CN1958877A - Periodic monocrystalline Nano structure of castellated ZnO, preparation method - Google Patents
Periodic monocrystalline Nano structure of castellated ZnO, preparation method Download PDFInfo
- Publication number
- CN1958877A CN1958877A CN 200610117268 CN200610117268A CN1958877A CN 1958877 A CN1958877 A CN 1958877A CN 200610117268 CN200610117268 CN 200610117268 CN 200610117268 A CN200610117268 A CN 200610117268A CN 1958877 A CN1958877 A CN 1958877A
- Authority
- CN
- China
- Prior art keywords
- zno
- nanostructure
- silicon chip
- silica tube
- quartz boat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
This invention discloses a method for preparing period tower-shaped ZnO monocrystal nanostructure. The nanostructure is layered and period tower-shaped ZnO monocrystal nanostructure assembled from hexagonal units from bottom to top on a Si wafer, and has a length of 20-30 mum, a bottom diameter of 3-10 mum, and a top diameter of 5-15 nm. The method comprises: utilizing Si wafer as the substrate, Zn powder as the evaporation source, and Ar as the carrier gas, and growing nanoscale ZnO monocrystals at 550-700 deg.C and atmospheric pressure on the substrate by heat evaporation. The nanoscale ZnO monocrystals have period tower-shaped nanostructure. The method has such advantages as simple process, low cost, high repeatability, and large-scale periodic tower-shaped ZnO monocrystal nanostructure on the substrate. The obtained nanostructure can be used as cathode material of field emission microelectronics, and probe of STM and AFM.
Description
Technical field
The present invention relates to periodicity monocrystal nanostructure of a kind of ZnO tower shape and preparation method thereof, specifically, relate to a kind of periodicity monocrystal nanostructure of the ZnO tower shape that forms by nano unit structure and with the method for thermal evaporation, under the condition of atmospheric pressure and 550～700 ℃, the method of the large-area this structure of preparation belongs to the technical field of photoelectron and semiconductor material and preparation method thereof on silicon chip substrate.
Background technology
ZnO is a kind of wide bandgap semiconductor, and have bigger exciton bind energy, very big application prospect is arranged in opto-electronic device, again because its thermostability, special property such as high mechanical strength and chemical stability has caused the interest of people to the field emission characteristic research of its nanostructure.Recently, people utilize the whole bag of tricks (solution method, molecular beam epitaxy, pulsed laser deposition, metal-organic chemical vapor deposition equipment etc.) prepared various One-Dimensional ZnO nanostructure, nano wire for example, nano belt, nanoneedle, nanometer pencil, nanometer rod etc., and the field emission characteristic of these nanostructures studied, the result shows to have the most advanced and sophisticated easier emitting electrons of those nanostructures, yet up to the present, all one dimension Nano structures are because its slick surface often all can only be from top emission electronic, limited the further raising of field emission performance, a kind ofly not only had the tip, and also had the structure of a lot of launching site to be used as the filed emission cathode material of a new generation from the teeth outwards so be necessary to make.On the other hand, want nano material is applied among the nano functional device, unidimensional nanometer tectonic element be self-assembled into the two dimension or three-dimensional nanostructure by different level be the problem that presses for solution that current nanotechnology faces, also be current many investigators' goal in research.
Summary of the invention
The objective of the invention is to propose a kind of periodicity monocrystal nanostructure of ZnO tower shape, it is characterized in that, this nanostructure is to have level and a periodic ZnO tower shape monocrystal nanostructure by what be grown in that hexagonal nano unit on the silicon chip assembles from bottom to top, and the length of described tower shape monocrystal nanostructure, bottom diameter and tip diameter are respectively 20～30 μ m, 3～10 μ m and 5～15nm.
Another object of the present invention provides a kind of method of periodicity monocrystal nanostructure of the ZnO of preparation tower shape.To achieve these goals, the present invention adopts following technical scheme.As substrate, as evaporation source, is carrier gas with Ar with the Zn powder with silicon chip, and under the condition of atmospheric pressure and 550～700 ℃, growth ZnO nano crystal obtains product, the periodicity monocrystal nanostructure of ZnO tower shape on substrate with thermal evaporation method.
Now describe technical scheme of the present invention in detail.
