CN101402466A - Method for producing monodisperse cube shaped pulmbous sulfide nanocrystalline - Google Patents
Method for producing monodisperse cube shaped pulmbous sulfide nanocrystalline Download PDFInfo
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- CN101402466A CN101402466A CNA2008101221063A CN200810122106A CN101402466A CN 101402466 A CN101402466 A CN 101402466A CN A2008101221063 A CNA2008101221063 A CN A2008101221063A CN 200810122106 A CN200810122106 A CN 200810122106A CN 101402466 A CN101402466 A CN 101402466A
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- deionized water
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- cube shaped
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Abstract
The invention relates to a method for preparing single-dispersed cubelike lead sulphide nano crystal. The method comprises the steps that lead acetate, thiacetamide, dodecyl sodium sulfate and hexadecyl trimethyl ammonium bromide are mixed into a reagent in the mol ratio of 1-2 to 2-3 to 0.15-0.2 to 0.2-0.3, the reagent is added into deionized water and stirred evenly, and the mass ratio of the reagent to the deionized water is 1 to between 20 and 40; and then a reaction solution is placed into a sealed reaction kettle, performs reaction at a temperature of between 120 and 160 DEG C for 8 to 16 hours, and is cooled to the room temperature, filtered, washed and dried. The method adopts simple controllable hydro-thermal reaction to prepare the single-dispersed cubelike lead sulphide nano crystal. The method has the advantages of easily obtained and cheap materials, simple process, low cost, high product purity and good repeatability, and is favorable for industrialized production on a large scale.
Description
Technical field
The invention belongs to the material technology field, relate to a kind of preparation of nanomaterials, be specifically related to the preparation method of monodisperse cube shaped pulmbous sulfide nanocrystalline.
Background technology
Lead sulfide (PbS) is a kind of cube of rock salt structure semiconductor material, has narrow band gap (0.41eV) and big Bohr's exciton radius (18nm).PbS is nanocrystalline to have strong quantum confined effect, its cubic non-linearity optical property approximately is 30 times of GaAs, 1000 times of CdSe have potentially at aspects such as near infrared communication, photon switch, heat and bio-imaging, photoelectric device and solar cells and to use.
Synthetic and the assembling of the control of nanostructure has in recent years become the focus of nano materials research, for solid basis has been established in the development of the nano-device " from bottom to top " of specific function.The research of PbS nanostructure is mainly still concentrated on nanocrystalline the synthesizing of PbS of different-shape at present both at home and abroad.As obtaining PbS nano particle (comprising quantum dot) in the decomposition of micella, sol-gel, glass, LB (Langmuir-Blogdett) film, polymeric matrix and organic lead-salt.Also obtained the PbS nanometer rod, passed through succsinic acid two (2-ethylhexyl) ester sulfonic acid lead (Pb (AOT) in octane-iso as [J.Phys.Chem.B, 2006,110,184] such as Zhang
2) and thioacetamide (TAA) prepared in reaction the PbS nanometer rod, Qian etc. [Mater.Chem.Phys., 2004,88,217] are by the PbS nanometer rod that water and oil phase surface reaction synthesize bunchy that acts on of tensio-active agent.The PbS of other pattern also has a spot of report, as [Adv.Mater., 2006 such as Zhao, 18,359] it is nanocrystalline to utilize anion and cation mixing surfactant low temperature to synthesize star PbS, [J.Am.Chem.Soc. such as Lee, 2002,124,11244] decompose precursor (PbS with o
2CNEt
2)
2The PbS that has obtained various patterns such as cubic, spherical, starlike is nanocrystalline.Zhou etc. [J.Phys.Chem.B, 2006,110,6543] adopt that the solution circumfluence method has obtained that star is flower-shaped, star racemosus shape and PbS such as cubic are nanocrystalline.The present invention prepares monodisperse cube shaped pulmbous sulfide nanocrystalline at low temperatures by the mol ratio of reconciliation statement surface-active agent sodium laurylsulfonate and cetyl trimethylammonium bromide.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing monodisperse cube shaped pulmbous sulfide nanocrystalline, this method raw material is cheap and easy to get, and technology is simple, cost is low, constant product quality is easy to realize control and good process repeatability that the diameter of the cube shaped pulmbous sulfide nanocrystalline of preparing is 80～100nm.
