CN103422155A - Method for preparing compact single crystal ZnO nanowire in porous template - Google Patents
Method for preparing compact single crystal ZnO nanowire in porous template Download PDFInfo
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- CN103422155A CN103422155A CN2013103945323A CN201310394532A CN103422155A CN 103422155 A CN103422155 A CN 103422155A CN 2013103945323 A CN2013103945323 A CN 2013103945323A CN 201310394532 A CN201310394532 A CN 201310394532A CN 103422155 A CN103422155 A CN 103422155A
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- die plate
- foraminous die
- porous
- single crystal
- zno
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- 239000002070 nanowire Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000013078 crystal Substances 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000003751 zinc Chemical class 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 239000004697 Polyetherimide Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229920001601 polyetherimide Polymers 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 150000003503 terephthalic acid derivatives Chemical class 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 abstract 4
- 235000010299 hexamethylene tetramine Nutrition 0.000 abstract 2
- 239000004312 hexamethylene tetramine Substances 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 93
- 239000011787 zinc oxide Substances 0.000 description 45
- 230000005540 biological transmission Effects 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 4
- 230000018199 S phase Effects 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a method for preparing a compact monocrystal ZnO nanowire in a porous template. Mainly through a double-chamber reactor, a porous template is arranged in the center of the reactor to divide the reactor into a double-chamber structure with equal volume. Respectively injecting zinc salt and Hexamethylenetetramine (HMT) solution with the same volume of 0.01-0.04 mol/L and 0.01-0.04 mol/L into two single chambers. And then the whole system is placed in a water bath at the temperature of 75-95 ℃ to be heated for 24-96 h. And finally, taking out the porous template, cleaning and drying. The method has the advantages of simple equipment, no special equipment, easy operation, uniform, compact and continuous prepared single crystal ZnO nanowire, low cost, obvious control effect and suitability for large-scale production.
Description
Technical field:
The present invention relates to a kind of method for preparing the single crystal ZnO nano wire, relate in particular to the method for the fine and close single crystal ZnO nano wire of preparation in a kind of foraminous die plate.
Background technology:
ZnO is the important low-cost semiconductor material of II-VI, is widely used in catalyzer, pressure-sensitive device, and photoelectron and photoelectrochemistry, receive people's concern this year.ZnO is higher at the visible region transmittance, suitably after doping, can conduct electricity, and this specific character is widely studied the transparency conductive electrode for flat-panel monitor and solar cell.ZnO structure and lattice dimensions and semi-conductor GaN are very approaching, so the two buffer layer or substrate each other, and this has more expanded the range of application of ZnO.
Foraminous die plate, because its cost is lower, controllability is good, has the nano level cylindrical cavity of uniform and ordered, and hole density is up to 10
9～10
12/ cm
2, the diameter in hole is about 5～200nm, and aperture is controlled, and hole depth is adjustable, has the preparation that good thermostability, chemical stability and the higher advantages such as thermal conductivity (046W/cmK) are widely used in monodimension nanometer material simultaneously.
At present, in template, making ZnO nano wire method mainly contains: electrochemical process, sol-gel method, physics or chemical Vapor deposition process, electrophoretic method etc.These procedures are loaded down with trivial details at present, and cost is higher, and the ZnO nano-wire major part of preparation belongs to polycrystalline structure.
Li Liang adopts the method for galvanic deposit to form gold plate on the foraminous die plate surface, then by the method for electrochemical deposition, has prepared ZnO nano-wire.This method need to be used electrochemical workstation, is unfavorable for simple, low-cost, the scale operation of ZnO nano-wire.
Gobinda Gopal Khan adopts in the simple wet chemistry method duct well distributed at AAO and prepares zinc oxide nano-wire array.Zinc oxide nanowire and AAO template table reveal very strong PL characteristic.But ZnO nano-wire prepared by the method is polycrystalline structure.
This seminar once utilized vulkacit H and soluble Zn reactant salt preparation zinc ammonia complex solution, then porous anodic alumina template directly was immersed in precursor solution while counting to last water-bath making ZnO nano wire.The nano-wire array of preparation presents discontinuity, is unsound.
Summary of the invention:
The objective of the invention is to provide in order to improve the deficiencies in the prior art the method for the fine and close single crystal ZnO nano wire of preparation in a kind of foraminous die plate.It is simple that the method has preparation technology, and low cost is applicable to extensive advantage of growing, and most critical is can in foraminous die plate, prepare to have the fine and close ZnO nano-wire of single crystal structure continuously.
Technical scheme of the present invention is: a kind of method of the fine and close single crystal ZnO nano wire of preparation in foraminous die plate, and its concrete steps are as follows:
Foraminous die plate is placed in reactor central authorities, and it is divided into to isopyknic double-chamber structure; By equal-volume concentration, be that 0.01～0.04mol/L zinc salt and 0.01～0.04mol/L vulkacit H solution are injected into respectively two single chambers; Then whole system is placed in to 75～95 ℃ of waters bath with thermostatic control and heats 24～96h; Finally foraminous die plate is taken out, clean, dry.
