CN102030362A - Method for preparing SnO2 nanomaterial by hydride deposition - Google Patents
Method for preparing SnO2 nanomaterial by hydride deposition Download PDFInfo
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- CN102030362A CN102030362A CN 201010500568 CN201010500568A CN102030362A CN 102030362 A CN102030362 A CN 102030362A CN 201010500568 CN201010500568 CN 201010500568 CN 201010500568 A CN201010500568 A CN 201010500568A CN 102030362 A CN102030362 A CN 102030362A
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Abstract
The invention relates to a method for preparing a stannic dioxide (SnO2) nanomaterial on the surface of a tungsten filament. The method is characterized in that: the tungsten filament coated with active carbon is used as a heating device and a substrate for material deposition; SnH4 produced by hydride generation is used as a precursor; and the SnO2 nanomaterial can be obtained by performing chemical vapor deposition under a normal pressure. The method has the advantages of no need of other large-sized equipment, simple device, short reaction time, small amount of used raw materials, mild reaction condition and low cost. The method for preparing the nanomaterial can be expected to be expanded to be used for the preparation of corresponding oxide nanomaterials of other elements capable of producing chemical vapor.
Description
Technical field
The invention belongs to technical field of material, relate to a kind of novel method of tin dioxide material preparation.
Background technology
Tindioxide is a kind of typical broad-band gap n N-type semiconductorN material, and bandwidth range is 3.6-4.0eV.Because its unique photoelectric properties and air-sensitive performance have widespread use in organic synthesis, ceramic industry, gas sensor, semiconductor material, electrode materials, area of solar cell.Tin dioxide material usually has multiple shape to satisfy different application, mainly contains tin dioxide powder, nanometer titanium dioxide tin thin film, nano belt, nano wire and nanometer rod etc.Present stage, the tin dioxide material that the research preparation is fit to the different field needs has become one of focus of people's research.It is a lot of to have the method for preparing tin dioxide material now, comprises solid phase method, and liquid phase method, vapor phase process can be used for synthesizing the material with different-shape.Relatively Chang Yong method has hydrothermal method, coprecipitation method, sol-gel method and chemical Vapor deposition process etc.Chen etc. are raw material with the tin tetrachloride, sodium hydroxide is precipitation agent, the combination water thermal synthesis method has synthesized the adjustable rutile-type nanometer tin dioxide rod of dimension in different reaction mediums, by reconciling the size [D.Chen that reaction medium can be controlled nanometer rod, L.Gao, Chemical Physics Letters, 398 (2004) 201-206]; Dai etc. are respectively with SnO and SnO
2Powder is a precursor, and it is constant with the argon gas flow velocity to keep-up pressure, and evaporation is 2 hours under differing temps, all obtaining width is monocrystalline stannic oxide nanometer band [Z.R.Dai, Z.W.Pan, the Z.L.Wang of 30-200nm even structure, Solid State Communications, 118 (2001) 351-354].The method for preparing at present tin dioxide material is more, because preparation technology's difference, the particle diameter that obtains, purity and the physicochemical property that had thereof also have nothing in common with each other.Existing preparation technology exists the route complexity mostly, the raw materials cost height, and defectives such as apparatus expensive, above several method or need expend long period and treatment step, or need expensive professional equipment and harsh synthesis condition.Therefore, design a kind of simple fast, synthesis of nano SnO with low cost
2The method of material and to expand its new range of application be very necessary.
Summary of the invention
The invention provides a kind of preparation method at the tungsten filament surface preparation nano tin dioxide material that is coated with gac, method occurs in based on hydride carries out chemical vapour deposition under the condition of normal pressure.By peristaltic pump with stannous chloride solution and solution of potassium borohydride hybrid reaction, with the SnH that generates
4Taken out of by argon gas stream, lead to the tungsten filament surface that is coated with gac and heating, deposition generates tin dioxide material thereon.This method is carried out under condition of normal pressure, and equipment is simple, and cost is low, easy handling.
The present invention realizes by following reactions steps:
1. the gac with the 10-100 milligram evenly is coated on the tungsten filament surface, is placed in the homemade quartz cover in laboratory, as the substrate of accepting of tin dioxide material.
2. by regulating tungsten filament current control tungsten filament temperature at 100-500 ℃.
By peristaltic pump with stannous chloride solution and solution of potassium borohydride hybrid reaction, the SnH of generation
4Blow out by argon gas, lead to the tungsten filament surface, deposit 5-120 minute.
4. after deposition is finished, tungsten filament is placed retort furnace,, obtain the nano oxidized tin material of vapour deposition on the tungsten filament surface 300 ℃ of calcinings 1-4 hour.
Advantage of the present invention:
Utilization of the present invention scribbles the tungsten filament of gac as heating unit and the sedimentary substrate of material, and the SnH that generates takes place by hydride
4As precursor, under condition of normal pressure, carry out chemical vapour deposition and can obtain nano tin dioxide material, do not need other main equipment, device is simple, and the reaction times is short, and the raw material consumption is few, the reaction conditions gentleness, cost is lower.This preparation method can be expected to be extended to the preparation that other can generate the relevant nanometer oxide material of chemical evapn element.
Description of drawings
Fig. 1 present method prepares the SEM figure of gained tin dioxide material
The EDS spectrogram of Fig. 2 material surface
Embodiment
Provide specific embodiment below so that the present invention is specifically described; be necessary to be pointed out that at this following examples can only be used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art of this area makes some nonessential improvement and adjusts according to the content of the invention described above and still belongs to protection scope of the present invention.
Embodiment one
1. get 100 milligrams of gacs after fully grinding, add 0.5 milliliter of dehydrated alcohol and several methyl-sulphoxides, stir, it is coated on the tungsten filament surface to pasty state.Afterwards tungsten filament is put in the retort furnace under 200 ℃ of conditions calcining 2 hours to remove ethanol and methyl-sulphoxide is standby.
