CN101798106A - Method for synthesizing ZnO nanometer stick array on large scale - Google Patents
Method for synthesizing ZnO nanometer stick array on large scale Download PDFInfo
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- CN101798106A CN101798106A CN200910311451A CN200910311451A CN101798106A CN 101798106 A CN101798106 A CN 101798106A CN 200910311451 A CN200910311451 A CN 200910311451A CN 200910311451 A CN200910311451 A CN 200910311451A CN 101798106 A CN101798106 A CN 101798106A
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Abstract
The invention discloses a method for synthesizing a ZnO nanometer stick array on a large scale and relates to a method for synthesizing the ZnO nanometer stick array. The method solves the problem that the synthesis of the conventional ZnO nanometer stick array needs to precast a ZnO seed layer on an underlayer and has a complex process. The method for synthesizing the ZnO nanometer stick array on the large scale comprises the following steps of: mixing zinc acetate and methenamine, and dissolving the mixture into deionized water to obtain mixed solution; and then simultaneously putting the mixed solution and a zinc plate into a high-pressure reaction kettle for heating reaction. The method of the invention has the advantages of simpleness and easy implementation, simple equipment, no need of modification of a zinc plate, high yield and low cost; the diameter of the obtained ZnO nanometer stick array is controllable and is between 20 and 60 nm; the ZnO nanometer stick array has good optical performance and hydrophobic performance, is suitable for industrialized large-scale production, has a water contact angle of between 105 and 115 degrees, is applied to the fields of gas-sensitive materials, sensors, photodetectors and the like, and can be used in cleaning equipment and solid oil.
Description
Technical field
The present invention relates to a kind of method of synthetic ZnO nanometer stick array.
Background technology
ZnO is a kind of important semiconductor material with wide forbidden band, except that having excellent optics, electric property, collect piezoelectric property simultaneously, hydrogen storage property, pyroelectric property, field emission performance, multiple performance such as gas-sensitive property have widely it and use in fields such as chemistry, bio-sensing, solar cell, photochemical catalysis, frequency transformer, photoelectron and flat pannel display.The preparation method of one-dimension zinc oxide nanostructure mainly contains two kinds of vapor phase process and liquid phase methods.Gas phase is synthetic generally to need higher temperature and expensive equipment, and output is lower, and reaction parameter is bigger to final pattern influence.Hydrothermal method is simple because of its required equipment, and temperature of reaction is low, and is easy to operate, is fit to scale operation and enjoys people to adopt.Yet existing hydrothermal method need at first prepare the ZnO Seed Layer, and the fine or not growth that directly influences postorder ZnO nanometer rod of the quality of ZnO Seed Layer, the step complexity, and ZnO nanometer rod quality is wayward.
Summary of the invention
The objective of the invention is for solve existing ZnO nanometer stick array synthetic need be on substrate the problem of prefabricated ZnO Seed Layer, complex process, the invention provides a kind of method of synthesizing ZnO nanometer stick array on large scale.
The method of a kind of synthesizing ZnO nanometer stick array on large scale of the present invention realizes by following steps: one, zinc acetate and six methynes, four ammonia are mixed in the back adding deionized water, stirring and dissolving 20～40min, and then adding ammoniacal liquor, stir mixing solutions, wherein the mol ratio of zinc acetate and six methynes, four ammonia is 1: 1, the mol ratio of ammoniacal liquor and zinc acetate is 0.2: 1, and the ratio of the molar weight of zinc acetate and deionized water volume is 1mol: 6L; Two, zinc metal sheet is placed dehydrated alcohol ultrasonic cleaning 20～40min; Three, the zinc metal sheet after the step 2 processing is put into autoclave with mixing solutions, autoclave is heated to 120～150 ℃ then, and is incubated 6～8h, then naturally cooling, take out zinc metal sheet, promptly get the ZnO nanometer stick array with the washed with de-ionized water after drying.
As long as the consumption of mixing solutions in the step 3 of the present invention is the submergence zinc metal sheet.
