CN100431970C - Method and device for preparing zinc oxide nano-crystal by microwave induced adulterant oxidation - Google Patents
Method and device for preparing zinc oxide nano-crystal by microwave induced adulterant oxidation Download PDFInfo
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- CN100431970C CN100431970C CNB2005100950645A CN200510095064A CN100431970C CN 100431970 C CN100431970 C CN 100431970C CN B2005100950645 A CNB2005100950645 A CN B2005100950645A CN 200510095064 A CN200510095064 A CN 200510095064A CN 100431970 C CN100431970 C CN 100431970C
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- reaktionsofen
- zinc oxide
- microwave
- hotchpotch
- crystal
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Abstract
The present invention relates to a method for preparing zinc oxide nanometer crystals, and a device. The device is composed of an O2 flowmeter, an Ar flowmeter, a reaction furnace and a heating furnace, and metallic zinc powder, a reaction cabin, small holes, microwaves, a K9 glass window, a reaction furnace, a vacuum pump, a base, a substrate, an adulterant metal plate and a working table are arranged in the device. In the present invention, the heat effect of the microwaves is used for heating adulterants to certain temperature above vaporization temperature for producing high-temperature plasma. Moreover, the plasma is partially expanded in a fixed direction, and reacts with oxygen and metallic zinc fume traveling along an Ar airflow in the reaction furnace. According to the action time difference of the microwaves and the metallicity of the adulterants, various zinc oxide nanometer crystals with particular shapes and the identical quality, such as nanometer threads, nanometer towers, nanometer particles, etc. are generated.
Description
Technical field:
The invention belongs to technical field of ceramic material, relate to the preparation method and the device of zinc oxide nano-crystal, refer in particular to a kind of method and apparatus that adopts preparing zinc oxide nano-crystal by microwave induced adulterant oxidation.
Background technology:
Common zinc oxide nano-crystal technology of preparing is to adopt physical vaporous deposition (PVD), chemical Vapor deposition process (CVD), pulsed laser deposition methods such as (PLD) that the temperature of metal zinc is raise, make the zinc powder vaporization, and the gas O in the reaction tubes (Reaktionsofen)
2React, return to room temperature after being incubated for some time then, zincite crystal deposits in the substrate (such as silicon chip).Some other metal ion is as additive or catalyzer if mix in reaction process, and nanocrystalline cognition shape of the ZnO of generation and different in kind have purposes widely.
200510094605.2) and the preparation method of ZnOw and device (application number: 94107349.1) thereof with the method and apparatus of the most approaching a kind of coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal of the present invention (number of patent application:, the former provides a kind of method and apparatus of coaxial oxygen transporting laser irradiation in-situ preparing zinc oxide nano-crystal, the preparation technology of zinc oxide nano-crystal is simplified, be easy to control, reduce the cost of preparation zinc oxide nano-crystal.This method be with the laser beam direct irradiation on the metal zine plate, by the position of controlling laser parameter (irradiation time, power etc.), oxygen concentration and passing through to move and rotate the control worktable, go out the nano zine oxide crystal of different dimensions in the surperficial direct growth of zine plate: the The latter chemical Vapor deposition process prepares four horn shape whiskers or single fibrous whisker zinc oxide nano-crystal.But the former exists the nano whisker of different dimensions to be difficult to separate, and the latter is because experiment condition is limit, and the zinc oxide nano-crystal shape and the character of generation are limited.
Summary of the invention:
The present invention seeks to provide a kind of method and apparatus of preparing zinc oxide nano-crystal by microwave induced adulterant oxidation, process furnace is heated to certain temperature, make metal zinc be vaporized into zinc fume, along with argon gas stream mobile direction moves to Reaktionsofen, at the doped metal ion of exit and microwave heating effect generation and the O that carries by under meter control
2React,, generate the on all four zinc oxide nano-crystal of multiple specific morphology and character according to the difference of experiment condition.
The invention is characterized in the heat effect of utilizing microwave reach tungsten, cobalt, manganese, aluminium, erbium fast, more than the indium metal hotchpotch vaporization temperature, make these metalic contamination vaporizations, form plasma body, as the hotchpotch that generates the ZnO nanocrystal, take place to answer with zinc fume and Oxygen Flow along with argon gas stream, the substrate deposition of placing at the left end of Reaktionsofen generates shape and the on all four ZnO nanocrystal of character, wherein control oxygen and argon flow amount speed is respectively 10～20sccm and 20～30sccm, and keep the air pressure of 2～4Torr in the stove.Argon gas can be used for keeping suitable gaseous tension in the whole stove on the one hand, and on the other hand, mobile metallic zinc steam in the process furnace can being transferred in the Reaktionsofen of argon gas reacts with hotchpotch metal ion and oxygen.
