CN105220229B - Preparation method of ZnO single crystal nanotube array - Google Patents
Preparation method of ZnO single crystal nanotube array Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002071 nanotube Substances 0.000 title abstract description 16
- 239000013078 crystal Substances 0.000 title abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 239000000758 substrate Substances 0.000 claims abstract description 23
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 78
- 238000010792 warming Methods 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 238000002207 thermal evaporation Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 15
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 description 7
- 239000010432 diamond Substances 0.000 description 7
- 229910003460 diamond Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- NQTSTBMCCAVWOS-UHFFFAOYSA-N 1-dimethoxyphosphoryl-3-phenoxypropan-2-one Chemical compound COP(=O)(OC)CC(=O)COC1=CC=CC=C1 NQTSTBMCCAVWOS-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000000101 transmission high energy electron diffraction Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 102000029749 Microtubule Human genes 0.000 description 1
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- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
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- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a ZnO single crystal nanotube array, which comprises the following steps: (1) putting zinc powder into a container, and putting the container and a substrate into a tube furnace; (2) vacuumizing the tube furnace, and filling compressed air; (3) heating the tubular furnace, and naturally cooling after reaction; (4) and taking out the substrate, wherein the growth on the substrate is the ZnO single crystal nanotube array. The method is economical, convenient, high in controllability and high in repeatability. The prepared ZnO nanotube has the advantages of thin tube wall, high crystallinity and regular arrangement, and has wide research value and application prospect in the fields of solar cells, photocatalysis, biological and gas sensors and the like.
Description
Technical field
The present invention relates to technical field of semiconductor.More particularly, to a kind of preparation of TiO2 monocrystal nano pipe array
Method.
Background technology
Japanese Scientists Sumio Iijima in 1991 reports discovery (the Iijima S.Helical of carbon nanotube for the first time
microtubules of graphitic carbon[J].nature,1991,354(6348):56-58), people has been caused since then
For this tubular nanometer material strong research enthusiasm.Nanotube increases with specific surface area more outstanding than nanometer rods
Potent fruit, this has a very important significance for improving the efficiency of photochemistry and photophysical process.For example, high-specific surface area can
It with reinforcing material adsorption of chemical species, absorbs light and limits the ability of light scattering, be conducive to the speed and right for improving catalysis reaction
In sensitivity (Vayssieres L, the et al.Three-dimensional array of highly of light absorption
oriented crystalline ZnO microtubes[J].Chemistry of Materials,2001,13(12):
4395-4398).Therefore people also attempt to prepare the tubular structure of other materials, among these, ZnO nanotube/becomes research
Hot spot.ZnO is a kind of typical direct band gap semiconductor material with wide forbidden band, its energy gap at normal temperatures is 3.37eV,
With excellent conduction, heat conductivility, chemical property is highly stable, is widely used in ceramics, rubber, coating and photoelectron
Equal fields.
The method for preparing ZnO nanotube/at present includes mainly metal organic chemical vapor deposition method (MOCVD) (Xu W Z, et
al.Quasi-aligned ZnO nanotubes grown on Si substrates[J].Applied Physics
Letters,2005,87(9):093110), two-step hydrothermal route method (Wei A, et al.Growth mechanism of
tubular ZnO formed in aqueous solution[J].Nanotechnology,2006,17(6):1740) and
Chemical vapour deposition technique (CVD) (Xing Y, et al.Optical properties of the ZnO nanotubes
synthesized via vapor phase growth[J].Applied Physics Letters,2003,83(9):
1689-1691).However above method all has different degrees of limitation.For example, the equipment and original that are used in mocvd method
Expect sufficiently expensive；Two-step hydrothermal route method process complexity is cumbersome, and product crystallinity is bad；The ZnO nanotube/that CVD method obtains is mixed
Disorderly lodging arranges, and is only suitable for being assembled into the device based on single ZnO nanotube/, the signal of this device using micro fabrication
It is very faint, and micro fabrication difficulty is big, time-consuming.In the present invention, we utilize simple and economical thermal evaporation for the first time
Method is prepared for TiO2 monocrystal nano pipe array, and obtained ZnO nanotube/pattern and structure is uniform, marshalling, crystallinity are high,
It is the ideal material of the devices such as solar cell, UV photodetector, chemical/biological sensors.
