CN101920987A - A kind of chemical process for preparing lead sulfide nanoparticles - Google Patents
A kind of chemical process for preparing lead sulfide nanoparticles Download PDFInfo
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- CN101920987A CN101920987A CN 201010227752 CN201010227752A CN101920987A CN 101920987 A CN101920987 A CN 101920987A CN 201010227752 CN201010227752 CN 201010227752 CN 201010227752 A CN201010227752 A CN 201010227752A CN 101920987 A CN101920987 A CN 101920987A
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- lead sulfide
- oleyl amine
- reactor
- sulfide nanoparticles
- lead
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Abstract
The present invention relates to a kind of chemical process for preparing lead sulfide nanoparticles, can prepare lead sulfide nanoparticles, can obtain stable near-infrared absorption spectrum, belong to technical field of nano material with good dispersiveness and particle size uniformity.Lead chloride and oleyl amine are joined in the reactor that has vacuum extractor, vacuumize, oil bath is heated to 120～180 ℃, stirs 0.5～2 hour; Obtain uniform leucosol; Sulphur powder and oleyl amine are joined in another reactor, be heated to 60～100 ℃, obtain wine-colored solution; Two solution are mixed, also be injected into fast in the cold toluene centrifuge tube through sampling in 10～30 minutes, solid impurity is removed in centrifugation; Supernatant liquor in the centrifuge tube is poured in the beaker, adds ethanol sedimentation lead sulfide then in beaker, ethanol is removed in centrifugation again, obtains lead sulfide nanoparticles.The present invention obtains the lead sulfide nanoparticles of good dispersity, even-grained different size.
Description
Technical field
The present invention relates to the chemical process of a kind of preparation lead sulfide (PbS) nano particle, can prepare lead sulfide (PbS) nano particle, can obtain stable near-infrared absorption spectrum, belong to technical field of nano material with good dispersiveness and particle size uniformity.
Background technology
Lead sulfide (PbS) nano particle is a kind of important direct band-gap semicondictor material, has big third-order nonlinear optical characteristic, at PHOTONIC DEVICE such as photon switch field the potential application prospect is arranged also.
Summary of the invention
The objective of the invention is to propose a kind of chemical process for preparing lead sulfide nanoparticles in order to obtain dispersed and even-grained lead sulfide nanoparticles.
The objective of the invention is to be achieved through the following technical solutions.
A kind of chemical process for preparing lead sulfide nanoparticles of the present invention is with lead chloride (PbCl
2), oleyl amine (C
18H
37N) and sulphur (S) powder be initial reactant, with toluene (CH
3C
6H
5) be auxiliary reagent; Its concrete steps are:
1) lead chloride and oleyl amine are joined in the reactor that has vacuum extractor, vacuumize, oil bath is heated to 120～180 ℃, stirs 0.5～2 hour; Obtain uniform leucosol;
2) sulphur powder and oleyl amine are joined in another reactor, be heated to 60～100 ℃, obtain wine-colored solution;
3) with step 2) in solution in the reactor be poured in the reactor in the step 1), through sampling in 10～30 minutes and be injected into fast in the cold toluene centrifuge tube, solid impurity is removed in centrifugation;
4) supernatant liquor in the centrifuge tube is poured in the beaker, adds ethanol sedimentation lead sulfide then in beaker, ethanol is removed in centrifugation again, obtains lead sulfide nanoparticles;
Lead chloride is 0.2～0.3g: 5mL with the ratio of oleyl amine in the above-mentioned step 1);
Above-mentioned step 2) the sulphur powder is 20～40mg: 5mL with the ratio of oleyl amine in.
Beneficial effect
The present invention obtains the lead sulfide nanoparticles of good dispersity, even-grained different size.
Description of drawings
Fig. 1 is the Electronic Speculum picture of PbS nanoparticle, and illustration is selected area electron diffraction figure.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
A kind of chemical process for preparing lead sulfide nanoparticles is with lead chloride (PbCl
2), oleyl amine (C
18H
37N) and sulphur (S) powder be initial reactant, with toluene (CH
3C
6H
5) be auxiliary reagent; Its concrete steps are:
1) 0.28g lead chloride and 5mL oleyl amine are joined in the reactor that has vacuum extractor, vacuumize, oil bath is heated to 140 ℃, stirs 1.5 hours; Obtain uniform leucosol;
2) 14mg sulphur powder and 2.5mL oleyl amine are joined in another reactor, be heated to 80 ℃, obtain wine-colored solution;
3) with step 2) in solution in the reactor be poured in the reactor in the step 1), solid impurity was removed in sampling and being injected into fast in the cold toluene centrifuge tube in the time of 10 minutes in centrifugal 3 minutes under 4000 rotating speeds;
4) supernatant liquor in the centrifuge tube is poured in the beaker, adds ethanol sedimentation lead sulfide then in beaker, ethanol is removed in centrifugation again, obtains lead sulfide nanoparticles, its Electronic Speculum picture as shown in Figure 1, illustration is selected area electron diffraction figure.
Embodiment 2
A kind of chemical process for preparing lead sulfide nanoparticles is with lead chloride (PbCl
2), oleyl amine (C
18H
37N) and sulphur (S) powder be initial reactant, with toluene (CH
3C
6H
5) be auxiliary reagent; Its concrete steps are:
1) 0.28g lead chloride and 5mL oleyl amine are joined in the reactor that has vacuum extractor, vacuumize, oil bath is heated to 150 ℃, stirs 1 hour; Obtain uniform leucosol;
2) 14mg sulphur powder and 2.5mL oleyl amine are joined in another reactor, be heated to 70 ℃, obtain wine-colored solution;
3) with step 2) in solution in the reactor be poured in the reactor in the step 1), solid impurity was removed in sampling and being injected into fast in the cold toluene centrifuge tube in the time of 20 minutes in centrifugal 3 minutes under 4000 rotating speeds;
4) supernatant liquor in the centrifuge tube is poured in the beaker, adds ethanol sedimentation lead sulfide then in beaker, ethanol is removed in centrifugation again, obtains lead sulfide nanoparticles.
