CN103641154A - Method for synthesizing aluminum-doped zinc oxide nanorod array structure under low temperature - Google Patents
Method for synthesizing aluminum-doped zinc oxide nanorod array structure under low temperature Download PDFInfo
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- CN103641154A CN103641154A CN201310682603.XA CN201310682603A CN103641154A CN 103641154 A CN103641154 A CN 103641154A CN 201310682603 A CN201310682603 A CN 201310682603A CN 103641154 A CN103641154 A CN 103641154A
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Abstract
The invention relates to the field of preparation of micro-nano materials and structures, and relates to a method and a device for preparing an aluminum-doped zinc oxide nanorod array structure under a low temperature by inverting a substrate in liquor. The method comprises the following steps of preparing formamide aqueous liquor with volume fraction of 5%-20% in a weighing bottle, spacing two rectangular zinc foils by keeping a distance away, and vertically immersing the two rectangular zinc foils in liquor; downwards placing a substrate coating surface coated with a buffer layer film on the tops of the two zinc foils to keep the substrate coating surface stable, and placing an aluminum foil at the bottom of the liquor, and covering the port of the weighing bottle by a glass cover in an inclined manner; and placing the weighing bottle in an oven of 50 DEG C-90 DEG C for reacting for 4 hours-20 hours, taking out the substrate, cleaning the substrate by deionized water, alcohol and acetone, and drying to obtain the aluminum-doped zinc oxide nanorod array structure. The method disclosed by the invention can obtain aluminum-doped zinc oxide nanorod arrays with different diameters and lengths by controlling height of the substrate; moreover, the method is simple, energy-saving, easy to operate, free from special requirements for equipment, and low in cost.
Description
Technical field
The present invention relates to micro Nano material and structure preparation field, relate to a kind of method and apparatus of preparing at low temperatures Al-Doped ZnO nano rod array structure in solution that substrate is inverted in.
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 is because nano effects such as having dimensional effect, table/interfacial effect shows the incomparable performance of other traditional material, at aspects such as optics, electricity, magnetics, mechanics, chemistry, show the characteristic differing widely with macro-scale material, because being widely used in the fields such as short-wavelength laser, photocatalyst, gas sensor, photodiode, solar cell; Wherein, the zinc oxide nano array of one dimension oriented growth more, because it is at the excellent properties aspect electric transmission, is considered to prepare the optimal candidate material of the photoelectric devices such as solar cel electrode, photodiode.
At present, the method for 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; In gas phase synthesis method, applying more is air-liquid-solid (VLS) method, gas phase-solid phase (VS) method and carbothermic method, and these methods all belong to the evaporation deposition method of high temperature, high energy consumption, and equipment cost is higher, and preparation condition harshness and operating process are complicated; In liquid phase synthesizing method, applying more is template, the hot method of water (solvent) etc., wherein template needs the special template of making, cost is high, and the pattern of synthetics and size-constrained in template, and the hot rule of water (solvent) have low temperature, low cost, easy and simple to handle, pollution-free, the advantage such as can big area prepare, in the preparation of zinc oxide nano array structure, embody its exclusive advantage; Formerly in technology, adopt the hot legal system of water (solvent) 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) are dissolved in the water and are 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 can be observed through cleaning, after dry Zinc oxide nano-rod array (referring to document: [1] X. Liu, 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, thereby change its electromagnetic performance and optical property, the nano zinc oxide material of various metals or nonmetal doping is synthesized, as utilize the hot method of above water (solvent), in solution, mix again a certain amount of aluminum nitrate, prepare the ZnO nanorod of mixing aluminium, the position of Zn in Al replacement ZnO, will at the bottom of conduction band, be full of the excess carriers of being introduced by impurity, the blue shift that causes the transmitting of nearly band edge, so-called Burstein-Mass effect is (referring to document: [1] Xu Di, Duan Xuechen, Li Zhonglan, Zhu Xiebin.
functional materials39 (2008) 695 ~ 697); But the ammonium salt (HMT or CTAB) that the preparation method of this class doping or the Zinc oxide nano-rod array structure that undopes adopts has relatively high toxicity, corrodibility and inflammableness conventionally, unfavorable to environment and personnel safety; Solution heats needed temperature higher (being conventionally greater than 90 ℃), and energy consumption is high and heat-up time is longer; The size of products therefrom and pattern are uneven, repeatable poor.
