CN100355657C - Method and device for in situ preparing zinc oxide nanometer crystal using coaxial oxygen transporting laser - Google Patents
Method and device for in situ preparing zinc oxide nanometer crystal using coaxial oxygen transporting laser Download PDFInfo
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- CN100355657C CN100355657C CNB2005100946052A CN200510094605A CN100355657C CN 100355657 C CN100355657 C CN 100355657C CN B2005100946052 A CNB2005100946052 A CN B2005100946052A CN 200510094605 A CN200510094605 A CN 200510094605A CN 100355657 C CN100355657 C CN 100355657C
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Abstract
The present invention relates to a method and a device for preparing zinc oxide nanometer crystals, particularly to a method and a device for preparing zinc oxide nanometer crystals by laser in situ. The present invention belongs to the technical field of ceramic materials. The device proposed by the method comprises a reaction furnace, an infrared thermoscope, a viewing window, a working table, a metallic zinc plate, annular oxygen stream, a laser beam, a coaxial oxygen conveying device, an air sending hole and a vacuum pump. In addition, the present invention has the preparing theory that a laser device is used for generating continuous laser heat effects so as to heat a metallic zinc plate to a certain temperature above a melting point. Thus, formed zinc steam reacts with oxygen coaxially conveyed by the laser beams on the basal body of the metallic zinc plate so as to produce zinc oxide nanometer crystals, and natural growth direction can be kept. Thus, one-dimensional, two-dimensional and three-dimensional zinc oxide nanometer crystals can be generated. A temperature zone of the metallic zinc plate can be realized by controlling laser power, laser spot diameters, lasing time and the working table.
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 coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal.
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 in the reaction tubes (Reaktionsofen) is (such as O
2, perhaps O
2With S, AL, the gas of additives such as IN) react, temperature returns to room temperature after insulation for some time then, and zincite crystal deposits in the substrate (such as silicon chip).If control correlated conditions such as air-flow, pressure well, these working methods can both obtain certain zinc oxide nano-crystal structure, but these zinc oxide preparation method conditional request is all very strict, and equipment is relatively costly, and can only obtain a kind of zincite crystal under some concrete conditions.
With the present invention the most approaching be that pulsed laser deposition prepares zinc oxide nano-crystal, this method 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 can only generate a certain zinc oxide nano-crystal, and sedimentary zincite crystal is non-directional, has brought difficulty for the extraction and the use of follow-up zinc oxide nano-crystal.
Summary of the invention:
The present invention seeks to provide 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 control laser parameter (irradiation time, power etc.), oxygen concentration and, by moving and rotate the position of control worktable, go out the nano zine oxide crystal of different dimensions in zine plate surface direct growth.
The invention is characterized in and utilize continuous laser at metal zine plate growth in situ zinc oxide nano-crystal, the while coaxial oxygen transporting, with continuous laser beam focussing force that laser apparatus produced in the zinc target material surface, make the zinc target material surface produce the High Temperature High Pressure plasma body, expand the taper spatial oxygen environment-development life with coaxial conveying of this plasma body directed local is reflected on the metal zine plate and forms zinc oxide nano-crystal.
Feature of the present invention also is to implement the temperature control of regional area, the area illumination of utilizing laser beam to set arbitrarily at zine plate, make its temperature in 420 ℃～850 ℃, produce the zinc oxide directional growth in situ nanocrystal that inspectable space distributes, shape and the character at the zinc oxide nano-crystal of some temperature regional area growth is consistent or similar like this.
Power by control laser is that 0.5kW～2.5kW, spot diameter are the position that is generally 1mm～3mm, action time 0.2-1.5 second and translation, rotary table in addition, guarantees at metal zine plate growth in situ nano zine oxide crystal.
Controlling oxygen flow simultaneously is certain speed, and 5.0～10.0sccm can satisfy the zinc oxide nano-crystal needed oxygen of growing, and can guarantee being grown on the metal zine plate of zinc oxide nano-crystal nature again.
