CN1789136A - Method for producing nano-wire or nano-belt of zinc oxide - Google Patents
Method for producing nano-wire or nano-belt of zinc oxide Download PDFInfo
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- CN1789136A CN1789136A CN 200510122214 CN200510122214A CN1789136A CN 1789136 A CN1789136 A CN 1789136A CN 200510122214 CN200510122214 CN 200510122214 CN 200510122214 A CN200510122214 A CN 200510122214A CN 1789136 A CN1789136 A CN 1789136A
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Abstract
The invention discloses a method for preparing zinc oxide nano line or zinc oxide nano belt, belonging to technology of preparing zinc oxide nano line and zinc oxide nano belt by adglutinating, comprising the flowing steps: mixing the polyvinyl alcohol and deionized water, batch-water heating until dissolves; mixing zinc acetate and polyvinyl alcohol, separating by mechanical stirring and supersonic wave, immersing the silicon, quarte or glass base plate into solution, layinf it on the bottom of the solution, putting the mixing solution into the baking box for procedure drying, transferring the dried sample into Muffle furnace for progressive warming up and calcining, zinc oxide nano line or zinc oxide nano belt is formed on the baseplate. The invention is characterized by the simple process and controllable shape of the zinc oxide nano line or zinc oxide nano belt. The process is compatible with current semiconductor technology because of the low calcining temperature.
Description
Technical field
The present invention relates to a kind of method for preparing zinc oxide nanowire or zinc oxide nano-belt, belong to the technology that sintering prepares zinc oxide nanowire and nano belt.
Background technology
Zinc oxide is a kind of broad-band gap (3.37eV) conductor oxidate, have high melt point and exciton bind energy (60meV), because zinc oxide nanowire and zinc oxide nano-belt depend on the photovoltaic effect of size, and nano structure of zinc oxide is with a wide range of applications in fields such as semiconductor laser, nanometer electronic device, gas sensor and sun power.Because factors such as structure, size and pattern have considerable influence to zinc oxide characteristic and application thereof, nano structure of zinc oxide has the character of a series of excellences, more company and R﹠D institution are engaged in nano structure of zinc oxide, as: the preparation research of nano wire, nano belt, nanometer rod, nano-comb etc.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 zinc oxide nanowire and nano belt, because of this class methods temperature of reaction is higher than 1000 ℃, atmospheric condition is strict, and apparatus expensive etc., be unfavorable for scale operation, incompatible with semiconductor technology, also be unfavorable for the integrated of device.The alumina formwork method is the diameter and the length of controlled oxidation zinc nano wire preferably, but because this method is easy to introduce impurity, also be unfavorable for the device research of nano zinc oxide material.The wet chemical preparation method of zinc oxide can't obtain long nano wire and nano belt at present, has limited the application of zinc oxide in nanometer electronic device.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing zinc oxide nanowire or zinc oxide nano-belt, this procedure is simple, and expense is lower; Can with the semiconductor technology compatibility.
The present invention is realized by the following technical programs: a kind of method for preparing zinc oxide nanowire or zinc oxide nano-belt is characterized in that comprising following process:
1) 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;
2) zinc acetate and polyvinyl alcohol solution are pressed zinc acetate and the mixing in 1: 5～5: 1 of polyvinyl alcohol mass ratio, adopt mechanical stirring and ultrasonic wave to combine and disperse more than the 0.5h;
3) with the mixing solutions of silicon, quartz or glass substrate immersion zinc acetate and polyvinyl alcohol, be tiled in the solution bottom;
4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～10 ℃/min; Speed with 2～8 ℃/min is warming up to 200～220 ℃, insulation 0.5～2h.
5) sample transfer that step 4) is made is in retort furnace, 290～310 ℃ of following roasting 0.5～1h; Speed with 5～10 ℃/min is warming up to 400～420 ℃, insulation 0.5～1h; With speed to 530～560 of 5～10 ℃/min ℃, insulation 0.5～3h forms zinc oxide nanowire or zinc oxide nano-belt on substrate.
Beneficial effect of the present invention is: adopt zinc acetate, polyvinyl alcohol to prepare zinc oxide nanowire or zinc oxide nano-belt, have advantages such as controllability is strong, simple to operate, expense is lower, the length of zinc oxide nanowire and zinc oxide nano-belt can reach more than the 10 μ m.Because polyvinyl alcohol has hydroxyl abundant, that be evenly distributed, hydroxyl on zinc cation and the polyvinyl alcohol interacts, make zinc acetate enrichment in the gap of polyvinyl alcohol, be rapidly heated through staged, in the gap that polyvinyl alcohol forms, decompose, realize zinc oxide nanowire or the controlled preparation of zinc oxide nano-belt by the polyvinyl alcohol water solution of sequence of control intensification and different concns.Because sintering temperature is low, can with the conventional semiconductor process compatible.
Description of drawings
Fig. 1 is scanning electronic microscope (SEM) photo of embodiment 1 prepared zinc oxide nanowire.
Fig. 2 is the SEM photo of embodiment 2 prepared zinc oxide nanowires and zinc oxide nano-belt.
Fig. 3 is the SEM photo of embodiment 3 prepared zinc oxide nano rod nano belt.
Fig. 4 is the SEM photo of embodiment 4 prepared zinc oxide nanowires and zinc oxide nano-belt.
Embodiment
Zinc oxide nanowire and zinc oxide nano-belt with zinc acetate, polyvinyl alcohol preparation are that example illustrates how to implement the present invention, the invention is not restricted to these embodiment.
