Method for preparing PbS spherical nano crystals by water-phase process

A nano-crystal and spherical technology, applied in the direction of lead sulfide, etc., can solve the problems of difficult control of orientation growth, few spherical nanostructures, unfavorable industrial application, etc., and achieve the effect of good crystal form, low cost and low toxicity

Inactive Publication Date: 2012-05-30
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since PbS quantum dots are isotropic materials, it is difficult to control the orientation growth during the preparation process, and there are relatively few reports on spherical nanostructures.
Some scholars use surfactants to control the synthesis of PbS zero-dimensional nanostructures, such as Lü et al. 6543) using lead acetate as the lead source, thioacetamide (TAA) as the sulfur source, reacting with the surfactant cetyltrimethylammonium bromide (CTAB) at a reaction temperature of 100°C for 30 minutes to obtain spherical PbS nanoparticles , but the spherical PbS particle diameter that this method makes is very big, is 40~50nm (far greater than 18nm); Zhao et al. Sargent, E.Kumacheva.Langmuir 2005, 21, 1086.) found that under the action of surfactant 1-mercaptoglycerol (TGL) and dimercaptoglycerol (DTG), the pH of the adjustment system=11.2, in a very short time Spherical PbS nanocrystals can be rapidly generated within a short period of time, but the two surfactants used in this method are imported reagents, which are expensive and unfavorable for industrial applications

Method used

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  • Method for preparing PbS spherical nano crystals by water-phase process
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  • Method for preparing PbS spherical nano crystals by water-phase process

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 8mL of distilled water, 4mL of 0.1M lead acetate solution, 7mL of 0.05M CTAB solution and 0.25mL (about 1.0mmol) of tert-dodecanethiol into a 100mL round-bottomed flask, mix the above solutions and place them in a constant temperature oil at 50°C. Stir evenly in the bath, then quickly inject 1mL of 0.1M sodium sulfide solution into the reactor, and reflux with tap water under stirring for 2 hours, 8 hours, 16 hours and 24 hours respectively. After the reaction, the centrifugation (12000rpm, 5min) was carried out after cooling to room temperature, the precipitate was washed successively with distilled water and absolute ethanol, and then the obtained precipitate was naturally dried at room temperature, and the obtained product was dark brown powder. By X-ray diffraction (XRD) (such as figure 1 shown) and electron diffraction pattern (as image 3 shown) shows that the product is a PbS nanocrystal; transmission electron microscopy (TEM) (such as figure 2 As shown), ...

Embodiment 2

[0022] Add 10mL of distilled water, 3mL of 0.1M lead acetate solution, 5mL of 0.05M CTAB solution and 0.25mL of tert-dodecanethiol (about 1.0mmol) into a 100mL round-bottomed flask, mix the above solutions and place them in a constant temperature oil at 100°C. Stir evenly in the bath, then quickly inject 2 mL of 0.1M sodium sulfide solution into the reactor, and reflux with tap water under stirring for 2 hours, 8 hours, 16 hours and 24 hours respectively. Then through the aftertreatment process of Example 1, the product form is obtained with Example 1. As the reflow time (2-24 hours) prolongs, the crystal form of PbS nanocrystals becomes better and the size increases.

Embodiment 3

[0024] Add 10mL of distilled water, 3mL of 0.1M lead acetate solution, 4mL of 0.05M CTAB solution and 0.25mL of tert-dodecylmercaptan (about 1.0mmol) into a 100mL round-bottomed flask, mix the above solutions and place them in a constant temperature oil at 100°C. Stir evenly in the bath, then quickly inject 3mL of 0.1M sodium sulfide solution into the reactor, and reflux with tap water under stirring for 2 hours, 8 hours, 16 hours and 24 hours respectively. Then through the aftertreatment process of Example 1, the product form is obtained with Example 1. As the reflow time (2-24 hours) prolongs, the crystal form of PbS nanocrystals becomes better and the size increases.

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Abstract

The invention discloses a method for preparing PbS spherical nano crystals by a water-phase process. In the method, lead acetate is used as a raw material and reacted with sodium sulfide under the coactions of the cetyl trimethyl ammonium bromide and tert-dodecanethiol surfactants, and the PbS spherical nano crystals are obtained by separating and purifying. The method adopts industrial raw materials which are cheap and readily available and ensures mild reaction conditions and simple and convenient operation.

Description

technical field [0001] The invention relates to the field of nano crystals, in particular to a method for preparing PbS spherical nano crystals by an aqueous phase method. Background technique [0002] PbS nanocrystals belong to Group IV~VI semiconductor nanocrystals (quantum dots), with a small energy band gap (0.41eV, 300K) and a large exciton Bohr radius (18nm), and its electronic energy band ranges from visible light to near In the infrared region, it has potential uses in the fields of nonlinear optical devices, infrared detectors, solar receivers, and biomarkers. The properties of nanomaterials based on PbS quantum dots are directly related to their microscopic morphology. Since PbS quantum dots are isotropic materials, it is difficult to control the orientation growth during the preparation process, and there are relatively few reports on spherical nanostructures. Some scholars use surfactants to control the synthesis of PbS zero-dimensional nanostructures, such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G21/21
Inventor 赵旭升干建群刘光华
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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