A kind of method for preparing the periodicity monocrystal nanostructure of ZnO tower shape is characterized in that, concrete processing step is as follows:
The first step cleaning silicon chip
With traditional method cleaning silicon chip;
Second step heating tubular type growth furnace
The tubular type growth furnace of horizontal positioned is heated to 550～700 ℃;
The 3rd step was placed evaporation source and silicon chip
With evaporation source, the Zn powder is put into quartz boat, and the silicon chip of handling through the first step is covered on quartz boat, collects resultant of reaction, and the distance of evaporation source and silicon chip is 3～8mm;
The 4th step was placed quartz boat
Quartz boat is put into the middle part of the tubular type growth furnace that heats through second step;
The 5th step fed carrier gas
With carrier gas, rare gas element Ar feeds the tubular type growth furnace, and the flow of carrier gas is 0.5L/min～2L/min, carries out thermal evaporation reaction 30～90min under the condition of atmospheric pressure and 550～700 ℃;
The 6th step made product
Take out quartz boat and silicon chip, the white translucent membranaceous thing that is grown on the silicon chip is exactly a product, the periodicity monocrystal nanostructure of ZnO tower shape.
Product has the identical structure of periodicity monocrystal nanostructure with above-mentioned ZnO tower shape.
Technical scheme of the present invention is further characterized in that, in second step, the tubular type growth furnace is made up of the silica tube of two different diameters, and the length and the diameter of big silica tube are respectively 110cm and 8cm, the length of little silica tube and diameter are respectively 140cm and 4cm, and little silica tube is inserted in the big silica tube; In the 4th step, quartz boat is placed on the middle part of little silica tube; In the 5th step, carrier gas feeds little silica tube.
Compare with existing synthetic technology and products thereof ZnO nanostructure, the present invention has following outstanding advantage:
(1) growth temperature is low, and pressure only is required to be normal pressure
Maximum growth temperature only needs 700 ℃, and pressure only is required to be normal pressure, has reduced the requirement to equipment.
(2) silicon chip is placed different
Existing synthetic method generally is placed on the dirty of air-flow to silicon substrate, with evaporation source at same level attitude, synthetic method of the present invention is placed directly in top with evaporation source to silicon chip.
(3) less demanding to carrier gas only needs Ar just passable, do not need logical people O
2Or other gases.
(4) method is simple, and cost is low, good reproducibility, and can be on silicon chip the periodicity monocrystal nanostructure of large area deposition ZnO tower shape.
Description of drawings
Fig. 1 is the X-ray diffractogram of the periodicity monocrystal nanostructure of ZnO tower shape.
Fig. 2 a is the SEM photo of the periodicity monocrystal nanostructure of a large amount of ZnO tower shapes.
Fig. 2 b is the SEM photo of high-amplification-factor of the periodicity monocrystal nanostructure of ZnO tower shape, and illustration wherein is the high-amplification-factor SEM photo of pinnacle of a pagoda.
Fig. 3 is the TEM photo of the periodicity monocrystal nanostructure of one ZnO tower shape.
Embodiment
All embodiment all operate by the preparation method's of above-mentioned superlong ZnO comb structure concrete processing step, and each embodiment is only enumerated crucial technical data.
Embodiment 1:
In second step, the tubular type growth furnace of horizontal positioned is heated to 550 ℃.In the 3rd step, with evaporation source, the Zn powder is put into quartz boat, and the distance of evaporation source and silicon chip is 3mm.In the 5th step, with carrier gas, rare gas element Ar feeds the tubular type growth furnace, and the flow of carrier gas is 0.5L/min, carries out thermal evaporation reaction 30min under the condition of atmospheric pressure and 550 ℃.
Embodiment 2:
In second step, the tubular type growth furnace of horizontal positioned is heated to 600 ℃.In the 3rd step, with evaporation source, the Zn powder is put into quartz boat, and the distance of evaporation source and silicon chip is 5mm.In the 5th step, with carrier gas, rare gas element Ar feeds the tubular type growth furnace, and the flow of carrier gas is 1L/min, carries out thermal evaporation reaction 60min under the condition of atmospheric pressure and 600 ℃.
Embodiment 3:
In second step, the tubular type growth furnace of horizontal positioned is heated to 700.In the 3rd step, with evaporation source, the Zn powder is put into quartz boat, and the distance of evaporation source and silicon chip is 8mm.In the 5th step, with carrier gas, rare gas element Ar feeds the tubular type growth furnace, and the flow of carrier gas is 2L/min, carries out thermal evaporation reaction 90min under the condition of atmospheric pressure and 700 ℃.
