CN100448778C - Method and device for preparing zinc oxide nanocrystals based on continuous laser or infrared rays - Google Patents
Method and device for preparing zinc oxide nanocrystals based on continuous laser or infrared rays Download PDFInfo
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- CN100448778C CN100448778C CNB2005100950626A CN200510095062A CN100448778C CN 100448778 C CN100448778 C CN 100448778C CN B2005100950626 A CNB2005100950626 A CN B2005100950626A CN 200510095062 A CN200510095062 A CN 200510095062A CN 100448778 C CN100448778 C CN 100448778C
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- reaktionsofen
- zinc oxide
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Abstract
本发明涉及氧化锌纳米晶体的制备方法和装置，其装置包括O2流量计、Ar流量计、反应炉、辅助加热炉以及设置在其内部的导光装置、工作台、金属锌板、非电离辐射、基底、基座和真空泵。本发明的制备方法是利用连续激光、红外线等非电离辐射的热效应将金属锌板加热到金属锌的汽化温度以上，使金属锌板表面产生高温等离子体，该等离子体定向局部膨胀与反应炉中的氧气发生反应，可以生长多种特定形貌和性质完全一致的纳米氧化锌晶体。具体的氧化锌纳米晶体的形貌和性质由非电离辐射的参数、照射时间、氧气浓度以及通过移动和旋转工作台控制金属锌板和非电离辐射线焦点的相对位置决定。其可以生成与传统的方法不能合成的氧化锌纳米晶体。
The present invention relates to the preparation method and device of zinc oxide nanocrystal, and its device comprises O2 flowmeter, Ar flowmeter, reaction furnace, auxiliary heating furnace and the light guiding device that is arranged in it, workbench, metal zinc plate, non-ionization Irradiation, substrates, pedestals and vacuum pumps. The preparation method of the present invention is to use the thermal effect of non-ionizing radiation such as continuous laser and infrared rays to heat the metal zinc plate above the vaporization temperature of the metal zinc, so that high-temperature plasma is generated on the surface of the metal zinc plate, and the plasma is oriented and locally expanded and heated in the reaction furnace. Oxygen reacts to grow a variety of nano-zinc oxide crystals with the same specific morphology and properties. The morphology and properties of the specific zinc oxide nanocrystals are determined by the parameters of the non-ionizing radiation, irradiation time, oxygen concentration, and the relative position of the metal zinc plate and the focus of the non-ionizing radiation controlled by moving and rotating the worktable. It can generate zinc oxide nanocrystals that cannot be synthesized by traditional methods.
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 for preparing zinc oxide nano-crystal based on continuous laser or ultrared gaseous 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, temperature returns to room temperature after insulation for some time then, and zincite crystal deposits in the substrate (as silicon chip).
With the present invention the most approaching be that pulsed laser deposition ( PLD ) and coaxial oxygen transporting laser in-situ method prepare zinc oxide nano-crystal ( number of patent application: 200510094605.2 ) .Pulsed laser deposition acts on the zinc target material surface with the high power pulsed laser beam focusing that laser apparatus produced； make the zinc target material surface produce the High Temperature High Pressure plasma body； this plasma body directed local expands and launches and formation of deposits zinc oxide nano-crystal in substrate.But this method has brought difficulty for the deposition of ZnO nanocrystal because target and substrate in same stove, can not form certain thermograde; The ZnO nanocrystal kind of coaxial oxygen transporting laser in-situ method preparation is many, and keeps the direction of growth of nature, is difficult to isolating deficiency but also exist. is in periodical " solid state chemistry " (" Journal ofSolid State Chemistry ") 173 (2003) 109-113 " four jiaos of whiskers of microwave plasma bulk-growth ZnO and high-resolution luminosity spectral characteristic " (" Microwave plasma growth and high spatial resolutioncathodoluminescent spectrum oftetrapod ZnO nanostructures ") document; Mentioned the fuel factor of utilizing microwave to produce and make zinc powder vaporization and oxygen reaction generate the ZnO nano crystal, but from patent of the present invention in utilize the fuel factor gaseous oxidation of continuous laser or infrared ray Non-ionizing radiation to prepare the method and apparatus of mentioning in the method and apparatus of zinc oxide nano-crystal and the document to have significantly different.
