CN101993108A - Method for effectively controlling dimensions of ZnO nano material - Google Patents
Method for effectively controlling dimensions of ZnO nano material Download PDFInfo
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- CN101993108A CN101993108A CN 200910067405 CN200910067405A CN101993108A CN 101993108 A CN101993108 A CN 101993108A CN 200910067405 CN200910067405 CN 200910067405 CN 200910067405 A CN200910067405 A CN 200910067405A CN 101993108 A CN101993108 A CN 101993108A
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Abstract
The invention discloses a method for effectively controlling dimensions of a ZnO nano material in the process of preparing the ZnO nano material by using a chemical method, wherein ice water is used as a solvent and the method comprises the processing steps of (1) ice-water solvent preparation, (2) reaction solution preparation and (3) thermal treatment. In the method, ionized water is replaced with the ice water, and the crystal nucleus nucleation speed of a solute in the initial growth process is controlled through reducing the dissolving speed of the solute in the ice water, thereby reducing the growth speed of the material to make the dimensions of the material reduced by about a half compared with a ZnO nano rod made in a normal-temperature solvent, and the controllable dimension growth of the powder material and the ZnO material on a substrate is realized so as to provide important materials for preparing nano electronic devices and nano optoelectronic devices and make the device application of an inorganic semiconductor material become true. The invention has the advantages of simple technical process, obvious control effect, stable optical property and wide application prospect, is economic and practical, is suitable for popularizing, can realize industrial mass production and the like, and the raw materials are wide in source range and can be obtained easily.
Description
Technical field: the present invention relates to take chemical process to prepare in the inorganic semiconductor material process the effectively processing method of its size of control, particularly relate to a kind of on substrate the processing method of the less ZnO nanometer rod of growth size.
Background technology: the one dimension semiconductor nano material has non-linear optical property, photoluminescence, high-luminous-efficiency, lower Laser emission threshold value because of its two-dimentional quantum confinement effect, and good physicalies such as superelevation physical strength, high chemical stability and thermostability are arranged, show huge application potential in a lot of fields, have broad application prospects.At present, the method for preparing the one dimension semiconductor nano material comprises physical method and chemical process two broad aspect, general gas phase transmission method, the thermal evaporation etc. of adopting for physical method.Yet these methods need special equipment, and cost is higher and process of growth is complicated.Comparatively speaking, chemical process, for example hydrothermal method, sol-gel method, microemulsion method and chemical coprecipitation etc., these chemical processes only with after the dissolving of reactant water equal solvent, are put into reaction vessels thermal treatment and are got final product mostly.Compare with physical method, they are easy to operate, and cost is lower and processing condition are simple, generally can finish under cold condition.But, no matter physics or chemical process, the one dimension semiconductor material of its growth, for example: the ZnO nanometer rod, its size is all bigger, can not realize that device uses.Therefore, the preparation that realizes one dimension small size nano material just seems and is even more important.
Summary of the invention: the purpose of this invention is to provide a kind of effective ways of the ZnO of control nano material size, mainly is its oversize problem that can not realize that device is used when solving chemical process and preparing the ZnO nano material.
The effective ways of a kind of ZnO of control nano material size of the present invention are as described below: it is to be solvent with the frozen water, with C
6H
12N
4(vulkacit H) and Zn (NO
3)
26H
2O (zinc nitrate hexahydrate) is a solute, realizes via configuration frozen water solvent, configuration reaction soln and thermal treatment three step process.
Described configuration frozen water solvent is that deionized water is being lower than under-18 ℃ of temperature ice, adds 2-3 times of deionized water again and melts the ice into 0-5 ℃ the frozen water that contains.
Described configuration reaction soln is by C
6H
12N
4With Zn (NO
3)
26H
2The mol ratio of O is 1: 1, C
6H
12N
4With frozen water, Zn (NO
3)
26H
2The weight proportion of O and frozen water is respectively (0.7-3.0): (100-200), (1.4-6.0): ratio (100-200) is with C
6H
12N
4, Zn (NO
3)
26H
2O puts into described frozen water solvent dissolving respectively and forms two kinds of pre-reaction solution, then with the C in two kinds of pre-reaction solution
6H
12N
4Frozen water solution is poured Zn (NO into
3)
26H
2Mix in the O frozen water solution and fully stir and form mixing solutions.
