CN101045553A - Preparation method of tin mixed with zinc oxide nanowire - Google Patents
Preparation method of tin mixed with zinc oxide nanowire Download PDFInfo
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- CN101045553A CN101045553A CN 200710065217 CN200710065217A CN101045553A CN 101045553 A CN101045553 A CN 101045553A CN 200710065217 CN200710065217 CN 200710065217 CN 200710065217 A CN200710065217 A CN 200710065217A CN 101045553 A CN101045553 A CN 101045553A
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Abstract
A process for preparing the Sn doped zinc oxide nanowires includes such steps as flushing the Si substrate by detergent, proportionally mixing ZnO powder, SnO powder and C powder by ball grinding, putting said substrate and powder mixture in a ceramic crucible, loading it in a quartz tube of tubular furnace, filling the mixture of argon gas and O2, heating at 850-950 deg.C while reacting, and cooling.
Description
Technical field
The invention belongs to the nano material preparation technical field, a kind of method of vapor phase production tin mixed with zinc oxide monodimension nanometer material particularly is provided, synthesis technique is simple and output is high, has realized the controllable growth under the low preparation temperature.
Background technology
Zinc oxide is direct band gap, and wide bandgap semiconductor belongs to the II-VI compounds of group.The energy gap of ZnO is about 3.37eV under the room temperature, and exciton binding energy higher (60meV) has piezoelectricity, and its photoelectric characteristic has good application prospects.While ZnO material cheapness, raw material abundance, stable chemical performance, good biocompatibility, thereby can be applied to fields such as optical material, matrix material, transmitter, catalyzer.The special one dimension Nano structure of one dimension semiconductor ZnO nano material has been given the ZnO material again in new physical propertys in aspect such as light, electricity, magnetic, simultaneously, the performance that can make the One-Dimensional ZnO nano material by mixing further is optimized and improves, and promotes the application of ZnO nano material aspect micro-nano photoelectric functional device.Thereby obtain suitable preparation technology and realize that the controlled of high-quality ZnO nano material size and photoelectric properties is the one-dimensional zinc oxide nanometer material key in application.
At present, prepared the accurate one-dimension zinc oxide nanostructure of the peacekeeping form of variform by different synthetic methods, these nanostructure forms comprise: zinc oxide nanowire, nano belt, four-acicular nanometer rod, nanotube, nanometer spiral, nanometer plate and nano-cable etc.Different nanostructure forms have different potential uses.The ZnO nano-material can be widely used in nano photoelectronic devices such as nanoscale laser apparatus, field effect transistor, transmitter as structural unit, can also be applied to an emission field as the cold-cathode field electron emission source.Sn mixes and can change electroconductibility, photoluminescence and the field emission performance of One-Dimensional ZnO nano material, helps to widen the Application Areas of One-Dimensional ZnO nano material.Up to now, about the preparation method of tin doping zinc oxide nanowire also seldom, exploitation effectively, reliable preparation seems very important.
The technical development that present stage prepares one-dimensional zinc oxide nanometer material is rapid, and the method for the nano material that comes in every shape of preparation constantly is in the news out, in these methods based on gas-phase deposition.The preparation method of doped one-dimensional nano zinc oxide material mainly contains two classes, and the first kind is directly Zn or ZnO to be mixed with hotchpotch, and methods such as employing thermal evaporation directly generate the doping zinc oxide nanometer structured material; The another kind of method for preparing the doped one-dimensional nano zinc oxide material then is to prepare the ZnO nano structural material earlier, adopts evaporation diffusion or method such as ion implantation to realize mixing then.Comparatively speaking, single stage method realizes that doping process is more simple, product quality height, and cost is low, helps the device assembling.The preparation temperature of physical vapor deposition that with the oxide powder and zinc is raw material is generally about 1400 ℃, and synthesis temperature is higher.In preparation process, add metal catalysts such as gold, cobalt and can reduce synthesis temperature, the easier control of product pattern and size, but product purity is subjected to very big influence.
Summary of the invention
The object of the invention is to provide a kind of method of preparing tin doping zinc oxide nanowire by vapor deposition, reduces preparation temperature, improves preparation technology's controllability, improves the quality of products and productive rate.Realize the doping of semi-conductor one-dimensional zinc oxide nanometer material, prepared tin doping zinc oxide nanowire.This method tentatively realizes the reliable preparation of tin doping zinc oxide nanowire, and preparation temperature reduces, and has improved its productive rate on a large scale.