Channel diameter 80～150nm in preferred described foraminous die plate, hole density is up to 10
9～10
12/ cm
2.Preferred described foraminous die plate is porous anodic alumina template, porous polyimide film, porous polyetherimide film, porous PEN or porous poly terephthalic acid class plastics film.Preferred described zinc salt is zinc acetate, zinc nitrate or zinc chloride etc.
Preferred above-mentioned cleaning process is for first using the deionized water washed product 3～5 times, then uses absolute ethanol washing 3～5 times.Preferably above-mentioned bake out temperature is 60～90 ℃.
Beneficial effect:
1. the shortcomings such as the traditional technology of making ZnO nano wire exists preparation process loaded down with trivial details in foraminous die plate, and cost is higher.Maximum characteristics of the present invention are to utilize the membrane cisterna method can in foraminous die plate, prepare fine and close continuous single crystal ZnO nano wire.
2. the inventive method equipment used is simple, does not use large-scale or specific equipment, and technical threshold is low, easy handling, and cost is low, is suitable for scale operation.
The accompanying drawing explanation:
Fig. 1 is the schematic diagram of the standby ZnO nano-wire of the membrane cisterna legal system that provides of the embodiment of the present invention; Wherein A is foraminous die plate, and B is water-bath;
Fig. 2 is ZnO nano-wire/foraminous die plate packaging assembly XRD figure; Wherein a is that embodiment 1 is prepared, and b is that embodiment 2 is prepared, and c is that embodiment 3 is prepared;
Fig. 3 is the profile scanning Electronic Speculum figure that the prepared foraminous die plate of embodiment 1 is filled ZnO nano-wire;
The transmission scanning electron microscope figure that Fig. 4 is the prepared ZnO nano-wire of embodiment 1 and electronic selection area diffraction figure;
Wherein a is ZnO nano-wire transmission scanning electron microscope figure; B is ZnO electronic selection area diffraction figure.
Embodiment:
To contribute to understand the present invention by following example, but not limit content of the present invention.
Embodiment 1
Two chambers reactor is made by Teflon, and diameter is about 120nm, and hole density is about 10
9/ cm
2Porous anodic alumina template be placed in the central authorities of square reactor, it is divided into to isopyknic double-chamber structure.Configure respectively mole 0.01mol/L Zn (CH such as 100ml
3COO)
22H
2O and vulkacit H solution.Then above-mentioned solution slowly is injected into respectively to two single chambers.Again whole system is placed in to 85 ℃ of waters bath with thermostatic control and heats 24h.Finally foraminous die plate is taken out, use respectively deionized water wash 4 times and absolute ethanol washing 3 times, then 80 ℃ of oven dry.Fig. 2 a is the present embodiment making ZnO/foraminous die plate packaging assembly XRD diffractogram, and the spectral line peak in figure conforms to substantially with JCPDS No.36-1451 card, and in the XRD diffracting spectrum, three characteristic strong peaks appear at 2 θ=31.2 °, 34.20 °, 35.60 °; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, and the diffraction peak of weak ZnO (102), (110), (103) face occurs near 47.5 °, 56.6 °, 62.9 °, show that prepared sample is six side's phase ZnO.The profile scanning Electronic Speculum figure that Fig. 3 is this example making ZnO in foraminous die plate, visible ZnO nano-wire densification is deposited in foraminous die plate.Fig. 4 a, for breaking away from the transmission scanning electron microscope figure of the single ZnO nano-wire of template, shows that the diameter of nano wire is about 120nm.The electronic selection zone collection of illustrative plates that Fig. 4 b is nano wire, show that the ZnO nano-wire of preparation is single crystal structure.
Two chambers reactor is made by Teflon, and diameter is about 100nm, and hole density is about 10
10/ cm
2The Kapton foraminous die plate be placed in the central authorities of square reactor, it is divided into to isopyknic double-chamber structure.Configure respectively mole 0.02mol/L ZnCl such as 100ml
2With vulkacit H solution.Then above-mentioned solution slowly is injected into respectively to two single chambers.Again whole system is placed in to 75 ℃ of waters bath with thermostatic control and heats 48h.Finally foraminous die plate is taken out, use respectively deionized water wash 3 times and absolute ethanol washing 3 times, then 70 ℃ of oven dry.Fig. 2 b is the present embodiment making ZnO/foraminous die plate packaging assembly XRD diffractogram, and the spectral line peak in figure conforms to substantially with JCPDS No.36-1451 card, and in the XRD diffracting spectrum, three characteristic strong peaks appear at 2 θ=31.2 °, 34.20 °, 35.60 °; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, and the diffraction peak of weak ZnO (102), (110), (103) face occurs near 47.5 °, 56.6 °, 62.9 °, show that prepared sample is six side's phase ZnO.Profile scanning Electronic Speculum figure has confirmed that the ZnO nano-wire densification is deposited in the Kapton foraminous die plate.Transmission scanning electron microscope characterizes and breaks away from the single ZnO nano-wire of template, and result shows that the diameter of nano wire is about 100nm.Electronic selection zone collection of illustrative plates has confirmed that the ZnO nano-wire of preparation is single crystal structure.
