CN103224249B - Synthesis method of zinc oxide aggregate - Google Patents
Synthesis method of zinc oxide aggregate Download PDFInfo
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- CN103224249B CN103224249B CN201310186314.0A CN201310186314A CN103224249B CN 103224249 B CN103224249 B CN 103224249B CN 201310186314 A CN201310186314 A CN 201310186314A CN 103224249 B CN103224249 B CN 103224249B
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Abstract
The invention discloses a synthesis method of a zinc oxide aggregate, which comprises the following steps: dissolving zinc acetate in a mixed solution composed of deionized water and anhydrous ethanol to obtain a mixed solution A; dissolving strong alkali in a mixed solution composed of deionized water and diethylene glycol to obtain a mixed solution B; mixing the solution A and solution B while stirring, adding a certain amount of deionized water, and heating to 40-75 DEG C to react for 4 hours; carrying out centrifugation or vacuum filtration on the solution; washing the obtained precipitate with deionized water 3-4 times, adding into an organic vessel, adding a certain amount of deionized water, and closing the organic vessel; putting the organic vessel filled with the solution into a high-pressure autoclave, and carrying out heat treatment at 130-200 DEG C for 4 hours; and centrifuging and collecting the obtained substance. The method has the advantages of novel and reasonable design, simple technique, low cost, simple operation, lower reaction temperature, controllable reaction conditions, controllable grain size and dimension of the prepared zinc oxide aggregate, and easy collection.
Description
Technical field
The present invention relates to a kind of materials synthesis field, specifically, particularly a kind of synthetic method of zinc oxide aggregate.
Background technology
At present, along with shortage and the rapid rise of price of fossil energy, and a large amount of serious environmental pollution using fossil oil to bring, force countries in the world actively to find new renewable free of contamination green energy resource.And sun power is inexhaustible, be the most promising green energy resource without any pollution that can develop in a large number, the development and utilization that a large amount of manpower and materials are devoted to sun power is all dropped in countries in the world.Existingly the most proven technique of sun power is utilized to be utilize silion cell to generate electricity, but the complex manufacturing process of silicon solar cell, energy consumption is high, expensive, is unsuitable for spread.In recent years due to the outstanding representation of a series of oxide-based nanomaterial such as titanium dioxide and zinc oxide in dye sensitization solar battery, photochemical catalyzing, organic photodegradation etc., people are made to see by oxide-based nanomaterial, a large amount of use hope of sun power and the possibility of environmental improvement aspect.In field of dye-sensitized solar cells, research shows, (TiO
2and ZnO) the scattering of light effect of respective wavelength that brings because of its submicron-scale of nanocrystalline coacervate and its relatively large specific surface area make it than common (TiO
2and ZnO) nano particle has higher electricity conversion.And tradition uses (160-180 degree) to be hydrolyzed the method for zinc acetate to obtain the temperature rise rate (wayward) that various zinc oxide aggregate needs to control solution in polyol medium, in addition solution is the organism that viscosity is higher, makes in collection material more difficult.。
Summary of the invention
The object of the present invention is to provide a kind of solution reaction synthetic method of zinc oxide aggregate, and the zinc oxide aggregate being easy to control reaction conditions and preparation is easy to collect.
For achieving the above object, technical scheme of the present invention is: a kind of synthetic method of zinc oxide aggregate, completes in accordance with the following steps:
(1), prepare A, B solution: be dissolved in by a certain amount of zinc acetate in the mixing solutions be made up of according to a certain ratio deionized water and dehydrated alcohol, fully stir simultaneously, make A mixing solutions; A certain amount of highly basic is dissolved in the mixing solutions be made up of according to a certain ratio deionized water and glycol ether, fully stirs simultaneously, make B mixing solutions; The concentration of zinc acetate solution is 0.013 ~ 0.034mol/l; The concentration of strong base solution is 0.018 ~ 0.66mol/l; Described deionized water and the proportioning of dehydrated alcohol are 1/150 ~ 3/150 by volume; Described deionized water and the proportioning of glycol ether are 1/50 ~ 3/50 by volume; Described highly basic and the mol ratio of zinc acetate are 1/2 ~ 1/1.5; Described highly basic is any one in NaOH, KOH, LiOH;
(2), step (1) solution A and B solution are under agitation mixed after, then add a certain amount of deionized water, be heated to 40 ~ 75 degree of reaction 4h; The volume of described deionized water be solution A and B solution volume and 0.1% ~ 1%;
(3), by the solution centrifugal of step (2) gained or suction filtration;
(4) the throw out deionized water wash, by step (3) obtained 3 ~ 4 times, to add in organic container and to add the deionized water of volume 4/5, throw out being disperseed in deionized water, and makes organic container closure;
(5), by step (4) the organic container of solution is housed and inserts autoclave, at 130 ~ 200 degree of thermal treatment 4h;
(6), material collection: by step (5) gained material collected by centrifugation.