Invention content
It is an object of the present invention to provide a kind of preparation methods of TiO2 monocrystal nano pipe array.Present invention preparation side
Method economy is convenient, and the raw material used is cheap, and only need to heat reaction by a step and can be completed, and obtains different sizes and is distributed close
The TiO2 monocrystal nano pipe of degree.
In order to achieve the above objectives, the present invention uses following technical proposals：
A kind of preparation method of TiO2 monocrystal nano pipe array, is prepared using thermal evaporation.
Preferably, thermal evaporation prepares TiO2 monocrystal nano pipe array and includes the following steps：
1) it takes zinc powder to be put into container, then container and substrate is put into tube furnace；
2) to tubular type stove evacuation, it is filled with compressed air；
3) tube furnace is heated up, makes tube furnace Temperature fall after reaction；
4) substrate is taken out, gained growth-gen is TiO2 monocrystal nano pipe array on substrate.
Preferably, in step 1), the purity of the zinc powder is 99.9% or more.
Preferably, in step 1), the substrate is one kind in metal mesh, silicon chip, quartz plate or sapphire sheet.
It is highly preferred that the metal mesh is molybdenum net or nickel screen.
Preferably, in step 1), the container is placed in the heating zone of tube furnace, and the high temperature for making zinc powder be located at tube furnace adds
Hot-zone；The substrate is placed in heating zone downstream.
Preferably, in step 1), the substrate is located at below zinc powder at 0-20cm.
Preferably, in step 2), described vacuumize refers to that pressure in tube furnace is down to 0.1-10Pa；It is described to be filled with compression
Air refers to that the compressed air of 10-30sccm is passed through in tube furnace, and control intraductal pressure is in 10-200Pa.
Preferably, in step 3), the heating refers to that diamond heating area is warming up to 550-900 DEG C, and heating rate is
10-25℃/min；The reaction time is 0.5-2 hours.
Beneficial effects of the present invention are as follows：
The present invention is prepared for the TiO2 monocrystal nano pipe array of proper alignment using thermal evaporation method for the first time.Nanotube battle array
It arranges with distinct hollow structure and specific surface area enhancing effect outstanding.
The present invention preparation method economy it is convenient and easy to operate, the raw material used be cheap zinc powder, and low cost
Compressed air is not necessarily to catalyst, only raw material and substrate need to be put into tube furnace, can be completed by step heating reaction, and
With the continuous rising of temperature, air-flow is constantly filled with and obtains reaction product.
This method controllability is strong and repeatability is high, by controlling heating temperature, intraductal pressure and air velocity, can stablize
Obtain the TiO2 monocrystal nano pipe of different sizes and distribution density.
TiO2 monocrystal nano tube wall that the present invention obtains is thin, crystallinity is high, marshalling, is urged in solar cell, light
There is extensive researching value and application prospect in the fields such as change, biology and gas sensor.
Description of the drawings
Specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.
In Fig. 1, (a) shows low power scanning electron microscope (SEM) image of the TiO2 monocrystal nano pipe array of embodiment 1；
(b) SEM image of the single TiO2 monocrystal nano pipe of embodiment 1 is shown.
Fig. 2 shows energy dispersion X-ray spectrometer (EDX) collection of illustrative plates of the TiO2 monocrystal nano pipe array of embodiment 1.
Fig. 3 shows X-ray diffraction (XRD) collection of illustrative plates of the TiO2 monocrystal nano pipe array of embodiment 1.
In Fig. 4, (a) shows high-resolution-ration transmission electric-lens (HRTEM) image of the TiO2 monocrystal nano pipe of embodiment 1；(b) show
Go out selection electronic diffraction (SAED) image of the TiO2 monocrystal nano pipe of embodiment 1.
Fig. 5 shows degradation rate and the illumination of the degradation methyl orange solution of the TiO2 monocrystal nano pipe array photo catalysis in embodiment 1
The curve of time, the light source used are 30mW ultraviolet lamps, optical source wavelength 254nm.
