CN101186329A - Method for preparing micron-level ZnO of octahedral structure - Google Patents
Method for preparing micron-level ZnO of octahedral structure Download PDFInfo
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- CN101186329A CN101186329A CNA2007100727393A CN200710072739A CN101186329A CN 101186329 A CN101186329 A CN 101186329A CN A2007100727393 A CNA2007100727393 A CN A2007100727393A CN 200710072739 A CN200710072739 A CN 200710072739A CN 101186329 A CN101186329 A CN 101186329A
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Abstract
The invention provides a preparation method of ZnO with micron grade octahedron structure. The specific method has the following steps: firstly, acetate zinc and ammonia are chosen as raw materials, the molar ratio of which is 1:2-4; secondly, ammonia is dripped to Zn(CH3COO)2 solution with stirring when the solution is heated to 45 to 50 DEG C, then, the dripping is stopped and the temperature is maintained and the stirring is carried on when the PH value equals 8, and when precipitation appears and ends, the heating and stirring is stopped ; thirdly, the precipitate is washed with deionized water, filtrated until the PH value equals 7; fourthly, the product gained from the third step is done with drying treatment when put in an alumina crucible at 70 to 80 DEG C, preserving the heat for 1 to 5 hours; fifthly, the dry powder is thermally processed at 300 to 900 DEG C with a temperature rising rate being kept 10 DEG C per minute, preserving the heat for 2 hours, thereby, the ZnO with the octahedron structure is achieved. The invention has the advantages of low cost, simple art, high yield and being adaptable for batch manufacturing, etc.
Description
(1) technical field:
The present invention relates to a kind of nanotechnology, be specifically related to the preparation method of a kind of ZnO of the micron order octahedral structure that forms by the nanoparticle self-assembly.
(2) background technology:
The controlled multidimensional nano material of preparation size is extremely important for development advanced catalyzer and gas sensor.Self-assembled material has big surface-area, therefore has the physicochemical property of many uniquenesses.ZnO is the direct band gap semiconductor material with wide forbidden band, has higher exciton binding energy, can at room temperature observe the existence of exciton, thereby good heat-resistance and thermostability are arranged.ZnO is a kind of multi-functional materials such as semiconductive, pyroelectricity and piezoelectricity that have concurrently, at the moving device of detector, catalyzer, transmitter, piezoelectricity frequency transformer, surface acoustic wave, and laser diode, solar battery etc.A peacekeeping of various forms two dimension ZnO structural research gets very manyly in the past few years, and as nano wire, nanotube, nano thin-film, nano-rings or the like, but it is still very difficult to control three-dimensional self-assembled structures at present.
(3) summary of the invention:
The objective of the invention is to propose the method for preparing micron-level ZnO of octahedral structure of advantages such as a kind of cost is low, technology is simple, productive rate is high, suitable batch process.
The object of the present invention is achieved like this: concrete steps comprise:
Step 1: selecting zinc acetate and ammoniacal liquor for use is raw material, and the mole of zinc acetate and ammoniacal liquor is 1: 2-4;
Step 2: when being heated to 45-50 ℃ to Zn (CH
3COO)
2Dropping ammonia and stirring in the solution stop to drip when PH=8, and temperature remains unchanged, and continues stirred solution, treat that appearance precipitation and whole post precipitation stop heated and stirred;
Step 3: PH=7 is washed and be filtered to precipitate with deionized water;
Step 4: the product in the step 3 is placed in the alumina crucible,, is incubated 1-5 hour in 70-80 ℃ of drying treatment;
Step 5: the exsiccant powder is heat-treated at 300-900 ℃, and temperature rise rate remains 10 ℃/min, is incubated 2h, promptly obtains the ZnO of octahedral structure.
The present invention also has some technical characterictics like this:
1, described zinc acetate be analytical pure, with the zinc acetate of two crystal water, ammoniacal liquor is 25% analytical pure ammoniacal liquor for the quality percentage composition.
What the present invention prepared is the micron-level ZnO of octahedral structure that is formed by the self-assembly of ZnO nanoparticle.At first adopt this easy method of sol-gel to make the ZnO presoma of octahedral structure, obtain the ZnO of octahedral structure again by the thermolysis presoma.
