CN1187267C - Process for preparing nano zinc oxide material - Google Patents
Process for preparing nano zinc oxide material Download PDFInfo
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- CN1187267C CN1187267C CNB031508642A CN03150864A CN1187267C CN 1187267 C CN1187267 C CN 1187267C CN B031508642 A CNB031508642 A CN B031508642A CN 03150864 A CN03150864 A CN 03150864A CN 1187267 C CN1187267 C CN 1187267C
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Abstract
The present invention discloses a process for preparing nanometer zinc oxide material, which is a precursor process by surface modification, namely that a micro amount of an anionic surfactant of sodium dodecyl sulfate (C12H25NaO4S) is added in a precursor composed of ammonium hydrogen carbonate and zinc chloride for the modification, and a loose filamentary precursor can be obtained; then, the filamentary precursor is calcined to obtain the nanometer zinc oxide material with good dispersibility and uniform linear distribution. Compared with the other existing methods for preparing the nanometer zinc oxide material, the present invention has the advantages of simple process, easy operation and low price, and the present invention is suitable for commercial process.
Description
Technical field
The present invention relates to the preparation method of semi-conductor low-dimension nano material, specifically be meant the preparation method of nano zinc oxide material.
Background technology
Zinc oxide (ZnO) is a kind of direct band gap broad stopband (Eg=3.37eV) semiconductor material, and bigger exciton bind energy (60meV) is arranged under the room temperature, and is bigger than the hot ionization energy of room temperature (26meV), thereby can guarantee that it at room temperature launches Ultra-Violet Laser.Therefore, compare with GaN (25meV) with other several broad stopbands luminescent material such as ZnSe (exciton bind energy 22meV), ZnS (40meV), ZnO is a kind of ultraviolet light emission material that is applicable under room temperature or the higher temperature, and has huge application potential, as blue light or ultraviolet light photo devices such as photodiode, laser diodes.
Compare with the body material, nano-ZnO has its special nature, because the size of material is little, specific surface area is big, surface key attitude is different with granule interior, the not congruent reason of surface atom coordination causes the activity site on surface to increase, and has formed scraggly atomic steps, strengthened the reaction contact surface, this makes nano zine oxide become a kind of up-and-coming catalyzer.Nano zine oxide also is one of a few oxide semiconductor of easily realizing quantum size effect, utilize its semiconductor property can make the discharge breakdown recording paper, it is unique material that can be luminous under the Low-voltage Electronic ray, be used for luminescent lamp can prolonging lamp tube work-ing life, utilize its piezoelectric property can make the piezoelectricity pronunciation and meaning, oscillator surface-duided wave filter etc.Nano zine oxide has also obtained widespread use in fields such as solar energy converting, varistor, pottery, gas sensor, stealth materials simultaneously.Therefore, present preparation about the nano-ZnO one-dimensional material has caused the great interest of people.
At present, the preparation method of nano ZnO material mainly contains template, gas-liquid-solid method, chemical Vapor deposition process (CVD) etc.Though these methods can obtain nano ZnO material good dispersity, purer since its to equipment and ingredient requirement height, yield poorly, therefore the production cost height is not suitable for suitability for industrialized production.
Summary of the invention
For solving the problem that exists among the existing nano ZnO material preparation method, it is low and to ingredient requirement preparation method not high, that be suitable for suitability for industrialized production to the objective of the invention is to propose a kind of production cost.
Preparation method of the present invention is the finishing precursor process, and this method is to prepare the wire presoma earlier, and then to wire presoma calcining, just can obtain good dispersity, linear distribution evenly and by the nano ZnO material of ball particle ordered arrangement.
We find to add the anionic (C of trace when the preparation presoma
12H
25NaO
4S) modify, the wire presoma that can obtain loosening, calcining wire presoma can obtain not only good dispersity, and the uniform nano-ZnO of linear distribution, all simpler, easy to operate and inexpensive than the existing method that other prepares nano ZnO material, be fit to suitability for industrialized production.
The preparation process of wire nano ZnO material is:
1. at room temperature, with chemical pure ammonium hydrogencarbonate (NH
4HCO
3) be dissolved in the distilled water, making its concentration is 1.6-2.4mol/L; Add anionic (C again
12H
25NaO
4S), making its concentration is 1 * 10
-4Mol/L; Under constantly stirring, slowly add analytical pure zinc chloride (ZnCl
2), making its concentration is 0.8-1.2mol/L, obtains white depositions at last.
With above-mentioned white depositions with the continuous filtering and washing of 95% ethanol three times, then throw out was toasted 3-4 hour in 40-60 ℃ of baking oven, desolvate to remove, obtain the wire presoma.
3. the wire presoma with oven dry places tube furnace, under the air atmosphere, tube furnace is warming up to 240-260 ℃, and the insulation calcining obtained the wire nano ZnO material in 0.81-1.2 hour.
The preparation process of cobblestone-appearance nano ZnO material is:
Repeat above-mentioned steps 1 and 2, obtain the wire presoma, the wire presoma of drying is placed tube furnace, under the air atmosphere, tube furnace is warming up to 580-620 ℃, be incubated 0.81-1.2 hour and can obtain the cobblestone-appearance nano ZnO material.
