CN101559920B - One-step method for preparing butterfly pattern ZnSe/GeSe grade heterojunction nano-wire - Google Patents
One-step method for preparing butterfly pattern ZnSe/GeSe grade heterojunction nano-wire Download PDFInfo
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Abstract
The invention relates to a one-step method for preparing a butterfly pattern ZnSe/GeSe grade heterojunction nano-wire, which comprises the following steps: (1) using a vacuum atmosphere tube electric furnace as a synthetic environment, mixing ZnSe powder and Ge powder according to a mass ratio of 3-2:2-1, putting the mixture on a central aluminum oxide boat, and simultaneously using a p-type silicon chip as a substrate; (2) vacuumizing continuously to control the pressure in the furnace to between 200 and 250 Torr, and simultaneously introducing argon gas into the furnace continuously; and (3)controlling the temperature of the reaction tube to between 1,100 and 1,200 DEG C, keeping the temperature for 1.5 to 3 hours, and cooling the product to the room temperature to obtain the butterfly pattern ZnSe/GeSe grade heterojunction nano-wire. The method has a simple and easy preparation process, is finished by adopting a one-step thermal evaporation, and has good repeatability; besides, in the prepared ZnSe/GeSe grade heterojunction nano-wire, a central framework consists of heterojunction structures formed by ZnSe and GeSe nano-wires through axis combination, and the ZnSe/GeSe grade heterojunction nano-wire has potential application in various fields of nano-device assembly, sensor manufacturing and the like.
Description
Technical field
The invention belongs to the preparation field of semiconductor heterojunction nanowire, particularly relate to one-step method for preparing butterfly shape ZnSe/GeSe grade heterojunction nano-wire.
Background technology
In recent years, the new kink characteristics that heterogeneous interface determined of one dimension hetero-junctions nano material because of constituting between its material component, shape, size and the heterogeneity, caused people's research boom, it is expected at the one-dimensional crystal pipe, Light-Emitting Diode (LED), FET, aspects such as solar cell have broad application prospects.
At present, obtaining progress definitely aspect the preparation of hetero-junctions nanostructured.The hetero-junctions nanostructured not only has important scientific meaning to the fundamental research of crystal growth, and has actual using value in micro-nano person in electronics.The preparation method of heterojunction nano-wire mainly contains chemical vapour deposition (CVD), laser ablation, template and hydro-thermal method etc.Said method is most to adopt the high temperature heating, multisteps are synthetic or other complicated supplementary means, preparation grade heterojunction nano-wire complex process and poor repeatability, and therefore to develop a simple one-step preparation method be very necessary and what be badly in need of also is challenging.
Summary of the invention
Technical problem to be solved by this invention provides one-step method for preparing butterfly shape ZnSe/GeSe grade heterojunction nano-wire, and preparation is simple for this, adopts one-step method to finish, and favorable repeatability.
One-step method for preparing butterfly shape ZnSe/GeSe grade heterojunction nano-wire of the present invention, be synthetic environment mainly with the vacuum atmosphere tube type electric furnace, with ZnSe powder and Ge powder is raw material, adopt the method for a step thermal evaporation to be prepared, thermal evaporation is a kind of method of the line of synthesis of nano simply and effectively, that is: progressively the raise temperature of reaction source makes its distillation, thereby makes it to deposit to the product that obtains needs on the substrate the transporting of current-carrying gas under the reaction source of distillation being transported to the lower zone of temperature.
Concrete steps are:
(1) being to mix place central alundum (Al boat at 3～2: 2～1 ZnSe powder and Ge powder according to mass ratio, is substrate with p type silicon chip simultaneously, puts into the alundum (Al boat of raw material leeward;
(2) continuing to vacuumize the control furnace pressure is 200～250Torr (1Torr ≈ 133Pa), and continuing simultaneously to feed flow is the argon gas of 100～150sccm;
(3) the control reaction tube temperature is 1100～1200 ℃, behind insulation 1.5～3h, is cooled to room temperature, obtains grey lint shape material, is butterfly shape ZnSe/GeSe grade heterojunction nano-wire.
