CN103359772B - Method for preparing antimony-doped zinc-oxide (ZnO) nanowire - Google Patents
Method for preparing antimony-doped zinc-oxide (ZnO) nanowire Download PDFInfo
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- CN103359772B CN103359772B CN201210433985.8A CN201210433985A CN103359772B CN 103359772 B CN103359772 B CN 103359772B CN 201210433985 A CN201210433985 A CN 201210433985A CN 103359772 B CN103359772 B CN 103359772B
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Abstract
The invention provides a method for preparing an antimony-doped zinc-oxide (ZnO) nanowire. The method is characterized by comprising the following steps of: preparing an antimony-doped solution and a hydrothermal synthesis solution, wherein the antimony-doped solution is the aqueous solution of antimony acetate, glycolic acid and sodium hydroxide, and the hydrothermal synthesis solution is the aqueous solution of zinc nitrate hexahydrate, hexamethylenetetramine and polyethyleneimine; weighing the antimony-doped solution and the hydrothermal synthesis solution according to the antimony doping proportion, mixing the antimony-doped solution with the hydrothermal synthesis solution, and adding aqueous ammonia to obtain a mixed solution; and finally carrying out hydrothermal synthesis in the mixed solution to obtain the antimony-doped ZnO nanowire, namely, putting a substrate with a ZnO seed crystal on the surface into the mixed solution to grow the antimony-doped ZnO nanowire hydrothermally. The method for preparing the antimony-doped ZnO nanowire through hydrothermal reaction is characterized by low preparation temperature and is suitable for preparing the antimony-doped ZnO nanowire on an organic matter and other flexible substrates.
Description
Technical field
The present invention relates to field of nano material preparation, particularly relate to a kind of zinc oxide nanowire preparation method who visits antimony doping.
Background technology
The monodimension nanometer material of doping has great significance and wide prospect in nanoelectronics field.The material of N-shaped and p-type doping combines can make p-n junction, and p-n junction has important application in light emitting diode, transistor and photovoltaic device.In view of zinc oxide is a kind of material that has semi-conductor and piezoelectric effect concurrently, and its synthetic method is relatively simple, stable and effectively, zinc oxide becomes the stay material in nano generator and piezoelectron.Natural less than the zinc oxide through deliberately doping is N-shaped semi-conductor, in recent years, utilizes extraneous element, and such as nitrogen, phosphorus, antimony etc. adulterated and be widely studied zinc oxide.The ability of the synthetic Homojeneous p-n Junction zinc oxide nanowire of success will make light emitting diode and logical circuit based on single nano-wire become possibility.
Although previously had been reported successfully, zinc oxide nanowire was carried out to p-type doping, synthetic method used need, by solid phase-liquid phase-gas phase (VLS) mechanism, need to be carried out at high temperature.This point has seriously limited the kind of the substrate that growth of zinc oxide nano line can use, the inapplicable zinc oxide nanowire of preparing p-type doping in the flexible substrates such as organism.
Summary of the invention
In order to overcome the existing zinc oxide nanowire p-type defect that need at high temperature carry out of adulterating, the object of the present invention is to provide a kind of method of preparing antimony (Sb) doped zinc oxide nano-wire at cold condition.
In order to achieve the above object, the invention provides a kind of preparation method of stibium-doped zinc oxide nano wire, the method comprises:
Preparation antimony doped solution and Hydrothermal Synthesis solution, wherein, described antimony doped solution is the aqueous solution of antimony acetate, oxyacetic acid and sodium hydroxide, described Hydrothermal Synthesis solution is the aqueous solution of zinc nitrate hexahydrate, Hexamine and polymine;
Measure described antimony doped solution and the mixing of Hydrothermal Synthesis solution according to antimony doping ratio, and add ammoniacal liquor to obtain mixing solutions;
The substrate that surface is prepared with to zinc oxide seed crystal is placed on and in described mixing solutions, carries out Hydrothermal Growth zinc oxide nanowire.