Embodiment 4:
Except for the following differences, remaining processing step and embodiment 1 are identical.
In second step, the tubular type growth furnace is made up of the silica tube of two different diameters, and the length and the diameter of big silica tube are respectively 110cm and 8cm, and the length of little silica tube and diameter are respectively 140cm and 4cm, and little silica tube is inserted in the big silica tube; In the 4th step, quartz boat is placed on the middle part of little silica tube; In the 5th step, carrier gas feeds little silica tube.
Embodiment 5:
Except for the following differences, remaining processing step and embodiment 2 are identical.
In second step, the tubular type growth furnace is made up of the silica tube of two different diameters, and the length and the diameter of big silica tube are respectively 110cm and 8cm, and the length of little silica tube and diameter are respectively 140cm and 4cm, and little silica tube is inserted in the big silica tube; In the 4th step, quartz boat is placed on the middle part of little silica tube; In the 5th step, carrier gas feeds little silica tube.
Embodiment 6:
Except for the following differences, remaining processing step and embodiment 3 are identical.
In second step, the tubular type growth furnace is made up of the silica tube of two different diameters, and the length and the diameter of big silica tube are respectively 110cm and 8cm, and the length of little silica tube and diameter are respectively 140cm and 4cm, and little silica tube is inserted in the big silica tube; In the 4th step, quartz boat is placed on the middle part of little silica tube; In the 5th step, carrier gas feeds little silica tube.
Periodicity monocrystal nanostructure with the ZnO tower shape of preparation method of the present invention preparation is specially adapted to as cathode material and microscopical probe such as STM, AFM in the emission microelectronics.
Claims (3)
1, a kind of periodicity monocrystal nanostructure of ZnO tower shape, it is characterized in that, this nanostructure is to have level and a periodic ZnO tower shape monocrystal nanostructure by what be grown in that hexagonal nano unit on the silicon chip assembles from bottom to top, and the length of described tower shape monocrystal nanostructure, bottom diameter and tip diameter are respectively 20～30 μ m, 3～10 μ m and 5～15nm.
2, a kind of method for preparing the periodicity monocrystal nanostructure of ZnO tower shape is characterized in that, concrete processing step is as follows:
The first step cleaning silicon chip
With traditional method cleaning silicon chip;
Second step heating tubular type growth furnace
The tubular type growth furnace of horizontal positioned is heated to 550～700 ℃;
The 3rd step was placed evaporation source and silicon chip
With evaporation source, the Zn powder is put into quartz boat, and the silicon chip of handling through the first step is covered on quartz boat, collects resultant of reaction, and the distance of evaporation source and silicon chip is 3～8mm;
The 4th step was placed quartz boat
Quartz boat is put into the middle part of the tubular type growth furnace that heats through second step;
The 5th step fed carrier gas
With carrier gas, rare gas element Ar feeds the tubular type growth furnace, and the flow of carrier gas is 0.5L/min～2L/min, carries out thermal evaporation reaction 30～90min under the condition of atmospheric pressure and 550～700 ℃;
The 6th step made product
Take out quartz boat and silicon chip, the white translucent membranaceous thing that is grown on the silicon chip is exactly a product, the periodicity monocrystal nanostructure of ZnO tower shape.
