CN101935875B - Sn-doped ZnO superfine nanowires and synthesis method thereof - Google Patents
Sn-doped ZnO superfine nanowires and synthesis method thereof Download PDFInfo
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- 238000001308 synthesis method Methods 0.000 title abstract 3
- 239000011701 zinc Substances 0.000 claims abstract description 15
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 13
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 12
- 229930195729 fatty acid Natural products 0.000 claims abstract description 12
- 239000000194 fatty acid Substances 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 238000009835 boiling Methods 0.000 claims abstract description 5
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 4
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 claims description 4
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- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- BRWZYZWZBMGMMG-UHFFFAOYSA-J dodecanoate tin(4+) Chemical compound [Sn+4].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O BRWZYZWZBMGMMG-UHFFFAOYSA-J 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229940038384 octadecane Drugs 0.000 claims description 2
- LPEBYPDZMWMCLZ-CVBJKYQLSA-L zinc;(z)-octadec-9-enoate Chemical compound [Zn+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O LPEBYPDZMWMCLZ-CVBJKYQLSA-L 0.000 claims description 2
- GBFLQPIIIRJQLU-UHFFFAOYSA-L zinc;tetradecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O GBFLQPIIIRJQLU-UHFFFAOYSA-L 0.000 claims description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 claims 2
- QMTFKWDCWOTPGJ-KVVVOXFISA-N (z)-octadec-9-enoic acid;tin Chemical compound [Sn].CCCCCCCC\C=C/CCCCCCCC(O)=O QMTFKWDCWOTPGJ-KVVVOXFISA-N 0.000 claims 1
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims 1
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical group CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims 1
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 claims 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims 1
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims 1
- WHMDKBIGKVEYHS-IYEMJOQQSA-L Zinc gluconate Chemical compound [Zn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O WHMDKBIGKVEYHS-IYEMJOQQSA-L 0.000 claims 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 claims 1
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims 1
- 229960004232 linoleic acid Drugs 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- UQCOBIQNBIHYJK-UHFFFAOYSA-N tetradecanoic acid;tin Chemical compound [Sn].CCCCCCCCCCCCCC(O)=O UQCOBIQNBIHYJK-UHFFFAOYSA-N 0.000 claims 1
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims 1
- WGIWBXUNRXCYRA-UHFFFAOYSA-H trizinc;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O WGIWBXUNRXCYRA-UHFFFAOYSA-H 0.000 claims 1
- GAAKLDANOSASAM-UHFFFAOYSA-N undec-10-enoic acid;zinc Chemical compound [Zn].OC(=O)CCCCCCCCC=C GAAKLDANOSASAM-UHFFFAOYSA-N 0.000 claims 1
- 239000004246 zinc acetate Substances 0.000 claims 1
- 239000011746 zinc citrate Substances 0.000 claims 1
- 235000006076 zinc citrate Nutrition 0.000 claims 1
- 229940068475 zinc citrate Drugs 0.000 claims 1
- 239000011670 zinc gluconate Substances 0.000 claims 1
- 235000011478 zinc gluconate Nutrition 0.000 claims 1
- 229960000306 zinc gluconate Drugs 0.000 claims 1
- 229940098697 zinc laurate Drugs 0.000 claims 1
- 229940012185 zinc palmitate Drugs 0.000 claims 1
- 229940118257 zinc undecylenate Drugs 0.000 claims 1
- ODNJVAVDJKOYFK-GRVYQHKQSA-L zinc;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Zn+2].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O.CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O ODNJVAVDJKOYFK-GRVYQHKQSA-L 0.000 claims 1
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 claims 1
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 claims 1
- XDWXRAYGALQIFG-UHFFFAOYSA-L zinc;propanoate Chemical compound [Zn+2].CCC([O-])=O.CCC([O-])=O XDWXRAYGALQIFG-UHFFFAOYSA-L 0.000 claims 1
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Abstract
The invention discloses Sn-doped ZnO superfine nanowires and a synthesis method thereof. The naowires have a hexagonal wurtzite structure, a diameter of 1 to 10 nanometers and a length of 2 to 10,000 nanometers. The synthesis method comprises the following steps of: mixing zinc fatty acid, tin fatty acid, fatty amine and a high boiling point organic solvent and putting the mixture into a reaction flask; heating to the temperature of between 50 and 200 DEG C with magnetic stirring under an inert protective atmosphere and keeping the temperature for 1 to 1,000 minutes; then heating to the temperature of between 200 and 350 DEG C under the inert protective atmosphere and keeping the temperature for 1 to 1,000 minutes; and centrifugally separating to obtain the Sn-doped ZnO superfine nanowires. The nanowires have the advantages of simple preparation process, low cost, high repeatability, easy industrial production and possible application to various fields such as transparent electroconductive films, flexible display devices, thin-film transistors, sensors and the like.