Beneficial effect of the present invention: this invention adopts frozen water to substitute the normal temperature ionized water as solvent, control its nucleus nucleation rate in the initial growth process by reducing the dissolution rate of solute in single solution and its frozen water of mixing solutions, thereby reach the speed of growth that reduces material, it not only can realize the controllable size of powder body material, can also be implemented in the controllable size ordering growth of ZnO material on most of substrates such as silicon substrate, smooth glass substrate, ITO Conducting Glass, finally realize the growth of small size ZnO nano material on substrate.And make material reduce size near half, thoroughly solved the conventional chemical method and prepared the bigger problem of scantling.Compared with prior art have outstanding substantive distinguishing features and obvious improvement.Because the frozen water conditional request is not high, other performance to material does not produce and should not influence, therefore this technology not only has the controlled outstanding advantage of scantling, and has a stable performance, with low cost, obviously improve the characteristics of product optical property, can provide important material for preparing nano electron device and nano photoelectronic devices.The device application of inorganic semiconductor material is become a reality.Realized goal of the invention reliably.Meanwhile, this invention has also that technological process is simple, raw material extensively is easy to get, control effect significantly, not only economy but also practicality, have a extensive future, be fit to promote, can realize advantages such as large-scale industrialization production.
Description of drawings:
Fig. 1 is the ZnO nanorod growth process synoptic diagram of the present invention and ordinary method preparation;
Fig. 2 is the SEM spectrogram of the ZnO nanometer rod of growing on silicon substrate;
Fig. 3 is the PL spectrogram of the ZnO nanometer rod of growing on silicon substrate;
Fig. 4 is the SEM spectrogram of the ZnO nanometer rod of growing on the ITO Conducting Glass.
Embodiment: the present invention is a solvent with the frozen water, with C
6H
12N
4(vulkacit H) and Zn (NO
3)
26H
2O (zinc nitrate hexahydrate) is a solute, at first is configuration frozen water solvent 1, the configuration of frozen water solvent be with deionized water-20---be frozen into ice under 22 ℃ of temperature condition, and then add 2 times of deionized waters and melt the ice into 0-5 ℃ containing frozen water and can use.With reaction raw materials C
6H
12N
4With Zn (NO
3)
26H
2O is according to C
6H
12N
4With Zn (NO
3)
26H
2The mol ratio of O is 1: 1, C
6H
12N
4With frozen water, Zn (NO
3)
26H
2The weight proportion of O and frozen water is put into the frozen water solvent dissolving that configures respectively in the ratio shown in the following table 1 and is formed pre-reaction solution.The proportioning that table 1 has provided 4 groups of two kinds of pre-reaction solution sees table 1 for details
The proportioning information slip of two kinds of pre-reaction solution of table 1 (unit is a weight part)
Then with the C in two kinds of pre-reaction solution of frozen water dissolution with solvents
6H
12N
4Frozen water solution is poured Zn (NO into
3)
26H
2Mix in the O frozen water solution and evenly stir to form mixing solutions and promptly dispose reaction soln 2, it is reaction soln that silicon substrate is tilted to place mixing solutions, heat-treats 3 again under 85-95 ℃ of temperature and gets final product.
In order more clearly to express the present invention, Fig. 1 has provided employing frozen water and two kinds of solvents of deionized water at normal temperature (hereinafter to be referred as frozen water solvent and normal temperature solvent) difference solubilizing reaction thing, the signal of ZnO nanorod growth process, the ZnO nucleus at first forms (step 1) in Fig. 1, makes the ZnO nucleus grow into the ZnO nanometer rod gradually through thermal treatment 3 afterwards.Owing to utilize frozen water to control the dissolution rate and the ZnO nucleation rate (step 2) of single solution and mixing solutions, cause ZnO nanometer rod (step 3) the size difference of finally on substrate, growing, this shows that this method is quite effective to control ZnO nanometer rod size.