3, the method for the periodicity monocrystal nanostructure of preparation ZnO tower shape according to claim 2, it is characterized in that, in second step, the tubular type growth furnace is made up of the silica tube of two different diameters, the length and the diameter of big silica tube are respectively 110cm and 8cm, the length of little silica tube and diameter are respectively 140cm and 4cm, and little silica tube is inserted in the big silica tube; In the 4th step, quartz boat is placed on the middle part of little silica tube; In the 5th step, carrier gas feeds little silica tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610117268 CN1958877A (en) | 2006-10-19 | 2006-10-19 | Periodic monocrystalline Nano structure of castellated ZnO, preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610117268 CN1958877A (en) | 2006-10-19 | 2006-10-19 | Periodic monocrystalline Nano structure of castellated ZnO, preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1958877A true CN1958877A (en) | 2007-05-09 |
Family
ID=38070722
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610117268 Pending CN1958877A (en) | 2006-10-19 | 2006-10-19 | Periodic monocrystalline Nano structure of castellated ZnO, preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1958877A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580405B (en) * | 2009-06-05 | 2011-07-27 | 华东师范大学 | Semiconductor material with ZnO cone-shaped nano structure compounded on silicon chip and preparation method thereof |
| CN102826587A (en) * | 2012-09-07 | 2012-12-19 | 天津大学 | Method for self assembling ZnO nanowire cluster structure at top end of metal needle point |
| CN112098390A (en) * | 2020-09-16 | 2020-12-18 | 燕山大学 | Surface enhanced Raman scattering substrate and preparation method thereof |
-
2006
- 2006-10-19 CN CN 200610117268 patent/CN1958877A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580405B (en) * | 2009-06-05 | 2011-07-27 | 华东师范大学 | Semiconductor material with ZnO cone-shaped nano structure compounded on silicon chip and preparation method thereof |
| CN102826587A (en) * | 2012-09-07 | 2012-12-19 | 天津大学 | Method for self assembling ZnO nanowire cluster structure at top end of metal needle point |
| CN112098390A (en) * | 2020-09-16 | 2020-12-18 | 燕山大学 | Surface enhanced Raman scattering substrate and preparation method thereof |
| CN112098390B (en) * | 2020-09-16 | 2021-12-14 | 燕山大学 | Surface enhanced Raman scattering substrate and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lu et al. | Hydrothermal growth of large-scale micropatterned arrays of ultralong ZnO nanowires and nanobelts on zinc substrate | |
| US7294417B2 (en) | Metal oxide nanostructures with hierarchical morphology | |
| Xu et al. | Density-controlled growth of aligned ZnO nanowire arrays by seedless chemical approach on smooth surfaces | |
| B Djurisic et al. | Recent progress in hydrothermal synthesis of zinc oxide nanomaterials | |
| KR101706353B1 (en) | Silicon nanowire comprising high density metal nanocluster and process for preparing the same | |
| Srivatsa et al. | Synthesis of aligned ZnO nanorod array on silicon and sapphire substrates by thermal evaporation technique | |
| CN101074492A (en) | Sulfide nano-tube array of semiconductor and its production | |
| CN1843932A (en) | Localized growth method of nanowire array of copper oxide | |
| CN100497179C (en) | Method for preparing nano zinc oxide film with different appearances through solution technique | |
| Zhang et al. | Controllable hydrothermal synthesis of ZnO nanowires arrays on Al-doped ZnO seed layer and patterning of ZnO nanowires arrays via surface modification of substrate | |
| CN1696358A (en) | Method of manufacturing nano-wire | |
| Sun et al. | Position and density control in hydrothermal growth of ZnO nanorod arrays through pre-formed micro/nanodots | |
| CN1958877A (en) | Periodic monocrystalline Nano structure of castellated ZnO, preparation method | |
| CN1843935A (en) | A tetrapod-like nanorod of zinc oxide, its preparation method and apparatus | |
| KR20070104034A (en) | Method of manufacturing tips for field emission, tips for field emission manufactured by the same, and device comprising the same | |
| KR20100104233A (en) | Fabrication of ultralong zno nanowire arrays with tunable density | |
| Yuan et al. | Growth of diameter-controlled ZnO nanorod arrays by hydrothermal technique for polymer solar cell application | |
| Liu et al. | Flexible orientation control of ultralong single-walled carbon nanotubes by gas flow | |
| CN107747130B (en) | A method of preparing metal phthalocyanine monocrystal thin films in the grapheme modified substrate of copper film | |
| Xie et al. | Template-guided growth of well-aligned ZnO nanocone arrays on FTO substrate | |
| CN109003883A (en) | The InGaN/GaN multiple quantum wells nano-pillar and preparation method thereof being grown in silicon/graphene compound substrate | |
| CN100349803C (en) | Tungsten oxide micron pipe and its preparation method | |
| US7132126B2 (en) | Room temperature synthesis of multiwalled carbon nanostructures | |
| CN1207452C (en) | High temperature molten salt reaction process of preparing one-dimensional ordered nano wire and nanotube array | |
| CN208570525U (en) | The InGaN/GaN multiple quantum wells nano-pillar being grown in silicon/graphene compound substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |