CN101049960A - Method for fabricating Nano rod of lead sulfide - Google Patents

Method for fabricating Nano rod of lead sulfide Download PDF

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Publication number
CN101049960A
CN101049960A CN 200710067681 CN200710067681A CN101049960A CN 101049960 A CN101049960 A CN 101049960A CN 200710067681 CN200710067681 CN 200710067681 CN 200710067681 A CN200710067681 A CN 200710067681A CN 101049960 A CN101049960 A CN 101049960A
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China
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joined
deionized water
nano rod
lead sulfide
thiocarbamide
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CN 200710067681
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CN100500574C (en
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祝华云
张孝彬
糜裕宏
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

This invention discloses a hydrothermal method for preparing PdS nanorods. The method comprises: adding sodium dodecyl sulfonate and hexadecyl trimethyl ammonium bromide into deionized water, stirring uniformly to obtain a transparent solution, adding lead acetate and thiourea, stirring uniformly, adding the solution into a hydrothermal reaction kettle, keeping at 80-160 deg.C for 6-24 h, cooling naturally to room temperature, washing the product with deionized water and absolute ethanol, centrifuging for filtration, and drying the precipitate to obtain the product. The method has such advantages as simple process, low reaction temperature, and low energy consumption.

Description

A kind of method for preparing Nano rod of lead sulfide
Technical field
The present invention relates to prepare the method for Nano rod of lead sulfide.
Background technology
Lead sulfide (PbS) is a kind of important semiconductor material, has narrower band gap (being about 0.41ev) and the bigger Bohr radius (being about 18nm) that excites.The PbS of nanoscale can be with from the near infrared blue shift to the visible region, present unusual optical property and electrical properties, big third-order nonlinear optical characteristic is arranged, the potential application prospect is arranged [referring to Kane R S, Cohen R E, Silbey R in fields such as PHOTONIC DEVICE such as photon switchs, J.Phys.Chem, 1996,100,7928].The PbS nano material also is expected to be used at infrared (IR) or near infrared (NIR) district the narrow gap semiconductor device that absorbs and launch is arranged.Especially PbS monodimension nanometer material because its less size and big non-linear is more outstanding on characteristics such as optical property, electric property and mechanical property, becomes hot research in recent years.Yet because PbS is three-dimensional isotropic material, its oriented growth is difficult to control, and its one dimension Nano structure research is less.Zhang etc. [referring to: Hua Zhang, Ming Zuo, Shun Tan, et al.Nanotechnology, 2006,17,2931~2936] be that the raw material heat obtains PbS superfine nano band and nano wire with activated carbon, sulphur and lead chloride, and studied the microstructure of nano belt and the grain boundary structure of nano wire.Wu etc. [referring to: Chien Wu, Jen-Bin Shi, Chih-Jung Chen, et al.MaterialsLetters, 2006,60,3618~3621] utilize anodic alumina films (AAM) to be template, preparing regular diameter is the PbS nano wire of 30nm.Consider that from application point of view it is more gentle to explore preparation condition, method is more simple, and suitable mass-produced preparation method with monodimension nanometer material of good crystal formation remains very big challenge.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, prepares the method for Nano rod of lead sulfide at low temperatures.
The method for preparing Nano rod of lead sulfide of the present invention, employing be hydrothermal method, its step is as follows:
1) sodium laurylsulfonate and cetyl trimethylammonium bromide are joined in the deionized water, fully stir and make both complete formation clear solutions soluble in water, the mass ratio of sodium laurylsulfonate and cetyl trimethylammonium bromide is 1: 2~1: 4;
2) lead acetate and thiocarbamide are joined in the clear solution, mix, the mass ratio of lead acetate and thiocarbamide is 5: 3~5: 4;
3) mixed solution is joined in the hydrothermal reaction kettle, sealed reactor at 80~160 ℃ of following insulation 6~24h, is opened reactor after waiting to naturally cool to room temperature, and with deionized water and absolute ethanol washing, centrifuging, dry sediment obtains final product.
For making sodium laurylsulfonate and cetyl trimethylammonium bromide be dissolved in the deionized water better, step 1) can be pined for carrying out adding, and treats that again room temperature being put in the solution cooling after sodium laurylsulfonate and cetyl trimethylammonium bromide dissolve fully carries out next step.
Beneficial effect of the present invention is: the preparation method is simple, and temperature of reaction is low, less energy consumption, and cost is low, helps suitability for industrialized production.
Description of drawings
Fig. 1 is the XRD figure of prepared Nano rod of lead sulfide;
Fig. 2 is the transmission electron microscope picture (TEM) of prepared Nano rod of lead sulfide.
Embodiment
Embodiment 1:
1) under the room temperature 0.15g sodium laurylsulfonate and 0.2g cetyl trimethylammonium bromide are joined in the deionized water of 120mL, heating and abundant the stirring make both soluble in water fully on magnetic stirring apparatus, form clear solution;
2) 0.75g lead acetate and 0.45g thiocarbamide are joined in the clear solution, continue to mix;
3) mixed solution is joined in the teflon-lined hydrothermal reaction kettle, sealed reactor, be incubated 12h down at 120 ℃, open reactor after waiting to naturally cool to room temperature, with deionized water and absolute ethanol washing, obtain throw out after the centrifuging, throw out obtains final product 50 ℃ of oven dry down.
Fig. 1 is the XRD figure of prepared product, and Fig. 2 is the transmission electron microscope picture (TEM) of prepared product.As seen from the figure, products therefrom is a Nano rod of lead sulfide.
Embodiment 2:
1) under the room temperature 0.3g sodium laurylsulfonate and 0.6g cetyl trimethylammonium bromide are joined in the deionized water of 120mL, heating and abundant the stirring make both soluble in water fully on magnetic stirring apparatus, form clear solution;
2) 1.5g lead acetate and 1.0g thiocarbamide are joined in the clear solution, continue to mix;
3) mixed solution is joined in the teflon-lined hydrothermal reaction kettle, sealed reactor, be incubated 12h down at 160 ℃, open reactor after waiting to naturally cool to room temperature, with deionized water and absolute ethanol washing, obtain throw out after the centrifuging, throw out obtains final product 50 ℃ of oven dry down.
Embodiment 3:
1) under the room temperature 0.2g sodium laurylsulfonate and 0.8g cetyl trimethylammonium bromide are joined in the deionized water of 120mL, heating and abundant the stirring make both soluble in water fully on magnetic stirring apparatus, form clear solution;
2) 3.0g lead acetate and 2.4g thiocarbamide are joined in the clear solution, continue to mix;
3) mixed solution is joined in the teflon-lined hydrothermal reaction kettle, sealed reactor is incubated 6h down at 80 ℃, open reactor after waiting to naturally cool to room temperature,, obtain throw out after the centrifuging with deionized water and absolute ethanol washing, throw out obtains final product 50 ℃ of oven dry down.

