CN103359772A - 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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- CN103359772A CN103359772A CN2012104339858A CN201210433985A CN103359772A CN 103359772 A CN103359772 A CN 103359772A CN 2012104339858 A CN2012104339858 A CN 2012104339858A CN 201210433985 A CN201210433985 A CN 201210433985A CN 103359772 A CN103359772 A CN 103359772A
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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 that antimony mixes that visits.
Background technology
The monodimension nanometer material that mixes has great significance in the nanoelectronics field and wide prospect.The material that N-shaped and p-type are mixed 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.Not natural through the zinc oxide that deliberately mixes is the N-shaped semi-conductor, in recent years, utilizes extraneous element, and such as nitrogen, phosphorus, antimony etc. zinc oxide being mixed is widely studied.The ability of the synthetic Homojeneous p-n Junction zinc oxide nanowire of success will be so that become possibility based on light emitting diode and the logical circuit of single nano-wire.
Although before had been reported and successful zinc oxide nanowire is carried out p-type mixed, used synthetic method need need to carry out under high temperature by solid phase-liquid phase-gas phase (VLS) mechanism.This point has seriously limited the kind of the substrate that the growth of zinc oxide nano line can use, the inapplicable zinc oxide nanowire that mixes in the flexible substrates such as organism preparation p-type.
Summary of the invention
The defective of mixing and need at high temperature carry out in order to overcome existing zinc oxide nanowire p-type the object of the present invention is to provide a kind of method for 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 the antimony doping ratio, and add ammoniacal liquor acquisition mixing solutions;
The substrate that the surface is prepared with the zinc oxide seed crystal is placed on and carries out the Hydrothermal Growth zinc oxide nanowire in the described mixing solutions.
Preferably, the step of described preparation antimony doped solution comprises:
Described oxyacetic acid and dissolution of sodium hydroxide are formed the aqueous solution of oxyacetic acid and sodium hydroxide in deionized water; Under the aqueous solution state that at the uniform velocity stirs described oxyacetic acid and sodium hydroxide, slowly add antimony acetate and form the 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 the surface is prepared with the zinc oxide seed crystal is placed on and carries out in the mixing solutions also comprising before the Hydrothermal Growth zinc oxide nanowire step: the step of the described mixing solutions of thermal pretreatment.
Preferably, the described mixing solutions step of described thermal pretreatment is 95 ℃ of insulations 1 hour.
Preferably, described antimony doping ratio is 0%-2%.
Preferably, behind the 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, at 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 the antimony doping ratio, and add ammoniacal liquor acquisition mixing solutions; The last Hydrothermal Synthesis that in described mixing solutions, carries out the stibium-doped zinc oxide nano wire.Adopt method of the present invention to prepare the stibium-doped zinc oxide nano wire in hydro-thermal reaction, preparation temperature is low, can be useful on 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 satisfy the requirement at single nano-wire preparation light emitting diode and logical circuit etc.
Description of drawings
Shown in accompanying drawing, above-mentioned and other purpose of the present invention, Characteristics and advantages will be more clear.Reference numeral identical in whole accompanying drawings 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 for preparing in the embodiment of the 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 to be mixed (a) and the electrical characterization of 2% antimony doping (b) zinc oxide nanowire;
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 invention, the technical scheme in the embodiment of the invention is clearly and completely described.Obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
Existing zinc oxide nanowire is carried out the p-type adulterating method need to be by solid phase-liquid phase-gas phase (VLS) mechanism, need to carry out under the high temperature, the inapplicable ZnO nano-wire that mixes in the flexible substrates such as organism preparations p-type, 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 the antimony doping ratio, and add ammoniacal liquor acquisition mixing solutions;
The substrate that the surface is prepared with the zinc oxide seed crystal is placed on and carries out the Hydrothermal Growth zinc oxide nanowire in the described mixing solutions.
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 on 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 satisfy the requirement at single nano-wire preparation light emitting diode and logical circuit etc.
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 comprises referring to Fig. 1:
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.
The mol ratio of antimony acetate, oxyacetic acid and sodium hydroxide is 1:12:12 in the described antimony doped solution, and the step of preparation antimony doped solution comprises: the aqueous solution that oxyacetic acid and dissolution of sodium hydroxide is formed oxyacetic acid and sodium hydroxide in deionized water; The aqueous solution of described oxyacetic acid and sodium hydroxide places centrifuge tube, and adds one piece of magnet rotor, is at the uniform velocity slowly adding antimony acetate formation antimony doped solution under the whipped state.Finally obtaining volume is 50mL, and concentration is the antimony doped solution of 0.1M, and this solution at room temperature can steady in a long-termly be preserved.
The mol ratio of zinc nitrate hexahydrate, Hexamine and polymine is 10:5:2 in the described Hydrothermal Synthesis solution, the step of preparation Hydrothermal Synthesis solution is for adding successively zinc nitrate hexahydrate, Hexamine and polymine in deionized water, be specially, in the 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 the 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 evenly mixing, measures the 50mL mentioned solution and pours reaction vessels into graduated cylinder.
Step S2 measures described antimony doped solution and the mixing of Hydrothermal Synthesis solution according to the antimony doping ratio, and adds ammoniacal liquor acquisition mixing solutions.
According to the antimony doping ratio, add an amount of antimony doped solution in the Hydrothermal Synthesis solution that in step S1, prepares and mix, the scope of doping ratio can be between 0% to 2% (antimony zinc atom ratio).In 50mL Hydrothermal Synthesis solution, add 25 μ L antimony doped solution in the present embodiment and mix, and the quality proportion of adding 2.7ml is 28% ammoniacal liquor and evenly mixes the sealed reaction vessel.
