CN1234611C - Method for preparing zinc oxide nanometer material with orientation arrangement nano-tubes - Google Patents
Method for preparing zinc oxide nanometer material with orientation arrangement nano-tubes Download PDFInfo
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- CN1234611C CN1234611C CN 200410015987 CN200410015987A CN1234611C CN 1234611 C CN1234611 C CN 1234611C CN 200410015987 CN200410015987 CN 200410015987 CN 200410015987 A CN200410015987 A CN 200410015987A CN 1234611 C CN1234611 C CN 1234611C
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 42
- 239000002071 nanotube Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title description 30
- 239000000758 substrate Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002086 nanomaterial Substances 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 10
- 150000003751 zinc Chemical class 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract 3
- 238000002360 preparation method Methods 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical group C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 229960001296 zinc oxide Drugs 0.000 description 33
- 235000012239 silicon dioxide Nutrition 0.000 description 12
- 239000003921 oil Substances 0.000 description 7
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005352 clarification Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229960005196 titanium dioxide Drugs 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- -1 varistor Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
一种纳米管定向排列的氧化锌纳米材料的制备方法，首先将锌盐、氨水、硫脲和铵盐按一定比例溶于去离子水，制备成薄膜生长反应液，然后将处理过的基片浸入制备好的薄膜生长反应液中，在预超声35～40分钟后，升温至94～97℃，反应45～60分钟即可获得致密的具有定向排列的纳米管定向排列的氧化锌纳米材料。本发明方法操作简单、成本低，生产周期短，制备的纳米管定向排列的氧化锌纳米材料由定向排列的纳米管组成，纳米管平均直径为500nm，厚度100nm，长度6μm。A method for preparing zinc oxide nanomaterials with aligned nanotubes. First, zinc salt, ammonia water, thiourea and ammonium salt are dissolved in deionized water in a certain proportion to prepare a film growth reaction solution, and then the treated substrate is Immerse in the prepared film growth reaction solution, pre-sonicate for 35-40 minutes, heat up to 94-97° C., and react for 45-60 minutes to obtain dense zinc oxide nanomaterials with aligned nanotubes. The method of the invention has the advantages of simple operation, low cost and short production cycle, and the prepared nanotube oriented zinc oxide nanomaterial is composed of oriented nanotubes, the average diameter of the nanotubes is 500nm, the thickness is 100nm, and the length is 6μm.
Description
Technical field
The present invention relates to a kind of preparation method of nano zinc oxide material, relate in particular to the nano zinc oxide material preparation method that a kind of nanotube aligns, adopt the chemical solution growth method to prepare the nano zinc oxide material that nanotube aligns.
Background technology
Nano material's structure and pattern have very big influence to the performance and the application of nano material, and the nano crystal material of preparing ad hoc structure and pattern has important meaning for the frontier of developing the nano material function.In the numerous pattern of nano material (nanometer ball, nanometer rod, nano wire, nano belt, nanofiber, nanotube), nanotube becomes the focus of research because of its particular structure.Since carbon nanotube in 1991 came out, the nanotube of a large amount of simple substance (silicon, germanium, copper, antimony etc.) and compound (vanadium oxide, zinc oxide, silicon-dioxide, titanium dioxide, gan, boron nitride, aluminium nitride, silicon carbide, molybdenumdisulphide etc.) is preparing by success successively.Among these tubular nanometer materials, zinc oxide owing to have good light, electricity, magnetic property at the uv-absorbing material, photocatalyst material is widely used on functional nano material such as varistor, electrode materials, solar cell and the device, thereby enjoys attention.The appearance of zinc oxide nano mitron is for the functional development of nano zinc oxide material has brought new life.But the research of nano zinc oxide material has two weak points at present, and one is that the preparation method requires height.The preparation method of the zinc oxide nano mitron of having reported at present has only two kinds of vapor phase process and solvent-thermal methods.And these two kinds of methods need extreme exacting terms such as high temperature, high pressure or high vacuum, and these conditions have brought very adverse influence for the cost and the efficient of material preparation, thereby need to be improved or replace.The another one weak point is that the zinc-oxide nano tube material of preparing at present all is Powdered random dispersion, and the application for nano-device also has certain distance like this.And the piped nano material is aligned on the semiconductor material and will the application of nano-device be had great significance according to certain mode.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide a kind of simple to operate, the preparation method of the nano zinc oxide material that the nanotube that temperature of reaction is low, cost is low, production efficiency is high aligns.
For realizing such purpose, in the technical scheme of the present invention, adopt chemical solution method to prepare the nano zinc oxide material that nanotube aligns.The substrate of handling is immersed in zinc salt, ammoniacal liquor, thiocarbamide and the ammonium salt mixing solutions for preparing, after pre-ultrasonic 35～40 minutes, be warming up to 94～97 ℃, react the zinc-oxide nano tube material that aligns that has that can obtain densification in 45～60 minutes.The nano zinc oxide material that the nanotube of preparation aligns is made up of the nanotube that aligns, and the mean diameter of nanotube is 500nm, thickness 100nm, length 6 μ m.