Description
Technical field
The present invention relates to technical field of nano material, relate in particular to a kind of Sn adulterated ZnO superfine nano line and compound method thereof.
Background technology
ZnO is a kind of II-VI group iii v compound semiconductor material, and energy gap is 3.37eV under the room temperature, and exciton bind energy is 60meV, is the ideal material of semiconductor laser, ultraviolet detector, royal purple light-emitting diode etc. under the gentle higher temperature of preparation room.The optics that is superior to the body material, electricity and the piezoelectric properties etc. that the ZnO monodimension nanometer material is had owing to quantum confined effect, surface effects, piezoelectric effect etc. have become the focus of current optoelectronic information research field.In the ZnO nano wire, carry out the doping of Sn, let Sn substitute the position of Zn, the adjusting that can realize being with and the change of electric property have good using value and Research Significance in fields such as preparing short wavelength's nano luminescent device and nano photoelectronic devices.
Some synthetic methods of mixing the ZnO nano wire of Sn are arranged at present; Mainly be divided into two big types of physical method and chemical processes; The former mainly comprises pulsed laser deposition, thermal evaporation etc., and the latter mainly comprises metal organic chemical vapor deposition, sol-gel method, hydrothermal method etc.These preparing methods' main deficiency is apparatus expensive or complex process, poor controllability, uniform doping property difference etc.; And the diameter of the Sn doped ZnO nano-wire that is obtained is generally in hundreds of nanometer to tens nanometer; Difficulty is observed tangible quantum confined effect, and uneven doped property has also limited its application in the nano photoelectric devices field widely simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of with low cost, controllability good, the Sn doping ZnO superfine nano line and the compound method thereof of high crystalline quality.
Sn doping ZnO superfine nano line of the present invention has hexagonal wurtzite structure, and the diameter of nano wire is 1～10 nanometer, and length is 2～10000 nanometers.
The compound method of Sn doping ZnO superfine nano line may further comprise the steps:
1) be that 200～350 ℃ organic solvent mixes and to place reaction flask with fatty acid zinc, lipid acid tin, oleyl amine and boiling point.Under inert protective atmosphere, magnetic agitation is even, be warming up to 50～200 ℃ after, be incubated 1～1000 minute, fatty acid zinc: the mol ratio of lipid acid tin 1: 1～100: 1, aliphatic amide: the mol ratio of the total amount of fatty acid zinc and lipid acid tin is 1: 1～50: 1;
2) under inert protective atmosphere, be heated to 200～350 ℃ then, be incubated 1～1000 minute, be cooled to room temperature;
3), obtain the adulterated ZnO superfine nano of Sn line with the reaction mixture spinning.
Among the present invention, described fatty acid zinc is a Zinic stearas.Lipid acid tin is Hydrocerol A tin.Aliphatic amide is an oleyl amine.
Among the present invention, described boiling point is that 200～350 ℃ organic solvent can be octyl ether, 1-octadecylene, phenyl ether.The medium that organic solvent carries out as fatty acid zinc, the dissolving of lipid acid tin and reaction, its consumption does not have special requirement.
Described inert protective gas is that purity is argon gas or the nitrogen more than 99%.
The present invention can control the length and the diameter of the adulterated ZnO superfine nano of Sn line through conditioned reaction heating solution temperature and reaction times; Can change actual doping content, the pattern of realization ZnO nano wire and the adjusting of dispersiveness of Sn in the ZnO nano wire through the mol ratio of regulating fatty acid zinc and lipid acid tin.Preparation technology of the present invention is simple, cost is lower, good reproducibility, be easy to suitability for industrialized production.The diameter of the Sn doping ZnO superfine nano line that obtains is 1～10 nanometer; Approaching with exciton Bohr radius 1.8 nanometers of ZnO body monocrystalline under the room temperature; Has very strong quantum confined effect; Simultaneously Sn mix change to electric property, be expected to be the ultraviolet detector on basis, flexible show and various fields such as transmitter are used in solution method.
