CN1314594C - Method for preparing nano-rod of zinc oxide or its ordered structure - Google Patents
Method for preparing nano-rod of zinc oxide or its ordered structure Download PDFInfo
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- CN1314594C CN1314594C CNB2005101222151A CN200510122215A CN1314594C CN 1314594 C CN1314594 C CN 1314594C CN B2005101222151 A CNB2005101222151 A CN B2005101222151A CN 200510122215 A CN200510122215 A CN 200510122215A CN 1314594 C CN1314594 C CN 1314594C
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Abstract
The present invention discloses a method for preparing a zinc oxide nano-rod or ordered structure of zinc oxide nano-rod, which belongs to the technology for preparing the zinc oxide nano-rod and nano-rod array by sintering. The method comprises the following steps that zinc acetate is dissolved in deionized water, sodium hydroxide powder is added and thoroughly reacts with the zinc acetate, and deposits are washed by the ionized water; polyvinyl alcohol solution is dissolved in water, and heated in water bath until dissolution; zinc hydroxide deposits and the polyvinyl alcohol solution are mixed, and separated by combining mechanical stirring and supersonic waves; the mixed solution is baked in a baking oven, the surface of a substrate is coated with a layer of film, the substrate coated with the film is transferred into a Muffle furnace and processed through heat treatment, and the zinc oxide nano-rod or the ordered structure of the zinc oxide nano-rod is formed on the substrate. The method of the present invention has the advantage of simple method, the prepared zinc oxide nano-rod or the ordered structure of the zinc oxide nano-rod can be widely used in fields of photology, electricity, etc., and the method can be compatible with the existing semiconductor technology.
Description
Technical field
The present invention relates to a kind of method for preparing zinc oxide nano rod or zinc oxide nano rod ordered structure, belong to the technology that sintering prepares zinc oxide nano rod and nanometer stick array.
Background technology
Zinc oxide is a kind of wide band gap semiconducter oxide compound, has high melt point and exciton bind energy, and zinc oxide has a good application prospect in fields such as photonic crystal, photodiode, transmitter, photo-detectors with its excellent photoelectric properties.Zinc oxide nano rod is a kind of potential Laser emission material, and nanometer stick array has excellent optical property, has the character of a series of excellences, and the preparation of zinc oxide nano rod and array thereof becomes a new research focus.The main at present transfer of metal catalytic gas phase, high temperature pyrolytic cracking (HTP) and the high-temperature physics method of evaporation of adopting prepares nanometic zinc oxide rod array, because of this class methods temperature of reaction height, severe reaction conditions, apparatus expensive, be unfavorable for scale operation, incompatible with semiconductor technology, also be unfavorable for the integrated of device.The alumina formwork method is the diameter of controlled oxidation zinc nanometer rod and the ordered arrangement of length and nanometer rod preferably, but because this method is easy to introduce impurity.Wet chemistry method prepares zinc oxide nano rod and also obtains certain progress, but complicated process of preparation,, structural controllability difference and cost be higher, the agglomeration of nanometer rod is serious, the diameter of nanometer rod also is unfavorable for the microminiaturization of zinc oxide photoelectric device greater than 100nm.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing zinc oxide nano rod or zinc oxide nano rod ordered structure, adopt the zinc oxide nano rod and the zinc oxide nano rod ordered structure of this method preparation can be widely used in fields such as optics, electricity.
The present invention is realized that by the following technical programs a kind of method for preparing zinc oxide nano rod or zinc oxide nano rod ordered structure is characterized in that comprising following process:
1) zinc acetate is dissolved in deionized water, the mol ratio of pressing zinc acetate and sodium hydroxide added sodium hydroxide powder in 1: 0.9～1: 1.2, with the precipitate with deionized water repetitive scrubbing, approached 7 until pH after fully reacting;
2) polyvinyl alcohol of the polymerization degree 1000～1500 is added in the deionized water under 90 ℃, be mixed with mass concentration and be 1～6% polyvinyl alcohol water solution;
3) zinc hydroxide precipitation and polyvinyl alcohol solution are pressed zinc hydroxide and the mixing in 1: 5～5: 1 of polyvinyl alcohol mol ratio, adopt mechanical stirring and ultrasonic wave to combine and disperse 0.5～3h;
4) mixing solutions is placed baking oven be warming up to 100～130 ℃, insulation 10～60min, silicon, quartz or the glass substrate of any surface finish are immersed mixed solution after etching, take out substrate, form the layer of even film at substrate surface, the substrate that is covered with film is placed baking oven, under 100～130 ℃, insulation 2～5h;
5) substrate that will be covered with film is transferred in the retort furnace, and under 500～590 ℃, thermal treatment 0.5～2h forms zinc oxide nano rod or zinc oxide nano rod ordered structure on substrate.
