CN109987623A - A kind of preparation method of six arris platform zinc oxide - Google Patents
A kind of preparation method of six arris platform zinc oxide Download PDFInfo
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- CN109987623A CN109987623A CN201910313396.8A CN201910313396A CN109987623A CN 109987623 A CN109987623 A CN 109987623A CN 201910313396 A CN201910313396 A CN 201910313396A CN 109987623 A CN109987623 A CN 109987623A
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- zinc oxide
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- ethylene glycol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The invention discloses a kind of preparation method of six arris platform zinc oxide, preparation process are as follows: 1) take the deionized water and ethylene glycol solution of certain volume, be configured to mixed solution after ultrasonic disperse；2) zinc oxide precursor and pattern controlling agent are sequentially added in above-mentioned mixed solution, ultrasonic dissolution；3) mixed liquor is transferred in water heating kettle, a period of time is reacted under high temperature；4) ethanol washing after filtering, high temperature drying；5) finally, the product after drying is carried out high-temperature calcination, it is hexaplanar zincite crystal that comparison zinc oxide X-ray diffraction standard card, which can be seen that product, meanwhile, it can be clearly seen that product is six arris platforms from field emission scanning electron microscope photo.A kind of advantages of the present invention: 1. hexaplanar terrace with edge Zinc oxide particles of asymmetric pattern；2. the different crystal face of zincite crystal exposure, controlled facets are for zinc oxide using most important.
Description
Technical field
The present invention relates to the technical fields of the asymmetric growth of zincite crystal and controlled facets zinc oxide to synthesize field, especially
It is a kind of preparation method of six arris platform zinc oxide.
Background technique
Zinc oxide because its unique property is widely used, such as: photocatalysis is lived as vulcanization in rubber industry
Agent, gas sensor, solar battery, photoelectricity and piezoelectricity field.The zinc oxide of the different crystal faces of exposure, corresponds to different answer
With field, therefore the zinc oxide for synthesizing different crystal faces, numerous scholars have carried out a large amount of research, wherein Pu Xian Gao
Et al. (Mesoporous Polyhedral Cages and Shells Formed byTextured Self-Assembly
Of ZnO Nanocrystals) Zinc oxide particles of various patterns are synthesized by the method for high-temperature calcination, such as: sheet, band
Shape, corynebacterium, it is needle-shaped etc..Eue Soon Jang et al. by control reaction condition successfully prepare corynebacterium with
And the zinc oxide of sheet.Xi Zhou etc. controls the growth of zincite crystal by solion, obtains the oxidation of Pyramid
Zinc.Zhong Ling Wang et al. has synthesized band-like and acicular zinc oxide by high temperature gas phase method.But due to crystalline substance
The relationship of body symmetry, zinc oxide tend to symmetric growth, are difficult to go it to the ratio of zinc oxide (001) and (001) crystal face
Effective regulation.The main object of the present invention is exactly effectively to be controlled the crystal face of zinc oxide exposure.
Summary of the invention
The purpose of the present invention is to provide a kind of synthetic methods of unsymmetric structure zinc oxide, by hydro-thermal reaction, in crow
Under the action of Lip river tropine and ethylene glycol, a kind of six arris platform zinc oxide are synthesized.The asymmetric growth of zincite crystal, different crystal faces
Ratio can be controlled by the change of experiment condition, finally obtain the controllable zinc oxide of crystal face.
Realize the object of the invention the technical solution adopted is as follows:
A kind of preparation method of six arris platform zinc oxide, includes the following steps:
1) the ethylene glycol mixed solution of certain volume score is prepared, it is spare after ultrasonic disperse.
2) zinc acetate of certain mass and methenamine are sequentially added in above-mentioned mixed solution, ultrasonic dissolution under room temperature.
3) 2) mixed solution in is transferred in the water heating kettle of certain volume, reacts under high temperature and takes out after a certain period of time.
4) washing suction filtration is carried out with ethyl alcohol after cooling, powder sample is placed in Muffle furnace after oven drying and carries out a period of time
High-temperature calcination is taken out after cooling and is made.
Preferably, the mixed solution of certain volume score described in step 1) refers to that the volume fraction of ethylene glycol is 30-
50%, the mass ratio of zinc acetate and methenamine described in step 2) is 1-2.
It is highly preferred that the reaction temperature of mixed solution is 85 DEG C -105 DEG C, the reaction time is -36h for 24 hours, meanwhile, high temperature is forged
The temperature of burning is 300 DEG C -500 DEG C, calcination time 2h-5h.