Specific implementation mode
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar component is indicated with identical reference numeral in attached drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
A kind of preparation method of TiO2 monocrystal nano pipe array, steps are as follows：
1. weighing the zinc powder that 1g purity is 99.9% to be put into ceramic boat, then ceramic boat is placed on to the heating of tube furnace
Area, it is ensured that zinc powder is located at the high-temperature heating area of heating zone；
2. by substrate molybdenum net be placed on heating zone downstream away from zinc powder 5cm at；
3. opening mechanical pump the compressed air of 30sccm to be passed through in tube furnace, pressure when pressure is down to 5Pa in stove
Control is in 200pa；
4. diamond heating area is warming up to 600 DEG C, heating rate is 15 DEG C/min, and the reaction time is 0.5 hour；
5. reaction terminates, after being naturally cooling to room temperature in tube furnace, substrate is taken out, Grown marshalling
TiO2 monocrystal nano pipe array.
(a) shows low power scanning electron microscope (SEM) image of the TiO2 monocrystal nano pipe array of embodiment 1 in Fig. 1,
It was found from the figure that the monodimension nanometer material of marshalling homoepitaxial on molybdenum mesh liner bottom；
(b) shows the SEM image of the single TiO2 monocrystal nano pipe of embodiment 1 in Fig. 1, it was found from the figure that, 1-dimention nano material
Material has tubular structure, and tube wall is thin, surface is smooth and pattern is regular；
Fig. 2 shows energy dispersion X-ray (EDX) collection of illustrative plates of the TiO2 monocrystal nano pipe array of embodiment 1, it was found from the figure that,
Nanotube is made of Zn elements and O elements；
Fig. 3 shows X-ray diffraction (XRD) collection of illustrative plates of the TiO2 monocrystal nano pipe array of embodiment 1, it was found from the figure that, nanometer
The ZnO of the side's Guan Youliu Wurzite structure is constituted；
(a) shows high-resolution-ration transmission electric-lens (HRTEM) image of the TiO2 monocrystal nano pipe of embodiment 1 in Fig. 4, from the figure
It is found that ZnO nanotube/is grown along [0001] direction；
(b) shows selection electronic diffraction (SAED) image of the TiO2 monocrystal nano pipe of embodiment 1 in Fig. 4, can from the figure
Know, the SAED images of TiO2 monocrystal nano piece are the electronic diffraction hot spots of rule, have typical single crystal diffraction feature, show ZnO
Single crystal nanoplate has good crystal quality.
Embodiment 2
A kind of preparation method of TiO2 monocrystal nano pipe array, steps are as follows：
1. weighing the zinc powder that 1.2g purity is 99.9% to be put into ceramic boat, then ceramic boat is placed on to the heating of tube furnace
Area, it is ensured that zinc powder is located at the high-temperature heating area of heating zone；
2. by silicon substrate be placed on heating zone downstream away from zinc powder 10cm at；
3. opening mechanical pump the compressed air of 20sccm to be passed through in tube furnace, pressure when pressure is down to 1Pa in stove
Control is in 100pa；
4. diamond heating area is warming up to 700 DEG C, heating rate is 15 DEG C/min, and the reaction time is 1 hour；
5. reaction terminates, after being naturally cooling to room temperature in tube furnace, sample is taken out, Grown marshalling
TiO2 monocrystal nano pipe array.
Embodiment 3
A kind of preparation method of TiO2 monocrystal nano pipe array, steps are as follows：
1. weighing the zinc powder that 2g purity is 99.9% to be put into ceramic boat, then ceramic boat is placed on to the heating of tube furnace
Area, it is ensured that zinc powder is located at the high-temperature heating area of heating zone；
2. by substrate sapphire piece be placed on heating zone downstream away from zinc powder 20cm at；The present invention is using nickel screen, silicon chip, potsherd
Or quartz plate substrate can reach identical effect.
3. opening mechanical pump the compressed air of 10sccm is passed through in tube furnace when pressure is down to 0.1Pa in stove, press
Strong control is in 50pa；
4. diamond heating area is warming up to 800 DEG C, heating rate is 25 DEG C/min, and the reaction time is 2 hours；
5. reaction terminates, after being naturally cooling to room temperature in tube furnace, substrate is taken out, Grown marshalling
TiO2 monocrystal nano pipe array.