Concrete technology of the present invention is as follows:
1, silicon (100) substrate is rinsed well with clean-out system, as deposition substrate.Silicon substrate can adopt pure silicon substrate or silicon-doped chip, but simultaneously on the substrate sputtering sedimentation one deck Ag, Au or Pt make catalyzer.Cleaning process is to use acetone and alcohol difference ultrasonic cleaning 20 minutes earlier, uses deionized water rinsing then;
2, with ZnO powder (purity＞99.9%), SnO powder (purity＞99.9%) and C powder [(5/6: 1/6)～(1/2: 1/2)] in molar ratio: 1 thorough mixing is even, mixed powder craft can utilize the method for ball milling, and mixed powder is positioned in the porcelain boat as reaction source, then with the silicon substrate back-off on porcelain boat;
3, the porcelain boat of carrying reaction source and substrate is put into the silica tube middle part of tube furnace, regulated under meter feeds argon gas and oxygen in silica tube mixed gas, total flux is 300～350cm
3/ min, oxygen proportion are 1～2%, under this atmosphere tube furnace are warming up to 850～950 ℃ of synthesis temperatures, are incubated 30～60 minutes then, and after preparation feedback finished, sample cooled to room temperature with the furnace, and products obtained therefrom is tin doping zinc oxide nanowire.
Silicon of the present invention (100) substrate adopts pure silicon substrate or silicon-doped chip, and sputtering sedimentation one deck Ag, Au or Pt make catalyzer on the substrate simultaneously; Use acetone and alcohol difference ultrasonic cleaning 20～30 minutes earlier, use deionized water rinsing then.
Discharge Zn steam and In steam by the carbothermic reduction effect in the experimentation, the reactant gases diffusion runs into silicon substrate, and a spot of oxygen action-reaction deposition generates tin doping zinc oxide nanowire in substrate surface and system.Preparation technology has reduced the sedimentary temperature of evaporation reaction, and the product that obtains is a hexagonal wurtzite structure.Regulate depositing temperature in more among a small circle, the total flux of argon gas and oxygen mixed gas and oxygen proportion can prepare the doped zinc oxide nano-wire of different size, guarantee that nano wire has higher purity, the crystalline quality height; On silicon substrate, utilize magnetron sputtering deposition layer of metal catalyzer, in conjunction with the auxiliary method of catalysis, effectively controlled doping nanowire size and pattern, make the doped zinc oxide nano-wire distribution of sizes more even, output is higher, the a small amount of pollution introduced in the affiliation that adds of catalyzer in product, reduce product purity.The prepared doped semiconductor nanocrystal line direction of growth is mainly [0001], and the nano wire shape is regular, is single crystal structure, and diameter dimension is even vertically, and size is 40～300nm, and nanowire length is at tens micrometer ranges.It is synthetic to adopt present method can obtain tin doping zinc oxide nanowire control in a big way, and output is higher.
Description of drawings
Fig. 1 is the XRD diffraction spectra of tin dope ZnO nano wire, and main diffraction peak is consistent with the zinc oxide diffracting spectrum of hexagonal wurtzite structure.
Fig. 2 is the stereoscan photograph of typical tin doped zinc oxide nano-wire, and as can be seen, a large amount of nano wires cover on the silicon substrate from the figure.
Fig. 3 is the high power stereoscan photograph of single nano-wire, and nanowire surface is level and smooth among the figure, and shape is regular, and the diameter dimension uniformity has high length-to-diameter ratio vertically.
Embodiment
The product quality that makes under following experiment condition is better.Experimental installation is a horizontal pipe furnace, specification: long 75cm, caliber 45mm, 1000 ℃ of maximum heating temperatures; Silica tube pipe range 100cm, caliber 32mm.
Embodiment 1: at first silicon (100) substrate is distinguished ultrasonic cleaning 20 minutes in acetone and dehydrated alcohol, rinse well with deionized water then.ZnO powder, SnO and C powder are pressed atomic ratio mix at 4: 1: 5,2 hours thorough mixing of ball milling evenly are put in the porcelain boat as raw material, and silicon substrate is placed on it.Then porcelain boat is put in the silica tube middle part in the tube furnace, regulates under meter and in pipe, feed argon (98%)/oxygen (2%) mixed gas (300sccm).With the speed of 20 ℃ of per minutes tube furnace is warming up to 900 ℃ and be incubated 40 minutes under this atmosphere, the velvet-like thing of sedimentary canescence is tin doping zinc oxide nanowire on the substrate.