In quartz beaker, the polyvinyl alcohol with the 2g polymerization degree 1000～1500 under 90 ℃ is dissolved in the 50ml deionized water; Add the 1g zinc acetate, adopt mechanical stirring 0.5h, rotating speed 800 commentaries on classics/min are with the ultrasonic dispersing 0.5h of 40KHz, 150W.Be tiled in the quartz beaker bottom with getting quartz base plate after the etching.Then quartz curette is placed baking oven and be warming up to 120 ℃ with the speed of 5 ℃/min, insulation 0.5h is until oven dry; Speed with 3 ℃/min is warming up to 200 ℃, insulation 1h.With sample transfer in retort furnace, 300 ℃ of following roasting 0.5h; Speed with 5 ℃/min is warming up to 400 ℃, insulation 0.5h; Speed with 8 ℃/min is warming up to 550 ℃, insulation 1h.SEM observes discovery, and formation diameter 30～50nm, length surpass the nano wire of 15 μ m and the nano belt that width 100～500nm, length surpass 20 μ m on substrate, as shown in Figure 1.
Embodiment 2
Present embodiment is similar to embodiment 1, and difference is that the consumption of zinc acetate and polyvinyl alcohol is respectively 2g in the step 1, is warming up to 130 ℃ with the speed of 9 ℃/min, and insulation 0.5h is until oven dry; Speed with 5 ℃/min is warming up to 210 ℃, insulation 1h.With sample transfer in retort furnace, 310 ℃ of following roasting 0.5h; Speed with 7 ℃/min is warming up to 400 ℃, insulation 1h; Speed with 10 ℃/min is warming up to 560 ℃, insulation 1h.SEM observes discovery, and product is by nano belt and about 2～6 μ m of area of the about 100～200nm of width, the about 15 μ m of length
2Zinc oxide squamous thin slice form, also have the nano wire of several about 20～60nm of diameter, as shown in Figure 2.
Embodiment 3
Present embodiment is similar to embodiment 1, and present embodiment is similar to embodiment 1, and difference is that the consumption of zinc acetate and polyvinyl alcohol is respectively 2g and 1g in the step 1, is warming up to 150 ℃ with the speed of 9 ℃/min, and insulation 1h is until oven dry; Speed with 3 ℃/min is warming up to 210 ℃, insulation 1.5h.With sample transfer in retort furnace, 310 ℃ of following roasting 1h; Speed with 10 ℃/min is warming up to 420 ℃, insulation 1h; Speed with 10 ℃/min is warming up to 560 ℃, insulation 3h.SEM observes discovery, and product is made up of the nano belt of width 100～1000nm, the about 6 μ m of length, as shown in Figure 3.
Embodiment 4
Present embodiment is similar to embodiment 3, and difference is that this step only adopts mechanical stirring 0.5h, rotating speed 800 commentaries on classics/min.SEM observes discovery, is made up of the nano belt of the about 200～500nm of width, the about 10 μ m of length in the product, also has the nano belt of the about 2.5 μ m of width, the about 5 μ m of length and the about 50nm of diameter, the length nano wire greater than 6 μ m, as shown in Figure 4.
Claims (1)
1. method for preparing zinc oxide nanowire or zinc oxide nano-belt is characterized in that comprising following process:
1) polyvinyl alcohol of 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;
2) zinc acetate and polyvinyl alcohol solution are pressed zinc acetate and the mixing in 1: 5～5: 1 of polyvinyl alcohol mass ratio, adopt mechanical stirring and ultrasonic wave to combine and disperse more than the 0.5h;
3) with the mixing solutions of silicon, quartz or glass substrate immersion zinc acetate and polyvinyl alcohol, be tiled in the solution bottom;
4) mixing solutions that is equipped with substrate of step 3) is placed baking oven and be warming up to 120～150 ℃, insulation 0.5～3h with the speed of 5～10 ℃/min; Speed with 2～8 ℃/min is warming up to 200～220 ℃, insulation 0.5～2h.
5) sample transfer that step 4) is made is in retort furnace, 290～310 ℃ of following roasting 0.5～1h; Speed with 5～10 ℃/min is warming up to 400～420 ℃, insulation 0.5～1h; Speed with 5～10 ℃/min is warming up to 530～560 ℃, and insulation 0.5～3h forms zinc oxide nanowire or zinc oxide nano-belt on substrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101222147A CN100336728C (en) | 2005-12-07 | 2005-12-07 | Method for producing nano-wire or nano-belt of zinc oxide |
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| CNB2005101222147A CN100336728C (en) | 2005-12-07 | 2005-12-07 | Method for producing nano-wire or nano-belt of zinc oxide |
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| CN100336728C CN100336728C (en) | 2007-09-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525155B (en) * | 2009-04-03 | 2010-12-08 | 天津大学 | Method for preparing manganese sesquioxide one dimension nano material |
| CN101624209B (en) * | 2009-08-19 | 2011-12-07 | 玉林师范学院 | Preparation method of ZnO nanorod |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5972835A (en) * | 1995-09-13 | 1999-10-26 | Research Triangle Institute | Fluidizable particulate materials and methods of making same |
| CN1238256C (en) * | 2003-07-08 | 2006-01-25 | 中国科学院过程工程研究所 | Process for preparing nano zinc oxide |
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2005
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101525155B (en) * | 2009-04-03 | 2010-12-08 | 天津大学 | Method for preparing manganese sesquioxide one dimension nano material |
| CN101624209B (en) * | 2009-08-19 | 2011-12-07 | 玉林师范学院 | Preparation method of ZnO nanorod |
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