Summary of the invention:
The object of the invention provides the method and apparatus that a kind of gaseous oxidation of adopting continuous laser or infrared rays nonionizing radiation prepares zinc oxide nano-crystal, utilize the heat effect of continuous laser or infrared rays nonionizing radiation, make metal zine plate surface form plasma body, and reach certain temperature, with oxygen in the Reaktionsofen generation zinc oxide nano-crystal that reacts.
The invention is characterized in and adopt continuous laser or ultrared heat effect, make metal zine plate surface form plasma body, and reach the vaporization temperature of metallic zinc, the plasma body of zinc and the oxygen generation zinc oxide nano-crystal that reacts in Reaktionsofen at first, then along with the argon gas stream in the Reaktionsofen keeps 450～600 ℃ of 20～30min at process furnace together, deposition generates shape and the on all four ZnO nanocrystal of character in the substrate of the downstream of process furnace placement, wherein control oxygen and argon flow amount speed is respectively 20sccm and 30sccm, and keep the air pressure of 2～4Torr in the stove.
And by controlling corresponding continuous laser or ultrared parameter, oxygen concentration and passing through to move and the relative position growth different-shape of rotary table control metal zine plate and nonionizing radiation focus and the nano zine oxide crystal of character.
Power by control laser is that 0.5kW～2.5kW, spot diameter are 1mm～3mm, action time: be generally the position of 0.2-1.5s and translation, rotary table, guarantee to produce at continuous laser radiation metal zine plate the plasma body of metallic zinc.
(wavelength is that 770～1000nm) irradiation time is 10～20min to the control infrared rays, and the position of translation, rotary table, guarantees to produce at continuous laser radiation metal zine plate the plasma body of metallic zinc.Control oxygen simultaneously and the argon gas velocity of flow is respectively 20sccm and 30sccm, satisfy the zinc oxide nano-crystal growth needs.
The device of implementing this method comprises O
2Under meter, Ar under meter, Reaktionsofen, process furnace, worktable, metal zine plate, continuous laser or infrared rays, substrate, pedestal and vacuum pump are formed, and wherein on the top of Reaktionsofen the K9 glass port are set, and connect O in the left side of Reaktionsofen
2Under meter and Ar under meter, be provided with the worktable of place work piece at the middle part of Reaktionsofen, above the Reaktionsofen of answering, be provided with continuous laser or infrared rays with it, be provided with the pedestal of placing substrate in the downstream of process furnace, on the other end of Reaktionsofen, vacuum pump is being set.
Wherein the guiding device of continuous laser adopts the K9 transparent glass, makes laser beam penetrate guiding device and produces heat effect; Common ultrared heat storing and heat preserving can make specimen surface produce 150 ℃ high temperature, but the metallic zinc vaporization is nowhere near, therefore ultrared guiding device adopts the concavees lens with the effect of gathering, the surface that makes infrared rays focus on the metal zine plate produces 900～1000 ℃ of high temperature, reaches the evaporating point of metallic zinc.
The invention has the advantages that:
(1) utilize the heat effect of continuous laser or infrared rays nonionizing radiation to make metal zine plate surface form the plasma body of zinc, and can reach a certain temperature by fast and stable, with oxygen in the Reaktionsofen generation zinc oxide nano-crystal that reacts, be the innovation on the preparation nanocrystal method.
(2) correlation parameter by control continuous laser or infrared rays nonionizing radiation, irradiation time, oxygen concentration and by moving and the relative position of rotary table control metal zine plate and continuous laser focus the on all four nano zine oxide crystal of can grow multiple specific morphology and character.Owing to adopt continuous laser or infrared rays nonionizing radiation, can generate with traditional method can not the synthetic zinc oxide nano-crystal.