Embodiment 3
Two chambers reactor is made by Teflon, and diameter is about 150nm, and hole density is about 10
12/ cm
2The polyetherimide foraminous die plate be placed in the central authorities of square reactor, it is divided into to isopyknic double-chamber structure.Configure respectively mole 0.04mol/L Zn (NO such as 100ml
3)
2With vulkacit H solution.Then above-mentioned solution slowly is injected into respectively to two single chambers.Again whole system is placed in to 95 ℃ of waters bath with thermostatic control and heats 64h.Finally foraminous die plate is taken out, use respectively deionized water wash 5 times and absolute ethanol washing 3 times, then 90 ℃ of oven dry.Fig. 2 c is the present embodiment making ZnO/foraminous die plate packaging assembly XRD diffractogram, and the spectral line peak in figure conforms to substantially with JCPDS No.36-1451 card, and in the XRD diffracting spectrum, three characteristic strong peaks appear at 2 θ=31.2 °, 34.20 °, 35.60 °; (100), (002), (101) face of these three the corresponding ZnO of strong peak difference, and the diffraction peak of weak ZnO (102), (110), (103) face occurs near 47.5 °, 56.6 °, 62.9 °, show that prepared sample is six side's phase ZnO.Profile scanning Electronic Speculum figure has confirmed that the ZnO nano-wire densification is deposited in the polyetherimide foraminous die plate.Transmission scanning electron microscope characterizes and breaks away from the single ZnO nano-wire of template, and result shows that the diameter of nano wire is about 150nm.Electronic selection zone collection of illustrative plates has confirmed that the ZnO nano-wire of preparation is single crystal structure.
Claims (6)
1. the method for the fine and close single crystal ZnO nano wire of preparation in a foraminous die plate, its concrete steps are as follows:
Foraminous die plate is placed in reactor central authorities, and it is divided into to isopyknic double-chamber structure; By equal-volume concentration, be that 0.01～0.04mol/L zinc salt and 0.01～0.04mol/L vulkacit H solution are injected into respectively two single chambers; Then whole system is placed in to 75～95 ℃ of waters bath with thermostatic control and heats 24～96h; Finally foraminous die plate is taken out, clean, dry.
2. method according to claim 1, is characterized in that the channel diameter on foraminous die plate is 80～150nm, and hole density is 10
9～10
12/ cm
2.
3. method according to claim 1, is characterized in that described foraminous die plate is porous anodic alumina template, porous polyimide film, porous polyetherimide film, porous PEN or porous poly terephthalic acid class plastics film.
4. method according to claim 1, is characterized in that described zinc salt is zinc acetate, zinc nitrate or zinc chloride.
5. method according to claim 1, is characterized in that cleaning as first using the deionized water washed product 3～5 times, then use absolute ethanol washing 3～5 times.
6. method according to claim 1, is characterized in that described bake out temperature is 60～90 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104815566A (en) * | 2015-04-28 | 2015-08-05 | 南京工业大学 | Preparation method of antibacterial dust removal film |
| CN112271247A (en) * | 2020-10-26 | 2021-01-26 | 中国科学院微电子研究所 | Pressure sensor based on thin film transistor and preparation method thereof |
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| CN102476823A (en) * | 2010-11-23 | 2012-05-30 | 国家纳米科学中心 | Zinc oxide micro-nano array and preparation method thereof |
| CN102492987A (en) * | 2011-12-23 | 2012-06-13 | 南京工业大学 | Method for growing ZnO nanowire array on flexible substrate by solution method |
| CN102949981A (en) * | 2011-08-17 | 2013-03-06 | 香港城市大学 | Porous substrate and one-dimensional nano-material composite material and its preparation method, and surface-modified composite material and its preparation method |
-
2013
- 2013-09-03 CN CN2013103945323A patent/CN103422155A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20100278720A1 (en) * | 2009-05-04 | 2010-11-04 | Wong Stanislaus S | Methods of Making Binary Metal Oxide Nanostructures and Methods of Controlling Morphology of Same |
| CN101974781A (en) * | 2010-11-08 | 2011-02-16 | 上海大学 | Method for preparing ZnO nano-rod array at normal temperature and normal pressure |
| CN102476823A (en) * | 2010-11-23 | 2012-05-30 | 国家纳米科学中心 | Zinc oxide micro-nano array and preparation method thereof |
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| CN102949981A (en) * | 2011-08-17 | 2013-03-06 | 香港城市大学 | Porous substrate and one-dimensional nano-material composite material and its preparation method, and surface-modified composite material and its preparation method |
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Cited By (2)
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| CN104815566A (en) * | 2015-04-28 | 2015-08-05 | 南京工业大学 | Preparation method of antibacterial dust removal film |
| CN112271247A (en) * | 2020-10-26 | 2021-01-26 | 中国科学院微电子研究所 | Pressure sensor based on thin film transistor and preparation method thereof |
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