The device of implementing this method comprises O
2The metal zinc of under meter, Ar under meter, Reaktionsofen, process furnace and the portion that sets within it, reaction cabin, aperture, microwave, K9 glass port, Reaktionsofen, vacuum pump, pedestal, substrate (deposit apex), hotchpotch powder and worktable are formed, wherein the K9 glass port is set on the top of Reaktionsofen, be provided with the worktable of placing the hotchpotch powder at the take over middle part of position of Reaktionsofen, above the Reaktionsofen of answering, be provided with microwave rf generator with it, be provided with the pedestal of placing substrate at the middle part of the position of taking back of Reaktionsofen, be connected with O at the rear of Reaktionsofen
2Under meter is at the left end connection vacuum pump of Reaktionsofen.Right side at process furnace connects the Ar under meter, is provided with the reaction cabin of placing metal zinc at the middle part of process furnace.
The invention has the advantages that:
(1) utilize the heat effect of microwave to reach tungsten, cobalt, manganese, aluminium, erbium, indium etc. fast more than the metalic contamination vaporization temperature, make metalic contamination vaporizations such as tungsten, cobalt, manganese, aluminium, erbium, indium, forming plasma body, as the hotchpotch that generates zinc oxide nano-crystal, is technologic innovation.
(2) utilize metalic contamination vaporizations such as tungsten that the heat effect of microwave radiation forms, cobalt, manganese, aluminium, erbium, indium, form plasma body, as the hotchpotch that generates zinc oxide nano-crystal, difference according to experiment condition, can generate the multiple zinc oxide nano-crystal that traditional method can not produce, such as nano wire, nanometer tower, nano particle etc.
Description of drawings:
The invention will be further described below in conjunction with Fig. 1:
A kind of microwave induced Doped Tungsten oxidation of Fig. 1 prepares the zinc oxide nano-crystal schematic representation of apparatus
The pattern of the ZnO nanocrystal that Fig. 2 hotchpotch prepares during for tungsten
The pattern of the ZnO nanocrystal that Fig. 3 hotchpotch prepares during for cobalt
The pattern of the ZnO nanocrystal that Fig. 4 hotchpotch prepares during for manganese
The pattern of the ZnO nanocrystal that Fig. 5 hotchpotch prepares during for erbium
The pattern of the ZnO nanocrystal that Fig. 6 hotchpotch prepares during for aluminium
The pattern of the ZnO nanocrystal that Fig. 7 hotchpotch prepares during for indium
1.Ar under meter 2. process furnace 3. metal zincs 4. reaction cabins 5. apertures 6. microwave 7.K9 glass port 8.O
2Under meter
9. Reaktionsofen 10. vacuum pumps 11. pedestals 12. substrates 13. hotchpotch metal sheets 14. worktable
Embodiment:
Describe the details and the working condition of the concrete device of the present invention's proposition in detail below in conjunction with accompanying drawing.
Carrying out gaseous oxidation with the present invention prepares the zinc oxide nano-crystal device and comprises: Ar under meter 1, process furnace 2, metal zinc 3, reaction cabin 4, aperture 5, microwave 6, K9 glass port 7, O
2Under meter 8, Reaktionsofen 9, vacuum pump 10, pedestal 11, substrate 12, hotchpotch metal sheet 13 and worktable 14.Wherein K9 glass port 7 is set on the top of Reaktionsofen 9, be provided with the worktable 14 of placing hotchpotch metal sheet 13 at the take over middle part of position of Reaktionsofen 9, above the Reaktionsofen 9 of answering, be provided with microwave 6 with it, be provided with the pedestal 11 of placing substrate 12 at the middle part of the position of taking back of Reaktionsofen 9, be connected with O at the rear of Reaktionsofen 9
2Under meter 8 is at the left end connection vacuum pump 10 of Reaktionsofen 9.Right side at process furnace 2 connects Ar under meter 1, is provided with the reaction cabin 4 of placing metal zinc 3 at the middle part of process furnace 2.
Preparation principle of the present invention is to use the heat effect of the microwave 6 that sees through K9 glass port 7 that certain hotchpotch metal sheet 13 on the worktable 14 is heated to more than the vaporization temperature (the vaporization temperature difference of different metals), form bigger vapour pressure, generate the plasma body and the O of this kind metalic contamination
2Oxygen that under meter is carried and the vapor generation of the metal zinc in process furnace reaction generate zinc oxide nano-crystal, and worktable 14 can move, rotate and be used for the moving of controlled doping thing.Process furnace 2 is the steam that is used for adding the thermogenesis hotchpotch, is to be used for depositing the ZnO nanocrystal in Reaktionsofen 9 substrate 12 that is arranged on the pedestal 11 of end of taking back, and vacuum pump 10 is set is the gas that is used in the abstraction reaction stove on the right side of Reaktionsofen 9, keeps O in the Reaktionsofen
2, Ar ratio, and keep certain air pressure (～4Torr).Pass through O simultaneously
2Under meter 8 and Ar under meter 1 control oxygen and argon flow amount speed are respectively 10～20sccm and 20～30sccm.