Preparation method of the present invention comprises following concrete steps:
1. the preparation of film growth reaction solution: zinc salt, ammoniacal liquor, thiocarbamide and ammonium salt are dissolved in deionized water by a certain percentage, are prepared into the film growth reaction solution.Contain zinc salt 0.01mol, 25% (mass ratio) ammoniacal liquor 5ml, thiocarbamide 0.01mol and ammonium salt 0.002mol in every 100ml reaction solution.
The said zinc salt of the present invention is a zinc nitrate hexahydrate; Ammonium salt is an ammonium chloride.
2. the pre-treatment of substrate: at first substrate was immersed in the vitriol oil of ebullient 98% 5～10 hours, was immersed in then in the acetone ultrasonic 30～60 minutes, next use a large amount of deionized water rinsings, at last substrate is dried in vacuum drying oven, stand-by.
The said substrate of the present invention is sheet glass or quartz substrate.
3. the nano zinc oxide material that aligns of nanotube is synthetic: before reaction, at first substrate is soaked in the above-mentioned film growth reaction soln for preparing; Then reaction soln is placed ultrasonic device, ultrasonic 35-40 minute; Reaction system is warming up to 94～97 ℃ again, temperature rise rate 10～20 degree/minute, reacted 45～60 minutes down at 94～97 ℃.Reaction finishes the back cools off fast with frozen water, substrate is put in deionized water for ultrasonic 1～2 minute then, uses a large amount of deionized water rinsings, can obtain the nano zinc oxide material that nanotube aligns through drying naturally after repeatedly washing.
Excellent results of the present invention is:
1. owing to adopted the buffered soln of ammoniacal liquor and ammonium salt as reaction solution, make in the process of zinc oxide nano mitron crystal growth reaction soln pH value keep stable to a certain extent, this even growth of arranging for nanotube provides good growth sublimity, thereby the zinc oxide nano mitron good uniformity of preparation.
2. because the chemical solution method temperature of reaction that this patent adopts is low, have only 94～97 ℃, reaction times is short, the shortest need 45 minutes, reaction raw materials is cheap, only needs zinc salt, ammoniacal liquor and ammonium salt commonly used, thereby the inventive method is simple to operate, cost is low, the efficient height, the nano zinc oxide material that the nanotube of preparation aligns is 500 nanometers by diameter, thickness is that the nanotube of the hexagonal prism shape of 6 microns of 100 nanometers, length aligns composition.
Description of drawings
The x-ray diffraction pattern of the nano zinc oxide material that Fig. 1 aligns for the embodiment of the invention 1 resulting nanotube.
The energy spectrogram (EDS) of the nano zinc oxide material that Fig. 2 aligns for the embodiment of the invention 1 resulting nanotube.
The electron scanning micrograph of the nano zinc oxide material that Fig. 3 aligns for the embodiment of the invention 1 resulting nanotube, wherein a figure is a photomacrograph, b figure is the high power enlarged photograph.
Embodiment
The following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1
1. in the ptfe plastic bottle of a 100mL, 0.01mol zinc nitrate, 0.01mol thiocarbamide, 0.002mol ammonium chloride are dissolved in the 95mL deionized water, be stirred to the ammoniacal liquor that adds 5ml 25% after whole dissolvings, continue when adding to stir, just be prepared into the reaction solution of zinc-oxide film growth after the solution clarification.
2. quartz plate that will the wide 20mm of long 50mm is immersed in the ebullient vitriol oil, and soak and immerse again in the acetone soln after 10 hours, ultrasonic 30 minutes, use a large amount of deionized water rinsings again, it is dry to put into vacuum drying oven at last.
3. will be immersed in according to the quartz substrate that 2. step is handled according in the reaction solution that is 1. disposed, ultrasonic 35 minutes, then reaction flask is placed oil bath pan, according to 10 the degree/minute speed temperature of reaction is risen to 95 ℃, kept 45 minutes.Then quartz substrate is immersed in the frozen water territory and cools off.After the cooling quartz substrate is immersed in deionized water for ultrasonic 2 minutes, uses a large amount of deionized water rinsings again.To dry under the quartz substrate room temperature at last, promptly obtain the nano zinc oxide material that nanotube aligns.
