CN103043707A - Preparation method of perpendicular array ZnO nanowire - Google Patents
Preparation method of perpendicular array ZnO nanowire Download PDFInfo
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- CN103043707A CN103043707A CN2013100127012A CN201310012701A CN103043707A CN 103043707 A CN103043707 A CN 103043707A CN 2013100127012 A CN2013100127012 A CN 2013100127012A CN 201310012701 A CN201310012701 A CN 201310012701A CN 103043707 A CN103043707 A CN 103043707A
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Abstract
The invention relates to a preparation method of a perpendicular array ZnO nanowire, belonging to the field of a nanowire preparation method. The method comprises the following processing steps: (1) precursor solution preparation: adding deionized water into a reaction vessel, then adding zinc salt and polyethyleneimine, and stirring at room temperature and normal pressure for 0.5-3 hours, thus obtaining the precursor solution; (2) ultrafiltration: performing ultrafiltration on the precursor solution; (3) spin coating: dropwisely adding the solution obtained through entrapping in the step (2) onto a substrate, and then coating rubber at a rotation speed of 500-3000 rpm; and (4) heat treatment: 1) keeping the rubber-coated substrate at 400-600 DEG C in a normal-pressure oxygen gas atmosphere for 30-120 minutes, and naturally cooling the substrate to room temperature after the expiration of the temperature keeping time; 2) keeping the substrate treated in the substep 1) at 800-1000 DEG C in a normal-pressure oxygen gas atmosphere for 1-10 minutes, and naturally cooling the substrate to room temperature after the expiration of the temperature keeping time; and 3) keeping the substrate treated in the substep 2) at 400-600 DEG C in a 100-3000 Pa oxygen gas atmosphere for 5-30 minutes.
Description
Technical field
The invention belongs to the fabricate of nanowires method field, particularly a kind of preparation method of orthogonal array ZnO nano-wire.
Background technology
Nano material exists following several effect different from traditional material: surface effects, small-size effect, quantum size effect and macro quanta tunnel effect owing to having unique dimensional structure in the nanoscale scope.
ZnO is a kind of direct band gap semiconductor material with wide forbidden band, and its energy gap is 3.37eV at normal temperatures, and high exciton binding energy is about 60meV.The One-Dimensional ZnO nano material has distinguishing feature in performances such as optics, electronic transport, photoelectricity, piezoelectricity, power electricity, an emission, rare magnetic, photochemical catalysis, suction ripples, has demonstrated good application prospect in fields such as sensing, optics, electronics, an emission, piezoelectricity, the energy, catalysis.The orthogonal array ZnO nano-wire is widely used in electronics, photoelectronics and dynamo-electric field of nanometer devices, for example solar cell, field emission device, ultraviolet laser, photodiode and nanometer engine.
The preparation method of orthogonal array ZnO nano-wire has metal organic chemical compound vapor deposition method, template assistant depositing method and solid-liquid-gas epitaxial growth method.(1) preparation flow of metal organic chemical compound vapor deposition: with zinc ethyl (Et
2Zn) and oxygen as reactant, respectively accurately control the two adopt different airsheds, and the Si substrate is placed on the air-flow below, namely get the orthogonal array ZnO nano-wire in 400-500 ℃ of lower thermal treatment 5-60min.The method exists the unmanageable shortcoming of airshed.(2) preparation flow of template assistant depositing method: gold-plated on porous anodic alumina template, template after gold-plated is tipped upside down on the corundum boat that the zinc source is housed, then put into together in the silica tube, being heated to 800-900 ℃ of reaction 10min in argon atmosphere evaporates the Zn powder fully, stop to pass into argon gas this moment, begin to pass into oxygen to normal pressure, treat that temperature is down to room temperature and namely gets the orthogonal array ZnO nano-wire.The shortcoming of the method is: 1. need to carry out gold-plated operation in template, this operation can be introduced unwanted impurity; 2. atmospheric condition is difficult to control.(3) preparation flow of solid-liquid-gas epitaxial growth method: at first need to be gold-plated in substrate, plated film, photoetching array pattern or need to select suitable substrate, then substrate is placed the air-flow lower end, the zinc source is placed on the air-flow upper end, preparation orthogonal array ZnO nano-wire in the mixed gas of argon gas or argon gas and oxygen.There is following shortcoming in the method: 1. need gold-plated in substrate or plated film comes the guide arrays nanowire growth, this process operation is complicated, and can introduce unwanted impurity, can cause simultaneously production cost higher; 2. need to select suitable substrate according to the lattice match degree, such as the GaN substrate, cause high cost; 3. need accurate controlled atmosphere reaction conditions, needed comparison in equipment is expensive.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of orthogonal array ZnO nano-wire is provided, to simplify the operation, improve controllability, and reduce production costs.