Adopt technique scheme, the present invention is a large amount of ethanol because reaction soln has, and makes solution viscosity less, thus can be easy to collect zinc oxide aggregate material; The variable factor (water yield, temperature of reaction) of this reaction is all easy to control, and temperature of reaction is relatively low;
Due to the low viscosity of solution, in order to cost-saving, cut the waste, in described step (3), centrifugal rotating speed is 8000 ~ 10000 turns/min, and the centrifugal time is 1 ~ 2min.
In order to reaction vessel can acid-fast alkali-proof high temperature resistant, in described step (4), organic container is tetrafluoroethylene reaction vessel.
Beneficial effect: the method is novel in design, rationally, technique is simple, with low cost, simple to operate and temperature of reaction is relatively low, the zinc oxide aggregate that reaction conditions is easy to control and prepare is easy to collect.
Accompanying drawing explanation
Fig. 1 is the scanning electronic microscope FESEM figure of the uniform ZnO coacervate of embodiments of the invention 1.
Fig. 2 is the X ray diffracting spectrum (XRD) of the zinc oxide aggregate of embodiments of the invention 1.
Fig. 3 is the scanning electronic microscope FESEM figure of the ZnO coacervate of the thermal treatment temp of embodiments of the invention 1.
Fig. 4 is the scanning electronic microscope FESEM figure of the uniform ZnO coacervate of embodiments of the invention 2.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated:
Embodiment 1
(1), preparing solution A: 5mMol (1.09g) zinc acetate is dissolved in 150ml ethanol and 2ml water; Preparation B solution: 5mMol (O.2g) NaOH is dissolved in 50ml glycol ether and 2ml water.Two solution stir 2h all at normal temperatures makes it fully dissolve.
(2), by step (1) obtain after A, B solution mix under stirring at normal temperature, then add 0.5ml water; Now solution is clarification.
(3), by the solution of step (2) gained be heated to 75 degree on hot plate, make mixing solutions under agitation react 4h.
(4) the milk shape solution centrifugal, by step (3) be obtained by reacting, centrifugal rotating speed is 8000 turns/min, and the centrifugal time is 1min.The intermediate product obtained to proceed to after washing 3 times with water in the tetrafluoroethylene reaction vessel of 50ml and adds 40ml deionized water.
(5) autoclave inserted by the tetrafluoroethylene reaction vessel that, by step (4) solution is housed, in the retort furnace of 200 degree, be incubated 4h.
(6), material collection: by step (5) gained material collected by centrifugation.
Fig. 1 scanning electronic microscope FESEM figure can find out that ZnO is agglomerated into more even bead.Fig. 2 provides X-ray diffraction (XRD) result, and it shows that synthetic product is the ZnO of hexagonal wurtzite structure.Fig. 3 can find out the size of ZnO crystallite under thermal treatment temp.
Embodiment 2
(1), solution A is prepared: 2mMol zinc acetate is dissolved in 150ml ethanol and 1ml water; Preparation B solution: 2mMol LiOH is dissolved in 50ml glycol ether and 1ml water.Two solution stir 1h all at normal temperatures makes it fully dissolve.
(2), by step (1) obtain after A, B solution mix under stirring at normal temperature, then add 0.2ml water; Now solution is clarification.
(3), by the solution of step (2) gained be heated to 40 degree on hot plate, make mixing solutions under agitation react 4h.
(4) the milk shape solution centrifugal, by step (3) be obtained by reacting, centrifugal rotating speed is 10000 turns/min, and the centrifugal time is 2min.The intermediate product obtained to proceed to after washing 4 times with water in the tetrafluoroethylene reaction vessel of 50ml and adds 40ml deionized water.
(5) autoclave inserted by the tetrafluoroethylene reaction vessel that, by step (4) solution is housed, in the retort furnace of 130 degree, be incubated 4h.