Summary of the invention
The object of this invention is to provide the controlled method and apparatus of preparing Al-Doped ZnO nano rod array structure under a kind of low temperature, the method can be 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:
The synthetic method of Al-Doped ZnO nano rod array structure low temperature, its concrete steps are:
The methane amide aqueous solution that dose volume mark is 5 ~ 20% in weighing bottle, two rectangle zinc paper tinsels are kept at a distance to separate and be dipped vertically in solution, the top that the substrate coated surface that is coated with buffer layer thin film is placed on to two zinc paper tinsels down can keep stable, and aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 50 ~ 90 ℃ and react 4 ~ 20 hours, take out substrate, after cleaning up and be dried with deionized water, ethanol and acetone.
In technical scheme, zinc paper tinsel height is 5 ~ 15 mm, and the edge lengths that 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 adopting is analytical pure commercialization reagent C H
3nO.
In technical scheme, the water adopting is pure water, deionized water or distilled water.
In technical scheme, zinc paper tinsel height has determined the height of substrate in solution, and it is (too short be difficult to pick and place) easy to operate in order both to guarantee 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 for guaranteeing the stable top that is placed on two zinc paper tinsels of substrate.
In technical scheme, the buffer layer thin film adopting can be 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 reducing between nucleus and substrate, thereby be lowered into nuclear barrier, the formation of accelerating oxidation zinc nano rod array structure; In prior art, be used for preparing the buffer layer thin film of Al-Doped ZnO nano rod array structure (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 implementing 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 leaned at weighing bottle bottleneck, both can stop pollutent to enter, and can ensure again enough air and enter and in bottle, participate in reaction.
Reaction mechanism of the present invention is speculated as: zinc paper tinsel and methane amide (HCONH
2) generation zinc-methane amide mixture ([Zn (HCONH first reacts
2)
n ]
2+) (Zn+1/2O
2+
nhCONH
2+ H
2o=[Zn (HCONH
2)
n ]
2++ 2OH
-), zinc-methane amide mixture thermolysis under 50 ~ 90 ℃ of conditions is subsequently 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 and decompose with formamide therebetween
2o
3crystallite, at ZnO and Al
2o
3form in the process of precipitation, coprecipitation phenomena occurs and form the ZnO that mixes aluminium.
Compared with prior art, the invention has the beneficial effects as follows:
1) only adopt methane amide reagent preparation reaction soln, its toxicity is little, and cost is low.
2) in the solution of whole reaction under 50 ~ 90 ℃ of lower temperature conditions, naturally carry out, can directly in substrate previous step, make Al-Doped ZnO nano rod array, easy and simple to handle, reaction conditions is gentle, and energy consumption is low, without special expensive equipment.
3) compare with the method conventionally substrate coated surface being kept flat upward, 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 be in solution any point nucleation, if the nucleus in solution is deposited on substrate, by the nano rod directivity variation that causes forming, if the impurity in same solution accumulates to the homogeneity variation that also can cause the nano rod that forms on substrate, plated film placed face down can finely be avoided the deposition of zinc oxide nucleus and other impurity in solution.
4) experiment showed, and adopt method of the present invention, when zinc paper tinsel height (being the height of substrate in solution) increases, diameter and the length of the Al-Doped ZnO nano rod of synthesized all reduce gradually, until change, tend towards stability; Therefore, the present invention can, simply by the control to zinc paper tinsel height (being the height of substrate in solution), 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.
The top view (a) of the Al-Doped ZnO nano rod array structure of gained and side-looking (b) SEM figure and energy spectrogram (c) in Fig. 2 embodiment 1.
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 of the Al-Doped ZnO nano rod array structure of gained figure in Fig. 4 embodiment 2.
The SEM of the Al-Doped ZnO nano rod array structure of gained figure in Fig. 5 embodiment 3.
The SEM of the Al-Doped ZnO nano rod array structure of gained figure in Fig. 6 embodiment 4.
