CN101941732A - Mass production method of zinc oxide nanowires - Google Patents
Mass production method of zinc oxide nanowires Download PDFInfo
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- CN101941732A CN101941732A CN 201010501373 CN201010501373A CN101941732A CN 101941732 A CN101941732 A CN 101941732A CN 201010501373 CN201010501373 CN 201010501373 CN 201010501373 A CN201010501373 A CN 201010501373A CN 101941732 A CN101941732 A CN 101941732A
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Abstract
The invention relates to a mass production method of zinc oxide nanowires in the technical field of the semiconductor nanometer material. The method comprises the following steps: selecting proper zinc source and oxygen source to ensure that zinc oxide and activated carbon fully react in a high temperature state and zinc is prepared by the reduction of carbon, and performing the recrystallization and preferred growth of zinc under the action of carrier gas and the mixed oxygen to obtain zinc oxide nanowires. The method of the invention has simple process, low cost and environmental friend, and is suitable for industrialized production.
Description
Technical field
What the present invention relates to is a kind of method of semiconductor nano material technical field, specifically is a kind of mass production method of zinc oxide nanowire.
Background technology
Zinc oxide (ZnO) is a kind of direct band-gap semicondictor material, has hexagonal wurtzite-type structure, and its energy gap at room temperature is 3.37eV.One-D nano zinc oxide is because small-size effect, its surface electronic structure and crystalline structure change, and have characteristics such as surface effects, volume effect, tunnel effect and quantum size effect that the common zinc oxide material do not have and polymolecularity, high-clarity.Show many special excellent specific properties in recent years, make it great application prospect and value be arranged in many fields such as medicine, biology, optics, chemical industry, electronics, potteries at aspects such as catalysis, optics, magnetics, mechanics.Nano zine oxide possesses the not available light of conventional common zinc oxide material, electricity, magnetic, thermal characteristics, product is active high, have sterilization, counter infrared ray and ultraviolet function, be widely used in the products such as shielding material, sanitary ware, sewage disposal and photocatalyst of sun-proof type makeup, antibacterial deodourizing and anti-ultraviolet new function fiber, self-cleaning antibacterial glass, pottery, anti-infrared, ultraviolet at present.
At present, a large amount of preparation methods of the nano zine oxide of having reported mainly are the preparation nano zinc oxide particles.Nano wire is compared and nanoparticle, has outstanding, excellent more performance.Find through literature search prior art, C.Y.Chang etc. are since 2006 the 88th volumes of " Appliedphysics letters " (Applied Physics communication) the 17th phase the 173503rd～173503-3 page or leaf is delivered " Electroluminescence from ZnO nanowire/polymer composite p-n junction " (electroluminescent of the compound p-n junction of Zinc oxide nano wire/polymer), and scientists has been studied based on the photodiode of zinc oxide nanowire film (LED), based on Field Emission Display (FED) de of zinc oxide nanowire etc. and show excellent performance.Yet,, still rest on laboratory stage and practicability in a large number based on the device of zinc oxide nanowire because a large amount of preparation zinc-oxide nano line technologies lack.
Therefore, a kind of preparation method that can prepare zinc oxide nanowire in a large number fast of exploitation has important scientific research and using value.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of mass production method of zinc oxide nanowire is provided, by selecting suitable zinc source, oxygen source, under the condition of high temperature, zinc oxide and activated carbon fully react, and carbon reduction goes out zinc, then under the effect of the oxygen that is mixed with in carrier gas of zinc, again the crystallization preferential growth obtains zinc oxide nanowire.Technology of the present invention is simple, and with low cost, environmental friendliness is fit to suitability for industrialized production.
The present invention is achieved by the following technical solutions, the present invention with zinc source power and carbon dust mixing and ball milling after under the nitrogen oxygen mixed gas environment sintering obtain zinc oxide nanowire.
The purity of described zinc source power is zinc, zinc oxide or the zinc carbonate of 99.999%wt;
The purity of described carbon dust is bamboo charcoal, gac or the carbon fiber of 99.999%wt;
Described mixing and ball milling is meant: is (0.5～1.5) with zinc source power and carbon dust with mass ratio: the mixed of (0.5～1.5), employing pure nitrogen gas or argon gas are used planetary ball mill ball milling 6～24 hours with 50～300rpm after charging into ball grinder and excluding air;
Described sintering is meant: nitrogen oxygen mixed gas is fed tube furnace and be warmed up to 800 ℃～1100 ℃ afterreactions 10～60 minutes.