The device of implementing this method comprises Reaktionsofen and the infrared thermometer of the portion that sets within it, viewing window, worktable, metal zine plate, taper Oxygen Flow, laser beam, coaxial oxygen transporting device, injection well and vacuum pump composition, wherein infrared thermometer is set on the top of Reaktionsofen, on the sidewall of Reaktionsofen, viewing window is set, the worktable of place work piece is set in the bottom of Reaktionsofen, above the Reaktionsofen of answering, being provided with the coaxial oxygen transporting device of forming by co-axial taper Oxygen Flow, laser beam, on another sidewall of Reaktionsofen, injection well and vacuum pump are set with it.
The invention has the advantages that:
(1) protection of coaxial Oxygen Flow helps zinc oxide nano-crystal and generates on the matrix of metal zine plate, and zinc oxide nano-crystal is on metal zine plate top layer, extracts easily, for the extraction and the use of follow-up zinc oxide nano-crystal brought convenience.
(2) utilize the heat effect of laser to shine the metal zine plate, around illuminated laser spot, form certain thermograde, generate the zinc oxide nano-crystal of shape and character basically identical in the corresponding regional original position of metal zine plate.
Description of drawings:
The invention will be further described below in conjunction with Fig. 1:
The three-dimensional zinc oxide nano-crystal of Fig. 1
Fig. 2 two dimensional oxidation zinc nanocrystalline body (ZnO nanometer plate)
Fig. 3 one-dimension zinc oxide nanocrystal array (ZnO nano wire)
Fig. 4 coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal schematic representation of apparatus
1. Reaktionsofen 2. infrared thermometers 3. viewing windows 4. worktable 5. metal zine plates 6. taper Oxygen Flow 7. laser beams 8. coaxial oxygen transporting devices 9. injection wells 10. 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 coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal device with the present invention comprises: Reaktionsofen 1, infrared thermometer 2, viewing window 3, worktable 4, metal zine plate 5, taper Oxygen Flow 6, laser beam 7, coaxial oxygen transporting device 8, injection well 9, vacuum pump 10.Wherein infrared thermometer 2 is set on the top of Reaktionsofen 1, viewing window 3 is set on the sidewall of Reaktionsofen 1, the worktable 4 of place work piece is set in the bottom of Reaktionsofen 1, above the Reaktionsofen 1 of answering, be provided with the coaxial oxygen transporting device of forming by co-axial taper Oxygen Flow 6, laser beam 78 with it, injection well 9 and vacuum pump 10 are being set on another sidewall of Reaktionsofen 1.
To be the laser beam 7 that produces with laser apparatus be heated to 4 metal zine plate 5 on the worktable more than the fusing point preparation principle of the present invention, form bigger vapour pressure, the zinc fume that generates and the oxygen 6 of the laser beam 7 coaxial conveyings generation zinc oxide that reacts, owing to be the moment oxidation, direct growth goes out zinc oxide nano-crystal on metallic zinc board substrate original position, and keeps the direction of growth.On make platform 4 and can move, rotate and be used for controlling moving of metal zine plate.Infrared thermometer 2 is used for detecting in real time the temperature on metal zine plate surface.Can come what happens in the viewing test process by viewing window 3.Injection well 9 is used for carrying the shielding gas that does not react (such as Ar, He, Ne and N
2Deng), also can be used for carrying other reactant gases (such as vaporous hotchpotchs such as sulphur, aluminium).
Under certain laser power, action time and the isoparametric condition of spot diameter size; zinc oxide nano-crystal can be on the metal zine plate self-sow; because the protection of coaxial Oxygen Flow is arranged; this helps zinc oxide nano-crystal more and generates on the matrix of metal zine plate; and zinc oxide nano-crystal extracts easily on metal zine plate top layer.In general, regional temperature is high more, and the zinc oxide nano-crystal of generation is complicated more, as shown in Figure 1 at the higher zone of temperature (＞850 ℃), generate to generate three-dimensional zinc oxide nano-crystal (such as plum blossom shape nanocrystal, four-footed nanocrystal etc.); As shown in Figure 2 be 850 ℃～600 ℃ in temperature, generate the zinc oxide nano-crystal of two dimension; The zone (420 ℃～600 ℃) at the fusing point of a little higher than zinc of surface temperature of metal zine plate as shown in Figure 3 generates the unidimensional zinc oxide nano-crystal.Concrete temperature province scope can realize by adjusting laser power, laser spot diameter, lasing time and worktable.