Description of drawings
Fig. 1 is the XRD figure of the adulterated ZnO superfine nano of Sn line;
Fig. 2 is the TEM photo of the adulterated ZnO superfine nano of Sn line;
Fig. 3 is the XPS figure of the adulterated ZnO superfine nano of Sn line;
Fig. 4 is the ultraviolet-visible absorption spectroscopy figure of the adulterated ZnO superfine nano of Sn line.
Embodiment
The instance that below synthesizes the adulterated ZnO superfine nano of Sn line for employing the inventive method, but the present invention is not limited to these embodiment.
Embodiment 1
1) take by weighing 1mmol Zinic stearas, 0.1mmol Triple Pressed Stearic Acid tin (mol ratio is 10: 1), the oleyl amine of 7mmol and the 1-octadecylene of 10ml and place the 50ml reaction flask, under inert protective atmosphere, magnetic agitation is warming up to 140 ℃, is incubated 20min then.
2) under inert protective atmosphere, rise to 340 ℃ to temperature, be incubated 30 minutes, to room temperature,, obtain the adulterated ZnO superfine nano of Sn line the reaction mixture spinning with the water-bath cooled reaction solution.
After the green product drying that obtains, carry out the XRD test, test result is seen Fig. 1.Peak among Fig. 1 all is the main peak position of wurtzite ZnO phase, proves that the product that obtains is a wurtzite structure; The TEM electromicroscopic photograph of product is seen Fig. 2, and as can be seen from the figure, the diameter of nano wire is 3～5 nanometers, and length is 50～200 nanometers.Nano wire is carried out XPS test, and test result is seen Fig. 3, from figure, can know that the signal of tin element in the nano wire is very strong, prove the Sn element entering ZnO nano wire that mixes really.Compare with the signal of zinc element, calculating both content is 16: 1 than Zn: Sn.Product is carried out UV, visible light absorb test; Test result is seen Fig. 4, can know from Fig. 4, and the ZnO nano wire of mixing Sn has tangible exciton absorption peak characteristic; And the obvious blue shift of peak position is to 332 nanometers, and this is effectively mixing and the strong coefficient result of quantum confined effect owing to Sn.
1) octyl ether that takes by weighing 1mmol Zinic stearas, 0.2mmol Hydrocerol A tin (mol ratio is 5: 1), 10mmol stearylamine and 10ml places the 50ml reaction flask, is incubated 10 minutes then.
2) under inert atmosphere protection, rise to 250 ℃ to temperature, and be incubated 60 minutes, to room temperature, with the reaction mixture spinning, obtaining diameter is that 2～6 nanometers, length are the adulterated ZnO superfine nano of the Sn line of 100～200 nanometers with the water-bath cooled reaction solution.
Embodiment 3
1) phenyl ether that takes by weighing 1mmol Zinic stearas, 0.3mmol Hydrocerol A tin (mol ratio is 10: 3), 5mmol amino dodecane and 12ml places the 50ml reaction flask, and under inert atmosphere protection, magnetic agitation is warming up to 150 ℃, is incubated 30 minutes then.
2) under inert atmosphere protection, rise to 210 ℃ to temperature, and be incubated 20 minutes, to room temperature, with the reaction mixture spinning, obtaining diameter is that 2～4 nanometers, length are the adulterated ZnO superfine nano of the Sn line of 100～300 nanometers with the water-bath cooled reaction solution.
Embodiment 4
1) eicosane that takes by weighing 1mmol Zinc tetradecanoate, 0.15mmol tin laurate (mol ratio is 100: 15), 7mmol amino dodecane and 15ml places the 50ml reaction flask, and under inert atmosphere protection, magnetic agitation is warming up to 160 ℃, is incubated 30 minutes then.
2) under inert atmosphere protection, rise to 280 ℃ to temperature, and be incubated 120 minutes, to room temperature, with the reaction mixture spinning, obtaining diameter is that 5～8 nanometers, length are the adulterated ZnO superfine nano of the Sn line of 100～700 nanometers with the water-bath cooled reaction solution.
Embodiment 5
1) octadecane that takes by weighing 1mmol zinc oleate, 0.25mmol lenoleic acid tin (mol ratio is 4: 1), 10mmol octylame and 15ml places the 50ml reaction flask, and under inert atmosphere protection, magnetic agitation is warming up to 110 ℃, is incubated 30 minutes then.
