gold layer electrochemical deposition one deck approximately 15～25 μ m are thick, the thick copper layer of preferred 20 μ m is as support substrates material and the cathode electroactive material of template.Polycarbonate membrane or polyester film nuclear track template are cleaned 1min in ultrasonic wave electrolytic solution, to get rid of the air in the aperture, make zinc oxide fully be deposited in the hole.Make anode with platinum filament, golden copper substrate is made negative electrode, and electrochemical deposition zinc oxide nanowire, electrolytic solution are 0.05～0.2mol/L KCl, 2～7mmol/L ZnCl
2, 3～8mmol/L H
2O
2Mixing solutions, this enforcement recommendation be 0.1mol/L KCl, 5mmol/L ZnCl
2, 5mmol/L H
2O
2Mixing solutions, all chemical reagent are all analytical pure, adopting the ultrapure water (＞18M Ω) of millipore filter system to come obtain solution, electrolytic solution is that pH value is 6.5～7.5 quasi-neutrality solution, the pH value of the present embodiment recommendation is 6.85.Adopt adjustable constant voltage instrument, regulating voltage is 0.8～1.5V, the present embodiment recommendation be 1.0V, the reaction that occurs on negative electrode is:
H
2O
2+2e
-→2OH
-
Zn
2++2OH
-→ZnO+H
2O
Deposit 1～5 hour, the present embodiment was recommended deposition 2.5 hours, and zinc oxide will deposit full nuclear track hole.Then the sample that has deposited zinc oxide is cleaned up in deionized water and dries.
After the zinc oxide nanowire preparation is completed, adopt methylene dichloride (CH
2Cl
2) solution dissolved polycarbonate film or polyester film nuclear track template, change a solution every 20min in dissolution process.Just can thoroughly dissolve after three times and reunite carbonic ether film or polyester film nuclear track template, zinc oxide nanowire just stands upright on copper substrate,
X-ray diffractometer and the demonstration of energy color dispersing X fluorescent spectrometer analytical results, the zinc oxide nanowire of preparation is to have highly purified hexagonal system nano zinc oxide material, and diameter is 400～500nm, and length is 6～7 μ m.
Obviously those skilled in the art can carry out various modifications and variations and not break away from the spirit and scope of the present invention the present invention.Like this, if of the present invention these revise and modification belongs in the scope of its equivalent technologies of claim of the present invention, the present invention also is intended to comprise these modifications and modification.
Claims (3)
1. zinc oxide nanowire preparation method, that the penetrating type nucleopore membranes as 100～600nm is template take the aperture, first at the gold layer of the one side plating 110～200nm of nucleopore membranes, then on the gold layer the thick copper layer of electrochemical deposition one deck 10-40 μ m, do support substrates material and cathode electroactive material; Then make anode with platinum filament, make negative electrode with golden brass, electrochemical deposition zinc oxide generates zinc oxide nanowire, and wherein electrolytic solution is 0.05～0.2mol/L KCl, 2～7mmol/L ZnCl
2, 3～8mmol/L H
2O
2Mixing solutions, the pH value is 6.5～7.5, electrolysis voltage is 0.8～1.5V, the electrochemical deposition time is 1～5 hour;
Described nucleopore membranes is selected polycarbonate or polyester material; The employing energy is that 80MeV, stream are strong for 20nA's
32The S ion irradiation; Etching condition after irradiation is: etching solution is that concentration is the NaOH solution of 6mol/L-7mol/L, and etch temperature is 55 ℃-65 ℃, and etching period is 6min-18min.
2. zinc oxide nanowire preparation method according to claim 1 is characterized in that: the described technique that Gold plated Layer adopts on nucleopore membranes is the method for vacuum-evaporation.
3. zinc oxide nanowire preparation method according to claim 1 is characterized in that: described polycarbonate or polyester material adopt the dichloromethane solution dissolving after the zinc oxide nanowire preparation is completed.
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|---|---|---|---|
| CN 201110129855 CN102220596B (en) | 2011-05-19 | 2011-05-19 | Preparation method of nano zinc oxide wire |
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|---|---|---|---|
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|---|---|
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| CN102220596B true CN102220596B (en) | 2013-06-12 |
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|---|---|---|---|---|
| CN102912437B (en) * | 2012-07-20 | 2016-02-24 | 浙江工业大学 | Flower-shaped multilevel-structure zinc oxide support frame and its preparation method and application |
| CN114150264B (en) * | 2022-02-10 | 2022-04-26 | 中国科学院近代物理研究所 | Method for preparing metal quasi-nano lattice and prepared product |
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| US8324703B2 (en) * | 2007-04-30 | 2012-12-04 | University Of Maryland | Approach to contacting nanowire arrays using nanoparticles |
| CN101255600B (en) * | 2007-12-07 | 2011-11-23 | 合肥工业大学 | Method for preparing ZnO-based diluted magnetic semiconductor nano-wire array |
| CN101456579B (en) * | 2008-12-05 | 2010-11-17 | 天津大学 | Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method |
| CN101498051B (en) * | 2009-01-16 | 2010-09-08 | 北京大学 | Preparation of zinc oxide nano-wire array |
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