CN101092744B - Preparation method of macroscopic ZnO monocrystal material in ramiform fractal structure - Google Patents
Preparation method of macroscopic ZnO monocrystal material in ramiform fractal structure Download PDFInfo
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- CN101092744B CN101092744B CN2007100391734A CN200710039173A CN101092744B CN 101092744 B CN101092744 B CN 101092744B CN 2007100391734 A CN2007100391734 A CN 2007100391734A CN 200710039173 A CN200710039173 A CN 200710039173A CN 101092744 B CN101092744 B CN 101092744B
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Abstract
This invention discloses a method for preparing macroscopic ZnO monocrystal material with tree-shaped fractal structure. The macroscopic ZnO monocrystal material is formed on a matrix via heat evaporation in a horizontal-pipe-type growth furnace with ZnO powder, graphite powder, and copper powder as the raw materials, and nitrogen as the gas source. The length and width of the macroscopic ZnO monocrystal material are 5-25 mm and 1-10 mm, respectively. The method has such advantages as mild conditions (normal pressure), low request for carrier gas, no need for oxygen, easy operation, high repeatability, abundant raw materials, and low cost. The method can be used in such fields as microelectronics and microelectronic photoelectric devices.
Description
Technical field
The present invention relates to macroscopic ZnO monocrystal material of a kind of tree-shaped fractal structure and preparation method thereof, belong to the technical field of Semiconductor Optoeletronic Materials and device.
Technical background
In recent years, because the ZnO structured material has excellent optics, electricity and piezoelectric property, so its research has been subjected to worldwide showing great attention to.As the ZnO structured material of wide bandgap semiconductor, transmitter, power device, ultraviolet light-emitting diode, solar cell have been widely used at present.Under the world, domestic Materials science worker's unremitting effort, can enough several different methods (as molecular beam epitaxy, pulsed laser deposition, magnetron sputtering, sol-gel method, thermal evaporation, Metalorganic Chemical Vapor Deposition etc.) prepare multiple ZnO structured material now, comprising ZnO nano structural material with shape characteristics such as " bar ", " line ", " band ", " ring ", " combs ".But at present report on these scantling lengths it all is on nanometer or micron order, it is rarely found that the better simply thermal evaporation of application art prepares the report of ZnO material of macrostructure.Wang Zhonglin professor seminar once reported a-Fe
20
3Tree-shaped fractal nano structure (Minhua Cao, etal.Single-Crystal Dendritic Micro-Pines of Magnetic a-Fe
2O
3: Large-Scale Synthesis, Formation Mechanism, and Properties, Angrew.Chem.int.Ed.2005.44,2-6), but the present report that does not have about the macroscopic ZnO monocrystal material of tree-shaped fractal structure.
Summary of the invention
An object of the present invention is to release a kind of macroscopic ZnO monocrystal material of tree-shaped fractal structure.This material is the macroscopic ZnO monocrystal structure that is attached to the tree-shaped fractal structure that length on the substrate and width be respectively 5mm～25mm and 1～10mm.
Another object of the present invention provides a kind of described preparation methods.For realizing above purpose, the present invention adopts following technical scheme.ZnO powder, Graphite Powder 99 and copper powder with commodity are done raw material, are source of the gas with the N2 that is easy to get, and adopt grow on the substrate macroscopic ZnO monocrystal material of tree-shaped fractal structure of thermal evaporation in the horizontal tube growth furnace, and this material is attached to the surface of substrate with absolute version.
Now describe technical scheme of the present invention in detail.A kind of preparation method of macroscopic ZnO monocrystal material of tree-shaped fractal structure is characterized in that, the concrete operations step:
The first step ultrasonic cleaning substrate also dries;
The temperature of second step with the horizontal tube growth furnace rises to 900～950 ℃;
The 3rd step charged into N in stove
2, flow is 0.8～2L/min;
The 4th step was placed on growth source ZnO powder, Graphite Powder 99 and pure copper powder mixing on the quartz boat, the air dried substrate places on the substrate holder, again quartz boat and substrate holder are placed in the flat-temperature zone of the horizontal tube growth furnace that has heated up, the purity of ZnO powder, Graphite Powder 99 and pure copper powder is respectively 99.99%, 99% and 99.999%, ZnO powder: Graphite Powder 99: the mass ratio of pure copper powder is 1: 1～2: 0.2～1, and the distance of substrate holder and growth source ZnO powder, Graphite Powder 99 and pure copper powder is 1～3cm;
Temperature in the 5th step holding tube, the ZnO material of the tree-shaped fractal structure of growth on substrate, the time is 60～90min;
The 6th step substrate is cooled to room temperature naturally with the horizontal tube growth furnace, opens the horizontal tube growth furnace, takes out substrate, obtains being grown in the macroscopic ZnO monocrystal material of the tree-shaped fractal structure of substrate surface.
Technical scheme of the present invention is further characterized in that described substrate is p type monocrystalline silicon piece, n type monocrystalline silicon piece or the porous silicon chip that deposits copper film.
Technical scheme of the present invention is further characterized in that, the method of the powder of mixing growth source ZnO powder, Graphite Powder 99 and pure copper powder is that selected mass ratio ZnO powder, Graphite Powder 99 and pure copper powder are mixed, add stirring behind an amount of dehydrated alcohol, ultrasonic vibration, oven dry and grinding, the growth source powder of mixing.
The advantage of method of the present invention:
1, method of the present invention only needs under normal pressure, and less demanding to carrier gas only needs N
2Just can, do not need to add O
2Wait other gas, airshed is not required strict control yet, simple, good reproducibility, raw material obtains easily, and preparation cost is cheap, is suitable for being used for preparing large-area ZnO single crystal structure.