The method for preparing monodisperse cube shaped pulmbous sulfide nanocrystalline of the present invention is plumbous source with plumbic acetate, is the sulphur source with the thioacetamide, carries out in closed reactor, and its step is as follows:
1) plumbic acetate, thioacetamide, sodium laurylsulfonate, cetyl trimethylammonium bromide are mixed into reactant in molar ratio at 1～2: 2～3: 0.15～0.2: 0.2～0.3, wherein plumbic acetate is that plumbous source, thioacetamide are that sulphur source, sodium laurylsulfonate are that anion surfactant, cetyl trimethylammonium bromide are cats product.
2) reactant is joined in the deionized water, stir 15～30 minutes as reaction soln, the mass ratio of reactant and deionized water is 1: 20～40.
3) reaction soln is put into closed reaction kettle, under 120～160 ℃ of temperature condition, reacted 8～16 hours, be cooled to normal temperature.
4) reacted solution is filtered, the filter residue deionized water wash is removed unreacted unnecessary ion, carries out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
The present invention prepares monodisperse cube shaped pulmbous sulfide nanocrystalline by the hydro-thermal reaction of simple controllable.This method raw material is cheap and easy to get, and technology is simple, and cost is low, the product purity height, and good reproducibility helps large-scale industrial production.
Description of drawings
Fig. 1 is the XRD figure of monodisperse cube shaped pulmbous sulfide nanocrystalline;
Fig. 2 is transmission electron microscope (TEM) photo of monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment
Embodiment 1
With 4.0 * 10
-3Mol analytical pure plumbic acetate, 1.2 * 10
-2Mol analytical pure thioacetamide, 0.8 * 10
-3Mol analytical pure sodium laurylsulfonate, 1.2 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 20, stir 15 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 160 ℃ of reactions 12 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, get final product monodisperse cube shaped pulmbous sulfide nanocrystalline.Product is accredited as lead sulfide (Fig. 1) through X-ray powder diffraction; TEM Electronic Speculum testing product pattern (Fig. 2); The sulfide nanocrystalline diameter is 80～120nm.
Embodiment 2
With 8.0 * 10
-3Mol analytical pure plumbic acetate, 8.0 * 10
-3Mol analytical pure thioacetamide, 0.6 * 10
-3Mol analytical pure sodium laurylsulfonate, 0.8 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 20, stir 25 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 140 ℃ of reactions 16 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 3
With 8.0 * 10
-3Mol analytical pure plumbic acetate, 8.0 * 10
-3Mol analytical pure thioacetamide, 0.8 * 10
-3Mol analytical pure sodium laurylsulfonate, 1.2 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 30, stir 20 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 120 ℃ of reactions 14 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 4
With 4.0 * 10
-3Mol analytical pure plumbic acetate, 1.2 * 10
-2Mol analytical pure thioacetamide, 0.6 * 10
-3Mol analytical pure sodium laurylsulfonate, 0.8 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 25, stir 15 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 150 ℃ of reactions 8 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 5
With 8.0 * 10
-3Mol analytical pure plumbic acetate, 1.2 * 10
-2Mol analytical pure thioacetamide, 0.6 * 10
-3Mol analytical pure sodium laurylsulfonate, 1.2 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 20, stir 20 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 140 ℃ of reactions 16 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 6
With 4.0 * 10
-3Mol analytical pure plumbic acetate, 8.0 * 10
-3Mol analytical pure thioacetamide, 0.8 * 10
-3Mol analytical pure sodium laurylsulfonate, 0.8 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 35, stir 30 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 130 ℃ of reactions 12 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 7
