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New method for preparing semiconductor nano-crystals containing tellurium, selenium or sulfur

A nanocrystal and semiconductor technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of expensive, toxic, flammable and explosive, and achieve the effect of easy operation, good repeatability and high application value

Inactive Publication Date: 2013-03-20
HENAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, Peng et al. and other groups have been using tributylphosphine (TBP) or trioctylphosphine (TOP) to dissolve tellurium, selenium or sulfur as tellurium, selenium or sulfur precursors when synthesizing tellurium, selenium or sulfur precursors. The precursor of sulfur, this method has application limitations because tributylphosphine or trioctylphosphine are toxic, flammable, explosive and relatively expensive drugs

Method used

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  • New method for preparing semiconductor nano-crystals containing tellurium, selenium or sulfur
  • New method for preparing semiconductor nano-crystals containing tellurium, selenium or sulfur
  • New method for preparing semiconductor nano-crystals containing tellurium, selenium or sulfur

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The preparation of embodiment 1 CdTe nanocrystal

[0028] Add 4 mmol Te powder to 20 g dioctylphosphine oxide (di-n-octylphosphine oxide, DOPO) and heat to 320 °C under nitrogen atmosphere until Te is completely dissolved to obtain a light yellow solution, which is the Te precursor, and cool it for later use.

[0029] Mix 0.2mmol cadmium oleate and 6g octadecene into a 25mL three-neck bottle, and heat to 240°C (180-350°C is acceptable) under nitrogen atmosphere to obtain a clear and uniform solution, namely the cadmium precursor.

[0030] Take 1g of Te precursor solution and inject it into the Cd solution at 280°C, and take samples for observation at different times. After reacting for 3 hours, cool down, add acetone to precipitate, and centrifuge to obtain CdTe nanocrystals. The fluorescence absorption spectra of CdTe nanocrystals obtained by sampling and testing at different times are as follows: figure 1 As shown, the TEM and HRTEM of CdTe nanocrystals are as figu...

Embodiment 2

[0031] The preparation of embodiment 2 ZnTe nanocrystals

[0032] 2mmol Te powder was added to 10g di-n-octylphosphinic acid (DOPA) and heated to 350°C under nitrogen atmosphere until Te was completely dissolved to obtain a light yellow solution, namely Te precursor, which was cooled for later use.

[0033] 0.4 mmol of zinc acetylacetonate and 6 g of octadecene were mixed into a 25 mL three-neck bottle, and heated to 240 °C (180-350 °C is acceptable) under nitrogen atmosphere to obtain a clear and homogeneous solution that is the zinc precursor.

[0034] Take 2g of Te precursor solution and inject it into the Zn solution at 310°C, and take samples for observation at different times. After reacting for 3 hours, cool down, add acetone to precipitate, and centrifuge to obtain ZnTe nanocrystals. TEM as image 3 As shown, the XRD pattern is as Figure 7 shown.

Embodiment 3

[0035] Example 3 Preparation of CuTe nanocrystals

[0036] 2mmol Te powder was added to 20g DOPO and heated to 320°C under nitrogen atmosphere until Te was completely dissolved to obtain a light yellow solution, namely Te precursor, which was cooled for later use.

[0037] Mix 0.2mmol copper stearate and 6g octadecene into a 25mL three-neck bottle, and heat to 240°C (180-350°C is acceptable) under nitrogen atmosphere to obtain a clear and homogeneous solution that is the copper precursor.

[0038] Take 2g of Te precursor solution and inject it into the Cu solution at 310°C, and take samples for observation at different times. After reacting for 3 hours, cool down, add acetone to precipitate, and centrifuge to obtain CuTe nanocrystals. TEM such as Figure 4 As shown, the XRD pattern is as Figure 7 shown.

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Abstract

The invention especially relates to a method for preparing nano-crystals containing tellurium, selenium or sulfur, wherein the method uses stable phosphine-containing organic compounds (such as dioctylphosphine oxide and the like) having similar structures as a novel solvent of tellurium powder, selenium powder or sulfur powder and uses a novel tellurium, selenium or sulfur solution as a precursor to prepare a plurality of nano-crystals containing tellurium, selenium or sulfur. The method avoids high cost and high risk caused by a case that tributylphosphine (TBP) or trioctylphosphine (TOP) is commonly and internationally used at present to dissolve tellurium, selenium or sulfur in order to generate the tellurium, selenium or sulfur precursor. The synthetic method has the advantages of safe operation, easy operation, and good repeatability, and medicines used in the method are routine and stable and have low toxicities. The nano-crystals containing tellurium, selenium or sulfur reaches even exceeds nano-crystals containing tellurium, selenium or sulfur synthesized through using flammable and explosive compounds comprising TOP / TBP and the like in quality. The method has very high application values in the laboratory field and the industrial production field.

Description

technical field [0001] The invention belongs to the technical field of synthesis of semiconductor nanocrystals, in particular to a new method for synthesizing semiconductor nanocrystals containing tellurium and selenium. Background technique [0002] Semiconductor nanoparticles, especially semiconductor nanoparticles containing tellurium, selenium or sulfur, are research hotspots in recent years. Semiconductor nanocrystals, also known as semiconductor quantum dots, have broad application prospects in optoelectronic devices, solar cells, and laser biomarkers due to their unique quantum size effects, dielectric confinement effects, and surface effects. Especially as the application in the fields of biomarkers and solar cells, it has attracted the attention of many scientific workers, and the research on its synthesis methods has also continued to deepen. In 2000, Peng et al. discovered a relatively cheap, inorganic, and relatively less toxic method to synthesize nanocrystals,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04C01B19/00B82Y30/00
Inventor 李林松申怀彬姜新东王素娟
Owner HENAN UNIVERSITY
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