Described nitrogen oxygen mixed gas is meant: the gas flow ratio of nitrogen and oxygen is (1～30ml/min): (1～3L/min).
A large amount of ZnO nano wires that preparation method of the present invention is prepared have overcome prior art and can only prepare the shortcoming of several micrograms to several milligrams of zinc oxide nanowires on substrates, can once prepare a large amount of zinc oxide nanowires fast.Present device requires simple, and green non-pollution in the preparation process is fit to large-scale industrialization production.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the zinc oxide nanowires that prepare in a large number with the inventive method institute.
Fig. 2 is the sem photograph of the sample that obtains with the inventive method embodiment 1.
Fig. 3 is the sem photograph of the sample that obtains with the inventive method embodiment 2.
Fig. 4 is the sem photograph of the sample that obtains with the inventive method embodiment 3.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
With high-purity oxide powder and zinc, quality of activated carbon ratio is 1: 1 thorough mixing, ball milling 15 hours under high pure nitrogen protection then, and the material that ball milling is good is put in the ceramic boat, and the ceramic boat that will be placed with material is again put into tube furnace.Tube furnace feeds the mixed gas be made up of high pure nitrogen (99.999%) and high purity oxygen gas (99.999%) (high purity oxygen gas flow: 20ml/min, high pure nitrogen flow: the 2L/min) carrier gas of Zu Chenging, and be rapidly heated 950 then
℃After, reacted a large amount of white cotton flower shape zinc oxide nano wires that in reaction process, can obtain spraying at the tubular type fire door 35 minutes., the electron scanning micrograph of material such as accompanying drawing 3.
As can be seen from Figure 1, present method the ZnO nano wires of a large amount of preparations consistent with standard diagram ZnO JCPDS 65-3411.
Embodiment 2
With high-purity zinc powder, bamboo charcoal mass ratio is 0.5: 1.5 thorough mixing, ball milling 6 hours under high-purity argon gas protection then, and the material that ball milling is good is put in the quartz boat, and the ceramic boat that will be placed with material is again put into tube furnace.Tube furnace feeds the mixed gas be made up of high pure nitrogen (99.999%) and high purity oxygen gas (99.999%) (high purity oxygen gas flow: 1ml/min, high pure nitrogen flow: the 1L/min) carrier gas of Zu Chenging, and be rapidly heated 800 then
℃After, reacted a large amount of white cotton flower shape zinc oxide nano wires that in reaction process, can obtain spraying at the tubular type fire door 10 minutes., the electron scanning micrograph of material such as accompanying drawing 4.
Embodiment 3
With high-purity carbonic acid zinc powder, carbon fiber mass ratio is 1.5: 0.5 thorough mixing, ball milling 24 hours under high pure nitrogen protection then, and the material that ball milling is good is put in the quartz boat, and the ceramic boat that will be placed with material is again put into tube furnace.Tube furnace feeds the mixed gas be made up of high pure nitrogen (99.999%) and high purity oxygen gas (99.999%) (high purity oxygen gas flow: 30ml/min, high pure nitrogen flow: the 3L/min) carrier gas of Zu Chenging, and be rapidly heated 1100 then
℃After, reacted a large amount of white cotton flower shape zinc oxide nano wires that in reaction process, can obtain spraying at the tubular type fire door 60 minutes., the electron scanning micrograph of material such as accompanying drawing 5.
Claims (4)
1. the mass production method of a zinc oxide nanowire, it is characterized in that, with after zinc source power and the carbon dust mixing and ball milling under the nitrogen oxygen mixed gas environment sintering obtain zinc oxide nanowire, described sintering is meant: nitrogen oxygen mixed gas is fed tube furnace and be warmed up to 800 ℃～1100 ℃ afterreactions 10～60 minutes; Described nitrogen oxygen mixed gas is meant: the gas flow ratio of nitrogen and oxygen is (1～30ml/min): (1～3L/min).