The preparation method of orthogonal array ZnO nano-wire of the present invention, processing step is as follows:
(1) preparation precursor aqueous solution
In reaction vessel, add deionized water, then add zinc salt and polymine, under room temperature, normal pressure, stir 0.5 ~ 3h, get precursor aqueous solution; The amount of described zinc salt, deionized water and polymine reaches 1:400:20 ~ 1:80:4 with the mass ratio of the zinc in the zinc salt, deionized water, polymine and is limited;
(2) ultra-filtration
Step (1) gained precursor aqueous solution is carried out ultra-filtration, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
Step (2) is held back gained solution under the rotating speed of 200 ~ 1000rpm, be added drop-wise in the substrate, then with rotating speed gluing 10 ~ 60s of 500 ~ 3000rpm;
(4) thermal treatment
1. the substrate behind step (3) the gained gluing is incubated 30 ~ 120min under normal pressure, oxygen atmosphere, 400 ~ 600 ℃ of conditions, soaking time naturally cools to room temperature with described substrate after expiring,
2. the substrate after 1. step being processed is incubated 1 ~ 10min under normal pressure, oxygen atmosphere, 800 ~ 1000 ℃ of conditions, soaking time naturally cools to room temperature with described substrate after expiring,
3. the substrate after 2. step being processed is incubated 5 ~ 30min under 100 ~ 3000Pa, oxygen atmosphere, 400 ~ 600 ℃ condition.
In the aforesaid method, described zinc salt is zinc nitrate, zinc acetate or zinc chloride.
In the aforesaid method, the molecular weight cut-off that described ultra-filtration operates employed ultra-filtration membrane is 400 ~ 10000 g/mol.
In the aforesaid method, described substrate be (0001) sapphire substrates,
Sapphire substrates,
Sapphire substrates,
In sapphire substrates, (111) silicon base any.
The present invention compared with prior art has following beneficial effect:
1, the precursor aqueous solution of the method for the invention after with ultra-filtration directly is spin-coated in the substrate and can heat-treats, need not in advance gold-plated in the substrate, plated film comes or gold-platedly on template come the guide arrays nanowire growth, not only simplify operation, and can not introduce impurity, and cost-saved.
2, the method for the invention need not to select particular substrate according to the lattice match degree to the wide adaptability of substrate, can save production cost.
3, the method for the invention adopts conventional equipment can realize the control of atmospheric condition, need not to adopt expensive equipment to come accurate controlled atmosphere condition, thereby can reduce production costs, and is easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the SEM photo of orthogonal array ZnO nano-wire under amplifying 10000 times of embodiment 1 preparation;
Fig. 2 is the SEM photo of orthogonal array ZnO nano-wire under amplifying 20000 times of embodiment 1 preparation;
Fig. 3 is the SEM photo of orthogonal array ZnO nano-wire under amplifying 100000 times of embodiment 1 preparation.
Embodiment
Below by embodiment the preparation method of orthogonal array ZnO nano-wire of the present invention is described further.The purity of the employed zinc salt of following each embodiment all 〉=99%, the molecular weight of polymine is 1000, purity is 99%; Employed high-temperature experimental furnace is produced by ring experimental electric furnace company limited in the Tianjin among following each embodiment, and model is SK-G06163-2T.
Embodiment 1
In the present embodiment, the preparation method of orthogonal array ZnO nano-wire is as follows:
(1) preparation precursor aqueous solution
In reaction vessel, add the 40g deionized water, then (mass ratio of the zinc in the zinc nitrate hexahydrate, deionized water, polymine is 1: 80:4) to add 2.275g zinc nitrate hexahydrate and 2g polymine, stirring 2h under the stirring velocity with 2000 rpm under room temperature, the normal pressure, get precursor aqueous solution;
(2) ultra-filtration
It is in the ultra-filtration centrifuge tube of 10000 g/mol that step (1) gained precursor aqueous solution is added molecular weight cut-off, then ultra-filtration centrifuge tube is put into whizzer with the rotating speed centrifugation of 3000rpm, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
(0001) sapphire substrates is put into spin coater, ultra-filtration membrane in the step (2) is held back gained solution in 18s, be added drop-wise under the rotating speed of 600rpm on (0001) sapphire substrates, then with the rotating speed gluing 30s of 2600rpm;
(4) thermal treatment
1. high-temperature experimental furnace is put in the substrate behind step (3) the gained gluing, to stove evacuation, when pressure in the stove reach-stop to vacuumize during 0.095MPa, then pass into high purity oxygen gas pressure to the stove in the stove and reach 0.03MPa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is normal pressure, stove is heated to 500 ℃ and described substrate is incubated 60min under this temperature and normal pressure, after soaking time expires, room temperature is taken out and is naturally cooled in substrate, 2. furnace temperature is risen to 900 ℃, stove is put in substrate after 1. step processed, to stove evacuation, when pressure in the stove reach-stop to vacuumize during 0.095MPa, then pass into high purity oxygen gas pressure to the stove in the stove and reach 0.03 MPa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is normal pressure, with described substrate at normal pressure, 900 ℃ of insulation 3min, after soaking time expires, room temperature is taken out and is naturally cooled in substrate, 3. furnace temperature is down to 500 ℃, stove is put in substrate after 2. step processed, to stove evacuation to furnace pressure reach-stop to vacuumize during 0.095MPa, then passing into high purity oxygen gas pressure to the stove in the stove reaches-0.0922Pa, then on one side pass into high purity oxygen gas in the stove and extract furnace gas out with mechanical pump on one side, keeping the pressure in the stove is 2800Pa, with described substrate at 2800Pa, 500 ℃ of insulation 10min are after soaking time expires, take out substrate, namely grow the orthogonal array ZnO nano-wire in the substrate.The orthogonal array ZnO nano-wire of the present embodiment preparation is that SEM photo under 10000 times, 20000 times, 100000 times is respectively such as Fig. 1, Fig. 2 and shown in Figure 3 in magnification.