In the step 1, according to chemical equation, zinc acetate and ammoniacal liquor amount of substance (mole) carried out proportioning by 1: 2, and ammoniacal liquor wants more excessive on this basis.In the step 2, after the raw material in the step 1 configured respectively, the limit was to Zn (CH between 45～50 ℃
3COO)
2Stir on the dropping ammonia limit in the solution.This process alkali and Zn reactant salt generate zinc hydroxide and polymkeric substance.When PH=8, stop to drip, be in gel state this moment.This process alkali and Zn reactant salt generate zinc hydroxide and polymkeric substance.Temperature-resistant, continue stirred solution, begin after 20 minutes precipitation to occur, treat that whole post precipitations stop heated and stirred.This process can be removed some little organic molecules and finish the transformation mutually of zinc hydroxide, has generated the ZnO presoma of octahedra shape.Step 3 is with the washing of the precipitate with deionized water in the step 2 and be filtered to PH=7.Step 4 is placed on the product in the step 3 in the alumina crucible, carries out drying at 70 ℃, is incubated 1～5 hour.Remove some moisture and little organic molecule, make the presoma crystallization.Step 5 is heat-treated exsiccant powder in the step 4 at 300～900 ℃, 10 ℃/min of temperature rise rate, and soaking time is 2h.This process mainly is that the presoma with octahedral structure carries out thermolysis, thereby obtains the ZnO of octahedral structure.
The present invention utilizes this easy method of sol-gel to prepare the ZnO presoma of octahedral structure first, again by the large-area micron order ZnO that has obtained octahedral structure of thermolysis presoma.This octahedron is to be that the ZnO particle self-assembly of 200nm forms by size of particles, does not have the situation of subsiding and occurs, and the ZnO octahedral structure that is stressed that this self-assembly in addition also is what not appear in the newspapers.The present invention has obtained to form micron-sized octahedral structure by the self-assembly of ZnO nanoparticle first, proposes a kind of method for preparing the ZnO octahedral structure that cost is low, technology is simple, productive rate is high, be fit to advantages such as batch process that has.The ZnO of this structure is expected to be applied in the moving device of detector, catalyzer, transmitter, piezoelectricity frequency transformer, surface acoustic wave, and aspects such as laser diode, solar battery.
(4) embodiment:
The present invention is further illustrated below in conjunction with specific embodiment:
Embodiment 1:
Take by weighing 65.7g and be dissolved in (1M) in the 300ml deionized water, 55ml ammoniacal liquor is dissolved in (2M) in the 400ml deionized water with the zinc acetate of two crystal water.On limit, 45 ℃ of left and right sides to Zn (CH
3COO)
2Stir on the dropping ammonia limit in the solution, when PH=8, stops to drip, and continues stirred solution, begins after 20 minutes precipitation to occur, treats that whole post precipitations stop heated and stirred.With deionized water wash and filter this throw out to PH=7.Carry out drying at 70 ℃ then, be incubated 1 hour.500 ℃ of thermal treatments 2 hours, what promptly obtain the well-crystallized formed the octahedral structure of micron order ZnO by the self-assembly of ZnO nanoparticle with the exsiccant powder, amounted to 20 grams.These octahedral size 5 μ m～10 μ m, wherein the mean sizes of ZnO particle is 100nm.
Embodiment 2:
Take by weighing 65.7g and be dissolved in (1M) in the 300ml deionized water, 55ml ammoniacal liquor is dissolved in (2M) in the 400ml deionized water with the zinc acetate of two crystal water.On limit, 45 ℃ of left and right sides to Zn (CH
3COO)
2Stir on the dropping ammonia limit in the solution, when PH=8, stops to drip, and continues stirred solution, begins after 20 minutes precipitation to occur, treats that whole post precipitations stop heated and stirred.With deionized water wash and filter this throw out to PH=7.Carry out drying at 70 ℃ then, be incubated 1 hour.600 ℃ of thermal treatments 2 hours, what promptly obtain the well-crystallized formed the octahedral structure of micron-sized ZnO by the self-assembly of ZnO nanoparticle with the exsiccant powder, amounted to 20 grams.These octahedral size 5 μ m～10 μ m are wherein about the size 120nm of ZnO particle.