Embodiment 2: the Ag that adopts magnetically controlled sputter method deposition 20nm on the silicon that cleans up (100) substrate will be coated with the silicon substrate of catalyzer as substrate as catalyzer; ZnO, SnO and C powder evenly are put in the porcelain boat as evaporation source by 1: 1: 2 thorough mixing, and silicon chip places on the porcelain boat, then porcelain boat are put into the silica tube middle part of tube furnace; Regulate under meter and in pipe, feed Ar and O
2Mixed gas 300cm
3Min
-1, oxygen proportion 1%, 930 ℃ of temperature of reaction, insulation is 30 minutes under this temperature, continues the ventilation body and is cooled to room temperature until tube furnace, takes out silicon substrate and promptly gets product.
Claims (3)
1, a kind of preparation method of tin doping zinc oxide nanowire is characterized in that: preparation technology is:
A. silicon (100) substrate is rinsed well with clean-out system, as deposition substrate;
B. with ZnO powder, SnO powder and C powder by atomic ratio [(5/6: 1/6)～(1/2: 1/2)]: 1 mixes, and mixed powder is positioned in the porcelain boat as reaction source, then with the silicon substrate back-off on porcelain boat;
C. porcelain boat is put into the silica tube middle part of tube furnace, the use traffic meter is regulated and is fed argon gas and the total flux of oxygen and the ratio of two kinds of gases in the reaction system, and argon gas and oxygen total flux are 300～350cm
3/ min, oxygen proportion are 1～2%; Under setting atmosphere tube furnace is warming up to synthesis temperature, synthesis temperature is 850～950 ℃, is incubated 30～60 minutes then, and preparation feedback finishes the back sample and cools to room temperature with the furnace, and products obtained therefrom is a tin doping zinc oxide nanowire.
2, in accordance with the method for claim 1, it is characterized in that: silicon (100) substrate adopts pure silicon substrate or silicon-doped chip, and sputtering sedimentation one deck Ag, Au or Pt make catalyzer on the substrate simultaneously; Use acetone and alcohol difference ultrasonic cleaning 20～30 minutes earlier, use deionized water rinsing then.
3, in accordance with the method for claim 1, it is characterized in that: ZnO powder, SnO powder and C powder mix the employing ball milling method.
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311365B (en) * | 2008-04-01 | 2010-07-21 | 北京科技大学 | Method for preparing room-temperature ferromagnetic Fe doped ZnO nanometer wire |
| CN101328609B (en) * | 2008-04-11 | 2010-12-08 | 北京科技大学 | Method for preparing tin doping zinc oxide nanowire by vapor deposition |
| CN101497127B (en) * | 2008-02-03 | 2010-12-22 | 中国科学院金属研究所 | Method for preparing zinc-zinc oxide composite nanostructure |
| CN101319369B (en) * | 2008-04-15 | 2011-06-22 | 辽宁师范大学 | Method of preparing type p ZnO nano-wire |
| CN102285634A (en) * | 2011-07-23 | 2011-12-21 | 北京科技大学 | Method for constructing flexible strain sensor based on ZnO micro/nano material |
| CN102320556A (en) * | 2011-07-22 | 2012-01-18 | 北京科技大学 | Method for constructing netty nano ZnO material strain transducer |
| CN101937732B (en) * | 2009-07-02 | 2012-02-15 | 国家纳米科学中心 | Nano cable made of magnetic material and half-metallic material and preparation method thereof |
| CN102942209A (en) * | 2012-11-07 | 2013-02-27 | 上海大学 | Method for preparing one-dimensional nanostructure zinc oxides through changing tin doping ratio |
| CN103382550A (en) * | 2013-07-18 | 2013-11-06 | 哈尔滨工业大学 | Method for preparing copper-doped zinc oxide nano-comb |
| CN104362512A (en) * | 2014-10-13 | 2015-02-18 | 北京大学 | Silicon-based nano laser manufacturing method |
| CN105129840A (en) * | 2015-07-17 | 2015-12-09 | 兰州思雪纳米科技有限公司 | Method of preparing monocrystal zinc oxide nano wire at high yield |
| CN105752947A (en) * | 2016-01-25 | 2016-07-13 | 广东工业大学 | Method for preparing tin selenide nanoribbon and tin selenide nanowire |