Embodiment 2
In the present embodiment, the preparation method of orthogonal array ZnO nano-wire is as follows:
(1) preparation precursor aqueous solution
In reaction vessel, add the 40g deionized water, then add 0.335g zinc acetate and 2g polymine (mass ratio of the zinc in the zinc acetate, deionized water, polymine is 1: 400: 20), stirring 0.5h under the stirring velocity with 2600 rpm under room temperature, the normal pressure, get precursor aqueous solution;
(2) ultra-filtration
It is in the ultra-filtration centrifuge tube of 400 g/mol that step (1) gained precursor aqueous solution is added molecular weight cut-off, then ultra-filtration centrifuge tube is put into whizzer with the rotating speed centrifugation of 1000rpm, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
(0001) sapphire substrates is put into spin coater, ultra-filtration membrane in the step (2) is held back gained solution in 5s, be added drop-wise under the rotating speed of 200rpm on (0001) sapphire substrates, then with the rotating speed gluing 60s of 500rpm;
(4) thermal treatment
1. high-temperature experimental furnace is put in the substrate behind step (3) the gained gluing, to stove evacuation, when pressure in the stove reach-stop to vacuumize during 0.095MPa, then pass into high purity oxygen gas pressure to the stove in the stove and reach 0.03MPa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is normal pressure, stove is heated to 400 ℃ and described substrate is incubated 120min under this temperature and normal pressure, after soaking time expires, room temperature is taken out and is naturally cooled in substrate, 2. furnace temperature is risen to 800 ℃, stove is put in substrate after 1. step processed, to stove evacuation, when pressure in the stove reach-stop to vacuumize during 0.095MPa, then pass into high purity oxygen gas pressure to the stove in the stove and reach 0.03MPa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is normal pressure, with described substrate at normal pressure, 800 ℃ of insulation 1min, after soaking time expires, room temperature is taken out and is naturally cooled in substrate, 3. furnace temperature is down to 400 ℃, stove is put in substrate after 2. step processed, to stove evacuation to furnace pressure reach-stop to vacuumize during 0.095MPa, then passing into high purity oxygen gas pressure to the stove in the stove reaches-0.0949Pa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is 100Pa, with described substrate at 100Pa, 400 ℃ of insulation 5min are after soaking time expires, take out substrate, namely grow the orthogonal array ZnO nano-wire in the substrate.The SEM photo of the orthogonal array ZnO nano-wire of the present embodiment preparation is similar to Fig. 1 ~ Fig. 3.