The SEM of the Al-Doped ZnO nano rod array structure of gained figure in Fig. 7 embodiment 5.
Embodiment
Fig. 1 is Al-Doped ZnO nano rod array structure synthesizer schematic diagram.Two zinc paper tinsels 1 are separated and are dipped vertically into along its length in the methane amide aqueous solution 3 that is contained in weighing bottle 2 and fix, the substrate 5 that is coated with buffer layer thin film 4 is placed on to the top of two zinc paper tinsels 1 down with coated surface, and a small pieces aluminium foil 6 is positioned over to solution bottom, then weighing bottle 2 use glass covers 7 are tilted to cover, move on the Stage microscope 9 in baking oven 8 and keep constant temperature to react, finally can on substrate 5, obtain Al-Doped ZnO nano rod array structure 10.
Below in conjunction with accompanying drawing, the present invention is further detailed explanation.
embodiment 1:the methane amide aqueous solution that dose volume mark is 5% in weighing bottle, two rectangle zinc paper tinsels are separated and are dipped vertically in solution, zinc paper tinsel height is that 15 mm(are edge lengths 15 mm that zinc paper tinsel is vertical), the silicon substrate coated surface that is coated with the thick Ag film of 10 nm is placed on to the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 90 ℃ and react 4 hours, take out silicon substrate, with deionized water, ethanol and acetone, clean up and be dried; Fig. 2 (a) and (b) shown in be respectively the top view of the Al-Doped ZnO nano rod array structure making and side-looking SEM figure on silicon substrate, the mean diameter of nano rod is that 240 nm, length are 2.6 μ m; From can spectrogram can finding out of Fig. 2 (c), except containing Zn element, O element, also contain Al element, prove that what obtain is the zinc oxide that contains aluminium; As can be seen from Figure 3, under these conditions, when changing zinc paper tinsel height (being the height of substrate in 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 variation 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:the methane amide aqueous solution that dose volume mark is 5% in weighing bottle, two rectangle zinc paper tinsels are separated and are dipped vertically in solution, zinc paper tinsel height is that 12 mm(are that the edge lengths that zinc paper tinsel is vertical is 12 mm), the silicon substrate coated surface that is coated with the thick ZnO film of 100 nm is placed on to the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 80 ℃ and react 8 hours, take out silicon substrate, with deionized water, ethanol and acetone, clean up and be dried; The SEM figure that Figure 4 shows that the Al-Doped ZnO nano rod array structure making on silicon substrate, the mean diameter of nano rod is 760 nm.
embodiment 3:the methane amide aqueous solution that dose volume mark is 10% in weighing bottle, two rectangle zinc paper tinsels are separated and are dipped vertically in solution, zinc paper tinsel height is that 10 mm(are that the edge lengths that zinc paper tinsel is vertical is 10 mm), the glass substrate coated surface that is coated with the thick ITO film of 200 nm is placed on to the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 70 ℃ and react 12 hours, take out glass substrate, with deionized water, ethanol and acetone, clean up and be dried; The SEM figure that Figure 5 shows that the Al-Doped ZnO nano rod array structure making in glass substrate, the mean diameter of nano rod is 700 nm.
embodiment 4:the methane amide aqueous solution that dose volume mark is 15% in weighing bottle, two rectangle zinc paper tinsels are separated and are dipped vertically in solution, zinc paper tinsel height is that 7 mm(are that the edge lengths that zinc paper tinsel is vertical is 7 mm), to be coated with coated surface at the bottom of the stainless steel lining of the thick AZO film of 500 nm and be placed on the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 60 ℃ and react 16 hours, at the bottom of taking out stainless steel lining, with deionized water, ethanol and acetone, clean up and be dried; The SEM figure that Figure 6 shows that the Al-Doped ZnO nano rod array structure making at the bottom of stainless steel lining, the diameter of nano rod is 200 ~ 650 nm.
embodiment 5:the methane amide aqueous solution that dose volume mark is 20% in weighing bottle, two rectangle zinc paper tinsels are separated and are dipped vertically in solution, zinc paper tinsel height is that 5 mm(are that the edge lengths that zinc paper tinsel is vertical is 5 mm), the glass substrate coated surface that is coated with the thick FTO film of 800 nm is placed on to the top of two zinc paper tinsels down, and a small pieces aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 50 ℃ and react 20 hours, take out glass substrate, with deionized water, ethanol and acetone, clean up and be dried; The SEM figure that Figure 7 shows that the Al-Doped ZnO nano rod array structure making in glass substrate, the mean diameter of nano rod is 600 nm.
