CN103641154B - A kind of method of Al-Doped ZnO nano rod array structure low temperature synthesis - Google Patents
A kind of method of Al-Doped ZnO nano rod array structure low temperature synthesis Download PDFInfo
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- CN103641154B CN103641154B CN201310682603.XA CN201310682603A CN103641154B CN 103641154 B CN103641154 B CN 103641154B CN 201310682603 A CN201310682603 A CN 201310682603A CN 103641154 B CN103641154 B CN 103641154B
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Abstract
The present invention relates to micro Nano material and structure preparation field, relate to and a kind ofly substrate is inverted in the method and apparatus preparing Al-Doped ZnO nano rod array structure in solution at low temperatures.The present invention's dose volume mark in weighing bottle is the methane amide aqueous solution of 5 ~ 20%, being kept at a distance to separate by two panels rectangle zinc paper tinsel is dipped vertically in solution, the top substrate coated surface being coated with buffer layer thin film being placed on two zinc paper tinsels down can keep stable, and aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, in the baking oven being placed in 50 ~ 90 DEG C, reaction 4 ~ 20 hours, takes out substrate, cleans up and after drying with deionized water, ethanol and acetone.The method can by obtaining the Al-Doped ZnO nano rod array of different diameter and length to the control of substrate height, method is simple, energy-conservation, processing ease, and to equipment without particular requirement, cost is low.
Description
Technical field
The present invention relates to micro Nano material and structure preparation field, relate to and a kind ofly substrate is inverted in the method and apparatus preparing Al-Doped ZnO nano rod array structure in solution at low temperatures.
Background technology
Zinc oxide is the semiconductor material under a kind of normal temperature with larger energy gap (3.37eV) and exciton bind energy (60 meV); Nano zine oxide shows the incomparable performance of other traditional material owing to having the nano effect such as dimensional effect, table/interfacial effect, the characteristic differed widely with macro-scale material is shown, because being widely used in the fields such as short-wavelength laser, photocatalyst, gas sensor, photodiode, solar cell in optics, electricity, magnetics, mechanics, chemistry etc.; Wherein, the zinc oxide nano array of one dimension oriented growth more due to its excellent properties in electric transmission, is considered to the optimal candidate material preparing the photoelectric device such as solar cel electrode, photodiode.
At present, the method preparing one dimension selective paraffin oxidation zinc nano array structure is a lot, and the difference based on reaction medium can be divided into gas phase synthesis method and liquid phase synthesizing method; Applying more in gas phase synthesis method is air-liquid-solid (VLS) method, gas phase-solid phase (VS) method and carbothermic method, these methods all belong to the evaporation deposition method of high temperature, high energy consumption, equipment cost is higher, and preparation condition is harsh and operating process is complicated; Applying more in liquid phase synthesizing method is template, water (solvent) hot method etc., wherein template needs to make template especially, cost is high, and the pattern of synthetics and size-constrained in template, and water (solvent) hot rule have low temperature, low cost, easy and simple to handle, pollution-free, big area the advantage such as can to prepare, the preparation of zinc oxide nano array structure embodies its exclusive advantage; In first technology, water (solvent) hot legal system is adopted to be generally for the method for Zinc oxide nano-rod array structure: zinc nitrate or zinc acetate and vulkacit H (HMT) or cetyl trimethylammonium bromide (CTAB) being dissolved in the water is made into mixing solutions, again by substrate level, inclination or be vertically positioned in solution, solution is heated and keeps certain hour, substrate is taken out and namely can be observed Zinc oxide nano-rod array (see document: [1] X. Liu after cleaning, drying, Z. Jin, S. Bu, J. Zhao, and Z. Liu.
materials Letters59 (2005) 3994 ~ 3999; [2] Y. Tong, Y. Liu, L. Dong, D. Zhao, J. Zhang, Y. Lu, D. Shen, and X. Fan.
the Journal of Physical Chemistry B110 (2006) 20263 ~ 20267; [3] H. Chen, X. Wu, L. Gong, C. Ye, F. Qu, and G. Shen.