Embodiment 3
In the present embodiment, the preparation method of orthogonal array ZnO nano-wire is as follows:
(1) preparation precursor aqueous solution
In reaction vessel, add the 40g deionized water, then (mass ratio of the zinc in the zinc chloride, deionized water, polymine is 1: 80:4) to add 1.042g zinc chloride and 2g polymine, stirring 3h under the stirring velocity with 1000 rpm under room temperature, the normal pressure, get precursor aqueous solution;
(2) ultra-filtration
It is in the ultra-filtration centrifuge tube of 1000 g/mol that step (1) gained precursor aqueous solution is added molecular weight cut-off, then ultra-filtration centrifuge tube is put into whizzer with the rotating speed centrifugation of 3000rpm, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
(111) silicon base is put into spin coater, ultra-filtration membrane in the step (2) is held back gained solution in 20s, be added drop-wise under the rotating speed of 1000rpm on (111) silicon base, then with the rotating speed gluing 10s of 3000rpm;
(4) thermal treatment
1. high-temperature experimental furnace is put in the substrate behind step (3) the gained gluing, to stove evacuation, when pressure in the stove reach-stop to vacuumize during 0.095MPa, then pass into high purity oxygen gas pressure to the stove in the stove and reach 0.03MPa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is normal pressure, stove is heated to 600 ℃ and described substrate is incubated 30min under this temperature and normal pressure, after soaking time expires, room temperature is taken out and is naturally cooled in substrate, 2. furnace temperature is risen to 1000 ℃, stove is put in substrate after 1. step processed, to stove evacuation, when pressure in the stove reach-stop to vacuumize during 0.095MPa, then pass into high purity oxygen gas pressure to the stove in the stove and reach 0.03 MPa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is normal pressure, with described substrate at normal pressure, 1000 ℃ of insulation 10min, after soaking time expires, room temperature is taken out and is naturally cooled in substrate, 3. furnace temperature is down to 600 ℃, stove is put in substrate after 2. step processed, to stove evacuation to furnace pressure reach-stop to vacuumize during 0.095MPa, then passing into high purity oxygen gas pressure to the stove in the stove reaches-0.092Pa, then on one side pass into high purity oxygen gas in the stove and discharge furnace gas on one side, keeping the pressure in the stove is 3000Pa, with described substrate at 3000Pa, 600 ℃ of insulation 30min are after soaking time expires, take out substrate, namely grow the orthogonal array ZnO nano-wire in the substrate.The SEM photo of the orthogonal array ZnO nano-wire of the present embodiment preparation is similar to Fig. 1 ~ Fig. 3.
Claims (5)
1. the preparation method of an orthogonal array ZnO nano-wire is characterized in that processing step is as follows:
(1) preparation precursor aqueous solution
In reaction vessel, add deionized water, then add zinc salt and polymine, under room temperature, normal pressure, stir 0.5 ~ 3h, get precursor aqueous solution; The amount of described zinc salt, deionized water and polymine reaches 1:400:20 ~ 1:80:4 with the mass ratio of the zinc in the zinc salt, deionized water, polymine and is limited;
(2) ultra-filtration
Step (1) gained precursor aqueous solution is carried out ultra-filtration, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
Step (2) is held back gained solution under the rotating speed of 200 ~ 1000rpm, be added drop-wise in the substrate, then with rotating speed gluing 10 ~ 60s of 500 ~ 3000rpm;
(4) thermal treatment
1. the substrate behind step (3) the gained gluing is incubated 30 ~ 120min under normal pressure, oxygen atmosphere, 400 ~ 600 ℃ of conditions, soaking time naturally cools to room temperature with described substrate after expiring,
2. the substrate after 1. step being processed is incubated 1 ~ 10min under normal pressure, oxygen atmosphere, 800 ~ 1000 ℃ of conditions, soaking time naturally cools to room temperature with described substrate after expiring,
3. the substrate after 2. step being processed is incubated 5 ~ 30min under 100 ~ 3000Pa, oxygen atmosphere, 400 ~ 600 ℃ condition.
2. the preparation method of described orthogonal array ZnO nano-wire according to claim 1 is characterized in that described zinc salt is zinc nitrate, zinc acetate or zinc chloride.
3. the preparation method of described orthogonal array ZnO nano-wire according to claim 1 and 2 is characterized in that the molecular weight cut-off that described ultra-filtration operates employed ultra-filtration membrane is 400 ~ 10000 g/mol.
4. the preparation method of described orthogonal array ZnO nano-wire according to claim 1 and 2, it is characterized in that described substrate for (0001) sapphire substrates,
Sapphire substrates,
Sapphire substrates,
In sapphire substrates, (111) silicon base any.
5. the preparation method of described orthogonal array ZnO nano-wire according to claim 3, it is characterized in that described substrate for (0001) sapphire substrates,
Sapphire substrates,
Sapphire substrates,
In sapphire substrates, (111) silicon base any.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183373A (en) * | 2013-04-18 | 2013-07-03 | 四川大学 | Horizontal array ZnO nano-wire and preparation method thereof |
| CN107176621A (en) * | 2017-05-03 | 2017-09-19 | 西南大学 | A kind of method and its application for preparing zinc oxide nano film under cryogenic |
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| US20120282645A1 (en) * | 2011-04-27 | 2012-11-08 | Natural History Museum | Nanoparticles |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183373A (en) * | 2013-04-18 | 2013-07-03 | 四川大学 | Horizontal array ZnO nano-wire and preparation method thereof |
| CN103183373B (en) * | 2013-04-18 | 2014-09-03 | 四川大学 | Horizontal array ZnO nano-wire and preparation method thereof |
| CN107176621A (en) * | 2017-05-03 | 2017-09-19 | 西南大学 | A kind of method and its application for preparing zinc oxide nano film under cryogenic |
| CN107176621B (en) * | 2017-05-03 | 2019-01-01 | 西南大学 | A kind of method and its application preparing zinc oxide nano film under cryogenic |
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