Claims (5)
1. the method for coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal, it is characterized in that utilizing continuous laser at metal zine plate growth in situ zinc oxide nano-crystal, the while coaxial oxygen transporting, with continuous laser beam focussing force that laser apparatus produced in metal zine plate surface, make metal zine plate surface produce the High Temperature High Pressure plasma body, expand the taper spatial oxygen environment-development life with coaxial conveying of this plasma body directed local is reflected on the metal zine plate and forms zinc oxide nano-crystal.
2. the method for coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal according to claim 1, it is characterized in that implementing the temperature control of regional area, the area illumination of utilizing laser beam to set arbitrarily at zine plate, make its temperature in 420 ℃～850 ℃, produce the zinc oxide directional growth in situ nanocrystal that inspectable space distributes.
3. the method for coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal according to claim 1, it is characterized in that the power by control laser is that 0.5kW～2.5kW, spot diameter are 1mm～3mm, action time to be the position of 0.2-1.5 second and translation, rotary table, guarantee at metal zine plate growth in situ nano zine oxide crystal.
4. the method for coaxial oxygen transporting laser in-situ preparing zinc oxide nano-crystal according to claim 1, it is characterized in that controlling oxygen flow is certain speed: 5.0～10.0sccm.
5. realize the device of the described coaxial oxygen transporting laser in-situ preparing of claim 1 zinc oxide nano-crystal method, it is characterized in that comprising Reaktionsofen, infrared thermometer, viewing window, worktable, the metal zine plate, the taper Oxygen Flow, laser beam, the coaxial oxygen transporting device, injection well and vacuum pump are formed, wherein infrared thermometer (2) is set on the top of Reaktionsofen (1), viewing window (3) is set on the sidewall of Reaktionsofen (1), the worktable (4) of place work piece is set in the bottom of Reaktionsofen (1), be provided with by co-axial taper Oxygen Flow (6) with its top over against the Reaktionsofen of answering (1), the coaxial oxygen transporting device (8) that laser beam (7) is formed is provided with injection well (9) and vacuum pump (10) on another sidewall of Reaktionsofen (1).
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100946052A CN100355657C (en) | 2005-09-29 | 2005-09-29 | Method and device for in situ preparing zinc oxide nanometer crystal using coaxial oxygen transporting laser |
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| CNB2005100946052A CN100355657C (en) | 2005-09-29 | 2005-09-29 | Method and device for in situ preparing zinc oxide nanometer crystal using coaxial oxygen transporting laser |
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| CN100355657C true CN100355657C (en) | 2007-12-19 |
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| CN112939060B (en) * | 2021-02-05 | 2022-02-15 | 中国人民解放军战略支援部队航天系统部装备部装备保障队 | Zinc oxide nano material and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001043165A2 (en) * | 1999-11-12 | 2001-06-14 | The Curators Of The University Of Missouri | Oxide films containing p-type dopant and process for preparing same |
| US6291085B1 (en) * | 1998-08-03 | 2001-09-18 | 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 |
| CN1458305A (en) * | 2002-05-13 | 2003-11-26 | 武汉科技大学 | ZnO nano crystal whisker material and its preparing method |
| CN1547264A (en) * | 2003-12-05 | 2004-11-17 | 中国科学院上海硅酸盐研究所 | Zinc oxide homogeneous p-n junction material and method for making same |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6291085B1 (en) * | 1998-08-03 | 2001-09-18 | The Curators Of The University Of Missouri | Zinc oxide films containing P-type dopant and process for preparing same |
| US6410162B1 (en) * | 1998-08-03 | 2002-06-25 | The Curators Of The University Of Missouri | Zinc oxide films containing P-type dopant and process for preparing same |
| WO2001043165A2 (en) * | 1999-11-12 | 2001-06-14 | The Curators Of The University Of Missouri | 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 |
| CN1458305A (en) * | 2002-05-13 | 2003-11-26 | 武汉科技大学 | ZnO nano crystal whisker material and its preparing method |
| CN1547264A (en) * | 2003-12-05 | 2004-11-17 | 中国科学院上海硅酸盐研究所 | Zinc oxide homogeneous p-n junction material and method for making same |
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