nanoscale Research Letters5 (2010) 570 ~ 575; [4] S. Sarkar, S. Patra, S.K. Bera, G.K. Paul, and R. Ghosh.
materials Letters64 (2010) 460 ~ 462; [5] L. Wang, Y. Kang, X. Liu, S. Zhang, W. Huang, and S. Wang.
sensors and Actuators B162 (2012) 237 ~ 243); Doping can change the level structure in zinc oxide forbidden band, thus change its electromagnetic performance and optical property, the nano zinc oxide material of various metal or nonmetal doping is synthesized, as utilized above water (solvent) hot method, mix a certain amount of aluminum nitrate more in the solution, prepare the ZnO nanorod mixing aluminium, when Al replaces the position of Zn in ZnO, the excess carriers introduced by impurity will be full of at the bottom of conduction band, cause the blue shift of nearly band-edge emission, namely so-called Burstein-Mass effect is (see document: [1] Xu Di, Duan Xuechen, Li Zhonglan, Zhu Xiebin.
functional materials39 (2008) 695 ~ 697); But the ammonium salt (HMT or CTAB) that this kind of doping or the preparation method undoping Zinc oxide nano-rod array structure adopt has relatively high toxicity, corrodibility and inflammableness usually, to environment and personnel safety unfavorable; Temperature higher (being usually greater than 90 DEG C) required for solution heating, energy consumption is high and heat-up time is longer; The size of products therefrom and pattern inequality, repeatable poor.
Summary of the invention
The object of this invention is to provide the method and apparatus of controlled synthesis Al-Doped ZnO nano rod array structure under a kind of low temperature, the method can by obtaining the Al-Doped ZnO nano rod array of different diameter and length to the control of substrate height, method is simple, energy-conservation, processing ease, to equipment without particular requirement, cost is low.
The technical solution adopted in the present invention is as follows:
A method for Al-Doped ZnO nano rod array structure low temperature synthesis, its concrete steps are:
In weighing bottle, dose volume mark is the methane amide aqueous solution of 5 ~ 20%, being kept at a distance to separate by two panels rectangle zinc paper tinsel is dipped vertically in solution, the top substrate coated surface being coated with buffer layer thin film being placed on two zinc paper tinsels down can keep stable, and aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, in the baking oven being placed in 50 ~ 90 DEG C, reaction 4 ~ 20 hours, takes out substrate, after cleaning up also drying with deionized water, ethanol and acetone.
In technical scheme, zinc paper tinsel height is 5 ~ 15 mm, and the edge lengths that namely zinc paper tinsel is vertical is 5 ~ 15 mm.
In technical scheme, buffer layer thin film thickness is 10 ~ 800 nm.
In technical scheme, the methane amide adopted is analytical pure commercial reagents CH
3nO.
In technical scheme, the water adopted is pure water, deionized water or distilled water.
In technical scheme, zinc paper tinsel height determines substrate height in the solution, and it is to both ensure easy to operate (too short being difficult to picks and places) in 5 ~ 15 mm scopes, again can support substrates (oversize rigidity is inadequate).
In technical scheme, the standard that zinc paper tinsel is kept at a distance is to ensure that substrate stablizes the top being placed on two zinc paper tinsels.
In technical scheme, the buffer layer thin film adopted is deposited on substrate material by existing coating technique, as chemical Vapor deposition process, sol-gel method, spray pyrolysis method, magnetron sputtering method, vacuum vapour deposition, pulsed laser deposition, its effect is the interfacial energy effectively reduced between nucleus and substrate, thus be lowered into nuclear barrier, the formation of accelerating oxidation zinc nano rod array structure; Be used for preparing the buffer layer thin film of Al-Doped ZnO nano rod array structure in prior art (as Ag film, Al film, Au film, ZnO film, AZO film, ito film, FTO film, TiO
2film) and substrate material (as silicon, glass, stainless steel) all can be used for implement the present invention; Above-mentioned technology is prior art, no longer describes in detail.
In technical scheme, glass cover tilts to cover weighing bottle mouth and refers to glass cover is leant against weighing bottle bottleneck, and pollutent both can have been stoped to enter, and can ensure again enough air and enter in bottle and participate in reaction.
