CN105293566A - Preparation method of mono-dispersed ZnO microspheres - Google Patents
Preparation method of mono-dispersed ZnO microspheres Download PDFInfo
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- CN105293566A CN105293566A CN201510724895.8A CN201510724895A CN105293566A CN 105293566 A CN105293566 A CN 105293566A CN 201510724895 A CN201510724895 A CN 201510724895A CN 105293566 A CN105293566 A CN 105293566A
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- zno microsphere
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The invention relates to a preparation method of mono-dispersed ZnO microspheres and belongs to the technical field of semiconductor materials. The preparation method of the mono-dispersed ZnO microspheres is characterized in that zinc nitrate hexahydrate, triethanolamine and PEG6000 are taken as raw materials and are mixed to obtain a mixed solution, ultrasonic reaction is carried out on the mixed solution to prepare mono-dispersed ZnO microsphere powder, triethanolamine is rapidly hydrolyzed and reacts with zinc ions on the surface of bubbles in an ultrasonic process, and mono-dispersed ZnO microspheres with different sizes can be prepared by changing ultrasonic reaction time.
Description
Technical field
The present invention relates to a kind of preparation method of single dispersing ZnO microsphere, belong to technical field of semiconductor.
Background technology
Under normal temperature, the dead band width of ZnO is 3.37eV, and exciton bind energy is 60meV, it is a kind of II-VI important race's semiconductor material, its stable chemical nature, nontoxic, there is good electrical property and biocompatibility simultaneously, be widely used in gas sensor, photodetector, photodiode, voltage dependent resistor, the aspects such as piezoelectric device, become the focus of electronic element device materials research gradually; Wherein, the based varistor prepared by monodisperse spherical nano zinc oxide material has good current/voltage non-linear character, can reduce the sintering temperature in preparation process simultaneously, reduces energy consumption; The method preparing different-shape and size ZnO has sol-gel method usually, hydrothermal synthesis method, chemical Vapor deposition process, spray pyrolysis is sent out, chemical precipitation method etc., but the usual complex process of method of more than preparation, equipment requirements is high, and energy consumption is large, and production cost is higher, also be difficult to pattern and the dispersiveness of controlled oxidization zinc simultaneously, therefore explore a kind of technique simple, cost is reasonable, less energy-consumption, it is necessary that eco-friendly preparation method synthesizes monodisperse spherical Zinc oxide powder, and relevant synthesis technique has become the focus of research and development.
Ultrasonic method is as a kind of method by ultrasonic radiation solution nano materials, simple process, high-efficiency environment friendly, ultrasonic method can produce a kind of strong cavitation in the solution because of its violent radiation vibration, bubble in solution can break instantaneously, the simultaneously hydroxy of bubble surface and metal ion reaction, thus control the growth of crystal, achieve dispersiveness and the morphology controllable of powder.
Therefore, the present invention for starting raw material, prepares single dispersing ZnO microsphere powder by ultrasonic reaction with zinc nitrate hexahydrate, trolamine, PEG6000, for place mat has been made in the extensive utilization of ultrasonic method in future in nano material.
Summary of the invention
The object of the invention is to overcome zinc oxide bad dispersibility prepared by traditional method, the shortcomings such as pattern is wayward, a kind of strong cavitation can be produced in the solution according to the radiation vibration that ultrasonic method is violent, namely release energy in the short period of time and cause solution localized hyperthermia high pressure, the official post of bubble external and internal pressure obtains bubbles burst, provide in a kind of ultrasonic procedure to be hydrolyzed rapidly at bubble surface trolamine and react with zine ion, thus generate the preparation method of controlled, the monodispersed ZnO microsphere of a kind of appearance and size.
The object of this invention is to provide a kind of preparation method of monodispersed ZnO microsphere, its reaction principle is as follows:
N(CH
2CH
2OH)
3+H
2O
NH
3+CO
2(1)
NH
3+H
2O
OH-+NH
4+(2)
Zn
2++OH-
Zn(OH)
2 ZnO(3)
Technical solution of the present invention is as follows:
A kind of preparation method of single dispersing ZnO microsphere, it is characterized in that: with zinc nitrate hexahydrate, trolamine, PEG6000 for raw material, three is mixed to get mixing solutions, mixing solutions prepares single dispersing ZnO microsphere powder by ultrasonic reaction, being hydrolyzed rapidly at bubble surface trolamine in ultrasonic procedure and reacting with zine ion, realizing the preparation of the single dispersing ZnO microsphere of different size by changing the ultrasonic reaction time.
Along with the ultrasonic reaction time increases, the particle diameter of ZnO microsphere becomes large.
A preparation method for single dispersing ZnO microsphere, is characterized in that concrete steps are as follows:
(1) be raw material with zinc nitrate hexahydrate, be solvent with distilled water, stirring and dissolving obtains transparent mixed solution.