| CN106215922A (en) * | 2016-08-08 | 2016-12-14 | 华南师范大学 | The composite catalyst of a kind of growing ZnO nano-wire on micron Cu ball and application thereof |
| CN106809869A (en) * | 2017-01-16 | 2017-06-09 | 华南师范大学 | A kind of preparation method of ZnO micro wires |
| CN107487780A (en) * | 2017-08-02 | 2017-12-19 | 淮阴工学院 | A kind of preparation method of high miller index surface constraint zinc oxide nano-belt |
| CN108658121A (en) * | 2018-04-09 | 2018-10-16 | 湖北大学 | A method of realizing zinc oxide nano-wire array grade doping |
| CN110923665A (en) * | 2019-11-27 | 2020-03-27 | 太原理工大学 | Ga with preferred orientation2O3And SnO2Preparation method of miscible membrane |
| CN114291839A (en) * | 2022-01-07 | 2022-04-08 | 辽宁师范大学 | Low-cost superfine beta-Ga2O3Method for preparing nano-wire |
| CN114314639A (en) * | 2021-12-30 | 2022-04-12 | 湘潭大学 | Preparation method of two-dimensional material layered zinc oxide nanosheet |
-
2007
- 2007-04-06 CN CN 200710065217 patent/CN101045553A/en active Pending
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497127B (en) * | 2008-02-03 | 2010-12-22 | 中国科学院金属研究所 | Method for preparing zinc-zinc oxide composite nanostructure |
| CN101311365B (en) * | 2008-04-01 | 2010-07-21 | 北京科技大学 | Method for preparing room-temperature ferromagnetic Fe doped ZnO nanometer wire |
| CN101328609B (en) * | 2008-04-11 | 2010-12-08 | 北京科技大学 | Method for preparing tin doping zinc oxide nanowire by vapor deposition |
| CN101319369B (en) * | 2008-04-15 | 2011-06-22 | 辽宁师范大学 | Method of preparing type p ZnO nano-wire |
| CN101937732B (en) * | 2009-07-02 | 2012-02-15 | 国家纳米科学中心 | Nano cable made of magnetic material and half-metallic material and preparation method thereof |
| CN102320556A (en) * | 2011-07-22 | 2012-01-18 | 北京科技大学 | Method for constructing netty nano ZnO material strain transducer |
| CN102285634A (en) * | 2011-07-23 | 2011-12-21 | 北京科技大学 | Method for constructing flexible strain sensor based on ZnO micro/nano material |
| CN102942209A (en) * | 2012-11-07 | 2013-02-27 | 上海大学 | Method for preparing one-dimensional nanostructure zinc oxides through changing tin doping ratio |
| CN103382550B (en) * | 2013-07-18 | 2016-05-11 | 哈尔滨工业大学 | A kind of method of preparing copper doped zinc oxide nano-comb |
| CN103382550A (en) * | 2013-07-18 | 2013-11-06 | 哈尔滨工业大学 | Method for preparing copper-doped zinc oxide nano-comb |
| CN104362512A (en) * | 2014-10-13 | 2015-02-18 | 北京大学 | Silicon-based nano laser manufacturing method |
| CN105129840A (en) * | 2015-07-17 | 2015-12-09 | 兰州思雪纳米科技有限公司 | Method of preparing monocrystal zinc oxide nano wire at high yield |
| CN105752947A (en) * | 2016-01-25 | 2016-07-13 | 广东工业大学 | Method for preparing tin selenide nanoribbon and tin selenide nanowire |
| CN106215922A (en) * | 2016-08-08 | 2016-12-14 | 华南师范大学 | The composite catalyst of a kind of growing ZnO nano-wire on micron Cu ball and application thereof |
| CN106809869A (en) * | 2017-01-16 | 2017-06-09 | 华南师范大学 | A kind of preparation method of ZnO micro wires |
| CN107487780A (en) * | 2017-08-02 | 2017-12-19 | 淮阴工学院 | A kind of preparation method of high miller index surface constraint zinc oxide nano-belt |
| CN108658121A (en) * | 2018-04-09 | 2018-10-16 | 湖北大学 | A method of realizing zinc oxide nano-wire array grade doping |
| CN110923665A (en) * | 2019-11-27 | 2020-03-27 | 太原理工大学 | Ga with preferred orientation2O3And SnO2Preparation method of miscible membrane |
| CN114314639A (en) * | 2021-12-30 | 2022-04-12 | 湘潭大学 | Preparation method of two-dimensional material layered zinc oxide nanosheet |
| CN114291839A (en) * | 2022-01-07 | 2022-04-08 | 辽宁师范大学 | Low-cost superfine beta-Ga2O3Method for preparing nano-wire |
| CN114291839B (en) * | 2022-01-07 | 2024-02-02 | 辽宁师范大学 | Low-cost superfine beta-Ga 2 O 3 Method for preparing nanowire |
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Open date: 20071003 |