CN103043707B - Preparation method of perpendicular array ZnO nanowire - Google Patents
Preparation method of perpendicular array ZnO nanowire Download PDFInfo
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- CN103043707B CN103043707B CN201310012701.2A CN201310012701A CN103043707B CN 103043707 B CN103043707 B CN 103043707B CN 201310012701 A CN201310012701 A CN 201310012701A CN 103043707 B CN103043707 B CN 103043707B
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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, owing to having unique dimensional structure, exists following several effect different from traditional material: surface effects, small-size effect, quantum size effect and macro quanta tunnel effect within the scope of nanoscale.
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.One-Dimensional ZnO nano material has distinguishing feature in the performances such as optics, electronic transport, photoelectricity, piezoelectricity, power electricity, a transmitting, rare magnetic, photochemical catalysis, suction ripple, has demonstrated good application prospect in fields such as sensing, optics, electronics, a transmitting, piezoelectricity, the energy, catalysis.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, accurately control respectively the two and adopt different airsheds, and Si substrate is placed on to air-flow below, at 400-500 DEG C, thermal treatment 5-60min obtains orthogonal array ZnO nano-wire.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 zinc source is housed, then put into together in silica tube, in argon atmosphere, being heated to 800-900 DEG C of reaction 10min evaporates Zn powder completely, now stop passing into argon gas, start to pass into oxygen to normal pressure, treat that temperature is down to room temperature and obtains orthogonal array ZnO nano-wire.The shortcoming of the method is: 1. need in template, carry out gold-plated operation, this operation can be introduced unwanted impurity; 2. atmospheric condition is difficult to control.(3) preparation flow of solid-liquid-gas epitaxial growth method: first need to be gold-plated in substrate, plated film, photoetching array pattern or need to select suitable substrate, then substrate is placed to air-flow lower end, zinc source is placed on to air-flow upper end, in the mixed gas of argon gas or argon gas and oxygen, prepare orthogonal array ZnO nano-wire.There is following shortcoming in the method: 1. need be in substrate gold-plated or plated film carry out guide arrays nanowire growth, this process operation complexity, and can introduce unwanted impurity can cause production cost higher simultaneously; 2. need to select suitable substrate according to lattice match degree, such as GaN substrate, cause high cost; 3. need accurate controlled atmosphere reaction conditions, needed comparison in equipment costliness.
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) prepare precursor aqueous solution
In reaction vessel, add deionized water, then add zinc salt and polymine, under room temperature, normal pressure, stir 0.5 ~ 3h, obtain 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 zinc salt, deionized water, polymine and is limited;
(2) ultra-filtration
Step (1) gained precursor aqueous solution is carried out to ultra-filtration, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
Step (2) is held back to gained solution and under the rotating speed of 200 ~ 1000rpm, be added drop-wise in substrate, then with rotating speed gluing 10 ~ 60s of 500 ~ 3000rpm;
(4) thermal treatment
1. the substrate after step (3) gained gluing is incubated to 30 ~ 120min under normal pressure, oxygen atmosphere, 400 ~ 600 DEG C of conditions, soaking time naturally cools to room temperature by described substrate after expiring,
2. by step 1. substrate after treatment under normal pressure, oxygen atmosphere, 800 ~ 1000 DEG C of conditions, be incubated 1 ~ 10min, soaking time at the expiration after, described substrate is naturally cooled to room temperature,
3. by step 2. substrate after treatment under 100 ~ 3000Pa, oxygen atmosphere, the condition of 400 ~ 600 DEG C, be incubated 5 ~ 30min.
In aforesaid method, described zinc salt is zinc nitrate, zinc acetate or zinc chloride.
In aforesaid method, the molecular weight cut-off that described ultra-filtration operates the ultra-filtration membrane using is 400 ~ 10000 g/mol.
In aforesaid method, described substrate be (0001) sapphire substrates,
sapphire substrates,
sapphire substrates,
any in sapphire substrates, (111) silicon base.
The present invention compared with prior art, has following beneficial effect:
1, the method for the invention is directly spin-coated on the precursor aqueous solution after ultra-filtration in substrate and can heat-treats, without gold-plated in substrate, plated film in advance come or in template gold-plated come guide arrays nanowire growth, not only simplify operation, and can not introduce impurity, and cost-saved.
2, the wide adaptability of the method for the invention to substrate, without selecting particular substrate according to lattice match degree, can save production cost.
3, the method for the invention adopts conventional equipment can realize the control of atmospheric condition, without adopting expensive equipment to carry out accurate controlled atmosphere condition, thereby can reduce production costs, and is easy to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the SEM photo of the orthogonal array ZnO nano-wire prepared of embodiment 1 under amplifying 10000 times;
Fig. 2 is the SEM photo of the orthogonal array ZnO nano-wire prepared of embodiment 1 under amplifying 20000 times;
Fig. 3 is the SEM photo of the orthogonal array ZnO nano-wire prepared of embodiment 1 under amplifying 100000 times.