2. tungsten filament is placed the homemade quartzy cover in laboratory, as the substrate of accepting of tin dioxide material, tungsten filament is by a DC power supply, by regulating tungsten filament current control tungsten filament temperature about 370 ℃.
By peristaltic pump with stannous chloride solution and solution of potassium borohydride hybrid reaction, the SnH of generation
4Take out of by argon gas, lead to the tungsten filament surface, deposit 30 minutes.
4. after deposition is finished, tungsten filament is placed retort furnace,, obtains the nano tin dioxide material of feeler shape 300 ℃ of calcinings 2 hours, its corresponding characterization data as depicted in figs. 1 and 2, about 1 micron of feeler length, about 100 nanometers of feeler top end diameter.
Embodiment two
The step of this processing method and embodiment one is identical substantially, and institute's difference is 100-200 ℃ of degree of control tungsten filament temperature in the process of growth.Specific practice is, turns down the tungsten filament electric current, allows SnH
4Calcine after 30 minutes at its surface deposition and to obtain the feeler shape nano tin dioxide material that feeler length and example are similar, length-to-diameter ratio is higher.
Embodiment three
The step of this processing method and embodiment one is identical substantially, and institute's difference is time to 2 hour of control chemical vapour deposition in the process of growth.Specific practice is, the working time of control peristaltic pump, with stannous chloride solution and solution of potassium borohydride hybrid reaction, allows SnH
4The tungsten filament surface deposition that is coated with gac calcine after 120 minutes obtain larger-size, length-to-diameter ratio and embodiment one similar feeler shape nano tin dioxide material.
Claims (4)
1. one kind based on the sedimentary preparation nano SnO of hydride
2The method of material is characterized in that, utilizes the gaseous state SnH of the hydride generation generation of Sn element
4As precursor, be loaded on the pre-warmed tungsten filament surface that scribbles gac by argon gas stream, the deposition by for some time prepares nano SnO
2Material obtains SnO
2Absorbent charcoal composite material.
2. preparation method as claimed in claim 1 is characterized in that, with tungsten filament as the heating deposition device, gac is coated on the tungsten filament surface, tungsten filament places the homemade quartz cover in laboratory, by a DC power supply, controls the tungsten filament surface temperature by regulating size of current.
3. preparation method as claimed in claim 1 is characterized in that, is under 100-500 ℃ the condition by regulating the tungsten filament surface temperature, can regulate institute and synthesize SnO
2The pattern of nano material.
4. preparation method as claimed in claim 1 is characterized in that, the tungsten filament surface deposition time that is coated with gac by adjusting is 5-120 minute, can regulate institute and synthesize SnO
2The size of nano material.
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| CN201010500568A CN102030362B (en) | 2010-10-08 | 2010-10-08 | Method for preparing SnO2 nanomaterial by hydride deposition |
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| CN102030362B CN102030362B (en) | 2012-08-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951677A (en) * | 2012-11-16 | 2013-03-06 | 四川大学 | Preparation method of stannic oxide micro-nano materials based on APCVD (atmospheric pressure chemical vapor deposition) method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58115025A (en) * | 1981-12-29 | 1983-07-08 | Nippon Sheet Glass Co Ltd | Method for forming tin oxide film |
| US6235343B1 (en) * | 1998-06-19 | 2001-05-22 | Saint-Gobain Vitrage | Process for depositing a metal-oxide-based layer on a glass substrate and glass substrate thus coated |
| CN1438179A (en) * | 2003-03-14 | 2003-08-27 | 中国科学院上海硅酸盐研究所 | Method for preparing nano tin-oxide powder |
| CN1762827A (en) * | 2005-08-23 | 2006-04-26 | 浙江大学 | Two-step method for preparing stannic oxide nano material |
| CN101306835A (en) * | 2008-04-22 | 2008-11-19 | 华东师范大学 | SnO2 complex three-dimensional nanostructure and method for preparing same |
| CN101372358A (en) * | 2008-10-21 | 2009-02-25 | 北京科技大学 | Method for preparing tin oxide nano-wire by normal atmosphere vapor deposition |
-
2010
- 2010-10-08 CN CN201010500568A patent/CN102030362B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58115025A (en) * | 1981-12-29 | 1983-07-08 | Nippon Sheet Glass Co Ltd | Method for forming tin oxide film |
| US6235343B1 (en) * | 1998-06-19 | 2001-05-22 | Saint-Gobain Vitrage | Process for depositing a metal-oxide-based layer on a glass substrate and glass substrate thus coated |
| CN1438179A (en) * | 2003-03-14 | 2003-08-27 | 中国科学院上海硅酸盐研究所 | Method for preparing nano tin-oxide powder |
| CN1762827A (en) * | 2005-08-23 | 2006-04-26 | 浙江大学 | Two-step method for preparing stannic oxide nano material |
| CN101306835A (en) * | 2008-04-22 | 2008-11-19 | 华东师范大学 | SnO2 complex three-dimensional nanostructure and method for preparing same |
| CN101372358A (en) * | 2008-10-21 | 2009-02-25 | 北京科技大学 | Method for preparing tin oxide nano-wire by normal atmosphere vapor deposition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951677A (en) * | 2012-11-16 | 2013-03-06 | 四川大学 | Preparation method of stannic oxide micro-nano materials based on APCVD (atmospheric pressure chemical vapor deposition) method |
| CN102951677B (en) * | 2012-11-16 | 2014-07-30 | 四川大学 | Preparation method of stannic oxide micro-nano materials based on APCVD (atmospheric pressure chemical vapor deposition) method |
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