(2) take polyethylene glycol 6000 as tensio-active agent, trolamine is stablizer, joins respectively in transparent mixed solution, stirring and dissolving, wherein zinc nitrate hexahydrate in mixing solutions: the mol ratio of trolamine is 1:7 ~ 1:9, the mass percentage concentration of polyethylene glycol 6000 is 0.5 ~ 1%.
(3) solution of three kinds of raw material mixing is put into 40Hz ultrasonic instrument and react 1-4h.
(4) centrifugation, washing, filtration, drying obtain single dispersing ZnO microsphere.
Further, described washing adopts distilled water and ethanol to take volume ratio as the mixing solutions washing that 1:2 mixes, and described drying refers under 80 DEG C of conditions dry.
Advantage of the present invention and positively effect: (1) can realize the preparation of different size and pattern single dispersing ZnO microsphere by changing the ultrasonic reaction time, method is simple; (2) the ZnO microsphere homogeneity prepared of the present invention is good, good dispersity; (3) use water to make solvent, polyethylene glycol 6000 makes tensio-active agent, pollution-free, production safety; (4) raw material is easy to get, and equipment is simple, and concise in technology, cost is lower.
Accompanying drawing explanation
Fig. 1 is the FTIR figure that embodiment 1 prepares sample; The absorption peak of 460cm-1Zn-O key as seen from Figure 1,1635cm-1 and 3385cm-1 is the vibration peak of water molecules and OH-1, shows that sample is ZnO.
Fig. 2 is the XRD figure that embodiment 1 prepares sample; As shown in Figure 2 100,002,101,102,110,103,200,112 is consistent with the standard feature peak of ZnO with 201 peaks, illustrates that this material is ZnO.
Fig. 3 is the SEM figure that embodiment 1 prepares sample, scale designation 10 μm.
Fig. 4 is the SEM figure that embodiment 1 prepares sample, scale designation 1 μm.
Fig. 5 is the SEM figure that embodiment 1 prepares sample, scale designation 200nm.
As can be seen from Fig. 3,4 and 5, sample powder is mono-dispersion microballoon, and its particle diameter is about 1.2 μm.
Embodiment
Below in conjunction with embodiment, the present invention is further described
Embodiment 1
2.1mmol zinc nitrate hexahydrate is dissolved in 100ml distilled water; 1g polyethylene glycol 6000 and 2ml trolamine are joined in above-mentioned solution, magnetic agitation becomes clear solution again, and by ultrasonic for mixing solutions 2h, then centrifugation, washs by the mixed solutions for many times of distilled water and ethanol by volume ratio 1:2 mixing, filter; At product being put into 80 DEG C, baking oven, drying obtains white solid powder.
FTIR spectrum (FTIR), X-ray optical diffraction (XRD), Scanning Electron microscope (SEM) is adopted to analyze product; Fig. 1, FTIR and XRD of 2 demonstrates successfully making ZnO microballoon; Fig. 3/4/5, be product SEM figure, can find out it is mono-dispersion microballoon, its particle diameter is about 1.2 μm.
Embodiment 2
2.1mmol zinc nitrate hexahydrate is dissolved in 100ml distilled water; 1g polyethylene glycol 6000 and 2ml trolamine are joined in above-mentioned solution, magnetic agitation becomes clear solution again, and by ultrasonic for mixing solutions 3h, then centrifugation, washs by the mixed solutions for many times of distilled water and ethanol by volume ratio 1:2 mixing, filter; At product being put into 80 DEG C, baking oven, drying obtains white solid powder; SEM figure, FTIR and XRD are similar to Example 1, but its particle diameter becomes about 2 μm.
Embodiment 3
2.1mmol zinc nitrate hexahydrate is dissolved in 100ml distilled water; 1g polyethylene glycol 6000 and 2ml trolamine are joined in above-mentioned solution, magnetic agitation becomes clear solution again, and by ultrasonic for mixing solutions 4h, then centrifugation, washs by the mixed solutions for many times of distilled water and ethanol by volume ratio 1:2 mixing, filter; At product being put into 80 DEG C, baking oven, drying obtains white solid powder; SEM figure, FTIR and XRD are similar to Example 1, but its particle diameter becomes about 2.4 μm.
Embodiment 4
2.5mmol zinc nitrate hexahydrate is dissolved in 100ml distilled water; 1g polyethylene glycol 6000 and 2ml trolamine are joined in above-mentioned solution, magnetic agitation becomes clear solution again, and by ultrasonic for mixing solutions 2h, then centrifugation, washs by the mixed solutions for many times of distilled water and ethanol by volume ratio 1:2 mixing, filter; At product being put into 80 DEG C, baking oven, drying obtains white solid powder; FTIR and XRD is similar to Example 1, but reduces due to the concentration of zine ion, and in SEM figure, ZnO powder dispersity reduces, and have reunion, diameter of particle is about 4 μm.