Preferably, the step of described preparation antimony doped solution comprises:
Described oxyacetic acid and dissolution of sodium hydroxide are formed in deionized water to the aqueous solution of oxyacetic acid and sodium hydroxide; Under the aqueous solution state that at the uniform velocity stirs described oxyacetic acid and sodium hydroxide, slowly add antimony acetate to form antimony doped solution; Wherein, the mol ratio of described antimony acetate, oxyacetic acid and sodium hydroxide is 1:12:12.
Preferably, the step of described preparation Hydrothermal Synthesis solution is for to add successively zinc nitrate hexahydrate, Hexamine and polymine in deionized water, wherein, zinc nitrate hexahydrate, Hexamine and polymine mol ratio be 10:5:2.
Preferably, the described substrate that surface is prepared with to zinc oxide seed crystal is placed in mixing solutions and carries out also comprising before Hydrothermal Growth zinc oxide nanowire step: the step of mixing solutions described in thermal pretreatment.
Preferably, described in described thermal pretreatment, mixing solutions step is 95 DEG C of insulations 1 hour.
Preferably, described antimony doping ratio is 0%-2%.
Preferably, after hydrothermal growth stibium-doped zinc oxide nano wire, also comprise the described stibium-doped zinc oxide nano wire step of annealing.
Compared with prior art, vibration detector of the present invention has following advantages:
The invention provides a kind of preparation method of stibium-doped zinc oxide nano wire, first prepare antimony doped solution and Hydrothermal Synthesis solution, wherein, described antimony doped solution is the aqueous solution of antimony acetate, oxyacetic acid and sodium hydroxide, and described Hydrothermal Synthesis solution is the aqueous solution of zinc nitrate hexahydrate, Hexamine and polymine; Then measure described antimony doped solution and the mixing of Hydrothermal Synthesis solution according to antimony doping ratio, and add ammoniacal liquor to obtain mixing solutions; The last Hydrothermal Synthesis that carries out stibium-doped zinc oxide nano wire in described mixing solutions.Adopt method of the present invention in hydro-thermal reaction, to prepare stibium-doped zinc oxide nano wire, preparation temperature is low, can be useful in the flexible substrates such as organism.
In addition, the preparation method of stibium-doped zinc oxide nano wire of the present invention can prepare the stibium-doped zinc oxide nano-wire array of overlength, and length can reach 60 microns, can meet the requirement of preparing light emitting diode and logical circuit etc. on single nano-wire.
Brief description of the drawings
Shown in accompanying drawing, above-mentioned and other object of the present invention, Characteristics and advantages will be more clear.In whole accompanying drawings, identical Reference numeral is indicated identical part.Deliberately do not draw accompanying drawing by physical size equal proportion convergent-divergent, focus on illustrating purport of the present invention.
Fig. 1 is the preparation method's of stibium-doped zinc oxide nano wire of the present invention schema;
Fig. 2 is the scanning electron microscope image of the stibium-doped zinc oxide nano wire prepared in the embodiment of the present invention;
Fig. 3 is the energy dispersion X ray spectrogram of the transmission electron microscope of single 2% stibium-doped zinc oxide nano wire;
Fig. 4 is for utilizing atomic force microscope 0.2% antimony adulterate (a) and the adulterate electrical characterization of (b) zinc oxide nanowire of 2% antimony;
Fig. 5 is the electrical measurement result of the stationary source drain bias scanning gate voltage that carries out of the field-effect transistor of single 0.2% stibium-doped zinc oxide the fabricate of nanowires.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Existing zinc oxide nanowire is carried out to p-type adulterating method need to be by solid phase-liquid phase-gas phase (VLS) mechanism, need to carry out at high temperature, the inapplicable ZnO nano-wire of preparing p-type doping in the flexible substrates such as organism, this has seriously limited the kind of the substrate that grow nanowire can use.