Reaction mechanism of the present invention is speculated as: zinc paper tinsel and methane amide (HCONH
2) the generation zinc that first reacts-methane amide mixture ([Zn (HCONH
2)
n ]
2+) (Zn+1/2O
2+
nhCONH
2+ H
2o=[Zn (HCONH
2)
n ]
2++ 2OH
-), the thermolysis under 50 ~ 90 DEG C of conditions of zinc subsequently-methane amide mixture is ZnO crystallite ([Zn (HCONH
2)
n ]
2+=Zn
2++
nhCONH
2, Zn
2++ 2OH
-=Zn (OH)
2, Zn (OH)
2=ZnO+H
2o).Aluminium foil also obtains Al by generating aluminium-methane amide mixture with formamide and decompose therebetween
2o
3crystallite, at ZnO and Al
2o
3formed in the process of precipitation, coprecipitation phenomena occurs and forms the ZnO mixing aluminium.
Compared with prior art, the invention has the beneficial effects as follows:
1) only adopt carboxamide agents preparation reaction soln, its toxicity is little, and cost is low.
2) naturally carry out in the solution of whole reaction under 50 ~ 90 DEG C of lower temperature conditions, directly can obtain Al-Doped ZnO nano rod array in substrate previous step, easy and simple to handle, reaction conditions is gentle, and energy consumption is low, without the need to special expensive equipment.
3) compared with the usual method kept flat upward by substrate coated surface, plated film placed face down is more conducive to homogeneous nucleation and the oriented growth of zincite crystal.Because the nucleation process of ZnO crystal is homogeneous nucleation in solution, crystal may any point nucleation in the solution, if the nucleus in solution is deposited on substrate, the nano rod directivity causing being formed is deteriorated, substrate also can cause the homogeneity of the nano rod formed be deteriorated if the impurity in same solution accumulates to, plated film placed face down then can avoid the deposition of zinc oxide nucleus and other impurity in solution very well.
4) experiment proves, adopt method of the present invention, when zinc paper tinsel height (i.e. substrate height in the solution) increases, diameter and the length of synthesized Al-Doped ZnO nano rod reduce all gradually, until change tends towards stability; Therefore, the present invention simply by the control to zinc paper tinsel height (i.e. substrate height in the solution), can synthesize the Al-Doped ZnO nano rod array of different diameter and length, to adapt to the needs of different application occasion easily.
Accompanying drawing explanation
Fig. 1 Al-Doped ZnO nano rod array structure synthesizer schematic diagram;
1 zinc paper tinsel, 2 weighing bottles, the 3 methane amide aqueous solution, 4 buffer layer thin films, 5 substrates, 6 aluminium foils, 7 glass covers, 8 baking ovens, 9 Stage microscopes, 10 Al-Doped ZnO nano rod array structures.
In Fig. 2 embodiment 1, the top view (a) of the Al-Doped ZnO nano rod array structure of gained is schemed and energy spectrogram (c) with side-looking (b) SEM.
The diameter of gained Al-Doped ZnO nano rod and the change curve of length when Fig. 3 changes the zinc paper tinsel height in embodiment 1.
The SEM figure of the Al-Doped ZnO nano rod array structure of gained in Fig. 4 embodiment 2.
The SEM figure of the Al-Doped ZnO nano rod array structure of gained in Fig. 5 embodiment 3.
The SEM figure of the Al-Doped ZnO nano rod array structure of gained in Fig. 6 embodiment 4.
The SEM figure of the Al-Doped ZnO nano rod array structure of gained in Fig. 7 embodiment 5.
Embodiment
Fig. 1 is Al-Doped ZnO nano rod array structure synthesizer schematic diagram.Two panels zinc paper tinsel 1 is separated in the methane amide aqueous solution 3 being dipped vertically into along its length and being contained in weighing bottle 2 also fixing, the substrate 5 being coated with buffer layer thin film 4 is placed on the top of two zinc paper tinsels 1 down with coated surface, and a small pieces aluminium foil 6 is positioned over bottom solution, then weighing bottle 2 glass cover 7 is tilted to cover, moving on the Stage microscope 9 in baking oven 8 keeps constant temperature to react, and finally can obtain Al-Doped ZnO nano rod array structure 10 on substrate 5.
