CN103991896A - Spherical zinc oxide nanometer material preparation method - Google Patents
Spherical zinc oxide nanometer material preparation method Download PDFInfo
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- CN103991896A CN103991896A CN201410137792.7A CN201410137792A CN103991896A CN 103991896 A CN103991896 A CN 103991896A CN 201410137792 A CN201410137792 A CN 201410137792A CN 103991896 A CN103991896 A CN 103991896A
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Abstract
The present invention discloses a spherical zinc oxide nanometer material preparation method, which comprises: dissolving zinc nitrate and hexamethylenetetramine in water, adding citric acid, adjusting the pH value of the solution to 6.0-7.0, carrying out a reaction at a temperature of 80-100 DEG C, filtering, washing, and drying to obtain the finished product. According to the method, the concentration of the citric acid is changed so as to achieve effective regulation of the zinc oxide morphology, and characteristics of mild condition, easily available raw material, simple equipment, simple process, low cost, high product purity, and good product dispersity are provided.
Description
Technical field
The present invention relates to a kind of preparation method of spherical nano zinc oxide material, belong to nano material preparing technical field.
Background technology
ZnO is a kind of important II-IV family direct band gap semiconductor material with wide forbidden band, under room temperature, can band gap be 3.37eV, is the focus of shortwave semiconductor laser device investigation of materials after GaN.And in the time that its size reaches nanometer scale, compared with common ZnO, nano-ZnO shows many excellences and special performance, as piezoelectric property, luminescence, transparent conductivity, biological safety and adaptability etc., make it gather around and have broad application prospects in fields such as piezoelectric, ultraviolet light detector, field effect transistor, surface acoustic wave, solar cell, gas sensor, biosensors.The preparation method of ZnO nano powder is study hotspot always, and the Preparation and characterization of the ZnO nano-structure of various patterns, dimension receives much attention.Traditional solid phase method needs complex apparatus, harsh preparation condition, and liquid phase synthetic be a kind of method of simple, quick, economic nano materials.Conventionally the chemical process of preparing nano-ZnO has the precipitator method, sol-gel method, water (solvent) Re Fa and microemulsion method etc.Hydro-thermal, solvent-thermal method reaction conditions be relatively gentle, be easy to amplify, and pollutes littlely, and solvent-thermal method needs a large amount of organic chemical reagents.Liquid phase method temperature of reaction taking water as solvent is low, reaction conditions is easy to control, gained powder purity is high, particle diameter is little, good uniformity, in actually operating, is widely used.
Summary of the invention
The object of this invention is to provide that a kind of pattern is controlled, the preparation method of the spherical nano zinc oxide material of good uniformity, good dispersity.
Implementation procedure of the present invention is as follows:
A preparation method for spherical zinc oxide, comprises the following steps:
(1) zinc nitrate and the hexamethylenetetramine that are 1:1 by mol ratio are water-soluble;
(2) in above-mentioned mixing solutions, add citric acid, wherein the mass percent concentration of citric acid is 0.25 ~ 0.5%, regulator solution pH value 6.0 ~ 7.0, and reaction at 80～100 DEG C, obtains spherical zinc oxide through washing, being dried.
In above-mentioned steps (1), the volumetric molar concentration of zinc nitrate and hexamethylenetetramine is 0.1 ~ 0.2mol/L.
In above-mentioned steps (2), the mass percent concentration of citric acid is 0.25 ~ 0.35%, adopts sodium hydroxide or potassium hydroxide regulator solution pH value.
Advantage of the present invention and positively effect:
can realize the preparation of spherical ZnO nano material by changing citric acid concentration, method is simple;
spherical ZnO nano material purity prepared by the present invention is high, good dispersity;
temperature of reaction is low, has reduced energy consumption and production cost;
making water is solvent, and nontoxic citric acid is tensio-active agent, environmental friendliness, production safety, and operating environment requires simple;
raw material is easy to get, equipment is simple, technique is succinct, with low cost, be easy to suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the XRD figure spectrum of the sample prepared of embodiment 1;
Fig. 2 is the EDS collection of illustrative plates of the sample prepared of embodiment 2;
Fig. 3 is the EDS collection of illustrative plates of the sample prepared of embodiment 3;
Fig. 4 is the XRD figure spectrum of the sample prepared of embodiment 4;
Fig. 5 is the SEM figure of the sample of embodiment 1,2,3,4 preparations.
Embodiment
Describe by the following examples implementation procedure of the present invention in detail.The phase composite of the zinc oxide nano-powder preparing adopts the analysis of the D/MAX-3CX of Rigaku company diffractometer, and its microscopic appearance is by the JSM-6700F of NEC company type scanning electron microscopic observation.
Embodiment 1
Take 1.4g hexamethylenetetramine (CH
2)
6n
4with 2.9g Zn (NO
3)
26H
2o is dissolved in 100mL deionized water, regulates at 6.5,90 DEG C of pH values and reacts and obtain zinc oxide nano-powder in 2 hours with sodium hydroxide, is designated as sample 1, and its powder diagram is shown in Fig. 1, and stereoscan photograph is shown in Fig. 5.
Embodiment 2
Similar to Example 1, difference is, in the mixing solutions of hexamethylenetetramine and zinc nitrate, has added 0.1g citric acid, regulate pH value 6.2,90 DEG C of reactions to obtain zinc oxide nano-powder in 2 hours with sodium hydroxide, be designated as sample 2, Fig. 2 is shown in by its EDS collection of illustrative plates, and stereoscan photograph is shown in Fig. 5.
Embodiment 3
Similar to Example 2, difference is that the add-on of citric acid is 0.2g, and gained Zinc oxide powder is designated as sample 3, and Fig. 3 is shown in by its EDS collection of illustrative plates, and stereoscan photograph is shown in Fig. 5.