The invention provides a kind of preparation method of stibium-doped zinc oxide nano wire, wherein, the method comprises:
Preparation antimony doped solution and Hydrothermal Synthesis solution, wherein, described antimony doped solution is the aqueous solution of antimony acetate, oxyacetic acid and sodium hydroxide, described Hydrothermal Synthesis solution is the aqueous solution of zinc nitrate hexahydrate, Hexamine and polymine;
Measure described antimony doped solution and the mixing of Hydrothermal Synthesis solution according to antimony doping ratio, and add ammoniacal liquor to obtain mixing solutions;
The substrate that surface is prepared with to zinc oxide seed crystal is placed on and in described mixing solutions, carries out Hydrothermal Growth zinc oxide nanowire.
The preparation method of stibium-doped zinc oxide nano wire of the present invention carries out in hydro-thermal reaction, and preparation temperature is low, can be useful in the flexible substrates such as organism.In addition, the preparation method of stibium-doped zinc oxide nano wire of the present invention can prepare the stibium-doped zinc oxide nano-wire array of overlength, and length can reach 60 microns, can meet the requirement of preparing light emitting diode and logical circuit etc. on single nano-wire.
Introduce in detail a specific embodiment of the present invention below in conjunction with accompanying drawing, the preparation method's of stibium-doped zinc oxide nano wire of the present invention schema, referring to Fig. 1, comprising:
Step S1, preparation antimony doped solution and Hydrothermal Synthesis solution, wherein, described antimony doped solution is the aqueous solution of antimony acetate, oxyacetic acid and sodium hydroxide, described Hydrothermal Synthesis solution is the aqueous solution of zinc nitrate hexahydrate, Hexamine and polymine.
In described antimony doped solution, the mol ratio of antimony acetate, oxyacetic acid and sodium hydroxide is 1:12:12, and the step of preparation antimony doped solution comprises: the aqueous solution that oxyacetic acid and dissolution of sodium hydroxide is formed in deionized water to oxyacetic acid and sodium hydroxide; The aqueous solution of described oxyacetic acid and sodium hydroxide is placed in centrifuge tube, and adds one piece of magnet rotor, at the uniform velocity under whipped state, is slowly adding antimony acetate to form antimony doped solution.Finally obtaining volume is 50mL, the antimony doped solution that concentration is 0.1M, and this solution at room temperature can steady in a long-termly be preserved.
In described Hydrothermal Synthesis solution, the mol ratio of zinc nitrate hexahydrate, Hexamine and polymine is 10:5:2, the step of preparation Hydrothermal Synthesis solution for adding successively zinc nitrate hexahydrate, Hexamine and polymine in deionized water, be specially, in 250ml deionized water, add successively zinc nitrate hexahydrate (Zn (NO
3)
26H
2o), Hexamine (HMTA) and polymine (PEI), make (Zn (the NO of zinc nitrate hexahydrate in solution
3)
26H
2o) concentration is 25mM(mM=1mmol/L, every liter of mmole), the concentration of Hexamine (HMTA) is that the concentration of 12.5mM and polymine (PEI) is 5mM, after even mixing, measures the above-mentioned solution of 50mL and pours reaction vessels into graduated cylinder.
Step S2, measures described antimony doped solution and the mixing of Hydrothermal Synthesis solution according to antimony doping ratio, and adds ammoniacal liquor to obtain mixing solutions.
According to antimony doping ratio, in the Hydrothermal Synthesis solution of preparing in step S1, add appropriate antimony doped solution to mix, the scope of doping ratio can be between 0% to 2% (antimony zinc atom ratio).In the present embodiment, in 50mL Hydrothermal Synthesis solution, add 25 μ L antimony doped solution to mix, and add the ammoniacal liquor that the quality proportion of 2.7ml is 28% and evenly mix sealed reaction vessel.
Step S3, the substrate that surface is prepared with to zinc oxide seed crystal is placed on and in described mixing solutions, carries out Hydrothermal Growth zinc oxide nanowire.