The present invention has the advantages that the asymmetric growth of 1. zincite crystals, six arris platforms, smooth surface, nothing is presented in pattern
Obvious shortcoming.2. the controlledly synthesis technology of zinc oxide crystal face may be implemented by control reaction condition.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram piece of case study on implementation 1；
Fig. 2 is the X ray diffracting spectrum of case study on implementation 1；
Fig. 3 is the scanning electron microscope diagram piece of case study on implementation 2；
Fig. 4 is the X ray diffracting spectrum of case study on implementation 2；
Fig. 5 is the scanning electron microscope diagram piece of case study on implementation 3；
Fig. 6 is the X ray diffracting spectrum of case study on implementation 3；
Fig. 7 is the scanning electron microscope diagram piece of case study on implementation 4；
Fig. 8 is the scanning electron microscope diagram piece of case study on implementation 5；
Fig. 9 is the scanning electron microscope diagram piece of case study on implementation 6；
Specific embodiment
The present invention provides a kind of preparation method of asymmetric developing zinc oxide crystallite, detailed process includes the following steps:
1) the ethylene glycol mixed solution of certain volume score is prepared, zinc acetate and methenamine are sequentially added after ultrasonic disperse, ultrasound
Dissolution；2) after above-mentioned mixed solution being placed in baking oven high temperature reaction a period of time, ethanol washing filtering, drying；It 3) finally, will
Obtained powder carries out high-temperature calcination.
Six side crystallographic system zinc oxide of different surface morphology in order to obtain, volume fraction and concentration to mixed solution carry out
Adjustment, meanwhile, reaction temperature and time are adjusted, contrast and experiment, obtain zinc oxide crystal face under different parameters.
Embodiment 1
1) preparation of mixed solution
The ethylene glycol of precise 16ml, the deionized water of 24ml, sequentially add after ultrasonic mixing 5.268 g zinc acetates and
3.364g methenamine, ultrasonic dissolution.
2) hydro-thermal reaction
Above-mentioned mixed solution is transferred in the water heating kettle of 100ml, is subsequently placed in 95 DEG C of baking oven and reacts for 24 hours, natural cooling
After take out.
3) high-temperature calcination
Washing is carried out to above-mentioned product using ethyl alcohol to filter three times, is then dried at 80 DEG C, finally, obtained powder is placed in
2h is calcined in 300 DEG C of Muffle furnace.The SEM picture of products therefrom is as shown in Figure 1, XRD map is as shown in Figure 2.
It is available to observe Fig. 1, product zinc oxide is in six arris platforms, and upper bottom surface is presented different sizes, and side is also not
The simple plane of symmetry, can significantly observe up and down two sides, about 1 μm of grain size.Compare hexaplanar zinc oxide
Standard diffraction map is it is found that gained zincite crystal is hexaplanar.
Embodiment 2
1) preparation of mixed solution
The ethylene glycol of precise 24ml, the deionized water of 24ml, sequentially add after ultrasonic mixing 5.268 g zinc acetates and
3.364g methenamine, ultrasonic dissolution.
2) hydro-thermal reaction
Above-mentioned mixed solution is transferred in the water heating kettle of 100ml, is subsequently placed in 95 DEG C of baking oven and reacts for 24 hours, natural cooling
After take out.
3) high-temperature calcination
Washing is carried out to above-mentioned product using ethyl alcohol to filter three times, is then dried at 80 DEG C, finally, obtained powder is placed in
2h is calcined in 300 DEG C of Muffle furnace.The SEM picture of products therefrom is as shown in figure 3, XRD map is as shown in Figure 4.
Observation Fig. 3 is available, and product zinc oxide is still in six arris platforms, and upper bottom surface ratio is significantly less than case one,
Simultaneously, it can clearly be seen that the ratio of upper and lower side, which arranges, is also obviously different from case one, and about 1 μm of grain size.It is brilliant to compare hexagonal
It is zinc oxide standard diffraction map it is found that gained zincite crystal is hexaplanar.
Embodiment 3
1) preparation of mixed solution
The ethylene glycol of precise 16ml, the deionized water of 24ml, sequentially add after ultrasonic mixing 5.268 g zinc acetates and
5.268g methenamine, ultrasonic dissolution.
2) hydro-thermal reaction
Above-mentioned mixed solution is transferred in the water heating kettle of 100ml, is subsequently placed in 95 DEG C of baking oven and reacts for 24 hours, natural cooling
After take out.
3) high-temperature calcination
Washing is carried out to above-mentioned product using ethyl alcohol to filter three times, is then dried at 80 DEG C, finally, obtained powder is placed in
2h is calcined in 500 DEG C of Muffle furnace.The SEM picture of products therefrom is as shown in figure 5, XRD map is as shown in Figure 6.
It is available to observe Fig. 3, six arris platforms are presented in product zinc oxide, and upper bottom surface is of different sizes, and upper and lower side is formed
Certain angle, about 1.5 μm of grain size.Hexaplanar zinc oxide standard diffraction map is compared it is found that gained zincite crystal
For hexaplanar.
Embodiment 4
1) preparation of mixed solution
The ethylene glycol of precise 10ml, the deionized water of 24ml, sequentially add after ultrasonic mixing 5.268 g zinc acetates and
5.268g methenamine, ultrasonic dissolution.
2) hydro-thermal reaction
Above-mentioned mixed solution is transferred in the water heating kettle of 100ml, is subsequently placed in 105 DEG C of baking oven and reacts 36h, natural cooling
After take out.