Fig. 2 is the ZnO nanometer rod SEM spectrogram that utilizes frozen water solvent and normal temperature solvent to grow on silicon substrate, wherein a and b are that the frozen water solvent is made, and b is that the high power of a is amplified SEM figure, and c and d are the SEM spectrograms of the made ZnO nanometer rod of normal temperature solvent, and d is that the high power of c is amplified SEM figure.Reaction times is 12h.
Fig. 3 is the PL spectrogram that utilizes the ZnO nanometer rod that frozen water solvent and normal temperature solvent grow on silicon substrate, and wherein a is for using the frozen water solvent made, and b is for using the normal temperature solvent made.
And utilize the SEM spectrogram of the ZnO nanometer rod that the normal temperature solvent grows on the ITO Conducting Glass to see a among Fig. 4, b, c, wherein a is growth 3h; B is growth 7h; C is growth 12h; Utilize the SEM spectrogram of the ZnO nanometer rod of frozen water solvent growth to see d among Fig. 4, e, f, wherein d is growth 3h; E is growth 7h; F is growth 12h.
In sum, the present invention is solvent with the frozen water, realize the low temperature obtain solution, by controlling the dissolution rate of single solution and mixing solutions, control and regulate the nucleation rate of nucleus, finally reach the purpose of the size of effective control ZnO nanometer rod, make the made ZnO nanometer rod of itself and normal temperature solvent compare size and reduce closely partly, thus the controllable growth of realization small size semiconductor material.And this methodological science effectively, popularization suits.
Claims (3)
1. effective ways of controlling ZnO nano material size, it is characterized in that: this method is to be solvent with the frozen water, and is made up of the processing step of configuration frozen water solvent (1), configuration reaction soln (2) and thermal treatment (3).
2. the effective ways of control ZnO nano material size according to claim 1, it is characterized in that: described configuration frozen water solvent (1) is that deionized water is being lower than under-18 ℃ of temperature ice, adds 2-3 times of deionized water again and melts the ice into 0-5 ℃ the frozen water that contains.
3. the effective ways of control ZnO nano material size according to claim 1, it is characterized in that: described configuration reaction soln (2) is by C
6H
12N
4With Zn (NO
3)
26H
2The mol ratio of O is 1, C
6H
12N
4With frozen water, Zn (NO
3)
26H
2The weight proportion of O and frozen water is respectively (0.7-3.0): (100-200), (1.4-6.0): ratio (100-200) is with C
6H
12N
4, Zn (NO
3)
26H
2O puts into the above frozen water solvent dissolving respectively and forms two kinds of pre-reaction solution, then with the C in two kinds of pre-reaction solution
6H
12N
4Frozen water solution is poured Zn (NO into
3)
26H
2Mix in the O frozen water solution and fully stir and form mixing solutions.
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|---|---|---|---|
| CN 200910067405 CN101993108A (en) | 2009-08-12 | 2009-08-12 | Method for effectively controlling dimensions of ZnO nano material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910067405 CN101993108A (en) | 2009-08-12 | 2009-08-12 | Method for effectively controlling dimensions of ZnO nano material |
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|---|---|
| CN101993108A true CN101993108A (en) | 2011-03-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106783186A (en) * | 2016-12-22 | 2017-05-31 | 广东昭信光电科技有限公司 | A kind of ZnO nanorod light anode and preparation method thereof, solar cell |
| CN109569563A (en) * | 2018-12-12 | 2019-04-05 | 东华大学 | A kind of preparation method of porous silicon/ZnO nanorod complex light anode |
-
2009
- 2009-08-12 CN CN 200910067405 patent/CN101993108A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106783186A (en) * | 2016-12-22 | 2017-05-31 | 广东昭信光电科技有限公司 | A kind of ZnO nanorod light anode and preparation method thereof, solar cell |
| CN109569563A (en) * | 2018-12-12 | 2019-04-05 | 东华大学 | A kind of preparation method of porous silicon/ZnO nanorod complex light anode |
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Application publication date: 20110330 |