Before completing and carrying out step S3 after antimony doped solution and Hydrothermal Synthesis solution mix, can also comprise the step of mixing solutions described in thermal pretreatment.The condition of concrete thermal pretreatment can be: the reaction vessels sealing in step S2 is placed in the thermostat container of 95 DEG C to heat-insulation preheating 1 hour.Described in thermal pretreatment, mixing solutions can make solution evenly mix.After mixing solutions is carried out to thermal pretreatment, the substrate that surface is prepared with to zinc oxide seed crystal in this step is placed on through carrying out Hydrothermal Growth zinc oxide nanowire in the mixing solutions of thermal pretreatment.
Taking the stibium-doped zinc oxide nano wire of growing in glass substrate as example, first sputtering zinc oxide inculating crystal layer in glass substrate, this glass substrate is inserted in the reaction vessels in step S2, after the hydrothermal growth of 24 hours, taken out substrate clean by rinsed with deionized water.So far, complete the preparation of stibium-doped zinc oxide nano wire.
In order to remove the organic residue on the stibium-doped zinc oxide nano wire of preparation, method of the present invention can also comprise annealing stibium-doped zinc oxide nano wire step after step S4, be specifically as follows, the substrate that is prepared with stibium-doped zinc oxide nano wire is toasted 1 hour at 300 DEG C, to remove organic substance residues.
The stibium-doped zinc oxide nano wire of preparing in the present embodiment is characterized, scanning electronic microscope, transmission electron microscope, atomic force microscope (AFM) and field-effect transistor measurement are used to characterize the pattern of synthetic nano wire, chemical component and electrical properties etc.
Shown in Fig. 2 is scanning electron microscope image, and wherein, nano wire (in Fig. 2 a and the b figure) length of 0.2% doping is 60 microns of left and right, diameter in 200 nanometers between 1000 nanometers; Length is 3 microns of left and right for the nano wire (c and d figure in Fig. 2) of 2% doping, and diameter is in 250 nanometer left and right.
In this method of preparing stibium-doped zinc oxide nano wire of the present invention, by the polymine adding in Hydrothermal Synthesis solution (PEI) as morphology control agent to obtain reaching the nano wire of 60 microns, simultaneously by glycollate ion, in the process of zinc oxide growth, antimony ion is mixed among its lattice.Adopt method of the present invention, the p-type doped zinc oxide nano-wire of overlength can be repeatedly, be stably produced out.
Fig. 3 utilizes the energy dispersion x-ray spectrometer of transmission electron microscope to measure the chemical component of single nano-wire, as shown in table 1, although added 2% antimony to adulterate, due to the material unaccounted-for (MUF) in building-up process, the doping content of actual nano wire is 0.55%.
Average weight and the atomic percent of the different elements in table 1.2% stibium doped nanometer line.
| Element | % by weight | Atom % |
| O(K) | 16.53 | 44.82 |
| Zn(K) | 81.91 | 54.61 |
| Sb(L) | 1.54 | 0.55 |
The piezoelectricity output characteristic of the zinc oxide nanowire of preparing in the present embodiment utilizes atomic force microscope to measure, as shown in Figure 4.After deformation, outward current is negative value, shows that zinc oxide nanowire is p-type doping.Reason is, it is one-way conduction that afm tip and zinc oxide nanowire form schottky junction, after the stressed bending of zinc oxide nanowire, Extrude Face is contrary with the electric charge symbol that compressing surface produces, the unidirectional general character of schottky junction makes, in the time that needle point contacts with two faces difference front and back, to only have one of them to have outward current.For N-shaped doping, just meeting conducting in the time that needle point contacts with compressing surface, corresponding to the positive current in measuring system; For p-type doping, just meeting conducting in the time that needle point contacts with compressing surface, corresponding to the negative current in measuring system.For 0.2% antimony doping (in Fig. 4 a) He 2% antimony adulterate (zinc oxide nanowire b) in Fig. 4, its maximum output current is respectively 30pA and 80pA, its maximum output voltage is respectively 7mV and 15mV.