The method of synthesizing ZnO nanometer stick array on large scale of the present invention is a kind of brand-new, easy synthetic method, and adopting zinc metal sheet is substrate and reactant, need not zinc metal sheet is modified growth ZnO Seed Layer directly synthetic ZnO nanometer rod on zinc metal sheet.The present invention adopts zinc acetate, ammoniacal liquor and six methynes, four ammonia common drugs, and organic solvent six methynes four ammonia need not purify, and cost is low; Appointed condition is simple, and the reaction conditions gentleness generally below 130 ℃, and does not produce obnoxious flavour in the reaction process; Can the disposable preparation of carrying out the high yield zinc oxide nano rod.
Description of drawings
Fig. 1 is the X-ray diffraction test curve figure of the ZnO nanometer stick array that obtains of embodiment one, and wherein * is the Zn characteristic peak; Fig. 2 is embodiment nine synthetic ZnO nanometer stick array scanning electronic microscope (SEM) pattern phenograms; Fig. 3 is embodiment nine synthetic ZnO nanometer stick array scanning electronic microscope (SEM) pattern phenograms; Fig. 4 is embodiment nine synthetic ZnO nanometer stick array transmission electron microscope (TEM) shape appearance figures; Fig. 5 is embodiment nine synthetic ZnO nanometer stick array electron diffraction diffractograms; Fig. 6 is embodiment nine synthetic ZnO nanometer stick array light at room temperature photoluminescence spectrograms; Fig. 7 is embodiment nine synthetic ZnO nanometer stick array contact angle test patterns.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for present embodiment synthesizing ZnO nanometer stick array on large scale realizes by following steps: one, zinc acetate and six methynes, four ammonia are mixed in the back adding deionized water, stirring and dissolving 20～40min, and then adding ammoniacal liquor, stir mixing solutions, wherein the mol ratio of zinc acetate and six methynes, four ammonia is 1: 1, the mol ratio of ammoniacal liquor and zinc acetate is 0.2: 1, and the ratio of the molar weight of zinc acetate and deionized water volume is 1mol: 6L; Two, zinc metal sheet is placed dehydrated alcohol ultrasonic cleaning 20～40min; Three, the zinc metal sheet after the step 2 processing is put into autoclave with mixing solutions, autoclave is heated to 120～150 ℃ then, and is incubated 6～8h, then naturally cooling, take out zinc metal sheet, promptly get the ZnO nanometer stick array with the washed with de-ionized water after drying.
As long as the consumption of mixing solutions in the present embodiment step 3 is the submergence zinc metal sheet.
The method of present embodiment is simple, and equipment is simple, operational safety, and the productive rate height, cost is low, the ZnO nanometer rod purity height that obtains, controllable diameter, repeatability are very high, are easy to large-scale industrialization production.
It is hexagonal wurtzite structure that present embodiment obtains the ZnO nanometer rod, prolongs quick, the evenly growth of (0001) direction, has fine crystalline quality and stoichiometric ratio, controllable diameter is 20～60nm, and length is at 3～4 microns, the size homogeneous, size is uniform distribution on (0001) direction.
Present embodiment is carried out X-ray diffraction test (XRD) with the ZnO nanometer stick array that obtains, test result as shown in Figure 1, by XRD curve among Fig. 1 as can be known, present embodiment synthetic zinc-oxide nano bar structure is hexagonal wurtzite structure (JCPDS No.36-1451), the peak that wherein is marked with " * " symbol is the characteristic peak of zinc simple substance, is designated as the characteristic peak of substrate zinc metal sheet.In addition, there is not any assorted peak again.Illustrate in product, except the zinc substrate that does not have to have reacted, not have other impurity again, the purity height.
The ZnO nanometer stick array that synthetic method of the present invention obtains is a hexagonal wurtzite structure, prolong quick, the evenly growth of (0001) direction, have fine crystalline quality and stoichiometric ratio, controllable diameter, be 20～60nm, length is at 3～4 microns, the size homogeneous, and size is uniform distribution on (0001) direction.
