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Method of preparing sulfide nano material of lead with calixarene adjusting solvent thermal system

A technology of chalcogen compounds and nanomaterials, applied in nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of high reaction temperature requirements, high cost, difficult to control the shape of toxic gas products, etc., and achieve low cost and easy operation Ease of use and low cost of production

Inactive Publication Date: 2007-02-07
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above reaction schemes all have problems such as high requirements on reaction temperature (above 600°C), high cost, generation of toxic gas, and difficult control of product morphology.

Method used

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  • Method of preparing sulfide nano material of lead with calixarene adjusting solvent thermal system
  • Method of preparing sulfide nano material of lead with calixarene adjusting solvent thermal system
  • Method of preparing sulfide nano material of lead with calixarene adjusting solvent thermal system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 0.001 mole of Pb(NO 3 ) 2 Solid and 0.01 g of calix[4]arene were placed in a 50 ml beaker, a small amount of toluene was added, and after stirring at 80°C for 1 hour, the mixture was transferred into a 40 ml polytetrafluoroethylene reactor, and then 0.001 mole of thiourea was added to the mixed solution. Add toluene to the reactor to 3 / 4 of the volume of the reactor, seal it, and react at 170°C for 24 hours. The reaction kettle was naturally cooled to room temperature. The obtained product was taken out, washed alternately with distilled water and absolute ethanol for 3-6 times, centrifuged, and vacuum-dried at 60° C. to obtain the desired product.

[0030] The morphology and structure of the product were characterized by transmission electron microscope (TEM) and X-ray powder diffractometer (XRD), as figure 1 The TEM shown shows that the product is a PbS quasi-nanorod with a diameter of 200 nm and a length of about 3.5 microns, as figure 2 The XRD results sh...

Embodiment 2

[0032] Weigh 0.001 mole of PbAc 2 Put the solid and 0.01 g of calix[4]arene into a 50 ml beaker, add a small amount of toluene, stir at 70 ° C for 1.5 hours, transfer the mixed solution into the reaction kettle, then add 0.001 mole of thiourea to the reaction kettle, and add toluene at the same time to 4 / 5 of the volume of the reactor, seal it, react at 150°C for 30 hours, cool the reactor to room temperature naturally, take out the obtained product, alternately wash with distilled water and absolute ethanol for 3-6 times, centrifuge and store at 70°C Dry under vacuum to obtain the desired product. The obtained product is a PbS quasi-nanorod with a diameter of about 200 nanometers and a length of about 3 microns, and the crystal system of the product is the same as that of Example 1. The product has high purity and good crystallinity. The optical performance is basically similar to Example 1.

Embodiment 3

[0034] Weigh 0.001 mole of Pb(NO 3 ) 2 Put the solid and 0.01 g of calix[4]arene into a 50 ml beaker, add a small amount of toluene, stir at 80°C for 1 hour, transfer the mixed solution into the reaction kettle, then add 0.001 mole of selenium powder to the reaction kettle, and add toluene at the same time to 3 / 4 of the volume of the reactor, sealed, reacted at 190°C for 20 hours, cooled the reactor to room temperature naturally, took out the obtained product, and cooled the reactor to room temperature naturally. The obtained product was taken out, washed alternately with distilled water and absolute ethanol for 3-6 times, centrifuged, and vacuum-dried at 80° C. to obtain the desired product. The obtained product is a PbS nanorod with a diameter of about 60 nanometers and a length of about 3 microns, and the crystal system of the product is the same as in Example 1. The product has high purity, good crystallinity and optical properties. The optical performance is basically ...

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Abstract

The invention belongs to the field of inorganic nanomaterials, and involves a preparation method for sulfur compounds of lead nanomaterial by calixarene in a specific thermal control system solvent. Said method comprises placing lead salt and calixarene in a container, using toluene as solvent, stirring at 70-90DEG C for 0.8-1.5 hours to obtain a mixture, transferring the mixture into a reactor and adding sulfur source, adding toluene to 3 / 5-4 / 5 of the reactor volume and sealing, reacting at 150-200DEG C for 18-30 hours and cooling to room temperature, washing, separating, and drying to obtain the final product. The molar ratio of sulfur source to lead salt is 1 : 1, wherein the lead salt is one of lead nitrate and lead acetate and sulfur source is one of thiourea, sulfur powders, and selenium powders. The raw materials of this invention are easy to get and cheap. This invention also has the advantages of simple operation and equipment, high purity, convenient treatment, and being easy for industrialization. This invention provides a new method for preparing nanomaterials by controlled synthesis.

Description

technical field [0001] The invention belongs to the field of inorganic nanometer materials, and relates to a synthesis method for preparing lead chalcogen compound nanomaterials. Specifically, it is a method for preparing lead chalcogen compound nanomaterials by regulating a solvothermal system with calixarene. Background technique [0002] Lead chalcogenide materials have important nonlinear optical properties, luminescent properties, quantum size effects and other important physical and chemical properties, and they have broad application prospects in electronics, optics, biology, coatings, medicine and other industries. Many scientific studies have confirmed that when normal substances are processed to extremely small scales, their optical, thermal, electrical, magnetic, mechanical and even chemical properties will also undergo correspondingly significant changes. Due to quantum size effects and surface effects, lead chalcogenide nanomaterials have more excellent optical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G21/21B82B3/00
Inventor 吴庆生尹蓉徽陈云贾润萍
Owner TONGJI UNIV
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