Claims (1)

1. method for preparing Nano rod of lead sulfide, its step is as follows:
1) sodium laurylsulfonate and cetyl trimethylammonium bromide are joined in the deionized water, fully stir and make both complete formation clear solutions soluble in water, the mass ratio of sodium laurylsulfonate and cetyl trimethylammonium bromide is 1: 2~1: 4;
2) lead acetate and thiocarbamide are joined in the clear solution, mix, the mass ratio of lead acetate and thiocarbamide is 5: 3~5: 4;
3) mixed solution is joined in the hydrothermal reaction kettle, sealed reactor at 80~160 ℃ of following insulation 6~24h, is opened reactor after waiting to naturally cool to room temperature, and with deionized water and absolute ethanol washing, centrifuging, dry sediment obtains final product.
CNB2007100676813A 2007-03-29 2007-03-29 Method for fabricating nano rod of lead sulfide Expired - Fee Related CN100500574C (en)

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CNB2007100676813A CN100500574C (en) 2007-03-29 2007-03-29 Method for fabricating nano rod of lead sulfide

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CN101049960A true CN101049960A (en) 2007-10-10
CN100500574C CN100500574C (en) 2009-06-17

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
MD241Z (en) * 2009-12-29 2011-03-31 Институт Прикладной Физики Академии Наук Молдовы Method for producing PbS nanoparticles stabilized with gelatine
MD242Z (en) * 2010-01-26 2011-03-31 Институт Прикладной Физики Академии Наук Молдовы Method for producing hydrophilic PbS nanocrystals
CN101319404B (en) * 2008-06-10 2012-05-16 浙江大学 Method for preparation of hollow spherical cadmium sulfide nanocrystalline
CN101955220B (en) * 2009-05-08 2012-05-30 中国科学院广州化学研究所 Method for preparing PbS spherical nano crystals by water-phase process

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101319404B (en) * 2008-06-10 2012-05-16 浙江大学 Method for preparation of hollow spherical cadmium sulfide nanocrystalline
CN101955220B (en) * 2009-05-08 2012-05-30 中国科学院广州化学研究所 Method for preparing PbS spherical nano crystals by water-phase process
MD241Z (en) * 2009-12-29 2011-03-31 Институт Прикладной Физики Академии Наук Молдовы Method for producing PbS nanoparticles stabilized with gelatine
MD242Z (en) * 2010-01-26 2011-03-31 Институт Прикладной Физики Академии Наук Молдовы Method for producing hydrophilic PbS nanocrystals

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