2, the macroscopic ZnO monocrystal material of the tree-shaped fractal structure that makes of method of the present invention is a kind of ZnO macroscopic viewization structured material with unique shape characteristic, is expected to obtain in fields such as microelectronics and microelectronics photoelectric devices important application.
Description of drawings
Fig. 1 is the X-ray diffractogram of the macroscopic ZnO monocrystal material of tree-shaped fractal structure.
Fig. 2 is the low power SEM photo of the macroscopic ZnO monocrystal material of tree-shaped fractal structure.
Fig. 3 be tree-shaped fractal structure macroscopic ZnO monocrystal material in times SEM photo.
Fig. 4 is the SEM photo of the macroscopic ZnO monocrystal material of isolated single tree-shaped fractal structure.
Embodiment
Now further specify technical scheme of the present invention in conjunction with the accompanying drawings and embodiments.According to the preparation method's of the macroscopic ZnO monocrystal material of above-mentioned tree-shaped fractal structure concrete operations step operation, succinct for making style of writing, each following embodiment is only enumerated crucial technical data to all embodiment fully.
Embodiment 1:
In the first step, substrate is a p type monocrystalline silicon piece; In second step, the temperature of horizontal tube growth furnace is risen to 930 ℃; In the 3rd step, flow is 1.5L/min; In the 4th step, ZnO powder: Graphite Powder 99: the mass ratio of pure copper powder is 1: 1: 0.5, and the distance of substrate holder and growth source ZnO powder, Graphite Powder 99 and pure copper powder is 2cm; In the 5th step, the time is 70min; In the 6th step, obtain being grown in the macroscopic ZnO monocrystal material of tree-shaped fractal structure of the white of substrate surface.
Embodiment 2:
In the first step, substrate is a n type monocrystalline silicon piece; In second step, the temperature of horizontal tube growth furnace is risen to 900 ℃; In the 3rd step, flow is 2L/min; In the 4th step, ZnO powder: Graphite Powder 99: the mass ratio of pure copper powder is 1: 1: 0.33, and the distance of substrate holder and growth source ZnO powder, Graphite Powder 99 and pure copper powder is 1.5cm; In the 5th step, the time is 60min; In the 6th step, obtain being grown in the macroscopic ZnO monocrystal material of tree-shaped fractal structure of the white of substrate surface.
Embodiment 3:
In the first step, substrate is the porous silicon of surface deposition copper film; In second step, the temperature of horizontal tube growth furnace is risen to 950 ℃; In the 3rd step, flow is 0.8L/min; In the 4th step, ZnO powder: Graphite Powder 99: the mass ratio of pure copper powder is 1: 2: 0.2, and the distance of substrate holder and growth source ZnO powder, Graphite Powder 99 and pure copper powder is 1cm; In the 5th step, the time is 70min; In the 6th step, obtain being grown in the macroscopic ZnO monocrystal material of tree-shaped fractal structure of the white of substrate surface.
Claims (4)
1. the preparation method of the macroscopic ZnO monocrystal material of a tree-shaped fractal structure is characterized in that, the concrete operations step:
The first step ultrasonic cleaning substrate also dries;
The temperature of second step with the horizontal tube growth furnace rises to 900～950 ℃;
The 3rd step charged into N in stove
2, flow is 0.8～2L/min;
The 4th step was placed on growth source ZnO powder, Graphite Powder 99 and pure copper powder mixing on the quartz boat, the air dried substrate places on the substrate holder, again quartz boat and substrate holder are placed in the flat-temperature zone of the horizontal tube growth furnace that has heated up, the purity of ZnO powder, Graphite Powder 99 and pure copper powder is respectively 99.99%, 99% and 99.999%, ZnO powder: Graphite Powder 99: the mass ratio of pure copper powder is 1: 1～2: 0.2～1, and the distance of substrate holder and growth source ZnO powder, Graphite Powder 99 and pure copper powder is 1～3cm;
Temperature in the 5th step holding tube, the ZnO material of the tree-shaped fractal structure of growth on substrate, the time is 60～90min;
The 6th step substrate is cooled to room temperature naturally with the horizontal tube growth furnace, opens the horizontal tube growth furnace, takes out substrate, obtains being grown in the macroscopic ZnO monocrystal material of the tree-shaped fractal structure of substrate surface.
2. the preparation method of the macroscopic ZnO monocrystal material of tree-shaped fractal structure according to claim 1 is characterized in that, described substrate is p type monocrystalline silicon piece, n type monocrystalline silicon piece or the porous silicon chip that deposits copper film.
3. the preparation method of the macroscopic ZnO monocrystal material of tree-shaped fractal structure according to claim 1, it is characterized in that, the method of the powder of mixing growth source ZnO powder, Graphite Powder 99 and pure copper powder is that selected mass ratio ZnO powder, Graphite Powder 99 and pure copper powder are mixed, add stirring behind an amount of dehydrated alcohol, ultrasonic vibration, oven dry and grinding, the growth source powder of mixing.
4. the preparation method of the macroscopic ZnO monocrystal material of tree-shaped fractal structure according to claim 1, it is characterized in that, described substrate is p type monocrystalline silicon piece, n type monocrystalline silicon piece or the porous silicon chip that deposits copper film, the method of the powder of mixing growth source ZnO powder, Graphite Powder 99 and pure copper powder is that selected mass ratio ZnO powder, Graphite Powder 99 and pure copper powder are mixed, add stirring behind an amount of dehydrated alcohol, ultrasonic vibration, oven dry and grinding, the growth source powder of mixing.
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