Described step (3) butterfly shape ZnSe/GeSe grade heterojunction nano-wire, its center framework forms heterojunction structure by ZnSe and GeSe nano wire and axle, and extension GeSe nanometer " wing " again on trunk GeSe nano wire, the GeSe nanocrystal of evenly growing again on " wing ".
Beneficial effect
(1) preparation is simple in the present invention, adopts one-step method to finish, and favorable repeatability;
(2) prepared ZnSe of the present invention/GeSe grade heterojunction nano-wire, the pattern novelty, its center framework forms heterojunction structure by ZnSe and GeSe nano wire and axle, and on trunk GeSe nano wire extension GeSe nanometer " wing " again, the GeSe nanocrystal of evenly growing again on " wing ";
(3) products therefrom of the present invention has potential application because of its unique pattern and structure in numerous areas such as nano-device assembling, sensor manufacturing.
Description of drawings
Fig. 1 is the experimental facilities schematic diagram;
Fig. 2 is the electron scanning micrograph of the ZnSe/GeSe grade heterojunction nano-wire of embodiment 1;
Fig. 3 is the electron scanning micrograph of the ZnSe/GeSe grade heterojunction nano-wire of embodiment 2;
Fig. 4 is an embodiment 3ZnSe/GeSe grade heterojunction nano-wire electron scanning micrograph a);
B) be embodiment 3ZnSe/GeSe grade heterojunction nano-wire X-ray diffractogram;
Fig. 5 (a) and (b) are the transmission electron microscope photo of the ZnSe/GeSe grade heterojunction nano-wire of embodiment 3, and wherein (a) is center framework, (b) are final butterfly shape grade heterojunction nano-wire; (c), (d) be wing part enlarged photograph, wherein (d) is the enlarged photograph of circle part in (c); (e), (f) is respectively the X-ray energy spectrum figure corresponding to circle part among the (a) and (b) figure.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
ZnSe and Ge powder mixed with 3: 1 mass ratio be placed on the reaction tube centre position.With p type silicon chip is substrate, puts into the alundum (Al boat of mixed-powder leeward, reaction tube one termination air supply system, a termination oil-sealed rotary pump.Continuing to feed flow is the argon gas of 100～150sccm, and reaction tube central authorities temperature is 1100 ℃ in the experiment, and deposition pressure is 200Torr (1Torr ≈ 133Pa), behind the insulation 1.5h, close heating power supply, naturally cool to room temperature, obtain the ZnSe/GeSe grade heterojunction nano-wire, as shown in Figure 2.
Embodiment 2
ZnSe and Ge powder mixed with 3: 1.5 mass ratio be placed on the reaction tube centre position.With p type silicon chip is substrate, puts into the alundum (Al boat of mixed-powder leeward, reaction tube one termination air supply system, a termination oil-sealed rotary pump.Continuing to feed flow is the argon gas of 100～150sccm, and crystal reaction tube central authorities temperature is 1100 ℃ in the experiment, and deposition pressure is 250Torr (1Torr ≈ 133Pa), behind the insulation 1.5h, close heating power supply, naturally cool to room temperature, obtain the ZnSe/GeSe grade heterojunction nano-wire, as shown in Figure 3.
Embodiment 3
ZnSe and Ge powder mixed with 3: 2 mass ratio be placed on the reaction tube centre position.Silica-based with the p type is substrate, puts into the alundum (Al boat of mixed-powder leeward, reaction tube one termination air supply system, a termination oil-sealed rotary pump.Continuing to feed flow is the argon gas of 100～150sccm, and reaction tube central authorities temperature is 1100 ℃ in the experiment, and deposition pressure is 200Torr (1Torr ≈ 133Pa), behind the insulation 1.5h, close heating power supply, naturally cool to room temperature, obtain the ZnSe/GeSe grade heterojunction nano-wire, as shown in Figure 4.