X-ray diffraction spectrogram such as Fig. 1 of the nano zinc oxide material that resultant nanotube aligns.Prepared as seen from Figure 1 material is pure zinc oxide, does not have other impurity, and crystalline form is a hexagonal crystal shape.For further proof degree of purity of production, the element EDS that product has been carried out scanning electron microscope analyzes, and Fig. 2 is the EDS figure of product, and as seen from the figure, product has only zinc and two kinds of elements of oxygen, does not have the impurity of element such as other sulphur.Electron scanning micrograph such as Fig. 3, wherein a figure is the positive Electronic Speculum picture of prepared nano material, b figure is the amplification picture of a figure.Prepared as seen from the figure zinc oxide material is made up of the nanotube of hexagonal prism shape, and the diameter of zinc oxide nano mitron is about 500 nanometers, and thickness is 100 nanometers, about 6 microns of length, and length-to-diameter ratio is about 12.
Embodiment 2
1. in the ptfe plastic bottle of a 100mL, 0.01mol zinc nitrate, 0.01mol thiocarbamide, 0.002mol ammonium chloride are dissolved in the 95mL deionized water, be stirred to the ammoniacal liquor that adds 5ml 25% after whole dissolvings, continue when adding to stir, just be prepared into the reaction solution of zinc-oxide film growth after the solution clarification.
2. sheet glass that will the wide 20mm of long 50mm is immersed in the ebullient vitriol oil, and soak and immerse again in the acetone soln after 10 hours, ultrasonic 60 minutes, use a large amount of deionized water rinsings again, it is dry to put into vacuum drying oven at last.
3. will be immersed in according to the glass substrate that 2. step is handled according in the reaction solution that is 1. disposed, ultrasonic 40 minutes, then reaction flask is placed oil bath pan, according to 20 the degree/minute speed temperature of reaction is risen to 97 ℃, kept 50 minutes.Then glass substrate is immersed in the frozen water territory and cools off.After the cooling glass substrate is immersed in deionized water for ultrasonic 1 minute, uses a large amount of deionized water rinsings again.To dry under the glass substrate room temperature at last, promptly obtain the nano zinc oxide material that nanotube aligns.
1. in the ptfe plastic bottle of a 100mL, 0.01mol zinc nitrate, 0.01mol thiocarbamide, 0.002mol ammonium chloride are dissolved in the 95mL deionized water, be stirred to the ammoniacal liquor that adds 5ml 25% after whole dissolvings, continue when adding to stir, just be prepared into the reaction solution of the nano zinc oxide material growth that nanotube aligns after the solution clarification.
2. quartz plate that will the wide 20mm of long 50mm is immersed in the ebullient vitriol oil, and soak and immerse again in the acetone soln after 8 hours, ultrasonic 45 minutes, use a large amount of deionized water rinsings again, it is dry to put into vacuum drying oven at last.
3. will be immersed in according to the quartz substrate that 2. step is handled according in the reaction solution that is 1. disposed, ultrasonic 38 minutes, then reaction flask is placed oil bath pan, according to 15 the degree/minute speed temperature of reaction is risen to 94 ℃, kept 60 minutes.Then quartz substrate is immersed in the frozen water territory and cools off.After the cooling quartz substrate is immersed in deionized water for ultrasonic 1 minute, uses a large amount of deionized water rinsings again.To dry under the quartz substrate room temperature at last, promptly obtain the nano zinc oxide material that nanotube aligns.
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410015987 CN1234611C (en) | 2004-01-19 | 2004-01-19 | Method for preparing zinc oxide nanometer material with orientation arrangement nano-tubes |
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| CN 200410015987 CN1234611C (en) | 2004-01-19 | 2004-01-19 | Method for preparing zinc oxide nanometer material with orientation arrangement nano-tubes |
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| CN1557718A CN1557718A (en) | 2004-12-29 |
| CN1234611C true CN1234611C (en) | 2006-01-04 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2649200C (en) * | 2005-04-14 | 2015-06-30 | Tallinn University Of Technology | Method of preparing zinc oxide nanorods on a substrate by chemical spray pyrolysis |
| CN100366793C (en) * | 2005-06-13 | 2008-02-06 | 中国科学院理化技术研究所 | Method and device for preparing doped single crystal zinc oxide nanotubes by vapor deposition |
| CN100360420C (en) * | 2005-11-02 | 2008-01-09 | 东南大学 | Method for growing nanotube-type zinc oxide by hydrothermal decomposition |
| 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 |
| CN100447089C (en) * | 2006-10-25 | 2008-12-31 | 哈尔滨工程大学 | Ultrasonic preparation method of zinc oxide nanotubes |
| CN100453711C (en) * | 2006-12-15 | 2009-01-21 | 付敏恭 | Zn0 crystallite material, and preparation method |
| CN103101961A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of zinc oxide nanotube array |
| CN104003434B (en) * | 2014-06-16 | 2015-10-21 | 安徽师范大学 | A three-dimensional self-assembled zinc oxide nano-heterogeneous material, preparation method and application thereof |
| CN113292249B (en) * | 2021-05-28 | 2022-05-03 | 厦门大学 | MoS2/ZnO/Ag2Preparation method of S coaxial nanotube array |
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