Embodiment 4
Similar to Example 3, difference is that the add-on of citric acid is 0.3g, and gained Zinc oxide powder is designated as sample 4, and its powder diagram is shown in Fig. 4, and stereoscan photograph is shown in Fig. 5.
Can find out from Fig. 1,4, all diffraction peaks in figure are consistent with all diffraction peaks on the standard card of zinc oxide (JPCDS 16-3451), prove that product is zinc oxide.In Fig. 1, diffraction peak intensity is high, and peak shape is sharp-pointed, is typical wurtzite.In Fig. 4, the diffraction peak intensity of 101 crystal faces reduces, and 100 and 110 crystal faces occur splitting point, illustrate that citric acid can effectively limit the longitudinal growth of zinc oxide.Can find out from the EDS collection of illustrative plates of Fig. 2 and Fig. 3, the composition of sample 2 and sample 3 only has O and Zn element, illustrates that product is zinc oxide.Can find out from the SEM photo of Fig. 5, without citric acid in the situation that, the ZnO nano material of gained grows into hexa-prism, is typical wurtzite; Add after citric acid, the pattern of ZnO changes, and when the massfraction concentration of citric acid solution is 0.1%, has occurred the ZnO of laminated structure, when the massfraction concentration of citric acid is increased to 0.2%, has occurred spherical ZnO structure in product.In the time that the massfraction concentration of citric acid reaches 0.3%, the zinc oxide in product all forms ball-like structure.Through experiment repeatedly, find the pattern of the concentration affects product of citric acid, in the time that its mass percent concentration is 0.25～0.5%, can obtain ball-like structure.
Claims (4)
1. a preparation method for spherical zinc oxide, is characterized in that comprising the following steps:
(1) zinc nitrate and the hexamethylenetetramine that are 1:1 by mol ratio are water-soluble;
(2) in above-mentioned mixing solutions, add citric acid, wherein the mass percent concentration of citric acid is 0.25 ~ 0.5%, regulator solution pH value 6.0 ~ 7.0, and reaction at 80～100 DEG C, obtains spherical zinc oxide through washing, being dried.
2. the preparation method of spherical zinc oxide according to claim 1, is characterized in that: in step (1), the volumetric molar concentration of zinc nitrate and hexamethylenetetramine is 0.1 ~ 0.2mol/L.
3. the preparation method of spherical zinc oxide according to claim 1, is characterized in that: in step (2), the mass percent concentration of citric acid is 0.25 ~ 0.35%.
4. the preparation method of spherical zinc oxide according to claim 1, is characterized in that: in step (2), adopt sodium hydroxide or potassium hydroxide regulator solution pH value.
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| CN201410137792.7A CN103991896A (en) | 2014-04-08 | 2014-04-08 | Spherical zinc oxide nanometer material preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036177A (en) * | 2015-07-20 | 2015-11-11 | 苏州宇希新材料科技有限公司 | Preparation method of nano-zinc oxide |
| CN107256811A (en) * | 2017-07-03 | 2017-10-17 | 武汉纽赛儿科技股份有限公司 | The synthetic method of nitrogen-doped carbon coating zinc oxide and its application |
| CN109939267A (en) * | 2019-04-04 | 2019-06-28 | 南昌大学 | A kind of antimicrobial form catheter polymer composite and preparation method thereof |
| KR101994980B1 (en) * | 2018-12-27 | 2019-07-01 | 주식회사 엘에스켐코리아 | A spherical zink oxide powder coated with natural materials, manufacturing method thereof and cosmetic comprising the same |
| CN110240192A (en) * | 2019-07-09 | 2019-09-17 | 常熟理工学院 | A kind of preparation method of the zinc oxide nanosphere of Superhydrophilic |
| CN111733591A (en) * | 2020-06-24 | 2020-10-02 | 上海工程技术大学 | Method for controlling growth of spherical zinc oxide on modified polyester fabric |
| CN115058894A (en) * | 2022-08-17 | 2022-09-16 | 江苏金呢工程织物股份有限公司 | Hydrolysis-resistant textile auxiliary for drying net |
-
2014
- 2014-04-08 CN CN201410137792.7A patent/CN103991896A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036177A (en) * | 2015-07-20 | 2015-11-11 | 苏州宇希新材料科技有限公司 | Preparation method of nano-zinc oxide |
| CN107256811A (en) * | 2017-07-03 | 2017-10-17 | 武汉纽赛儿科技股份有限公司 | The synthetic method of nitrogen-doped carbon coating zinc oxide and its application |
| KR101994980B1 (en) * | 2018-12-27 | 2019-07-01 | 주식회사 엘에스켐코리아 | A spherical zink oxide powder coated with natural materials, manufacturing method thereof and cosmetic comprising the same |
| CN109939267A (en) * | 2019-04-04 | 2019-06-28 | 南昌大学 | A kind of antimicrobial form catheter polymer composite and preparation method thereof |
| CN110240192A (en) * | 2019-07-09 | 2019-09-17 | 常熟理工学院 | A kind of preparation method of the zinc oxide nanosphere of Superhydrophilic |
| CN110240192B (en) * | 2019-07-09 | 2022-02-11 | 常熟理工学院 | Preparation method of super-hydrophilic zinc oxide nanospheres |
| CN111733591A (en) * | 2020-06-24 | 2020-10-02 | 上海工程技术大学 | Method for controlling growth of spherical zinc oxide on modified polyester fabric |
| CN115058894A (en) * | 2022-08-17 | 2022-09-16 | 江苏金呢工程织物股份有限公司 | Hydrolysis-resistant textile auxiliary for drying net |
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Application publication date: 20140820 |