Description of drawings:
The invention will be further described below in conjunction with Fig. 1:
Fig. 1 embodiment of the invention---prepare the zinc oxide nano-crystal schematic representation of apparatus based on the gaseous oxidation of continuous laser
1.O
2Under meter 2.Ar under meter 3. worktable, 4. metal zine plate 5.K9 glass port 6. continuous lasers or infrared rays 7. Reaktionsofens 8. process furnace 9. substrates 10. pedestals 11. vacuum pumps
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: O
2Under meter 1, Ar under meter 2., worktable 3, metal zine plate 4, K9 glass port 5, continuous laser, Reaktionsofen 7, process furnace 8, substrate 9, pedestal 10, vacuum pump 11.
Wherein K9 glass port 5 is set, connects O in the left side of Reaktionsofen 7 on the top of Reaktionsofen 7
2Under meter 1 and Ar under meter 2, be provided with the worktable 3 of placing metal zine plate 4 at the middle part of Reaktionsofen 7, above the Reaktionsofen 7 of answering, be provided with continuous laser with it, be provided with the pedestal 10 of placing substrate 9 in the downstream of process furnace 7, vacuum pump 11 is being set on the right side of process furnace 8.
When adopting infrared heating, guiding device adopts the concavees lens with the effect of gathering to replace K9 glass port 5 in the device.
Preparation principle of the present invention is to use the heat effect of the continuous laser 6 that sees through K9 glass port 5 that the metal zine plate 4 on the worktable 3 is heated to more than the vaporization temperature (850 ℃), form bigger vapour pressure, the plasma body of the zinc that generates and the oxygen in the Reaktionsofen generation zinc oxide nano-crystal that reacts, worktable 3 can move, rotate and be used for controlling the mobile of metal zine plate.Process furnace 8 is to be used for heating maintenance constant temperature, the substrate 9 that is arranged on the pedestal 10 at process furnace 8 right-hand members is to be used for depositing the ZnO nanocrystal, vacuum pump 11 is set is the gas that is used in the abstraction reaction stove on the right side of process furnace 8, keep certain air pressure (2～4Torr).Pass through O simultaneously
2Under meter 1 and Ar under meter 2 control oxygen and argon flow amount speed are respectively 20sccm and 30sccm.
Under the condition of certain continuous laser or infrared rays 6 nonionizing radiation relevant parameters, the heat effect that continuous laser or infrared rays 6 produce makes the metallic zinc vaporization, react the on all four nano zine oxide crystal of to grow multiple specific morphology and character with the oxygen in the Reaktionsofen.The pattern of concrete zinc oxide nano-crystal and character are by relevant parameter, irradiation time, the oxygen concentration of continuous laser or infrared rays 6 nonionizing radiations and the relative position decision of controlling metal zine plate and nonionizing radiation line focus by mobile and rotary table.
Claims (5)
1. method for preparing the ZnO nanocrystal based on continuous laser or ultrared gaseous oxidation, it is characterized in that adopting continuous laser or ultrared heat effect, make metal zine plate surface form plasma body, and reach the vaporization temperature of metallic zinc, at first the plasma body of zinc and oxygen react in Reaktionsofen, then along with the argon gas stream in the Reaktionsofen keeps 450～600 ℃ of 20～30min at process furnace together, deposition generates shape and the on all four ZnO nanocrystal of character in the substrate of the downstream of process furnace placement, wherein control oxygen and argon flow amount speed is respectively 20sccm and 30sccm, and keep the air pressure of 2～4Torr in the stove.
2. according to claim 1ly prepare the method for ZnO nanocrystal based on continuous laser or ultrared gaseous oxidation, the power that it is characterized in that controlling laser is that 0.5kW～2.5kW, spot diameter are that 1mm～3mm, action time are 0.2-1.5s.