Below in conjunction with accompanying drawing, the present invention is further detailed explanation.
embodiment 1:in weighing bottle, dose volume mark is the methane amide aqueous solution of 5%, being separated by two panels rectangle zinc paper tinsel is dipped vertically in solution, zinc paper tinsel height is edge lengths 15 mm that 15 mm(and zinc paper tinsel are vertical), the silicon substrate coated surface being coated with the thick Ag film of 10 nm is placed on the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, reaction 4 hours in the baking oven being placed in 90 DEG C, take out silicon substrate, clean up with deionized water, ethanol and acetone and drying; The top view and the side-looking SEM that are respectively Al-Doped ZnO nano rod array structure obtained on a silicon substrate shown in Fig. 2 (a) He (b) scheme, and the mean diameter of nano rod is 240 nm, length is 2.6 μm; As can be seen from Fig. 2 (c) can spectrogram, except containing Zn element, O element, also containing Al element, what prove to obtain is the zinc oxide containing aluminium; As can be seen from Figure 3, under these conditions, when changing zinc paper tinsel height (i.e. substrate height in the solution), the diameter of Al-Doped ZnO nano rod and length all reduce along with the increase of zinc paper tinsel length, when zinc paper tinsel height reaches 12 mm, the diameter of nano rod and the change of length tend towards stability, and illustrate that zinc paper tinsel height has certain regulating and controlling effect to the diameter of Al-Doped ZnO nano rod and length.
embodiment 2:in weighing bottle, dose volume mark is the methane amide aqueous solution of 5%, being separated by two panels rectangle zinc paper tinsel is dipped vertically in solution, zinc paper tinsel height is the edge lengths that 12 mm(and zinc paper tinsel are vertical is 12 mm), the silicon substrate coated surface being coated with the thick ZnO film of 100 nm is placed on the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, reaction 8 hours in the baking oven being placed in 80 DEG C, take out silicon substrate, clean up with deionized water, ethanol and acetone and drying; Figure 4 shows that the SEM figure of Al-Doped ZnO nano rod array structure obtained on a silicon substrate, the mean diameter of nano rod is 760 nm.
embodiment 3:in weighing bottle, dose volume mark is the methane amide aqueous solution of 10%, being separated by two panels rectangle zinc paper tinsel is dipped vertically in solution, zinc paper tinsel height is the edge lengths that 10 mm(and zinc paper tinsel are vertical is 10 mm), the glass substrate coated surface being coated with the thick ito film of 200 nm is placed on the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, reaction 12 hours in the baking oven being placed in 70 DEG C, take out glass substrate, clean up with deionized water, ethanol and acetone and drying; Figure 5 shows that the SEM figure of Al-Doped ZnO nano rod array structure obtained on a glass substrate, the mean diameter of nano rod is 700 nm.
embodiment 4:in weighing bottle, dose volume mark is the methane amide aqueous solution of 15%, being separated by two panels rectangle zinc paper tinsel is dipped vertically in solution, zinc paper tinsel height is the edge lengths that 7 mm(and zinc paper tinsel are vertical is 7 mm), coated surface at the bottom of the stainless steel lining being coated with the thick AZO film of 500 nm is placed on the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, reaction 16 hours in the baking oven being placed in 60 DEG C, take out at the bottom of stainless steel lining, clean up with deionized water, ethanol and acetone and drying; Figure 6 shows that the SEM figure of Al-Doped ZnO nano rod array structure obtained at the bottom of stainless steel lining, the diameter of nano rod is 200 ~ 650 nm.
embodiment 5:in weighing bottle, dose volume mark is the methane amide aqueous solution of 20%, being separated by two panels rectangle zinc paper tinsel is dipped vertically in solution, zinc paper tinsel height is the edge lengths that 5 mm(and zinc paper tinsel are vertical is 5 mm), the glass substrate coated surface being coated with the thick FTO film of 800 nm is placed on the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, reaction 20 hours in the baking oven being placed in 50 DEG C, take out glass substrate, clean up with deionized water, ethanol and acetone and drying; Figure 7 shows that the SEM figure of Al-Doped ZnO nano rod array structure obtained on a glass substrate, the mean diameter of nano rod is 600 nm.
