CN1792773A - Process for preparing aqueous phase lead selenide nano material - Google Patents
Process for preparing aqueous phase lead selenide nano material Download PDFInfo
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- CN1792773A CN1792773A CN 200510119122 CN200510119122A CN1792773A CN 1792773 A CN1792773 A CN 1792773A CN 200510119122 CN200510119122 CN 200510119122 CN 200510119122 A CN200510119122 A CN 200510119122A CN 1792773 A CN1792773 A CN 1792773A
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Abstract
A process for preparing water-phase nano-lead selenide features the reaction between lead acetate, selenourea and coating agent chosen from mercaptoacetic acid, mercaptopropionic acid, cysteine, thioglycerin, and mercaptoethanol at 60-180 deg.C for 15-90 min.
Description
Technical field
The present invention relates to prepare the method for aqueous phase lead selenide nano material.
Background technology
The nano material particularly research of nano semiconductor material is acknowledged as 21st century one of the most promising subject.And will help understanding crystalline nucleation and growth on atom or molecular level to the preparation and the research of one dimension or accurate 1-dimention nano semiconductor material, help further to explore the relation between quantum size effect and the unique physicochemical property, to being implemented in the future design on the molecular level, making microelectronic device and have important directive significance.Especially the one dimension semiconductor nano material has caused the great interest of people because of it has unique physical and chemical properties and the application of the potential on nano-device.Lead selenide is a kind of semiconductor material, the interest that can cause scientist is the character that it is unique, its forbidden band is positioned at middle infrared and visible region, it can be applicable in infrared detector and the thermal imaging, and the structure of this class material can be responsive more to the infrared light of some designated frequency through overregulating.In addition, the Bohr radius of the electronics of lead selenide, hole, exciton is relatively large, is respectively 23nm, 23nm, 46nm, and an approach near this extreme quantum limit zone is provided, therefore have all characteristics of strong quantum limit, smaller such as influenced by surface effects.Lead selenide has the stronger high dielectric radio and little electronics and the virtual mass in hole of comprising to make its quantum effect more remarkable, and also causing its Bohr radius is more than the octuple of cadmium selenide.Therefore, the nanocrystalline fields such as photoelectron, biology that can be applicable to of lead selenide.The lead selenide nano material that how to prepare effectively and control different shapes and size is the problem that a lot of in the last few years researchists explore.
Up to the present, can take many kinds of methods to prepare lead selenide nano material, wherein mainly comprise solid phase decomposition method (Applied Physics communication, 1997,71,3406; Appl.Phy.Lett.1997,71,3406), hydrothermal method is synthesized (nanometer communication, 2002,2,1321; Nano.Lett.2002,2,1321), template (Applied Physics, 2004,96,615; J.Appl.Phys.2004,96,615; Investigation of materials, 1994,9,1014; J.Mater.Res.1994,9,1014) and the organic method of metal (American Chemical Society, 2005,127,7140; J.Am.Chem.Soc.2005,127,7140).Have only the nanocrystalline narrow size distribution of lead selenide prepared in the organic method of metal in these methods, and nanocrystalline quality is higher.Can only be dispersed in the organic solvent but institute's synthetic is nanocrystalline, be unfavorable for application at biological field.
Summary of the invention
The purpose of this invention is to provide a kind of can preparation size and pattern is controlled and preparation method that can stably be scattered in the lead selenide nano material of aqueous phase.
The monomer that adopts among the present invention is: plumbic acetate or selenourea; Coating is: dredge guanidine-acetic acid, thin basic propionic acid, halfcystine, thioglycerol or dredge basic ethanol; Solvent is: deionized water.
Preparation process is as follows:
The mol ratio of monomer and coating is 15-1: 1, plumbic acetate is dissolved in the deionized water, and add coating by proportioning then, with sodium hydroxide the pH value of solution is adjusted to 7-10, make plumbous precursor solution.Selenourea is dissolved in makes the selenium precursor solution in the ionized water, the mol ratio of plumbic acetate and selenourea is 1: 8-4: 1.Then the selenium precursor solution is poured into to plumbous precursor solution, is heated to 60 ℃-180 ℃, react 15-90 minute stopped reaction, treat solution cooling, with water and Virahol wash, centrifugal, drying makes aqueous phase lead selenide nano material.