3) high-temperature calcination
Washing is carried out to above-mentioned product using ethyl alcohol to filter three times, is then dried at 80 DEG C, finally, obtained powder is placed in
4h is calcined in 500 DEG C of Muffle furnace.The SEM picture of products therefrom is as shown in Figure 7.
It is available to observe Fig. 3, six arris platforms are presented in product zinc oxide, and upper bottom surface size is still different, grain size
About 2 μm.Unlike case before, terrace with edge obtained is without upper and lower two kinds of sides under this condition.
Embodiment 5
1) preparation of mixed solution
The ethylene glycol of precise 16ml, the deionized water of 24ml, sequentially add after ultrasonic mixing 5.268 g zinc acetates and
2.634g methenamine, ultrasonic dissolution.
2) hydro-thermal reaction
Above-mentioned mixed solution is transferred in the water heating kettle of 100ml, is subsequently placed in 95 DEG C of baking oven and reacts 36h, natural cooling
After take out.
3) high-temperature calcination
Washing is carried out to above-mentioned product using ethyl alcohol to filter three times, is then dried at 80 DEG C, finally, obtained powder is placed in
4h is calcined in 500 DEG C of Muffle furnace.The SEM picture of products therefrom is as shown in Figure 8.
Embodiment 6
1) preparation of mixed solution
The ethylene glycol of precise 24ml, the deionized water of 24ml, sequentially add after ultrasonic mixing 5.268 g zinc acetates and
2.634g methenamine, ultrasonic dissolution.
2) hydro-thermal reaction
Above-mentioned mixed solution is transferred in the water heating kettle of 100ml, is subsequently placed in 95 DEG C of baking oven and reacts 36h, natural cooling
After take out.
3) high-temperature calcination
Washing is carried out to above-mentioned product using ethyl alcohol to filter three times, is then dried at 80 DEG C, finally, obtained powder is placed in
2h is calcined in 300 DEG C of Muffle furnace.The SEM picture of products therefrom is as shown in Figure 9.
Claims (6)
1. a kind of preparation method of six arris platform zinc oxide, characterized by the following steps:
(1) mixed solution is prepared: at room temperature, being prepared the ethylene glycol mixed solution of certain volume score, is successively added after ultrasonic disperse
Enter the zinc oxide precursor and pattern controlling agent of certain mass, again ultrasonic disperse.
(2) pyroreaction: above-mentioned mixed liquor being transferred in the water heating kettle of a constant volume, and it is anti-that water heating kettle is placed in baking oven high temperature
It should a period of time.
(3) calcination processing: the product in (2) is washed and is filtered, powder is placed in Muffle furnace after drying, at one section of high-temperature calcination
Between after take out.
2. the preparation method according to requiring 1, which is characterized in that the volume fraction of ethylene glycol mixed solution is in step (1)
30-50%.
3. the preparation method according to requiring 1, which is characterized in that the presoma of zinc is zinc acetate, pattern control in step (1)
Agent is methenamine, and the mass ratio of the two is 1-2.
4. the preparation method according to requiring 2 or 3, which is characterized in that when ethylene glycol mixed solution volume fraction be 40%,
When the mass ratio of zinc acetate and methenamine is 1.56, zincite crystal pattern is the most regular.
5. the preparation method according to requiring 1, which is characterized in that the temperature and time difference of step (2) high temperature reaction
Control -36h at 85 DEG C -105 DEG C and for 24 hours.
6. the preparation method according to requiring 1, which is characterized in that the temperature and time difference of step (3) high temperature calcining
For 300 DEG C -500 DEG C and 2h-5h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862105A (en) * | 2019-11-22 | 2020-03-06 | 郑州大学 | Pyramid-shaped zinc oxide nano-particles with enhanced fluorescence intensity as well as preparation method and application thereof |
| CN112607763A (en) * | 2021-01-05 | 2021-04-06 | 昆明理工大学 | Method for controllably preparing multi-morphology micro-nano zinc oxide by hydrothermal method |
| CN113277490A (en) * | 2021-05-14 | 2021-08-20 | 同济大学 | Carbon-based composite material based on biomass and preparation method and application thereof |
-
2019
- 2019-04-18 CN CN201910313396.8A patent/CN109987623A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| S YIN ET AL.: ""Synthesis of Plate-like Zinc Oxide Particles by the Transcription of Precursor"s Shape"", 《IOP CONFERENCE SERIES：MATERIALS SCIENCE AND ENGINEERING》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862105A (en) * | 2019-11-22 | 2020-03-06 | 郑州大学 | Pyramid-shaped zinc oxide nano-particles with enhanced fluorescence intensity as well as preparation method and application thereof |
| CN112607763A (en) * | 2021-01-05 | 2021-04-06 | 昆明理工大学 | Method for controllably preparing multi-morphology micro-nano zinc oxide by hydrothermal method |
| CN113277490A (en) * | 2021-05-14 | 2021-08-20 | 同济大学 | Carbon-based composite material based on biomass and preparation method and application thereof |
| CN113277490B (en) * | 2021-05-14 | 2022-10-04 | 同济大学 | Carbon-based composite material based on biomass and preparation method and application thereof |
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Application publication date: 20190709 |