2. the mass production method of zinc oxide nanowire according to claim 1 is characterized in that, the purity of described zinc source power is zinc, zinc oxide or the zinc carbonate of 99.999%wt.
3. the mass production method of zinc oxide nanowire according to claim 1 is characterized in that, the purity of described carbon dust is bamboo charcoal, gac or the carbon fiber of 99.999%wt.
4. the mass production method of zinc oxide nanowire according to claim 1, it is characterized in that, described mixing and ball milling is meant: is (0.5～1.5) with zinc source power and carbon dust with mass ratio: the mixed of (0.5～1.5), employing pure nitrogen gas or argon gas are used planetary ball mill ball milling 6～24 hours with 50～300rpm after charging into ball grinder and excluding air.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318946A (en) * | 2013-06-04 | 2013-09-25 | 上海大学 | Method of preparing ZnO nano-line with higher length-diameter ratio through carbon thermal reduction technology |
| CN103449505A (en) * | 2013-08-28 | 2013-12-18 | 哈尔滨工业大学（威海） | Preparation method of nano zinc oxide material |
| CN103523817A (en) * | 2013-10-30 | 2014-01-22 | 刘景顺 | Zinc oxide nano-wire and preparation method thereof |
| CN104986792A (en) * | 2015-06-13 | 2015-10-21 | 温州生物材料与工程研究所 | Method for preparing na-doped p-type zinc oxide nanowire with assistance of graphene |
| CN105129840A (en) * | 2015-07-17 | 2015-12-09 | 兰州思雪纳米科技有限公司 | Method of preparing monocrystal zinc oxide nano wire at high yield |
| CN106374013A (en) * | 2016-11-19 | 2017-02-01 | 西北工业大学 | Preparation method of MgZnO nanowire array for ultraviolet photoelectric detectors |
| CN112299471A (en) * | 2020-11-25 | 2021-02-02 | 中南大学 | Method for synchronously preparing nano zinc oxide by efficiently separating zinc from zinc-containing electronic waste |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407335A (en) * | 2008-08-27 | 2009-04-15 | 上海理工大学 | Method for preparing zinc oxide nano-wire by using zinc nano-particle |
| KR20090097244A (en) * | 2008-03-11 | 2009-09-16 | 금오공과대학교 산학협력단 | Zinc oxide nano wire and method for manufacturing the same |
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2010
- 2010-10-11 CN CN 201010501373 patent/CN101941732A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20090097244A (en) * | 2008-03-11 | 2009-09-16 | 금오공과대학교 산학협력단 | Zinc oxide nano wire and method for manufacturing the same |
| CN101407335A (en) * | 2008-08-27 | 2009-04-15 | 上海理工大学 | Method for preparing zinc oxide nano-wire by using zinc nano-particle |
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| 《云南化工》 20071231 白慧萍 等 氧化锌纳米线的制备及其应用研究 49-53 1-4 第34卷, 第6期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318946A (en) * | 2013-06-04 | 2013-09-25 | 上海大学 | Method of preparing ZnO nano-line with higher length-diameter ratio through carbon thermal reduction technology |
| CN103449505A (en) * | 2013-08-28 | 2013-12-18 | 哈尔滨工业大学（威海） | Preparation method of nano zinc oxide material |
| CN103523817A (en) * | 2013-10-30 | 2014-01-22 | 刘景顺 | Zinc oxide nano-wire and preparation method thereof |
| CN103523817B (en) * | 2013-10-30 | 2016-03-02 | 刘景顺 | A kind of zinc oxide nanowire and preparation method thereof |
| CN104986792A (en) * | 2015-06-13 | 2015-10-21 | 温州生物材料与工程研究所 | Method for preparing na-doped p-type zinc oxide nanowire with assistance of graphene |
| CN105129840A (en) * | 2015-07-17 | 2015-12-09 | 兰州思雪纳米科技有限公司 | Method of preparing monocrystal zinc oxide nano wire at high yield |
| CN106374013A (en) * | 2016-11-19 | 2017-02-01 | 西北工业大学 | Preparation method of MgZnO nanowire array for ultraviolet photoelectric detectors |
| CN112299471A (en) * | 2020-11-25 | 2021-02-02 | 中南大学 | Method for synchronously preparing nano zinc oxide by efficiently separating zinc from zinc-containing electronic waste |
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