Embodiment 5
3.0mmol zinc nitrate hexahydrate is dissolved in 100ml distilled water; 1g polyethylene glycol 6000 and 2ml trolamine are joined in above-mentioned solution, magnetic agitation becomes clear solution again, and by ultrasonic for mixing solutions 1h, then centrifugation, washs by the mixed solutions for many times of distilled water and ethanol by volume ratio 1:2 mixing, filter; At product being put into 80 DEG C, baking oven, drying obtains white solid powder; FTIR and XRD is similar to Example 1, but the concentration of zine ion reduces, and the reaction times is short, and in SEM figure, ZnO morphology microstructure is irregular, and particle diameter is 1 ~ 5 μm.
Embodiment 6
3.5mmol zinc nitrate hexahydrate is dissolved in 100ml distilled water; 0.5g polyethylene glycol 6000 and 2ml trolamine are joined in above-mentioned solution, magnetic agitation becomes clear solution again, and by ultrasonic for mixing solutions 2h, then centrifugation, washs by the mixed solutions for many times of distilled water and ethanol by volume ratio 1:2 mixing, filter; At product being put into 80 DEG C, baking oven, drying obtains white solid powder; FTIR and XRD is similar to Example 1, and dosage of surfactant is few, and in SEM figure, ZnO morphology microstructure is irregular, has a large amount of reunion, dispersed low, particle diameter 5 ~ 8 μm.
Claims (4)
1. the preparation method of a single dispersing ZnO microsphere, it is characterized in that: with zinc nitrate hexahydrate, trolamine, PEG6000 for raw material, three is mixed to get mixing solutions, mixing solutions prepares single dispersing ZnO microsphere powder by ultrasonic reaction, being hydrolyzed rapidly at bubble surface trolamine in ultrasonic procedure and reacting with zine ion, realizing the preparation of the single dispersing ZnO microsphere of different size by changing the ultrasonic reaction time.
2. the preparation method of a kind of single dispersing ZnO microsphere as claimed in claim 1, is characterized in that concrete steps are as follows:
(1) be raw material with zinc nitrate hexahydrate, be solvent with distilled water, stirring and dissolving obtains transparent mixed solution;
(2) take polyethylene glycol 6000 as tensio-active agent, trolamine is stablizer, joins respectively in transparent mixed solution, stirring and dissolving, wherein zinc nitrate hexahydrate: the mol ratio of trolamine is 1:7 ~ 1:9, the mass percentage concentration of polyethylene glycol 6000 is 0.5 ~ 1%;
(3) solution of three kinds of raw material mixing is put into 40Hz ultrasonic instrument and react 1-4h;
(4) centrifugation, washing, filtration, drying obtain single dispersing ZnO microsphere.
3. the preparation method of a kind of single dispersing ZnO microsphere as claimed in claim 2, is characterized in that: along with the ultrasonic reaction time increases, and the particle diameter of ZnO microsphere becomes large.
4. the preparation method of a kind of single dispersing ZnO microsphere as claimed in claim 2, is characterized in that: described washing adopts distilled water and ethanol to take volume ratio as the mixing solutions washing that 1:2 mixes, and described drying refers under 80 DEG C of conditions dry.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoid-shaped zinc oxide |
| WO2012010949A1 (en) * | 2010-07-23 | 2012-01-26 | Indian Institute Of Technology, Bombay | PROCESS FOR SYNTHESIS OF Tb DOPED ZnO NANOPARTICLES FOR TOTAL CONTROL OVER THE UV TO GREEN LUMINESCENCE (GL) INTENSITY RATIO AND THE TUNABILITY OF UV LUMINESCENCE (UVL) |
| CN102442694A (en) * | 2011-10-14 | 2012-05-09 | 太原理工大学 | Preparation method of nanometer ZnO full sphere |
| CN103922389A (en) * | 2014-04-21 | 2014-07-16 | 天津师范大学 | Preparation method of graded zinc oxide nanodisk material |
-
2015
- 2015-11-02 CN CN201510724895.8A patent/CN105293566A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoid-shaped zinc oxide |
| WO2012010949A1 (en) * | 2010-07-23 | 2012-01-26 | Indian Institute Of Technology, Bombay | PROCESS FOR SYNTHESIS OF Tb DOPED ZnO NANOPARTICLES FOR TOTAL CONTROL OVER THE UV TO GREEN LUMINESCENCE (GL) INTENSITY RATIO AND THE TUNABILITY OF UV LUMINESCENCE (UVL) |
| CN102442694A (en) * | 2011-10-14 | 2012-05-09 | 太原理工大学 | Preparation method of nanometer ZnO full sphere |
| CN103922389A (en) * | 2014-04-21 | 2014-07-16 | 天津师范大学 | Preparation method of graded zinc oxide nanodisk material |
Non-Patent Citations (3)
| Title |
|---|
| HORST STOCKER: "《物理手册》", 30 April 2005 * |
| 张三奇等: "《药物合成新方法》", 30 September 2005 * |
| 邓崇海: "超声化学制备ZnO 单分散纳米球及光学性能", 《合肥学院学报（自然科学版）》 * |
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