CN100372775C - Process for preparing uni-dimensional zinc oxide nano-materials - Google Patents
Process for preparing uni-dimensional zinc oxide nano-materials Download PDFInfo
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- CN100372775C CN100372775C CNB2005100763263A CN200510076326A CN100372775C CN 100372775 C CN100372775 C CN 100372775C CN B2005100763263 A CNB2005100763263 A CN B2005100763263A CN 200510076326 A CN200510076326 A CN 200510076326A CN 100372775 C CN100372775 C CN 100372775C
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- dimensional nanomaterial
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Abstract
The present invention relates to a method for preparing one-dimensional zinc oxide nanometer materials, which is characterized in that the preparing method comprises the following steps: step 1, inorganic zincate and sodium sulfide with the same mole are respectively added in water/ alcohol binary solution to be stirred to form homogeneous solution; step 2, the sodium sulfide is added drop by drop in the inorganic zincate solution to react for forming zinc sulfide deposit; step 3, the produced deposit is respectively washed with ionized water and organic alcohol, and then is dried; step 4, the dried zinc sulfide is oxidized to obtain the one-dimensional zinc oxide nanometer materials.
Description
Technical field
The present invention relates to a kind of preparation of nanomaterials, particularly relate to a kind of method for preparing zinc oxide one-dimensional nanomaterial by oxidation presoma zinc sulphide.
Background technology
ZnO is a kind of important II-VI family broad stopband, direct band-gap semicondictor material, energy gap is 3.37eV under the room temperature, exciton bind energy is 60meV, be considered to another novel photoelectric material after ZnSe, GaN, can be applicable to fields such as short wavelength laser, ultraviolet detector, photodiode, solar cell, field-effect transistor, chemical sensor.
Monodimension nanometer material is meant that current carrier only can free movement in a direction, at the then bound material system of two other direction.In recent years, monodimension nanometer material is one of field, forward position comparatively active in the nano science research always, major cause is that it has peculiar structure, physics and chemical property, this not only provides valuable research object for fundamental research, also aspect the structure nano-device extremely important status is being arranged.At present, the research of Application and Development ZnO monodimension nanometer material has been subjected to paying close attention to widely.The method for preparing the ZnO monodimension nanometer material is a lot, mainly comprises molecular beam epitaxy, organic chemical vapor deposition, template etc.Yet, high, the complicated operation of condition harshness, equipment price that these methods adopted.
Summary of the invention
Deficiency at existing preparation method exists the object of the present invention is to provide a kind of method for preparing zinc oxide one-dimensional nanomaterial, has characteristics such as cost is low, simple to operate, suitability is extensive.
A kind of method for preparing zinc oxide one-dimensional nanomaterial of the present invention is characterized in that its preparation method is as follows:
(1) equimolar inorganic zinc salt and sodium sulphite are joined respectively in the binary solution of water/alcohol, stir and form homogeneous solution;
(2) under agitation condition, sodium sulfide solution is dropwise joined in the inorganic zinc salt solution, reaction forms the zinc sulphide precipitation;
(3) precipitation that will generate spends ionized water and organic alcohol washing, drying respectively;
(4), obtain zinc oxide one-dimensional nanomaterial with dried zinc sulphide oxidation.
Wherein said exsiccant temperature is 50～100 ℃.
The temperature of wherein said zinc sulphide oxidation is 700～900 ℃.
The time of wherein said zinc sulphide oxidation is 1～3 hour.
Wherein inorganic zinc salt comprises zinc chloride, zinc nitrate and zinc acetate, and alcohol comprises methyl alcohol and ethanol.
Wherein the ratio of water/pure mixed solvent is 0.4～1.
It is raw material that the present invention adopts cheap inorganic zinc salt, sodium sulphite, adopts simple experimental apparatus, prepared zinc oxide one-dimensional nanomaterial, so the present invention has characteristics such as cost is low, simple to operate, suitability is extensive.
Description of drawings
Fig. 1 is the comparison diagram of the X-ray powder diffraction of prepared zinc sulphide presoma of the present invention and zinc oxide one-dimensional nanomaterial.
Embodiment
A kind of method for preparing zinc oxide one-dimensional nanomaterial of the present invention, its preparation method is as follows:
(1) equimolar inorganic zinc salt and sodium sulphite are joined respectively in the binary solution of water/alcohol, stir and form homogeneous solution, wherein inorganic zinc salt comprises zinc chloride, zinc nitrate and zinc acetate, and alcohol comprises methyl alcohol and ethanol; Wherein the ratio of water/pure mixed solvent is 0.4～1;
(2) under agitation condition, sodium sulfide solution is dropwise joined in the inorganic zinc salt solution, reaction forms the zinc sulphide precipitation;
(3) precipitation that will generate spends ionized water and organic alcohol washing, drying respectively; Described exsiccant temperature is 50～100 ℃;
(4), obtain zinc oxide one-dimensional nanomaterial with dried zinc sulphide oxidation; The temperature that described zinc sulphide oxidation is done is 700～900 ℃; The time of described zinc sulphide oxidation is 1～3 hour.