Embodiment provided by the present invention is only described technical scheme, and does not limit.
Claims (6)
1. the method for an Al-Doped ZnO nano rod array structure low temperature synthesis, it is characterized in that concrete steps are as follows: dose volume mark is the methane amide aqueous solution of 5 ~ 20% in weighing bottle, being kept at a distance to separate by two panels rectangle zinc paper tinsel is dipped vertically in solution, the top substrate coated surface being coated with buffer layer thin film being placed on two zinc paper tinsels down can keep stable, and aluminium foil is positioned over bottom solution, tilt to cover weighing bottle mouth with glass cover again, reaction 4 ~ 20 hours in the baking oven being placed in 50 ~ 90 DEG C, take out substrate, with deionized water, after ethanol and acetone clean up also drying, wherein zinc paper tinsel height is 5 ~ 15 mm, and the edge lengths that namely zinc paper tinsel is vertical is 5 ~ 15 mm, and zinc paper tinsel height determines substrate height in the solution, when substrate height in the solution increases zinc paper tinsel height in other words, diameter and the length of synthesized Al-Doped ZnO nano rod reduce all gradually, until change tends towards stability, the diameter of Al-Doped ZnO nano rod and length are respectively 0.20-0.76 μm and 2.4 μm-4.5 μm.
2. the method for a kind of Al-Doped ZnO nano rod array structure low temperature synthesis as claimed in claim 1, is characterized in that: buffer layer thin film thickness is 10 ~ 800 nm.
3. the method for a kind of Al-Doped ZnO nano rod array structure low temperature synthesis as claimed in claim 1, is characterized in that: the methane amide adopted is analytical pure commercial reagents CH
3nO, the water adopted is pure water.
4. the method for a kind of Al-Doped ZnO nano rod array structure low temperature synthesis as claimed in claim 1, is characterized in that: the standard that zinc paper tinsel is kept at a distance is to ensure that substrate stablizes the top being placed on two zinc paper tinsels.
5. the method for a kind of Al-Doped ZnO nano rod array structure low temperature synthesis as claimed in claim 1, it is characterized in that: the buffer layer thin film adopted is deposited on substrate material by existing coating technique, described coating technique is chemical Vapor deposition process, sol-gel method, spray pyrolysis method, magnetron sputtering method, vacuum vapour deposition or pulsed laser deposition, its effect is the interfacial energy effectively reduced between nucleus and substrate, thus be lowered into nuclear barrier, the formation of accelerating oxidation zinc nano rod array structure; Described buffer layer thin film is Ag film, Al film, Au film, ZnO film, AZO film, ito film, FTO film or TiO
2film, described substrate material is silicon, glass or stainless steel.
6. the method for a kind of Al-Doped ZnO nano rod array structure low temperature synthesis as claimed in claim 1, it is characterized in that: glass cover tilts to cover weighing bottle mouth and refers to glass cover is leant against weighing bottle bottleneck, both pollutent can have been stoped to enter, enough air can have been ensured again and enter participation reaction in bottle.
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| CN103059629A (en) * | 2012-12-28 | 2013-04-24 | 中国科学院过程工程研究所 | Zinc oxide nanowire conductive coating and preparation method thereof |
| CN103159253A (en) * | 2013-03-01 | 2013-06-19 | 中国科学院深圳先进技术研究院 | Aluminum-doped zinc oxide one-dimensional nanorod and preparation method thereof |
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| CN102050481A (en) * | 2009-11-04 | 2011-05-11 | 中国科学院半导体研究所 | Method for preparing zinc oxide nano material |
| CN103059629A (en) * | 2012-12-28 | 2013-04-24 | 中国科学院过程工程研究所 | Zinc oxide nanowire conductive coating and preparation method thereof |
| CN103159253A (en) * | 2013-03-01 | 2013-06-19 | 中国科学院深圳先进技术研究院 | Aluminum-doped zinc oxide one-dimensional nanorod and preparation method thereof |
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