The ZnO nanometer stick array that the present invention obtains has good hydrophobicity, with the contact angle of water be 105 °～115 °.The ZnO nanometer stick array that the present invention obtains has good optical property simultaneously, is light at room temperature photoluminescence under the condition of 245nm at the incident peak, and a broadband emission peak is arranged at the 383nm place.
Method of the present invention is simple, and equipment is simple, operational safety, and the productive rate height, cost is low, the ZnO nanometer stick array controllable diameter that obtains, repeatability is very high, is easy to large-scale industrialization production; The ZnO nanometer stick array that obtains can be applicable to fields such as gas sensitive, transmitter, photo-detector, can be used on automatically cleaning equipment and solid oil simultaneously.
Embodiment two: what present embodiment and embodiment one were different is that stirring and dissolving 30min gets mixing solutions in the step 1.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment is different with embodiment one or two is that to adopt model in the step 2 be the numerical control supersonic cleanser of KQ2200DB, with 50% ~ 99% ultrasonic power ultrasonic cleaning of rated output.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different with embodiment one or two is that to adopt model in the step 2 be the numerical control supersonic cleanser of KQ2200DB, with 99% ultrasonic power ultrasonic cleaning of rated output.Other step and parameter are identical with embodiment one or two.
Embodiment five: that present embodiment and embodiment one to four are different is ultrasonic cleaning 30min in the step 2.Other step and parameter are identical with embodiment one to four.
Embodiment six: what present embodiment and embodiment one to five were different is that zinc metal sheet is that quality purity is 99.98% in the step 2.Other step and parameter are identical with embodiment one to five.
Embodiment seven: what present embodiment and embodiment one to six were different is in the step 3 autoclave to be heated to 125～140 ℃, and is incubated 6.5～7.5h.Other step and parameter are identical with embodiment one to six.
Embodiment eight: present embodiment and embodiment one to six are not in the step 3 autoclave to be heated to 130 ℃ on an equal basis, and insulation 7h.Other step and parameter are identical with embodiment one to six.
Embodiment nine: the method for present embodiment synthesizing ZnO nanometer stick array on large scale realizes by following steps: one, 5mmol zinc acetate and 5mmol six methynes four ammonia are mixed in the back adding 30mL deionized water, stirring and dissolving 30min gets mixing solutions; Two, zinc metal sheet is placed dehydrated alcohol ultrasonic cleaning 30min; Three, the zinc metal sheet after the step 2 processing is put into autoclave with mixing solutions, autoclave is heated to 130 ℃ then, and insulation 7h, naturally cooling takes out zinc metal sheet then, promptly gets the ZnO nanometer stick array with the washed with de-ionized water after drying.
As long as the consumption of mixing solutions in the present embodiment step 3 is the submergence zinc metal sheet.
Present embodiment is carried out scanning electronic microscope (SEM) pattern with synthetic ZnO nanometer stick array and is characterized, and shape appearance figure respectively as shown in Figures 2 and 3.As seen from Figure 2, synthetic ZnO nanometer stick array direction of growth unanimity, size homogeneous; As seen from Figure 3, synthetic ZnO nanometer stick array diameter is 20～60nm, and length is at 3～4 microns, and the top of each nanometer rod and surface all are slick.
Present embodiment is carried out transmission electron microscope (TEM) pattern with synthetic ZnO nanometer stick array and is characterized, shape appearance figure as shown in Figure 4, as seen from Figure 4, the size of ZnO nanometer rod is along direction of growth uniform distribution, be about 20nm, and the ZnO nanorod structure does not have defective.
Present embodiment is carried out the electron diffraction test to synthetic ZnO nanometer stick array, and the gained electron-diffraction diagram as shown in Figure 5.As seen from Figure 5, the direction of growth of nanometic zinc oxide rod array is along (0001) direction, the direction of zinc oxide optimum growth just; By Fig. 5 we also can to draw synthetic ZnO nanometer rod be the hexagonal wurtzite single crystal structure.