Above-mentioned reaction is expressed as follows with chemical equation:
Zn
2++S
2-＝ZnS↓
2ZnS+3O
2＝2ZnO＋2SO
2↑
Embodiment
Below for adopting the inventive method to prepare the example of zinc oxide one-dimensional nanomaterial.
The inorganic zinc salt that is adopted comprises zinc chloride, zinc nitrate, zinc acetate etc., and the concentration of inorganic zinc salt and sodium sulfide solution is controlled at 0.05～0.1mol/l.
Take by weighing 0.9g analytical pure zinc acetate and place the binary solution of water/methyl alcohol, stir and form homogeneous solution.Take by weighing 0.4g analytical pure sodium sulphite and place the binary solution of another water/methyl alcohol, stir and form homogeneous solution.Sodium sulfide solution is dropwise joined in the zinc acetate solution, form the zinc sulphide precipitation of white.To precipitate and spend ionized water and methanol wash respectively, and place baking oven dry down then in 50 ℃.Zinc sulphide after the oven dry is put into box-type furnace, and heating is 1 hour under 700 ℃, in the air atmosphere, naturally cools to room temperature then.Shown in accompanying drawing 1b, after 700 ℃ of oxidations, zinc sulphide presoma complete oxidation is a zinc oxide.The TEM transmission electron microscope detects the zinc oxide pattern: diameter is that 30～80 nanometers, length are that 0.2～0.5 micron, two ends only are several nanometers.Single nano zine oxide electron diffraction proof product is a monocrystalline.Under the same conditions, temperature of reaction is controlled at 800,900 ℃, will be controlled in the reaction times 2,3 hours, inorganic zinc salt adopts zinc chloride or zinc nitrate, all can obtain zinc oxide one-dimensional nanomaterial.
By conditioned reaction temperature and reaction times, can prepare the zinc oxide one-dimensional nanomaterial of different length-to-diameter ratios.
Claims (6)
1. method for preparing zinc oxide one-dimensional nanomaterial is characterized in that its preparation method is as follows:
(1) equimolar inorganic zinc salt and sodium sulphite are joined respectively in the binary solution of water/alcohol, stir and form homogeneous solution;
(2) under agitation condition, sodium sulfide solution is dropwise joined in the inorganic zinc salt solution, reaction forms the zinc sulphide precipitation;
(3) precipitation that will generate spends ionized water and alcohol washing, drying respectively;
(4), obtain zinc oxide one-dimensional nanomaterial with dried zinc sulphide oxidation.
2. the preparation method of zinc oxide one-dimensional nanomaterial as claimed in claim 1 is characterized in that, wherein said exsiccant temperature is 50～100 ℃.
3. the preparation method of zinc oxide one-dimensional nanomaterial as claimed in claim 1 is characterized in that, the temperature of wherein said zinc sulphide oxidation is 700～900 ℃.
4. the preparation method of zinc oxide one-dimensional nanomaterial as claimed in claim 1 is characterized in that, the time of wherein said zinc sulphide oxidation is 1～3 hour.
5. the preparation method of zinc oxide one-dimensional nanomaterial as claimed in claim 1 is characterized in that, wherein inorganic zinc salt comprises zinc chloride, zinc nitrate and zinc acetate, and alcohol comprises methyl alcohol and ethanol.
6. the preparation method of zinc oxide one-dimensional nanomaterial as claimed in claim 1 is characterized in that, wherein the ratio of water/pure mixed solvent is 0.4～1.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100763263A CN100372775C (en) | 2005-06-14 | 2005-06-14 | Process for preparing uni-dimensional zinc oxide nano-materials |
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| CNB2005100763263A CN100372775C (en) | 2005-06-14 | 2005-06-14 | Process for preparing uni-dimensional zinc oxide nano-materials |
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| CN1880227A CN1880227A (en) | 2006-12-20 |
| CN100372775C true CN100372775C (en) | 2008-03-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104437072B (en) * | 2014-11-21 | 2016-03-16 | 太原理工大学 | A kind of preparation method of middle desulfurizing agent for high-temp gas |
| CN106830921B (en) * | 2017-01-23 | 2019-11-15 | 九江学院 | A kind of ZnO transparent ceramics and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462258A (en) * | 2001-05-08 | 2003-12-17 | Lg化学株式会社 | Method for preparing single crystalline ZnS powder for phosphor |
| US6710091B1 (en) * | 1999-02-23 | 2004-03-23 | Bayer Aktiengesellschaft | Nanoparticulate, redispersible zinc oxide gels |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6710091B1 (en) * | 1999-02-23 | 2004-03-23 | Bayer Aktiengesellschaft | Nanoparticulate, redispersible zinc oxide gels |
| CN1462258A (en) * | 2001-05-08 | 2003-12-17 | Lg化学株式会社 | Method for preparing single crystalline ZnS powder for phosphor |
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