Embodiment provided by the present invention only describes technical scheme, and does not limit.
Claims (7)
1. the synthetic method of Al-Doped ZnO nano rod array structure low temperature, it is characterized in that concrete steps are as follows: the methane amide aqueous solution that dose volume mark is 5 ~ 20% in weighing bottle, two rectangle zinc paper tinsels are kept at a distance to separate and be dipped vertically in solution, the top that the substrate coated surface that is coated with buffer layer thin film is placed on to two zinc paper tinsels down can keep stable, and aluminium foil is positioned over to solution bottom, with glass cover, tilt to cover weighing bottle mouth again, be placed in the baking oven of 50 ~ 90 ℃ and react 4 ~ 20 hours, take out substrate, with deionized water, after ethanol and acetone clean up and are dried.
2. the synthetic method of a kind of Al-Doped ZnO nano rod array structure low temperature as claimed in claim 1, is characterized in that: zinc paper tinsel height is 5 ~ 15 mm, and the edge lengths that zinc paper tinsel is vertical is 5 ~ 15 mm, and zinc paper tinsel height has determined the height of substrate in solution; When zinc paper tinsel height is when the height of substrate in solution increases in other words, diameter and the length of the Al-Doped ZnO nano rod of synthesized all reduce gradually, until change, tend towards stability; The diameter of Al-Doped ZnO nano rod and length are respectively 0.20-0.76 μ m and 2.4 μ m-4.5 μ m.
3. the synthetic method of a kind of Al-Doped ZnO nano rod array structure low temperature as claimed in claim 1, is characterized in that: buffer layer thin film thickness is 10 ~ 800 nm.
4. the synthetic method of a kind of Al-Doped ZnO nano rod array structure low temperature as claimed in claim 1, is characterized in that: the methane amide adopting is analytical pure commercialization reagent C H
3nO, the water adopting is pure water, deionized water or distilled water.
5. the synthetic method of a kind of Al-Doped ZnO nano rod array structure low temperature as claimed in claim 1, is characterized in that: the standard that zinc paper tinsel is kept at a distance is for guaranteeing the stable top that is placed on two zinc paper tinsels of substrate.
6. the synthetic method of a kind of Al-Doped ZnO nano rod array structure low temperature as claimed in claim 1, it is characterized in that: the buffer layer thin film adopting 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 reducing between nucleus and substrate, thereby 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.
7. the synthetic method of a kind of Al-Doped ZnO nano rod array structure low temperature as claimed in claim 1, it is characterized in that: glass cover tilts to cover weighing bottle mouth and refers to glass cover is leaned at weighing bottle bottleneck, both can stop pollutent to enter, and can ensure again enough air and enter participation reaction in bottle.
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Cited By (2)
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| CN108793766A (en) * | 2018-06-12 | 2018-11-13 | 西安理工大学 | The electrochomeric films and preparation method thereof of ir transmissivity in a kind of effective modulation |
| CN110790301A (en) * | 2019-12-11 | 2020-02-14 | 大连理工大学 | Device and method for preparing high-quality-density uniform vertical zinc oxide nanorod array |
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| CN108793766A (en) * | 2018-06-12 | 2018-11-13 | 西安理工大学 | The electrochomeric films and preparation method thereof of ir transmissivity in a kind of effective modulation |
| CN108793766B (en) * | 2018-06-12 | 2021-05-25 | 西安理工大学 | Electrochromic film capable of effectively modulating mid-infrared transmittance and preparation method thereof |
| CN110790301A (en) * | 2019-12-11 | 2020-02-14 | 大连理工大学 | Device and method for preparing high-quality-density uniform vertical zinc oxide nanorod array |
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