The present invention utilize selenourea at a certain temperature decomposition and emit plasma selenium, with the plumbous source effect that coating that can be water-soluble coats, it is nanocrystalline that reaction generates lead selenide under normal pressure or under the high pressure, the lead selenide of generation is nanocrystalline stably to be dispersed in aqueous phase.This method has overcome the nanocrystalline of organic synthesis on the one hand can not be applied to biological field, and inferior position such as environmental pollution is bigger.The lead selenide that has synthesized different-shape and size on the other hand again effectively is nanocrystalline, makes material can be applicable to different fields.The preparation process of the whole material of the present invention has the reaction conditions gentleness, and raw materials cost is cheap and less to the pollution of environment, the characteristics that method is simple, and preparation cycle is short, thereby be easy to realize industrialization., the pattern of the lead selenide nano material of preparation has nano particle, nanometer rod, nano wire
Embodiment
Embodiment 1:
Dredge guanidine-acetic acid and coat the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL deionized water, add 27 μ L (0.4mmol) and dredge guanidine-acetic acid, with the sodium hydroxide of 1M the pH value of solution is adjusted to 7 then, make plumbous precursor solution.0.39g (3.2mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 60 ℃, react stopped reaction after 15 minutes, treat solution cooling back with water and Virahol wash, centrifugal, drying makes aqueous phase lead selenide nano material, pattern is a nano particle, and diameter range is at 15-25nm.
Embodiment 2:
Dredge basic propionic acid and coat the nanocrystalline preparation of lead selenide
Take by weighing 0.30g (0.8mmol) plumbic acetate earlier, it is dissolved in the 40mL deionized water, add 136 μ L (1.6mmol) and dredge basic propionic acid, with the sodium hydroxide of 1M the pH value of solution is adjusted to 10 then, make plumbous precursor solution.0.39g (3.2mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 120 ℃, react stopped reaction after 30 minutes, after treating solution cooling, with water and Virahol wash, centrifugal, drying, make aqueous phase lead selenide nano material, pattern is a nano particle, and diameter range is at 20-30nm.
Embodiment 3:
Halfcystine coats the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL water, add 0.07g (0.6mmol) halfcystine, with the sodium hydroxide of 1M the pH value of solution is adjusted to 9 then, make plumbous precursor solution.0.39g (3.2mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 180 ℃, react stopped reaction after 45 minutes, after treating solution cooling, with water and Virahol wash, centrifugal, drying, make aqueous phase lead selenide nano material, pattern is a nanometer rod, and diameter range is at 30-50nm, and length range is at 80-500nm.
Embodiment 4:
Thioglycerol coats the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL water, add 0.22g (2.0mmol) thioglycerol, with the sodium hydroxide of 1M the pH value of solution is adjusted to 10 then, make plumbous precursor solution.0.01g (0.1mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 80 ℃, react stopped reaction after 90 minutes, treat solution cooling back with water and Virahol wash, centrifugal, drying makes aqueous phase lead selenide nano material, and pattern is a nanometer rod, diameter range is at 25-37nm, and length is at 80-600nm.
Embodiment 5:
Dredge basic ethanol and coat the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL water, add 0.08g (1.0mmol) and dredge basic ethanol, with the sodium hydroxide of 1M the pH value of solution is adjusted to 10 then, make plumbous precursor solution.0.04g (0.4mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 100 ℃, react stopped reaction after 60 minutes, after treating solution cooling, with water and Virahol wash, centrifugal, drying, make aqueous phase lead selenide nano material, pattern is a nano particle, and diameter range is at 15-30nm.
Embodiment 6:
Dredge basic propionic acid and coat the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL water, add 60 μ L (0.6mmol) and dredge basic propionic acid, with the sodium hydroxide of 1M the pH value of solution is adjusted to 10 then, make plumbous precursor solution.0.20g (1.6mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 150 ℃, react stopped reaction after 45 minutes, after treating solution cooling, with water and Virahol wash, centrifugal, drying, make aqueous phase lead selenide nano material, pattern is a nano wire, and diameter range is at 15-30nm, and length range is at 100-2000nm.
Embodiment 7:
Halfcystine coats the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL water, add 0.05g (0.4mmol) halfcystine, with the sodium hydroxide of 1M the pH value of solution is adjusted to 7 then, make plumbous precursor solution.0.01g (0.8mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 180 ℃, react stopped reaction after 90 minutes, after treating solution cooling, with water and Virahol wash, centrifugal, drying, make aqueous phase lead selenide nano material, pattern is a nano particle, and diameter range is at 15-23nm.