Beneficial effect of the present invention is: adopt zinc acetate, sodium hydroxide and polyvinyl alcohol to prepare zinc oxide nano rod or zinc oxide nano rod ordered structure, promptly have advantages such as controllability is strong, reaction conditions gentleness.Because the micropore that polyvinyl alcohol forms in the substrate surface self-assembly, the hydroxyl interaction through on zinc hydroxide and the polyvinyl alcohol makes zinc hydroxide enrichment in micropore, forms zinc oxide nano rod gradually under 120 ℃; Through the thermal decomposition process of high temperature crystallization and polyvinyl alcohol, form zinc oxide nano rod under 550 ℃, form ordered structure when nanometer rod is intensive at substrate surface.Because sintering temperature is low, preparation technology is simple, can with the conventional semiconductor process compatible.
Description of drawings
Fig. 1 is scanning electronic microscope (SEM) photo of embodiment 1 prepared zinc oxide nano rod.
Fig. 2 is the SEM photo of embodiment 2 prepared zinc oxide nano rods.
Fig. 3 is the SEM photo of embodiment 3 prepared zinc oxide nano rod ordered structures.
Fig. 4 is the SEM photo of embodiment 4 prepared zinc oxide nano rods.
Embodiment
Zinc oxide nano rod or zinc oxide nano rod ordered structure with zinc acetate, sodium hydroxide and polyvinyl alcohol preparation are that example illustrates how to implement the present invention, the invention is not restricted to these embodiment.
The 1g zinc acetate is dissolved in the 30ml deionized water, adds the 1.1g sodium hydroxide powder, with the precipitate with deionized water repetitive scrubbing, approach 7 after fully reacting until pH.In the quartz beaker, the polyvinyl alcohol of the 2g polymerization degree 1000～1500 is mixed with 4% the aqueous solution, 90 ℃ of following heating in water bath are until dissolving.Zinc hydroxide precipitation and polyvinyl alcohol solution are mixed, adopt mechanical stirring 0.5h, rotating speed 800 commentaries on classics/min are with the ultrasonic dispersing 1h of 40KHz, 150W.Place baking oven to be rapidly heated mixing solutions, during liquid thickness to be mixed, silicon substrate is immersed mixed solution, extract the back and form a skim at substrate surface to 120 ℃.The substrate that is covered with film is placed baking oven, under 120 ℃, insulation 2h.The substrate that is covered with film is transferred in the retort furnace, under 550 ℃, thermal treatment 1h.SEM observes discovery, generates the about 40～60nm of some amount diameter, about 0.4～0.7 μ m nanometer rod of length at substrate surface, as shown in Figure 1.
Embodiment 2
Present embodiment is similar to embodiment 1, difference is that the consumption of zinc acetate and polyvinyl alcohol is respectively 1g in the step 1, storing temperature is 110 ℃, maturing temperature is 560 ℃, SEM observes discovery, generate the about 50～80nm of a fairly large number of diameter, about 0.4～0.7 μ m nanometer rod of length at substrate surface, as shown in Figure 2.
Present embodiment is similar to embodiment 1, difference is that the consumption of zinc acetate and polyvinyl alcohol is respectively 2g and 1g in the step 1, maturing temperature is 580 ℃, generated the ordered structure of forming by the zinc oxide nano rod of the about 50～80nm of diameter at substrate surface, the zinc oxide tabular crystal that is mingled with some amount in the ordered structure, as shown in Figure 3.
