Method for preparing zinc blende nano particle and zinc blende nano particle prepared thereby

A technology of nano-particles and zinc sulfide, applied in the direction of zinc sulfide, nanostructure manufacturing, nanotechnology, etc., can solve the problems of easy oxidation of sulfide, unreachable samples, and easy occurrence of danger, etc., and achieve low reaction temperature and no pollution Effect

Inactive Publication Date: 2008-08-27
CHINA BUILDING MATERIALS ACAD
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Problems solved by technology

Existing high-temperature solid-phase method (Tsuzuki T, Ding J, McCormick P G. "Mechanochemical synthesis of ultrafine zinc sulfide partiales". PhysicaB, 1997, 239: 378) and precipitation method (R.Vacassy, ​​S.M.Scholz, et al. , "Synthesis of controlledspherical zinc sulfide particles by precipitation from homogeneous solutions" J.Am.Ceram.Soc.81(1998) 2699) method for preparing ZnS particles, but because sulfides are relatively easy to oxidize, traditional high-temperature solid-phase methods often use Inert atmosphere or reducing atmosphere is used for protection, which not only consumes a lot of energy but is also prone to danger, and the samples prepared by direct precipitation method cannot reach the nanometer level

Method used

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  • Method for preparing zinc blende nano particle and zinc blende nano particle prepared thereby
  • Method for preparing zinc blende nano particle and zinc blende nano particle prepared thereby
  • Method for preparing zinc blende nano particle and zinc blende nano particle prepared thereby

Examples

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preparation example Construction

[0022] (1) Preparation of ZnS precursor:

[0023] Select the microemulsion system of CTAB / n-butanol / cyclohexane / water, cyclohexane is the oil phase, CTAB (cetyltrimethylammonium bromide) is the surfactant, and n-butanol is the co-surfactant agent, Zn(NO 3 ) 2 ·6H 2 O solution and Na 2 S·9H 2 The O solution is the aqueous phase. Two microemulsions, I and II, need to be configured during the test. The aqueous phase in microemulsion I was 0.5M Zn(NO 3 ) 2 ·6H 2 O solution, the aqueous phase in microemulsion II is 0.5M Na 2 S solution. 2g CTAB, 20ml cyclohexane and 4ml n-butanol were mixed and dissolved. Under constant stirring, slowly add 2.4ml of 0.5M Zn(NO 3 ) 2 ·6H 2 O solution, to ensure that the system is in a transparent state without delamination, to obtain microemulsion I. Microemulsion II differs in that 0.5M Na 2 S solution replaced 0.5M Zn(NO 3 ) 2 ·6H 2 O solution. The two transparent and stable microemulsions I and II were quickly mixed and stirre...

Embodiment 1

[0026] Example 1 : Preparation of ZnS powder

[0027] Preparation of ZnS precursor: Mix 2g CTAB, 20ml cyclohexane and 4ml n-butanol to dissolve CTAB to form an oil phase solution. Slowly add 2.4ml of 0.5M Zn(NO 3 ) 2 ·6H 2 O solution to obtain microemulsion I. Similarly, slowly add 2.4ml of 0.5M Na to the oil phase solution 2S solution to obtain microemulsion II. The microemulsion I and microemulsion II were rapidly mixed and stirred continuously for 30 minutes to obtain an emulsion containing a white precipitate. Let it stand at room temperature for 12h, then add the demulsifier acetone and separate the precipitate with a centrifuge. The precipitate was washed 5 times with acetone, 3 times with ethanol, and 3 times with deionized water, and then dried at room temperature to obtain the ZnS precursor.

[0028] Hydrothermal reaction: move the prepared ZnS precursor into a 100ml polytetrafluoroethylene-lined autoclave, add distilled water to 70% of the volume of the auto...

Embodiment 2

[0031] Example 2 : Preparation of ZnS powder

[0032] The ZnS precursor was prepared by the same method as in Example 1.

[0033] Hydrothermal reaction: move the prepared ZnS precursor into a 100ml polytetrafluoroethylene-lined autoclave, add distilled water to 70% of the volume of the autoclave, seal it, and react at a hydrothermal temperature of 160°C for 12 hours. After washing with distilled water for 3 times and absolute ethanol for 3 times, dry in a vacuum oven at 60°C for 6 hours to obtain a powder which is the product.

[0034] Identification: The product is identified as cubic phase ZnS by X-ray diffraction (XRD), such as image 3 (b) shown. The transmission electron microscope observation shows that the product is composed of uniformly dispersed spherical particles with an average size of 5 nm, such as figure 1 (b) shown.

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Abstract

Disclosed is a preparing process for zinc sulfide nanometer particles, which comprises steps that a hydrothermal synthesis process is employed, Zn (NO3) 2, 6H2O and Na2S, 9H2O are selected as reaction materials and H2O is used as hydrothermal reaction medium. The process selects microemulsion systems of CTAB / n-butanol / cyclohexane / water to be a zinc sulfide precursor, thereby obtaining the zinc sulfide nanometer particles in hydrothermal reaction in 8-16 hours under the temperature of 120 DGE C-200 DGE C. The preparing process is capable of obtaining the zinc sulfide nanometer particles with sizes of 5-20 nm in adequate distribution and can be used for substrates of light emitting materials.

Description

Technical field: [0001] The invention relates to the field of chemical synthesis, in particular to a novel preparation method of zinc sulfide nanoparticles. Background technique: [0002] ZnS is one of the best hosts for electroluminescent materials so far, and it is used in many fields, such as: plasma and electroluminescence, flat panel display (such as field emission display), cathode ray tube (for radar, TV and oscilloscope) materials . In addition, it is also used in sensors, X-ray fluorescence detection, and can also be used to make photoelectric (solar) sensitive components, nanomaterial laser production and photoelectric identification marks for special wavelength control. The excellent performance of ZnS has attracted more and more attention from material scientists, and people have been exploring synthetic methods to control the size and shape of particles. Existing high-temperature solid-phase method (Tsuzuki T, Ding J, McCormick P G. "Mechanochemical synthesis ...

Claims

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Application Information

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IPC IPC(8): C01G9/08B82B3/00
Inventor 马峻峰刘俊林波涛任仰姜晓辉孙勇刘振森
Owner CHINA BUILDING MATERIALS ACAD
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