Embodiment 3:
Take by weighing 65.7g and be dissolved in (1M) in the 300ml deionized water, 55ml ammoniacal liquor is dissolved in (2M) in the 400ml deionized water with the zinc acetate of two crystal water.On limit, 45 ℃ of left and right sides to Zn (CH
3COO)
2Stir on the dropping ammonia limit in the solution, when PH=8, stops to drip, and continues stirred solution, begins after 20 minutes precipitation to occur, treats that whole post precipitations stop heated and stirred.With deionized water wash and filter this throw out to PH=7.Carry out drying at 70 ℃ then, be incubated 1 hour.With the exsiccant powder 900 ℃ of thermal treatments 2 hours, furnace cooling, the octahedral structure form does not become, but is sticked together between the ZnO nanoparticle, amounts to 20 grams.
Embodiment 4:
Take by weighing 10.95g and be dissolved in (0.5M) in the 100ml deionized water, 15ml ammoniacal liquor is dissolved in (0.5M) in the 400ml deionized water with the zinc acetate of two crystal water.On limit, 50 ℃ of left and right sides to Zn (CH
3COO)
2Stir on the dropping ammonia limit in the solution, when PH=8, stops to drip, and continues stirred solution, begins after 20 minutes precipitation to occur, treats that whole post precipitations stop heated and stirred.With deionized water wash and filter this throw out to PH=7.Carry out drying at 70 ℃ then, be incubated 3.5 hours.500 ℃ of thermal treatments 2 hours, what promptly obtain the well-crystallized formed the octahedral structure of micron order ZnO by the self-assembly of ZnO nanoparticle with the exsiccant powder, amounted to 3 grams.These octahedral size 5 μ m～8 μ m are wherein about the size 50nm of ZnO particle.
Claims (2)
1. the preparation method of a micron-level ZnO of octahedral structure is characterized in that:
Step 1: selecting zinc acetate and ammoniacal liquor for use is raw material, and the mol ratio of zinc acetate and ammoniacal liquor is 1: 2-4;
Step 2: when being heated to 45-50 ℃ to Zn (CH
3COO)
2Dropping ammonia and stirring in the solution stop to drip when PH=8, and temperature remains unchanged, and continues stirred solution, treat that appearance precipitation and whole post precipitation stop heated and stirred;
Step 3: PH=7 is washed and be filtered to precipitate with deionized water;
Step 4: the product in the step 3 is placed in the alumina crucible,, is incubated 1-5 hour in 70-80 ℃ of drying treatment;
Step 5: the exsiccant powder is heat-treated at 300-900 ℃, and temperature rise rate remains 10 ℃/min, is incubated 2h, promptly obtains the ZnO of octahedral structure.
2. the preparation method of a kind of micron-level ZnO of octahedral structure according to claim 1 is characterized in that: described zinc acetate is analytical pure, with the zinc acetate of two crystal water, and ammoniacal liquor is 25% analytical pure ammoniacal liquor for the quality percentage composition.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100727393A CN101186329A (en) | 2007-09-04 | 2007-09-04 | Method for preparing micron-level ZnO of octahedral structure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774875A (en) * | 2012-07-30 | 2012-11-14 | 西安理工大学 | Preparation method of octahedral zinc oxide crystals with micrometer-nanometer pore micro structures |
| CN106006708A (en) * | 2016-05-23 | 2016-10-12 | 渤海大学 | Preparation method of lengthened octahedral hierarchical structure material of ZnO |
| CN108163884A (en) * | 2018-03-21 | 2018-06-15 | 淮阴师范学院 | A kind of polyhedron zinc oxide and preparation method thereof |
| CN111924871A (en) * | 2020-07-27 | 2020-11-13 | 广州大学 | Octahedral zinc oxide/carbon composite material and preparation method and application thereof |
-
2007
- 2007-09-04 CN CNA2007100727393A patent/CN101186329A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774875A (en) * | 2012-07-30 | 2012-11-14 | 西安理工大学 | Preparation method of octahedral zinc oxide crystals with micrometer-nanometer pore micro structures |
| CN106006708A (en) * | 2016-05-23 | 2016-10-12 | 渤海大学 | Preparation method of lengthened octahedral hierarchical structure material of ZnO |
| CN106006708B (en) * | 2016-05-23 | 2017-10-31 | 渤海大学 | A kind of zinc oxide elongates the preparation method of octahedra hierarchical organization material |
| CN108163884A (en) * | 2018-03-21 | 2018-06-15 | 淮阴师范学院 | A kind of polyhedron zinc oxide and preparation method thereof |
| CN111924871A (en) * | 2020-07-27 | 2020-11-13 | 广州大学 | Octahedral zinc oxide/carbon composite material and preparation method and application thereof |
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