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Preparing method for lead-sulfide nanocrystalline material

A nanocrystalline material, lead sulfide technology, applied in the direction of lead sulfide, nanotechnology, analytical materials, etc., can solve the problems of complex preparation process and limitations, and achieve the effect of simple method, huge application value and good application prospect.

Active Publication Date: 2018-02-23
INST OF NEW MATERIALS & IND TECH WENZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, the above-mentioned preparation process is complicated, and many key process parameters need to be considered in the preparation process, which is still greatly limited in practical application.

Method used

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  • Preparing method for lead-sulfide nanocrystalline material
  • Preparing method for lead-sulfide nanocrystalline material
  • Preparing method for lead-sulfide nanocrystalline material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] S1: Put 0.1mol of lead nitrate and 0.2mol of sodium dimethylaminodithioformate (sodium thiocarbamate) into a 200ml beaker respectively, add 100ml of high-purity water, stir, then sonicate for 30min, let it react completely, and then filter it with suction. Wash and dry at 120°C for 2 hours to obtain a white lump product, grind it into powder in a mortar, pack it in a glass bottle, and place it in a drying oven for use.

[0040] S2: Weigh out 0.05 mmol of the precursor lead dimethylaminodithiocarbamate, measure 50 ml of ethylene glycol, and put it into a 50 ml long-necked double-necked round bottom flask. It was placed in an ultrasonic cleaner for 20 min and heated to 50°C.

[0041] S3: Under the ultrasonic stirring power of 200W, the precursor reaction solution obtained in step S2 is heated to 120°C by microwave at room temperature, and the heating temperature gradient is 35-40°C / min to obtain the first reaction solution; the first reaction solution is continued Microw...

Embodiment 2-4

[0044] The only difference with Example 1 is that the weighed amounts of lead dimethyl dithiocarbamate in this Example 2-4 are respectively 0.01mol, 0.03mol and 0.06mol, and others are the same as Example 1. To repeat, the obtained lead sulfide nanocrystalline materials are respectively named as PbS-2, PbS-3 and PbS-4.

Embodiment 5-7

[0046] The only difference from Example 1 is that the powers of ultrasonic stirring in Examples 5-7 are respectively 100W, 300W and 400W, and others are the same as in Example 1, and will not be repeated here, and the obtained lead sulfide nanocrystalline materials are respectively named are PbS-5, PbS-5 and PbS-7.

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Abstract

The invention discloses a preparing method for a lead-sulfide nanocrystalline material. The preparing method for the lead-sulfide nanocrystalline material is characterized by including the following steps that a lead compound and sodium dimethyldithiocarbamate are added into pure water and stirred and then subjected to ultrasonic for 30 min to 40 min, suction filtration, washing and drying are carried out, and a lead-source precursor is obtained; the lead-source precursor is added into an organic solvent, the mixture is fully stirred and mixed and subjected to ultrasonic washing for 20 min to30 min, and precursor reaction liquid is obtained; under the ultrasonic stirring power of 100 W to 400 W, the precursor reaction liquid is subjected to gradient microwave heating, wherein gradient microwave heating is heated to be 110 DEG C to 120 DEG C, first reaction liquid is obtained, and the heating temperature gradient is 35 DEG C / min to 40 DEG C / min; the heating temperature is 130 DEG C to180 DEG C, heat preservation is carried out for 4 min to 6 min, second reaction liquid is obtained, and the heating temperature gradient is 2 DEG C / min to 30 DEG C / min; the second reaction liquid is naturally cooled to the room temperature, centrifuged, precipitated and washed, and the lead-sulfide nanocrystalline material is obtained.

Description

field of invention [0001] The invention relates to a preparation method of a nanocrystalline material, in particular to a preparation method of a lead sulfide nanocrystalline material, belonging to the field of nanocrystalline materials. Background technique [0002] Nanomaterials are an important development direction of modern material science. It has four major effects, namely quantum size effect, small size effect, surface effect, and macroscopic quantum tunneling effect, thus showing optical, electrical, magnetic, thermal, mechanical, chemical, diffusion and sintering properties different from traditional materials. [0003] Semiconductor nanomaterials have attracted extensive attention from scientists, and the different sizes and structures of materials have opened up new opportunities to explore their chemical and physical properties. Lead sulfide (PbS) has a narrow band gap (0.41eV) and a large Bohr radius. At the same time, as an important and typical direct band g...

Claims

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Application Information

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IPC IPC(8): C01G21/21G01N21/65B82Y40/00
CPCB82Y40/00C01G21/21C01P2002/01C01P2002/72C01P2002/82C01P2002/85C01P2002/88C01P2004/03C01P2004/04C01P2004/30G01N21/658
Inventor 王舜刘爱丽金辉乐王继昌董小妹郑皓源鲁霞毛心楠
Owner INST OF NEW MATERIALS & IND TECH WENZHOU UNIV
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