The uniform butterfly shape of large tracts of land size grade heterojunction nano-wire has covered whole silicon chip as can be seen from Fig. 4 (a) photo, and its diameter is less than 1 μ m, and length is from hundreds of nanometer to tens micron.Diffraction maximum among Fig. 4 (b) can be distinguished index, and (JCPDS is 88-2345) with quadrature GeSe (JCPDS, diffraction maximum 74-0372) mutually for cube phase ZnSe.From Fig. 5 (a) photo as can be seen, the center framework of nano wire is and the axle nano wire that diameter is in 50nm, and is very even; Can find out clearly that from Fig. 5 (b) this grade heterojunction nano-wire is the butterfly pattern.Little crystal grain that can the clear GeSe of seeing among Fig. 5 (c) relatively is evenly distributed on the wing, and Fig. 5 (d) has showed about tens nanometers of the small particle diameters of GeSe clearly.Fig. 5 (e), (f) show that the center framework composition is the also axle nano wire of ZnSe and GeSe, and wing then is that GeSe stretches out, the result of diauxic growth.The above results shows, this invention prepared ZnSe/GeSe grade heterojunction nano-wire, its center framework forms hetero-junctions by ZnSe and GeSe nano wire and axle and constitutes, and on trunk GeSe nano wire extension GeSe nanometer " wing " again, the GeSe nanocrystal of evenly growing again on " wing ".
Claims (3)
1. one-step method for preparing butterfly shape ZnSe/GeSe grade heterojunction nano-wire comprises:
(1) being synthetic environment with the vacuum atmosphere tube type electric furnace, is that (3: 2)～(3: 1) are mixed and placed on the central alundum (Al boat with ZnSe and Ge according to mass ratio, is substrate with p type silicon chip simultaneously, puts into the alundum (Al boat of raw material leeward;
(2) continuing to vacuumize the control furnace pressure is 200～250Torr, continues to feed argon gas simultaneously;
(3) the control reaction tube temperature is 1100～1200 ℃, behind the insulation 1.5h, is cooled to room temperature, promptly gets butterfly shape ZnSe/GeSe grade heterojunction nano-wire.
2. one-step method for preparing butterfly shape ZnSe/GeSe grade heterojunction nano-wire according to claim 1 is characterized in that: the mass ratio of ZnSe powder and Ge powder is 3: 2,3: 1.5 or 3: 1 in the described step (1).
3. one-step method for preparing butterfly shape ZnSe/GeSe grade heterojunction nano-wire according to claim 1, it is characterized in that: the butterfly shape ZnSe/GeSe grade heterojunction nano-wire of gained in the described step (3), its center framework forms heterojunction structure by ZnSe and GeSe nano wire and axle, and extension GeSe nanometer " wing " again on trunk GeSe nano wire, the GeSe nanocrystal of evenly growing again on " wing ".
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004050547A2 (en) * | 2002-09-12 | 2004-06-17 | The Trustees Of Boston College | Metal oxide nanostructures with hierarchical morphology |
| CN1727524A (en) * | 2004-11-30 | 2006-02-01 | 中国科学院长春光学精密机械与物理研究所 | The method for preparing low temperature catalyst-free needle-like Zn0 nano wire |
| CN1908250A (en) * | 2006-07-26 | 2007-02-07 | 北京科技大学 | Method of preparing room temperature ferromagnetism Zn(1-X)Mn(X)O diluted magnetic semiconductor nano-line |
| JP2008311396A (en) * | 2007-06-14 | 2008-12-25 | National Institute For Materials Science | Hetero-junction containing magnesium nitride nano wire and gallium nano wire thin-wall covered with graphitic carbon nano tube content |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004050547A2 (en) * | 2002-09-12 | 2004-06-17 | The Trustees Of Boston College | Metal oxide nanostructures with hierarchical morphology |
| CN1727524A (en) * | 2004-11-30 | 2006-02-01 | 中国科学院长春光学精密机械与物理研究所 | The method for preparing low temperature catalyst-free needle-like Zn0 nano wire |
| CN1908250A (en) * | 2006-07-26 | 2007-02-07 | 北京科技大学 | Method of preparing room temperature ferromagnetism Zn(1-X)Mn(X)O diluted magnetic semiconductor nano-line |
| JP2008311396A (en) * | 2007-06-14 | 2008-12-25 | National Institute For Materials Science | Hetero-junction containing magnesium nitride nano wire and gallium nano wire thin-wall covered with graphitic carbon nano tube content |
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