The model that present embodiment adopts U.S. SPEX company to produce synthetic ZnO nanometer stick array is that the Ultraluminescence spectrograph of FL-272 is to carry out light at room temperature photoluminescence test under the condition of 245nm at the incident peak, gained light at room temperature photoluminescence collection of illustrative plates as shown in Figure 6, as seen from Figure 6, only one wide emission peak is arranged at about 383nm place, do not have other assorted peaks again, illustrate that the synthetic nanometer stick array has good crystalline quality and stoichiometric ratio.
Present embodiment is carried out contact angle test with synthetic ZnO nanometer stick array, test result as shown in Figure 7, as seen from Figure 7, the water contact angle of synthetic ZnO nanometer stick array is at 110 °.Illustrate that the synthetic nanostructure has good hydrophobic performance.
To sum up, present embodiment synthetic ZnO nanometer rod has good optical property and hydrophobic performance, can be used for fields such as gas sensitive, transmitter, photo-detector, can be used on automatically cleaning equipment and solid oil simultaneously.
Claims (6)
1. the method for a synthesizing ZnO nanometer stick array on large scale, the method that it is characterized in that synthesizing ZnO nanometer stick array on large scale realizes by following steps: one, zinc acetate and six methynes, four ammonia are mixed in the back adding deionized water, stirring and dissolving 20～40min, and then adding ammoniacal liquor, stir mixing solutions, wherein the mol ratio of zinc acetate and six methynes, four ammonia is 1: 1, the mol ratio of ammoniacal liquor and zinc acetate is 0.2: 1, and the ratio of the molar weight of zinc acetate and deionized water volume is 1mol: 6L; Two, zinc metal sheet is placed dehydrated alcohol ultrasonic cleaning 20～40min; Three, the zinc metal sheet after the step 2 processing is put into autoclave with mixing solutions, autoclave is heated to 120～150 ℃ then, and is incubated 6～8h, then naturally cooling, take out zinc metal sheet, promptly get the ZnO nanometer stick array with the washed with de-ionized water after drying.
2. the method for a kind of synthesizing ZnO nanometer stick array on large scale according to claim 1 is characterized in that stirring and dissolving 30min gets mixing solutions in the step 1.
3. the method for a kind of synthesizing ZnO nanometer stick array on large scale according to claim 1 and 2 is characterized in that ultrasonic cleaning 30min in the step 2.
4. the method for a kind of synthesizing ZnO nanometer stick array on large scale according to claim 3 is characterized in that zinc metal sheet is that quality purity is 99.98% in the step 2.
5. according to the method for claim 1,2 or 4 described a kind of synthesizing ZnO nanometer stick array on large scale, it is characterized in that in the step 3 autoclave being heated to 125～140 ℃, and be incubated 6.5～7.5h.
6. according to the method for claim 1,2 or 4 described a kind of synthesizing ZnO nanometer stick array on large scale, it is characterized in that in the step 3 autoclave being heated to 130 ℃, and insulation 7h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092774A (en) * | 2010-12-28 | 2011-06-15 | 电子科技大学 | Preparation method of zinc oxide nano linear array |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
| CN103011255A (en) * | 2012-12-27 | 2013-04-03 | 浙江大学 | Wet chemical preparation method of ultralong zinc oxide nanowire |
-
2009
- 2009-12-15 CN CN200910311451A patent/CN101798106A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092774A (en) * | 2010-12-28 | 2011-06-15 | 电子科技大学 | Preparation method of zinc oxide nano linear array |
| CN102092774B (en) * | 2010-12-28 | 2012-05-23 | 电子科技大学 | Preparation method of zinc oxide nano linear array |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
| CN103011255A (en) * | 2012-12-27 | 2013-04-03 | 浙江大学 | Wet chemical preparation method of ultralong zinc oxide nanowire |
| CN103011255B (en) * | 2012-12-27 | 2014-08-06 | 浙江大学 | Wet chemical preparation method of ultralong zinc oxide nanowire |
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Open date: 20100811 |