Embodiment 8:
Dredge guanidine-acetic acid and coat the nanocrystalline preparation of lead selenide
Take by weighing 0.15g (0.4mmol) plumbic acetate earlier, it is dissolved in the 30mL water, add 35 μ L (0.6mmol) and dredge guanidine-acetic acid, with the sodium hydroxide of 1M the pH value of solution is adjusted to 10 then, make plumbous precursor solution.0.39g (3.2mmol) selenourea is dissolved in makes the selenium precursor solution in the deionized water.Rapidly the selenium precursor solution is poured into to plumbous precursor solution then, be heated to 60 ℃, react stopped reaction after 90 minutes, treat solution cooling back with water and Virahol wash, centrifugal, drying makes aqueous phase lead selenide nano material, and pattern is a nanometer rod, diameter range is at 9-20nm, and length is at 30-100nm.
Claims (1)
1. the preparation method of an aqueous phase lead selenide nano material is characterized in that, the monomer of employing is: plumbic acetate or selenourea; Coating is: dredge guanidine-acetic acid, thin basic propionic acid, halfcystine, thioglycerol or dredge basic ethanol; Solvent is: deionized water;
Preparation process and condition are as follows:
The proportioning of monomer and coating is mol ratio 15-1: 1, plumbic acetate is dissolved in the deionized water, and add coating by proportioning then, with sodium hydroxide the pH value of solution is adjusted to 7-10, make plumbous precursor solution; Selenourea is dissolved in makes the selenium precursor solution in the deionized water, the mol ratio of plumbic acetate and selenourea is 1: 8-4: 1; Then the selenium precursor solution is poured into to plumbous precursor solution, is heated to 60 ℃-180 ℃, react 15-90 minute stopped reaction, treat solution cooling, with water and Virahol wash, centrifugal, drying makes aqueous phase lead selenide nano material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384740C (en) * | 2006-10-13 | 2008-04-30 | 中国科学院上海硅酸盐研究所 | Method for preparing sulfure family compound nano tube of lead by cysteine biological molecule assisted self assembling |
| CN101070183B (en) * | 2007-05-24 | 2010-06-02 | 上海大学 | Electronic-beam radiation synthesizing method for nano lead-selenide |
| CN101871127A (en) * | 2010-05-31 | 2010-10-27 | 武汉大学 | Size-controllable synthesis method for MSe (M equal to Cd, Pb) nanocrystals |
| CN102795605A (en) * | 2012-08-06 | 2012-11-28 | 西北工业大学 | Method for preparing nanometer material lead selenide by aqueous phase method |
| CN106634985A (en) * | 2016-09-22 | 2017-05-10 | 上海洞舟实业有限公司 | Preparation for novel down-conversion infrared emission material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9518910D0 (en) * | 1995-09-15 | 1995-11-15 | Imperial College | Process |
| CN1159211C (en) * | 2002-06-07 | 2004-07-28 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
-
2005
- 2005-12-28 CN CNB2005101191223A patent/CN1323027C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100384740C (en) * | 2006-10-13 | 2008-04-30 | 中国科学院上海硅酸盐研究所 | Method for preparing sulfure family compound nano tube of lead by cysteine biological molecule assisted self assembling |
| CN101070183B (en) * | 2007-05-24 | 2010-06-02 | 上海大学 | Electronic-beam radiation synthesizing method for nano lead-selenide |
| CN101871127A (en) * | 2010-05-31 | 2010-10-27 | 武汉大学 | Size-controllable synthesis method for MSe (M equal to Cd, Pb) nanocrystals |
| CN101871127B (en) * | 2010-05-31 | 2012-03-21 | 武汉大学 | Size-controllable synthesis method for MSe (M equal to Cd, Pb) nanocrystals |
| CN102795605A (en) * | 2012-08-06 | 2012-11-28 | 西北工业大学 | Method for preparing nanometer material lead selenide by aqueous phase method |
| CN106634985A (en) * | 2016-09-22 | 2017-05-10 | 上海洞舟实业有限公司 | Preparation for novel down-conversion infrared emission material |
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| CN1323027C (en) | 2007-06-27 |
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Granted publication date: 20070627 Termination date: 20100128 |