With 8.0 * 10
-3Mol analytical pure plumbic acetate, 1.2 * 10
-2Mol analytical pure thioacetamide, 0.8 * 10
-3Mol analytical pure sodium laurylsulfonate, 0.8 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 20, stir 25 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 120 ℃ of reactions 16 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 8
With 4.0 * 10
-3Mol analytical pure plumbic acetate, 8.0 * 10
-3Mol analytical pure thioacetamide, 0.6 * 10
-3Mol analytical pure sodium laurylsulfonate, 1.2 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 25, stir 15 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 140 ℃ of reactions 14 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Embodiment 9
With 6.0 * 10
-3Mol analytical pure plumbic acetate, 1.0 * 10
-2Mol analytical pure thioacetamide, 0.7 * 10
-3Mol analytical pure sodium laurylsulfonate, 1.0 * 10
-3Mol analytical pure cetyl trimethylammonium bromide is mixed into reactant, reactant is joined in the deionized water, the mass ratio of reactant and deionized water is 1: 30, stir 30 minutes as reaction soln, reaction soln is put into the airtight withstand voltage reactor of 150ml Stainless Steel, 160 ℃ of reactions 10 hours, be cooled to normal temperature, open reactor, reacted solution is filtered, and the filter residue deionized water wash is removed unreacted unnecessary ion, carry out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
Claims (1)
1, a kind of method for preparing monodisperse cube shaped pulmbous sulfide nanocrystalline is characterized in that this method is plumbous source, is the sulphur source with the thioacetamide that with plumbic acetate carry out, concrete steps are as follows in closed reactor:
1) plumbic acetate, thioacetamide, sodium laurylsulfonate, cetyl trimethylammonium bromide are mixed into reactant in molar ratio at 1～2: 2～3: 0.15～0.2: 0.2～0.3, wherein plumbic acetate is that plumbous source, thioacetamide are that sulphur source, sodium laurylsulfonate are that anion surfactant, cetyl trimethylammonium bromide are cats product;
2) reactant is joined in the deionized water, stir 15～30 minutes as reaction soln, the mass ratio of reactant and deionized water is 1: 20～40;
3) reaction soln is put into closed reaction kettle, under 120～160 ℃ of temperature condition, reacted 8～16 hours, be cooled to normal temperature;
4) reacted solution is filtered, the filter residue deionized water wash is removed unreacted unnecessary ion, carries out vacuum-drying then, can prepare monodisperse cube shaped pulmbous sulfide nanocrystalline.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102557119A (en) * | 2012-03-16 | 2012-07-11 | 西南大学 | Method for preparing lead sulfide nanotubes |
| CN102674440A (en) * | 2012-05-23 | 2012-09-19 | 许昌学院 | Chemical method for preparing PbS film with peony-shaped surface appearance by ethylenediamine assisted in-situ preparation |
| CN108793235A (en) * | 2018-09-20 | 2018-11-13 | 昌吉学院 | A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid |
-
2008
- 2008-10-28 CN CNA2008101221063A patent/CN101402466A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102557119A (en) * | 2012-03-16 | 2012-07-11 | 西南大学 | Method for preparing lead sulfide nanotubes |
| CN102674440A (en) * | 2012-05-23 | 2012-09-19 | 许昌学院 | Chemical method for preparing PbS film with peony-shaped surface appearance by ethylenediamine assisted in-situ preparation |
| CN102674440B (en) * | 2012-05-23 | 2013-12-25 | 许昌学院 | Chemical method for preparing PbS film with peony-shaped surface appearance by ethylenediamine assisted in-situ preparation |
| CN108793235A (en) * | 2018-09-20 | 2018-11-13 | 昌吉学院 | A method of preparing vulcanized lead using ammonia process of desulfurization waste liquid |
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Open date: 20090408 |