2) under inert atmosphere protection, rise to 230 ℃ to temperature, and be incubated 40 minutes, to room temperature, with the reaction mixture spinning, obtaining diameter is that 3～5 nanometers, length are the adulterated ZnO superfine nano of the Sn line of 100～250 nanometers with the water-bath cooled reaction solution.
Claims (6)
1. the compound method of the adulterated ZnO superfine nano of a Sn line is characterized in that may further comprise the steps:
1) be that 200～350 ℃ organic solvent mixes and to place reactor drum with fatty acid zinc, lipid acid tin, aliphatic amide and boiling point; Stir at the inert protective atmosphere lower magnetic force; Be incubated 1～1000 minute after being warming up to 50～200 ℃; Fatty acid zinc: the mol ratio of lipid acid tin is 1: 1～100: 1, aliphatic amide: the mol ratio of the total amount of fatty acid zinc and lipid acid tin is 1: 1～20: 1;
2) under inert protective gas, be heated to 200～350 ℃ then, be incubated 1～1000 minute, be cooled to room temperature;
3), obtain the adulterated ZnO superfine nano of Sn line with the reaction product spinning;
The adulterated ZnO superfine nano of described Sn line has hexagonal wurtzite structure, and the diameter of nano wire is 1～10 nanometer, and length is 2～10000 nanometers.
2. the compound method of the adulterated ZnO superfine nano of a kind of Sn according to claim 1 line, it is characterized in that: described fatty acid zinc is zinc acetate, zinc propionate, Zinc Undecylenate, Zinc Gluconate, Zinc Heptylate, zinc citrate, Zinc tetradecanoate, zinc laurate, zinc palmitate, zinc oleate, zinc linoleate or Zinic stearas.
3. the compound method of the adulterated ZnO superfine nano of a kind of Sn according to claim 1 line is characterized in that described lipid acid tin is tin acetate, glucono-tin, tetradecanoic acid tin, tin laurate, palmitinic acid tin, oleic acid tin, linolic acid tin or Hydrocerol A tin.
4. the compound method of the adulterated ZnO superfine nano of a kind of Sn according to claim 1 line is characterized in that described aliphatic amide is hexylamine, octylame, decyl amine, amino dodecane, tetradecy lamine, cetylamine, stearylamine or oleyl amine.
5. the compound method of the adulterated ZnO superfine nano of a kind of Sn according to claim 1 line is characterized in that described boiling point is that 200～350 ℃ organic solvent is octyl ether, phenyl ether, the tetradecane, n-Hexadecane, octadecane, eicosane or 1-octadecylene.
6. the compound method of the adulterated ZnO superfine nano of a kind of Sn according to claim 1 line is characterized in that said inert protective gas is that purity is argon gas or the nitrogen more than 99%.
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| CN102442787B (en) * | 2011-09-23 | 2013-09-04 | 青岛海信电器股份有限公司 | Nano air-sensitive thin film and preparation method thereof |
| CN102826527B (en) * | 2012-08-21 | 2014-07-09 | 西北大学 | Preparation method of rare earth-doped Ca-PO4-CO3 solid solution ultrafine nano-wires |
| KR102093625B1 (en) | 2013-04-30 | 2020-03-26 | 엘지디스플레이 주식회사 | Quantum rod and Method of fabricating the same |
| JP6515419B2 (en) * | 2014-05-27 | 2019-05-22 | 国立大学法人信州大学 | Method of manufacturing metal oxide nanowire and nanowire |
| CN105420808B (en) * | 2015-11-06 | 2018-09-18 | 昆山龙腾光电有限公司 | The synthetic method of the ZnO nano crystalline substance of In, Ga codope |
| CN105702857B (en) * | 2016-03-21 | 2018-10-19 | 南昌大学 | A kind of non-volatile more bit micro-/ nano resistance-variable storing devices and application method based on trap states regulation and control |
| CN106186041A (en) * | 2016-07-06 | 2016-12-07 | 常州大学 | A kind of method that nano-ZnO is prepared in microwave-assisted pyrolysis |
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| CN101328609A (en) * | 2008-04-11 | 2008-12-24 | 北京科技大学 | Method for preparing tin doping zinc oxide nanowire by vapor deposition |
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| CN101328609A (en) * | 2008-04-11 | 2008-12-24 | 北京科技大学 | Method for preparing tin doping zinc oxide nanowire by vapor deposition |
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