3. according to claim 1ly prepare the method for ZnO nanocrystal based on continuous laser or ultrared gaseous oxidation, it is characterized in that controlling Infrared wavelength is 770～1000nm, and irradiation time is 10～20min.
4. realizing that claim 1 is described prepares the device of the method for zinc oxide nano-crystal based on continuous laser or ultrared gaseous oxidation, it is characterized in that comprising O
2Under meter (1), Ar under meter (2), Reaktionsofen (7), process furnace (8), worktable (3), metal zine plate (4), continuous laser or infrared rays (6), substrate (9), pedestal (10) and vacuum pump (11) are formed, wherein guiding device is set, connects O in the left side of Reaktionsofen (7) on the top of Reaktionsofen (7)
2Under meter (1) and Ar under meter (2), be provided with the worktable (3) of placing metal zine plate (4) at the middle part of Reaktionsofen (7), be provided with continuous laser or infrared rays (6) with its top over against the Reaktionsofen of answering (7), be provided with the pedestal (10) of placing substrate (9) in the downstream of process furnace (8), vacuum pump (11) be set on the right side of process furnace (8).
5. the device for preparing the method for zinc oxide nano-crystal based on continuous laser or ultrared gaseous oxidation according to claim 4, guiding device is K9 glass port (5) when it is characterized in that adopting continuous laser, and guiding device adopts the concavees lens with the effect of gathering when adopting infrared rays.
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| CNB2005100950626A CN100448778C (en) | 2005-10-27 | 2005-10-27 | Method and device for preparing zinc oxide nanocrystals based on continuous laser or infrared rays |
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| CN100448778C true CN100448778C (en) | 2009-01-07 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003034510A1 (en) * | 2001-10-19 | 2003-04-24 | Bluetron Inc. | P-type zinc oxide thin film, compound semiconductor using the same and method for producing the same |
| 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 |
| CN1489182A (en) * | 2003-08-20 | 2004-04-14 | 东南大学 | Preparation Method of Periodic Structure Wide Bandgap Semiconductor Zinc Oxide Thin Film |
| CN1523641A (en) * | 2003-09-09 | 2004-08-25 | 山东大学 | Method for preparing zinc oxide-based magnetic semiconductor material by sub-nanometer composite method |
-
2005
- 2005-10-27 CN CNB2005100950626A patent/CN100448778C/en not_active Expired - Fee Related
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 |
| WO2003034510A1 (en) * | 2001-10-19 | 2003-04-24 | Bluetron Inc. | P-type zinc oxide thin film, compound semiconductor using the same and method for producing the 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 |
| CN1489182A (en) * | 2003-08-20 | 2004-04-14 | 东南大学 | Preparation Method of Periodic Structure Wide Bandgap Semiconductor Zinc Oxide Thin Film |
| CN1523641A (en) * | 2003-09-09 | 2004-08-25 | 山东大学 | Method for preparing zinc oxide-based magnetic semiconductor material by sub-nanometer composite method |
Non-Patent Citations (5)
| Title |
|---|
| PLD法生长硅基ZnO薄膜的特性. 何建廷等.电子元件与材料，第24卷第5期. 2005 * |
| Si表面上生长的ZnO薄膜的阴极射线荧光. 许小亮等.发光学报，第24卷第2期. 2003 * |
| Synthesis of Nanoscale Metal Oxide Particles Using LaserVaporization/Condensation in a Diffusion Cloud Chamber. M.Samy El-Shall et al.The Journal of Physical Chemistry,Vol.98 No.12. 1994 * |
| ZnO纳米结构薄膜的三阶非线性折射特性. 熊瑛等.光电子·激光，第15卷第11期. 2004 * |
| 激光蒸凝法工艺参数对Zn/ZnO纳米粒子性能的影响及临界粒子半径r*的研究. 李强等.应用激光，第23卷第5期. 2003 * |
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