(6), material collection: by step (5) gained material collected by centrifugation.
Fig. 4 scanning electronic microscope FESEM figure can find out that ZnO is agglomerated into more even bead.
Embodiment 3
(1), solution A is prepared: 3mMol zinc acetate is dissolved in 150ml ethanol and 3ml water; Preparation B solution: 3mMol NaOH is dissolved in 50ml glycol ether and 3ml water.Two solution stir 3h all at normal temperatures makes it fully dissolve.
(2), by step (1) obtain after A, B solution mix under stirring at normal temperature, then add 2ml water; Now solution is clarification.
(3), by the solution of step (2) gained be heated to 60 degree on hot plate, make mixing solutions under agitation react 4h.
(4) the milk shape solution centrifugal, by step (3) be obtained by reacting, centrifugal rotating speed is 9000 turns/min, and the centrifugal time is 1min.The intermediate product obtained to proceed to after washing 3 times with water in the tetrafluoroethylene reaction vessel of 50ml and adds 40ml deionized water.
(5) autoclave inserted by the tetrafluoroethylene reaction vessel that, by step (4) solution is housed, in the retort furnace of 180 degree, be incubated 4h.
(6), material collection: by step (5) gained material collected by centrifugation.
Claims (3)
1. a synthetic method for zinc oxide aggregate, is characterized in that: complete in accordance with the following steps:
(1), prepare A, B solution: be dissolved in by a certain amount of zinc acetate in the mixing solutions be made up of according to a certain ratio deionized water and dehydrated alcohol, fully stir simultaneously, make A mixing solutions; A certain amount of highly basic is dissolved in the mixing solutions be made up of according to a certain ratio deionized water and glycol ether, fully stirs simultaneously, make B mixing solutions; The concentration of zinc acetate solution is 0.013 ~ 0.034mol/l; The concentration of strong base solution is 0.018 ~ 0.066mol/l; Described deionized water and the proportioning of dehydrated alcohol are 1/150 ~ 3/150 by volume; Described deionized water and the proportioning of glycol ether are 1/50 ~ 3/50 by volume; Described highly basic and the mol ratio of zinc acetate are 1/2 ~ 1/1.5; Described highly basic is any one in NaOH, KOH, LiOH;
(2), step (1) solution A and B solution are under agitation mixed after, then add a certain amount of deionized water, be heated to 40 ~ 75 degree of reaction 4h; The volume of described deionized water be solution A and B solution volume and 0.1% ~ 1%;
(3), by the solution centrifugal of step (2) gained or suction filtration;
(4) the throw out deionized water wash, by step (3) obtained 3 ~ 4 times, to add in organic container and to add the deionized water of volume 4/5, throw out being disperseed in deionized water, and makes organic container closure;
(5), by step (4) the organic container of solution is housed and inserts autoclave, at 130 ~ 200 degree of thermal treatment 4h;
(6), material collection: by step (5) gained material collected by centrifugation.
2. the synthetic method of a kind of zinc oxide aggregate according to claim 1, is characterized in that: in described step (3), and centrifugal rotating speed is 8000 ~ 10000 turns/min, and the centrifugal time is 1 ~ 2min.
3. the synthetic method of a kind of zinc oxide aggregate according to claim 1, is characterized in that: in described step (4), and organic container is tetrafluoroethylene reaction vessel.
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| CN106986374B (en) * | 2017-05-08 | 2018-11-16 | 济南大学 | A kind of high specific surface area and mesoporous zinc-oxide nano cluster and preparation method thereof |
| CN110078112A (en) * | 2019-05-08 | 2019-08-02 | 中国航空发动机研究院 | By the preparation method for the ZnO microsphere that nano dot forms |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101704544A (en) * | 2009-11-13 | 2010-05-12 | 无锡泰达纺织科技有限公司 | Method for preparing zinc oxide nano rod applied to sewage treatment |
| CN101979324A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing monodisperse zinc oxide microspheres |
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| US8268287B2 (en) * | 2010-05-12 | 2012-09-18 | National Chung Cheng University | Zinc oxide nanorod thin film and method for making same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101704544A (en) * | 2009-11-13 | 2010-05-12 | 无锡泰达纺织科技有限公司 | Method for preparing zinc oxide nano rod applied to sewage treatment |
| CN101979324A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing monodisperse zinc oxide microspheres |
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