In microwave frequency is 245O MHz and certain effect 20～30min, the heat effect that microwave produces makes metalic contamination vaporizations such as tungsten, cobalt, manganese, aluminium, erbium, indium, vapor generation reaction with oxygen in the Reaktionsofen and the metal zinc in the process furnace, difference and hotchpotch metalline decision action time according to microwave, generate the on all four zinc oxide nano-crystal of multiple specific morphology and character, as Fig. 2～7, such as nano wire, nanometer tower, nano particle etc.
Claims (2)
1. method that adopts preparing zinc oxide nano-crystal by microwave induced adulterant oxidation, it is characterized in that utilizing the heat effect of microwave to reach tungsten fast, cobalt, manganese, aluminium, erbium, more than the indium metal hotchpotch vaporization temperature, make these metalic contamination vaporizations, form plasma body, as the hotchpotch that generates the ZnO nanocrystal, take place to answer with zinc fume and Oxygen Flow along with argon gas stream, the substrate deposition of placing at the left end of Reaktionsofen generates shape and the on all four ZnO nanocrystal of character, wherein control oxygen and argon flow amount speed is respectively 10～20sccm and 20～30sccm, and keep the air pressure of 2～4Torr in the stove.
2. realize the device of the method for the described preparing zinc oxide nano-crystal by microwave induced adulterant oxidation of claim 1, it is characterized in that comprising: Ar under meter (1), process furnace (2), metal zinc (3), reaction cabin (4), aperture (5), microwave (6), K9 glass port (7), O
2Under meter (8), Reaktionsofen (9), vacuum pump (10), pedestal (11), substrate are deposit apex (12), hotchpotch metal sheet (13) and worktable (14), wherein K9 glass port (7) is set on the top of Reaktionsofen (9), be provided with the worktable (14) of placing hotchpotch metal sheet (13) at the take over middle part of position of Reaktionsofen (9), be provided with microwave (6) with its top over against the Reaktionsofen of answering (9), be provided with the pedestal (11) of placing substrate (12) at the middle part of the position of taking back of Reaktionsofen (9), be connected with O at the rear of Reaktionsofen (9)
2Under meter (8), the left end connection vacuum pump (10) at Reaktionsofen (9) connects Ar under meter (1) on the right side of process furnace (2), is provided with the reaction cabin (4) of placing metal zinc (3) at the middle part of process furnace (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100950645A CN100431970C (en) | 2005-10-27 | 2005-10-27 | Method and device for preparing zinc oxide nano-crystal by microwave induced adulterant oxidation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100950645A CN100431970C (en) | 2005-10-27 | 2005-10-27 | Method and device for preparing zinc oxide nano-crystal by microwave induced adulterant oxidation |
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| CN1785819A CN1785819A (en) | 2006-06-14 |
| CN100431970C true CN100431970C (en) | 2008-11-12 |
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| CNB2005100950645A Expired - Fee Related CN100431970C (en) | 2005-10-27 | 2005-10-27 | Method and device for preparing zinc oxide nano-crystal by microwave induced adulterant oxidation |
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| CN103241765A (en) * | 2013-04-26 | 2013-08-14 | 湖南凯新陶瓷科技有限公司 | Microwave synthesis method of superfine zinc oxide powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1405902A (en) * | 2002-10-25 | 2003-03-26 | 华东师范大学 | Erbium-doped zinc oxide near-infrared light source |
| US6610141B2 (en) * | 1998-08-03 | 2003-08-26 | The Curators Of The University Of Missouri | Zinc oxide films containing p-type dopant and process for preparing same |
| US6624442B1 (en) * | 2002-03-27 | 2003-09-23 | Young-Chang Kim | Method of forming p-n junction on ZnO thin film and p-n junction thin film |
| CN1527361A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | N and In codoping process in preparing hole type zinc oxide film |
| CN1542917A (en) * | 2003-11-04 | 2004-11-03 | 浙江大学 | Method for growing p type zinc oxide crystal film by real-time nitrogen doping |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6610141B2 (en) * | 1998-08-03 | 2003-08-26 | The Curators Of The University Of Missouri | Zinc oxide films containing p-type dopant and process for preparing same |
| US6624442B1 (en) * | 2002-03-27 | 2003-09-23 | Young-Chang Kim | Method of forming p-n junction on ZnO thin film and p-n junction thin film |
| CN1405902A (en) * | 2002-10-25 | 2003-03-26 | 华东师范大学 | Erbium-doped zinc oxide near-infrared light source |
| CN1527361A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | N and In codoping process in preparing hole type zinc oxide film |
| CN1542917A (en) * | 2003-11-04 | 2004-11-03 | 浙江大学 | Method for growing p type zinc oxide crystal film by real-time nitrogen doping |
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