Embodiment 3
A kind of chemical process for preparing lead sulfide nanoparticles is with lead chloride (PbCl
2), oleyl amine (C
18H
37N) and sulphur (S) powder be initial reactant, with toluene (CH
3C
6H
5) be auxiliary reagent; Its concrete steps are:
1) 0.28g lead chloride and 5mL oleyl amine are joined in the reactor that has vacuum extractor, vacuumize, oil bath is heated to 160 ℃, stirs 0.5 hour; Obtain uniform leucosol;
2) 14mg sulphur powder and 2.5mL oleyl amine are joined in another reactor, be heated to 80 ℃, obtain wine-colored solution;
3) with step 2) in solution in the reactor be poured in the reactor in the step 1), solid impurity was removed in sampling and being injected into fast in the cold toluene centrifuge tube in the time of 30 minutes in centrifugal 3 minutes under 4000 rotating speeds;
4) supernatant liquor in the centrifuge tube is poured in the beaker, adds ethanol sedimentation lead sulfide then in beaker, ethanol is removed in centrifugation again, obtains lead sulfide nanoparticles.
Claims (1)
1. chemical process for preparing lead sulfide nanoparticles, it is characterized in that: with lead chloride, oleyl amine and sulphur powder is initial reactant, is auxiliary reagent with toluene; Its concrete steps are:
1) lead chloride and oleyl amine are joined in the reactor that has vacuum extractor, vacuumize, oil bath is heated to 120～180 ℃, stirs 0.5～2 hour; Obtain uniform leucosol;
2) sulphur powder and oleyl amine are joined in another reactor, be heated to 60～100 ℃, obtain wine-colored solution;
3) with step 2) in solution in the reactor be poured in the reactor in the step 1), through sampling in 10～30 minutes and be injected into fast in the cold toluene centrifuge tube, solid impurity is removed in centrifugation;
4) supernatant liquor in the centrifuge tube is poured in the beaker, adds ethanol sedimentation lead sulfide then in beaker, ethanol is removed in centrifugation again, obtains lead sulfide nanoparticles;
Lead chloride is 0.2～0.3g: 5mL with the ratio of oleyl amine in the above-mentioned step 1);
Above-mentioned step 2) the sulphur powder is 20～40mg: 5mL with the ratio of oleyl amine in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010227752 CN101920987A (en) | 2010-07-16 | 2010-07-16 | A kind of chemical process for preparing lead sulfide nanoparticles |
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|---|---|---|---|
| CN 201010227752 CN101920987A (en) | 2010-07-16 | 2010-07-16 | A kind of chemical process for preparing lead sulfide nanoparticles |
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|---|---|
| CN101920987A true CN101920987A (en) | 2010-12-22 |
Family
ID=43336244
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633239A (en) * | 2012-05-11 | 2012-08-15 | 兰州大学 | Preparation method of PbSxSe1-x ternary nanocrystal |
| CN106433634A (en) * | 2016-09-19 | 2017-02-22 | 武汉华思创新科技有限公司 | Preparation method of monodisperse PbS quantum dot |
| CN106517318A (en) * | 2016-09-30 | 2017-03-22 | 华东师范大学 | Method for preparation of lead sulfide ultrafine powder from waste lead-acid battery lead paste |
| CN111635759A (en) * | 2020-06-16 | 2020-09-08 | 南昌大学 | Preparation method of lead sulfide colloidal quantum dots |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050036938A1 (en) * | 2003-08-13 | 2005-02-17 | Taegwhan Hyeon | Method for synthesizing nanoparticles of metal sulfides |
-
2010
- 2010-07-16 CN CN 201010227752 patent/CN101920987A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050036938A1 (en) * | 2003-08-13 | 2005-02-17 | Taegwhan Hyeon | Method for synthesizing nanoparticles of metal sulfides |
Non-Patent Citations (2)
| Title |
|---|
| 《中国博士学位论文全文数据库 工程科技I辑 》 20091215 司华艳 应用表面功能化的纳米颗粒制备新型纳米复合物的研究 1 , 第12期 2 * |
| 《功能材料（增刊）》 20061231 刘凌 胶体法合成PbS和CdS纳米材料 837-839，843 1 第37卷, 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633239A (en) * | 2012-05-11 | 2012-08-15 | 兰州大学 | Preparation method of PbSxSe1-x ternary nanocrystal |
| CN106433634A (en) * | 2016-09-19 | 2017-02-22 | 武汉华思创新科技有限公司 | Preparation method of monodisperse PbS quantum dot |
| CN106433634B (en) * | 2016-09-19 | 2018-10-12 | 武汉华思创新科技有限公司 | A kind of preparation method of monodisperse pulmbous sulfide quantum dot |
| CN106517318A (en) * | 2016-09-30 | 2017-03-22 | 华东师范大学 | Method for preparation of lead sulfide ultrafine powder from waste lead-acid battery lead paste |
| CN111635759A (en) * | 2020-06-16 | 2020-09-08 | 南昌大学 | Preparation method of lead sulfide colloidal quantum dots |
| CN111635759B (en) * | 2020-06-16 | 2021-08-06 | 南昌大学 | Preparation method of lead sulfide colloidal quantum dots |
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Open date: 20101222 |