Step S3, the substrate that the surface is prepared with the zinc oxide seed crystal is placed on and carries out the Hydrothermal Growth zinc oxide nanowire in the described mixing solutions.
Before after finishing the mixing of antimony doped solution and Hydrothermal Synthesis solution, carrying out step S3, can also comprise the step of the described mixing solutions of thermal pretreatment.The condition of concrete thermal pretreatment can for: the reaction vessels that seals among the step S2 was placed in 95 ℃ the thermostat container heat-insulation preheating 1 hour.The described mixing solutions of thermal pretreatment can make solution evenly mix.Mixing solutions is carried out after the thermal pretreatment, and the substrate that the surface is prepared with the zinc oxide seed crystal in this step is placed on through carrying out the Hydrothermal Growth zinc oxide nanowire in the mixing solutions of thermal pretreatment.
To grow the stibium-doped zinc oxide nano wire as example in glass substrate, sputtering zinc oxide inculating crystal layer on glass substrate at first, this glass substrate is inserted in the reaction vessels among the step S2, behind 24 hours hydrothermal growth, taken out substrate and clean with rinsed with deionized water.So far, finish the preparation of stibium-doped zinc oxide nano wire.
For the organic residue on the stibium-doped zinc oxide nano wire of removing preparation, method of the present invention can also comprise annealing stibium-doped zinc oxide nano wire step after step S4, be specifically as follows, to be prepared with the substrate of stibium-doped zinc oxide nano wire 300 ℃ of lower bakings 1 hour, to remove organic substance residues.
The stibium-doped zinc oxide nano wire for 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 Figure 2 is scanning electron microscope image, and wherein, 0.2% nano wire that mixes (a and b figure among Fig. 2) length is about 60 microns, diameter in 200 nanometers between 1000 nanometers; Length is about 3 microns for 2% nano wire that mixes (c and d figure among Fig. 2), and diameter is about 250 nanometers.
In this method for preparing the stibium-doped zinc oxide nano wire of the present invention, by the polymine that adds in the Hydrothermal Synthesis solution (PEI) as the morphology control agent to obtain reaching 60 microns nano wire, simultaneously by the 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, stably be 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, mix although added 2% antimony, because the material unaccounted-for (MUF) in the building-up process, the doping content of actual nano wire is 0.55%.
Average weight and the atomic percent of the different elements in the 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 for 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 that p-type is mixed.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, the electric charge opposite in sign that Extrude Face and compressing surface produce, the unidirectional general character of schottky junction is so that when needle point contacts with two faces difference front and back, only have one of them to have outward current.Mix for N-shaped, when needle point contacts with compressing surface, just understand conducting, corresponding to the positive current in the measuring system; Mix for p-type, when needle point contacts with compressing surface, just understand conducting, corresponding to the negative current in the measuring system.Mixing for 0.2% antimony, (a) and the mix zinc oxide nanowire of (b among Fig. 4) of 2% antimony, its maximum output current is respectively 30pA and 80pA among Fig. 4, and its maximum output voltage is respectively 7mV and 15mV.
At last, the field-effect transistor of the single zinc oxide nanowire that mixes based on 0.2% antimony is produced, and has carried out the source and leak 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 that synthesize be the p-type doping.
The above only is preferred embodiment of the present invention, the present invention is not done any pro forma restriction.Any those skilled in the art can utilize above-mentioned disclosed method and technology contents that technical scheme of the present invention is made multiple possible modification and modification, or be revised as the equivalent embodiment of equivalent variations in the situation that do not break away from the technical solution of the present invention scope.Therefore, every content that does not break away from technical solution of the present invention to any simple modification, equivalent modifications and modification that above embodiment does, all belongs to the scope of technical solution of the present invention protection according to technical scheme of the present invention.
Claims (7)
1. the preparation method of a 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 the antimony doping ratio, and add ammoniacal liquor acquisition mixing solutions;
The substrate that the surface is prepared with the zinc oxide seed crystal is placed on and carries out the Hydrothermal Growth zinc oxide nanowire in the described mixing solutions.
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 the aqueous solution of oxyacetic acid and sodium hydroxide in deionized water; Under the aqueous solution state that at the uniform velocity stirs described oxyacetic acid and sodium hydroxide, slowly add antimony acetate and form the 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: add successively zinc nitrate hexahydrate, Hexamine and polymine in deionized water; Zinc nitrate hexahydrate, Hexamine and polymine mol ratio be 10:5:2.
4. the described preparation method of any one according to claim 1-3, wherein, the method also comprises: before the substrate that the surface is prepared with the zinc oxide seed crystal is placed on and carries out the Hydrothermal Growth zinc oxide nanowire in the described mixing solutions: the step of described mixing solutions being carried out thermal pretreatment.
5. preparation method according to claim 4 wherein, carries out the step of thermal pretreatment for being incubated 1 hour at 95 ℃ to described mixing solutions.
6. preparation method according to claim 1, wherein, described antimony doping ratio is 0%-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 that will obtain is annealed.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104176766A (en) * | 2014-09-02 | 2014-12-03 | 中国科学院上海硅酸盐研究所 | Praseodymium-doped zinc oxide nanowire and preparation method thereof |
| 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 |
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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 |
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| CN104176766A (en) * | 2014-09-02 | 2014-12-03 | 中国科学院上海硅酸盐研究所 | Praseodymium-doped zinc oxide nanowire and preparation method thereof |
| 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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