Embodiment 4
Embodiment 2 is repeated, difference lies in be changed to " the waiting for that pressure is down to 1Pa in stove " in step 3 " to wait for that pressure drops in stove
To 0.1Pa ", other steps are constant, and the TiO2 monocrystal nano pipe array of marshalling is prepared.
Embodiment 5
Embodiment 2 is repeated, difference lies in be changed to " pressure control in 100pa " in step 3 that " pressure control exists
10pa ", other steps are constant, and the TiO2 monocrystal nano pipe array of marshalling is prepared.
Embodiment 6
Embodiment 1 is repeated, difference lies in be changed to " diamond heating area being warming up to 600 DEG C " in step 4 " by tubular type
Stove heat area is warming up to 550 DEG C ", other steps are constant, and the TiO2 monocrystal nano pipe array of marshalling is prepared.
Embodiment 7
Embodiment 1 is repeated, difference lies in " will be warming up to 600 DEG C, heating rate 15 in step 4 by diamond heating area
DEG C/min " is changed to " diamond heating area is warming up to 900 DEG C, heating rate is 10 DEG C/min ", and other steps are constant, are prepared into
To the TiO2 monocrystal nano pipe array of marshalling.
There is the TiO2 monocrystal nano pipe being prepared in embodiment unique hollow structure and specific surface area outstanding to enhance
Effect, thus can be applied to the fields such as photocatalysis, solar cell.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (5)
1. a kind of preparation method of TiO2 monocrystal nano pipe array, it is characterised in that：The TiO2 monocrystal nano pipe array is to use
What thermal evaporation was prepared；
The thermal evaporation includes the following steps：
1) it takes zinc powder to be put into container, then container and substrate is put into tube furnace, wherein the substrate is located at zinc powder downstream
At 5cm, 10cm or 20cm；
2) to tubular type stove evacuation, it is filled with compressed air；
3) tube furnace is heated up, makes tube furnace Temperature fall after reaction；
4) substrate is taken out, gained growth-gen is TiO2 monocrystal nano pipe array on substrate；
In step 1), the substrate is metal mesh, and the metal mesh is molybdenum net or nickel screen.
2. preparation method according to claim 1, it is characterised in that：In step 1), the purity of the zinc powder is 99.9%
More than.
3. preparation method according to claim 1, it is characterised in that：In step 1), the container is placed in adding for tube furnace
Hot-zone, and zinc powder is made to be located at the high-temperature heating area of tube furnace；The substrate is placed in heating zone downstream.
4. preparation method according to claim 1, it is characterised in that：In step 2), described vacuumize refers to by tube furnace
Interior pressure is down to 0.1-10Pa；The compressed air that is filled with refers to that the compressed air of 10-30sccm is passed through in tube furnace, control
Intraductal pressure is in 10-200Pa.
5. preparation method according to claim 1, it is characterised in that：In step 3), the heating refers to adding tube furnace
Hot-zone is warming up to 550-900 DEG C, and heating rate is 10-25 DEG C/min；The reaction time is 0.5-2 hours.
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| CN1618738A (en) * | 2003-11-18 | 2005-05-25 | 北京大学 | Zinc oxide nano-wire and its preparation method and application |
| CN102618849A (en) * | 2012-03-15 | 2012-08-01 | 中国科学院理化技术研究所 | One-dimensional ZnO/SnO2Preparation method of core-shell structure nano heterojunction semiconductor material |
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| CN100396615C (en) * | 2006-06-30 | 2008-06-25 | 华东师范大学 | Process for preparing nano ZnO |
| KR100836890B1 (en) * | 2007-04-05 | 2008-06-11 | 한국과학기술원 | Method for vertical growth of zno nanowires on ito substrate |
| CN101412534A (en) * | 2008-11-18 | 2009-04-22 | 北京科技大学 | Method for preparing high yield tetrapod-shaped nano zinc oxide by autocatalysis |
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| CN1618738A (en) * | 2003-11-18 | 2005-05-25 | 北京大学 | Zinc oxide nano-wire and its preparation method and application |
| CN102618849A (en) * | 2012-03-15 | 2012-08-01 | 中国科学院理化技术研究所 | One-dimensional ZnO/SnO2Preparation method of core-shell structure nano heterojunction semiconductor material |
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