Finally, the field-effect transistor of the single zinc oxide nanowire based on 0.2% antimony doping is produced, and has carried out source leakage fixed bias, the electrical measurement of scanning gate voltage, and measurement of correlation the results are shown in Figure 5.This result further strict proof the zinc oxide nanowire of synthesized be p-type doping.
The above, be only preferred embodiment of the present invention, the present invention do not done to any pro forma restriction.Any those skilled in the art, in the situation that not departing from technical solution of the present invention scope, can utilize above-mentioned disclosed method and technology contents to make multiple possible modification and modification to technical scheme of the present invention, or are revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not depart from technical solution of the present invention, to any simple modification made for any of the above embodiments, equivalent modifications and modification, all belongs to the scope of technical solution of the present invention protection according to technical scheme of the present invention.
Claims (7)
1. a preparation method for stibium-doped zinc oxide nano wire, is characterized in that, the method comprises:
Preparation antimony doped solution and Hydrothermal Synthesis solution, wherein, described antimony doped solution is the aqueous solution of antimony acetate, oxyacetic acid and sodium hydroxide, described Hydrothermal Synthesis solution is the aqueous solution of zinc nitrate hexahydrate, Hexamine and polymine;
Measure described antimony doped solution and the mixing of Hydrothermal Synthesis solution according to antimony doping ratio, and add ammoniacal liquor to obtain mixing solutions;
The substrate that surface is prepared with to zinc oxide seed crystal is placed on and in described mixing solutions, carries out Hydrothermal Growth zinc oxide nanowire.
2. preparation method according to claim 1, wherein, the step of preparation antimony doped solution is:
Described oxyacetic acid and dissolution of sodium hydroxide are formed in deionized water to the aqueous solution of oxyacetic acid and sodium hydroxide; Under the aqueous solution state that at the uniform velocity stirs described oxyacetic acid and sodium hydroxide, slowly add antimony acetate to form antimony doped solution; The mol ratio of described antimony acetate, oxyacetic acid and sodium hydroxide is 1:12:12.
3. preparation method according to claim 1, wherein, the step of described preparation Hydrothermal Synthesis solution is: in deionized water, add successively zinc nitrate hexahydrate, Hexamine and polymine; Zinc nitrate hexahydrate, Hexamine and polymine mol ratio be 10:5:2.
4. according to the preparation method described in any one in claim 1-3, wherein, the method also comprises: the substrate that surface is prepared with to zinc oxide seed crystal is placed in described mixing solutions and carries out before Hydrothermal Growth zinc oxide nanowire: the step of described mixing solutions being carried out to thermal pretreatment.
5. preparation method according to claim 4, wherein, carries out the step of thermal pretreatment for being incubated 1 hour at 95 DEG C to described mixing solutions.
6. preparation method according to claim 1, wherein, described antimony doping ratio is 0.2%-2%.
7. preparation method according to claim 1, wherein, the method also comprises the step that the stibium-doped zinc oxide nano wire of the hydrothermal growth obtaining is annealed.
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| CN104792827A (en) * | 2015-04-03 | 2015-07-22 | 东北大学 | Self-powered humidity sensor adopting antimony doped zinc oxide nano array and preparation method of self-powered humidity sensor |
| CN110526275A (en) * | 2019-07-26 | 2019-12-03 | 集美大学 | A kind of preparation method of new-type impurity addition zinc oxide nanowire |
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| CN101319370A (en) * | 2008-06-24 | 2008-12-10 | 济南大学 | Method for controlling orientation and profile characteristic of zinc oxide nano-stick/nano-tube array |
| 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 |
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| CN101319370A (en) * | 2008-06-24 | 2008-12-10 | 济南大学 | Method for controlling orientation and profile characteristic of zinc oxide nano-stick/nano-tube array |
| 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 |
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