The nano zinc oxide material of the inventive method preparation has following advantage:
1. Zhi Bei nano material good dispersity, good uniformity, pattern is single, and crystallinity is good.
2. do not need complicated plant and instrument, save the energy, and cost is low, is easy to suitability for industrialized production.
Description of drawings
Fig. 1. the transmission electron microscope of wire zinc oxide precursor of the present invention (TEM) photo.
Fig. 2. the transmission electron microscope of wire nano zinc oxide material of the present invention (TEM) photo.
Fig. 3. the X-ray diffraction of wire nano zinc oxide material of the present invention (XRD) test result.
Fig. 4. the transmission electron microscope of cobblestone-appearance nano zine oxide of the present invention (TEM) photo.
Embodiment
Below we are further described the present invention by embodiment:
1. clean used vessel:
The beaker that the preparation material is used, graduated cylinder, glass stick, volumetric flask, porcelain boat etc. clean once with dilute hydrochloric acid earlier, then with the tap water flushing, again with distillation washing 3 times.Washed vessel are standby after 4 hours in baking under 50 ℃ the temperature.
2. the preparation of presoma
At room temperature, with chemical pure ammonium hydrogencarbonate (NH
4HCO
3) 8.0 the gram be dissolved in 100 ml distilled waters, add 5 milliliter 1 * 10
-4Anionic (the C of mol/L
12H
25NaO
4S) aqueous solution slowly adds 6.84 gram zinc chloride (ZnCl then under constantly stirring
2), obtain white depositions.
Use 95% ethanol to above-mentioned white depositions filtering and washing three times then, the white depositions after the filtering and washing is placed 40-60 ℃ baking oven baking 3-4 hour, obtain the wire presoma, see Fig. 1.
3. the preparation of wire nano zinc oxide material
Get a certain amount of wire presoma and put into the porcelain boat that had cleaned and dried, place tube furnace, under air atmosphere, tube furnace is warming up to 250 ℃, the insulation calcining is 1 hour then, obtains the wire nano zinc oxide material, sees Fig. 2.Wire nano zinc oxide material orientation of the present invention is along [101] direction, sees Fig. 3.
Fig. 4 is incubated the cobblestone-appearance nano zinc oxide material that obtains after 1 hour for the tube furnace temperature is increased to 600 ℃.
Claims (1)
1. the preparation method of a nano zinc oxide material is characterized in that this preparation method in turn includes the following steps:
A. at room temperature, with chemical pure ammonium hydrogencarbonate (NH
4HCO
3) be dissolved in the distilled water, making its concentration is 1.6-2.4mol/L; Add anionic (C again
12H
25NaO
4S), making its concentration is 1 * 10
-4Mol/L; Under constantly stirring, slowly add analytical pure zinc chloride (ZnCl
2), making its concentration is 0.8-1.2mol/L, obtains white depositions at last;
B. with above-mentioned white depositions with the continuous filtering and washing of 95% ethanol three times, then throw out was placed in the 40-60 ℃ of baking oven baking 3-4 hour, desolvate to remove, obtain the wire presoma;
C. the wire presoma with oven dry places tube furnace, under air atmosphere, tube furnace is warming up to 240-260 ℃, and the insulation calcining obtained the wire nano zine oxide in 0.8-1.2 hour;
D. after A, B step, the wire presoma of drying is placed tube furnace, under air atmosphere, tube furnace is warming up to 580-682 ℃, be incubated 0.8-1.2 hour and can obtain the cobblestone-appearance nano zine oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031508642A CN1187267C (en) | 2003-09-09 | 2003-09-09 | Process for preparing nano zinc oxide material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031508642A CN1187267C (en) | 2003-09-09 | 2003-09-09 | Process for preparing nano zinc oxide material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1491895A CN1491895A (en) | 2004-04-28 |
| CN1187267C true CN1187267C (en) | 2005-02-02 |
Family
ID=34240650
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031508642A Expired - Fee Related CN1187267C (en) | 2003-09-09 | 2003-09-09 | Process for preparing nano zinc oxide material |
Country Status (1)
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301217C (en) * | 2004-11-03 | 2007-02-21 | 西北工业大学 | Method for chemically preparing zinc oxide nanometer rod using low temperature wet method |
| CN105236467B (en) * | 2014-08-01 | 2017-06-16 | 阜阳师范学院 | A kind of a large amount of technique and its applications for preparing nano zine oxide |
| CN104118898B (en) * | 2014-08-14 | 2015-07-08 | 安徽工业大学 | Preparation method of zinc carbonate nanoneedle |
| CN104355331A (en) * | 2014-10-28 | 2015-02-18 | 常州市创捷防雷电子有限公司 | Biological environment-friendly method for preparing mono-dispersed nano-zinc oxide |
| CN105566681B (en) * | 2015-12-22 | 2018-03-16 | 贵州金马包装材料有限公司 | A kind of auxiliary agent for lifting compound art post paperboard printing performance and preparation method thereof |
| CN108226233B (en) * | 2018-01-08 | 2020-01-31 | 中国工程物理研究院化工材料研究所 | Hierarchical ZnO @ ZnO nanocomposite gas-sensitive material and preparation method thereof |
| CN108864764A (en) * | 2018-06-15 | 2018-11-23 | 安徽艾米伦特建材科技有限公司 | Modified material and preparation method thereof for water-repellent paint |
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2003
- 2003-09-09 CN CNB031508642A patent/CN1187267C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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