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Synthesis of nano hollow balls of zinc selenide

A synthesis method, zinc selenide technology, applied in chemical instruments and methods, binary selenium/tellurium compounds, zinc compounds, etc., can solve the problem of micron-scale ZnSe hollow spheres that cannot be synthesized, and micron-sized hollow particles that cannot be synthesized with zinc selenide Balls, unable to be further assembled into photonic crystals, etc., to achieve the effects of easy control, cheap raw materials, and stable product quality

Inactive Publication Date: 2003-06-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the traditional synthesis methods and the methods reported in the literature cannot synthesize micron-scale ZnSe hollow spheres, so that they cannot be further assembled into structural materials such as photonic crystals, which limits the application of zinc selenide.
Such as, Holland "Materials Chemistry and Physics" (Materials Chemistry and Physics) 1999 60 volumes 99 pages have reported to react the zinc selenide of particle shape with element selenium and element zinc in alkaline solution; British "Chemical Communications" (Chemical Communications) ) 14 volumes 1243 pages in 2000 reported the metal organic compound of zinc as a precursor to synthesize the nanoparticles of zinc selenide; A method for synthesizing monodisperse zinc selenide nanoparticles with organic compounds as precursors, the method is expensive in raw materials and complicated in operation
Other methods include synthesizing zinc selenide nanoparticles in the microemulsion system through reverse micelles, and using molecular beam epitaxy to grow zinc selenide films, but none of them can synthesize micron hollow spheres of zinc selenide

Method used

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  • Synthesis of nano hollow balls of zinc selenide
  • Synthesis of nano hollow balls of zinc selenide
  • Synthesis of nano hollow balls of zinc selenide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Weigh 0.002 mole of analytical pure ZnSO 4 ·7H 2 O is placed in a 40 ml reaction kettle, add 20 ml of 1M NaOH solution to dissolve it, add equimolar amount of sodium selenite and 1 times molar excess of hydrazine hydrate into this reaction kettle, add deionized water to the total volume 70%, seal the reactor, and react at 100°C for 2 hours. Then it was cooled to room temperature, the reaction kettle was opened, filtered with a cloth funnel, washed with deionized water, and a yellow powder was obtained. The product was identified as zinc selenide by X-ray powder diffraction, and it was identified as a micron-level zinc selenide ball by scanning electron microscopy, with a diameter of about 3 microns (attached figure 2 ). After grinding the zinc selenide ball, it was identified with a scanning electron microscope, and it was found that the ball has a hollow structure (attached Figure 4 ).

[0050] Under the same conditions, replace hydrazine hydrate with a molar excess of 5...

Embodiment 2

[0052] Weigh 0.003 moles of analytical pure ZnCl 2 Placed in a 40 ml reaction kettle, add 20 ml of 2M NaOH solution to dissolve, and the AgNO 3 Add it to the solution at the ratio of Zn:Ag=100:5, and add it with ZnCl 2 And 1 / 2 times AgNO 3 The sum of moles of ammonium selenite, 2 times excess of hydrazine sulfate, and finally add deionized water to 70% of the total volume, seal the reactor and react at 120°C for 4 hours to prepare a Zn:Ag ratio of 100:5 Ag doped composite zinc selenide micron hollow spheres.

[0053] Under the same conditions, replace hydrazine hydrate with sodium borohydride, potassium borohydride, hydroxylamine or hydrazine sulfate, and control the reaction temperature at 100, 150, 200℃, and adjust the reaction time to 48, 32, 16, 8, 2 hours , Can get micron-sized Ag-doped zinc selenide hollow spheres.

Embodiment 3

[0055] Weigh 0.002 mole analytically pure Zn (NO 3 ) 2 Placed in a 40 ml reaction kettle, add 20 ml of 1M KOH solution to dissolve, and MnSO 4 Add it to the solution at the ratio of Zn:Ni=100:10, and add it with Zn(NO 3 ) 2 And NiSO 4 The sum of the molar amount of selenous acid, the excess of sodium borohydride 4 times, and finally add deionized water to 70% of the total volume, seal the reactor, and react at 160°C for 32 hours to prepare a Zn:Ni ratio of 100:10 Ni-doped composite zinc selenide micron hollow sphere (attached Figure 5 ).

[0056] Under the same conditions, replace hydrazine hydrate with sodium borohydride, potassium borohydride, hydroxylamine or hydrazine sulfate, control the reaction temperature at 100, 140, 200℃, and adjust the reaction time to 48, 32, 16, 8, 4 hours , Can get micron-scale Ni-doped zinc selenide hollow spheres.

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Abstract

A process for synthesizing a micro-class hollow zinc selenide sphere features that hydrothermal reduction reaction between zincic acid radical ions and seleninic acid or soluble selerate under action of hydrazine hydrate as reducer in strong alkaline condition at 100-200 deg.C in a sealed reaction. It is possible to dope it or coat it. Its advantages are low cost and high quality.

Description

Technical field [0001] The invention relates to the synthesis of micron-sized ZnSe hollow spheres and their internal doping (including manganese, iron, cobalt, nickel, copper, silver, cadmium, tin, antimony, lead, and bismuth) and surface coating (including manganese, The process method of iron, cobalt, nickel, copper, silver, cadmium, tin, antimony, lead, bismuth oxide, sulfide, selenide) belongs to the technical field of inorganic material preparation technology. Background technique [0002] Zinc selenide is an important semiconductor material with special optical and electrical properties, and has a wide range of applications in blue lasers, solar cells and other fields. At present, traditional synthesis methods and methods reported in the literature are unable to synthesize micron-sized ZnSe hollow spheres, and thus cannot be further assembled into structural materials such as photonic crystals, which limits the application of zinc selenide. For example, the Netherlands "Mat...

Claims

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Application Information

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IPC IPC(8): C01B19/04C01G9/00
Inventor 李亚栋彭卿董亚杰
Owner TSINGHUA UNIV
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