Embodiment 4
Present embodiment is similar to embodiment 1, difference is to adopt in the step 1 mechanical stirring 0.5h, become the about 30～60nm of comparatively small amt diameter, about 0.3～0.5 μ m zinc oxide nano rod of length at substrate surface dirt, the zinc oxide grain that most of zone is particle diameter 200～400nm is formed, as shown in Figure 4
Claims (1)
1. method for preparing zinc oxide nano rod or zinc oxide nano rod ordered structure is characterized in that comprising following process:
1) zinc acetate is dissolved in deionized water, the mol ratio of pressing zinc acetate and sodium hydroxide added sodium hydroxide powder in 1: 0.9～1: 1.2, with the precipitate with deionized water repetitive scrubbing, approached 7 until pH after fully reacting;
2) polyvinyl alcohol of the polymerization degree 1000～1500 is added in the deionized water under 90 ℃, be mixed with mass concentration and be 1～6% polyvinyl alcohol water solution;
3) zinc hydroxide precipitation and polyvinyl alcohol solution are pressed zinc hydroxide and the mixing in 1: 5～5: 1 of polyvinyl alcohol mol ratio, adopt mechanical stirring and ultrasonic wave to combine and disperse 0.5～3h;
4) mixing solutions is placed baking oven be warming up to 100～130 ℃, insulation 10～60min, silicon, quartz or the glass substrate of any surface finish are immersed mixed solution after etching, take out substrate, form the layer of even film at substrate surface, the substrate that is covered with film is placed baking oven, under 100～130 ℃, insulation 2～5h;
5) substrate that will be covered with film is transferred in the retort furnace, and under 500～590 ℃, thermal treatment 0.5～2h forms zinc oxide nano rod or zinc oxide nano rod ordered structure on substrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101222151A CN1314594C (en) | 2005-12-07 | 2005-12-07 | Method for preparing nano-rod of zinc oxide or its ordered structure |
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| CNB2005101222151A CN1314594C (en) | 2005-12-07 | 2005-12-07 | Method for preparing nano-rod of zinc oxide or its ordered structure |
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| CN1789137A CN1789137A (en) | 2006-06-21 |
| CN1314594C true CN1314594C (en) | 2007-05-09 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100360421C (en) * | 2006-07-31 | 2008-01-09 | 浙江理工大学 | Process for preparing zinc oxide nano-stick |
| CN100582012C (en) * | 2006-09-26 | 2010-01-20 | 中国科学院上海硅酸盐研究所 | Nano porous zinc oxide thin film with high C-axis orientation and preparation method thereof |
| CN101580269B (en) * | 2009-06-22 | 2010-09-01 | 浙江理工大学 | Method for preparing green emission ZnO nano-rod |
| CN101624209B (en) * | 2009-08-19 | 2011-12-07 | 玉林师范学院 | Preparation method of ZnO nanorod |
| CN102199770B (en) * | 2010-03-26 | 2013-03-13 | 中国科学院金属研究所 | Large-area preparation method for zinc oxide nanorod array |
| CN106477621B (en) * | 2016-10-21 | 2018-04-13 | 中南大学 | Stratiform zinc hydroxide, the preparation of zinc-oxide nano cone and stripping means |
| CN114314639A (en) * | 2021-12-30 | 2022-04-12 | 湘潭大学 | Preparation method of two-dimensional material layered zinc oxide nanosheet |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6224937B1 (en) * | 1995-05-08 | 2001-05-01 | Matsushita Electric Industrial Co., Ltd. | Method of manufacturing a zinc oxide varistor |
| CN1557716A (en) * | 2004-01-13 | 2004-12-29 | 上海大学 | Method for manufacturing nano-zinc oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6224937B1 (en) * | 1995-05-08 | 2001-05-01 | Matsushita Electric Industrial Co., Ltd. | Method of manufacturing a zinc oxide varistor |
| CN1557716A (en) * | 2004-01-13 | 2004-12-29 | 上海大学 | Method for manufacturing nano-zinc oxide |
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