Embodiment
Below by embodiment, the preparation method of orthogonal array ZnO nano-wire of the present invention is described further.All >=99%, the molecular weight of polymine is 1000 to the purity of the zinc salt that following each embodiment uses, and purity is 99%; The high-temperature experimental furnace using in following each embodiment is produced by Tianjin Zhong Huan experimental electric furnace company limited, 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) prepare precursor aqueous solution
In reaction vessel, add 40g deionized water, then (mass ratio of zinc in zinc nitrate hexahydrate, deionized water, polymine is 1: 80:4) to add 2.275g zinc nitrate hexahydrate and 2g polymine, under stirring velocity with 2000 rpm under room temperature, normal pressure, stir 2h, obtain 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 to molecular weight cut-off, then ultra-filtration centrifuge tube is put into the rotating speed centrifugation of whizzer with 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 step (2) is held back to gained solution and under the rotating speed of 600rpm, in 18s, be added drop-wise in (0001) sapphire substrates, then with the rotating speed gluing 30s of 2600rpm;
(4) thermal treatment
1. the substrate after step (3) gained gluing is put into high-temperature experimental furnace, to stove evacuation, in the time of reach-0.095MPa of pressure in stove, stop vacuumizing, then reach 0.03MPa to passing into high purity oxygen gas to pressure in stove in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is normal pressure, stove is heated to 500 DEG C and described substrate is incubated to 60min under this temperature and normal pressure, after soaking time expires, substrate is taken out and is naturally cooled to room temperature, 2. furnace temperature is risen to 900 DEG C, by step 1. substrate after treatment put into stove, to stove evacuation, in the time of reach-0.095MPa of pressure in stove, stop vacuumizing, then reach 0.03 MPa to passing into high purity oxygen gas to pressure in stove in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is normal pressure, by described substrate at normal pressure, 900 DEG C of insulation 3min, after soaking time expires, substrate is taken out and is naturally cooled to room temperature, 3. furnace temperature is down to 500 DEG C, by step 2. substrate after treatment put into stove, during to reach-0.095MPa of stove evacuation to furnace pressure, stop vacuumizing, then to passing into high purity oxygen gas in stove to reach-0.0922Pa of pressure in stove, then on one side extract furnace gas out with mechanical pump on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is 2800Pa, by described substrate at 2800Pa, 500 DEG C of insulation 10min, after soaking time expires, take out substrate, in substrate, grow orthogonal array ZnO nano-wire.Orthogonal array ZnO nano-wire prepared by the present embodiment magnification be SEM photo under 10000 times, 20000 times, 100000 times respectively as shown in Figure 1, Figure 2 and Figure 3.
Embodiment 2
In the present embodiment, the preparation method of orthogonal array ZnO nano-wire is as follows:
(1) prepare precursor aqueous solution
In reaction vessel, add 40g deionized water, then add 0.335g zinc acetate and 2g polymine (mass ratio of zinc in zinc acetate, deionized water, polymine is 1: 400: 20), under stirring velocity with 2600 rpm under room temperature, normal pressure, stir 0.5h, obtain 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 to molecular weight cut-off, then ultra-filtration centrifuge tube is put into the rotating speed centrifugation of whizzer with 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 step (2) is held back to gained solution and under the rotating speed of 200rpm, in 5s, be added drop-wise in (0001) sapphire substrates, then with the rotating speed gluing 60s of 500rpm;
(4) thermal treatment
1. the substrate after step (3) gained gluing is put into high-temperature experimental furnace, to stove evacuation, in the time of reach-0.095MPa of pressure in stove, stop vacuumizing, then reach 0.03MPa to passing into high purity oxygen gas to pressure in stove in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is normal pressure, stove is heated to 400 DEG C and described substrate is incubated to 120min under this temperature and normal pressure, after soaking time expires, substrate is taken out and is naturally cooled to room temperature, 2. furnace temperature is risen to 800 DEG C, by step 1. substrate after treatment put into stove, to stove evacuation, in the time of reach-0.095MPa of pressure in stove, stop vacuumizing, then reach 0.03MPa to passing into high purity oxygen gas to pressure in stove in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is normal pressure, by described substrate at normal pressure, 800 DEG C of insulation 1min, after soaking time expires, substrate is taken out and is naturally cooled to room temperature, 3. furnace temperature is down to 400 DEG C, by step 2. substrate after treatment put into stove, during to reach-0.095MPa of stove evacuation to furnace pressure, stop vacuumizing, then to passing into high purity oxygen gas in stove to reach-0.0949Pa of pressure in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is 100Pa, by described substrate at 100Pa, 400 DEG C of insulation 5min, after soaking time expires, take out substrate, in substrate, grow orthogonal array ZnO nano-wire.The SEM photo of orthogonal array ZnO nano-wire prepared by the present embodiment 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) prepare precursor aqueous solution
In reaction vessel, add 40g deionized water, then (mass ratio of zinc in zinc chloride, deionized water, polymine is 1: 80:4) to add 1.042g zinc chloride and 2g polymine, under stirring velocity with 1000 rpm under room temperature, normal pressure, stir 3h, obtain 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 to molecular weight cut-off, then ultra-filtration centrifuge tube is put into the rotating speed centrifugation of whizzer with 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 step (2) is held back to gained solution and under the rotating speed of 1000rpm, in 20s, be added drop-wise in (111) silicon base, then with the rotating speed gluing 10s of 3000rpm;
(4) thermal treatment
1. the substrate after step (3) gained gluing is put into high-temperature experimental furnace, to stove evacuation, in the time of reach-0.095MPa of pressure in stove, stop vacuumizing, then reach 0.03MPa to passing into high purity oxygen gas to pressure in stove in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is normal pressure, stove is heated to 600 DEG C and described substrate is incubated to 30min under this temperature and normal pressure, after soaking time expires, substrate is taken out and is naturally cooled to room temperature, 2. furnace temperature is risen to 1000 DEG C, by step 1. substrate after treatment put into stove, to stove evacuation, in the time of reach-0.095MPa of pressure in stove, stop vacuumizing, then reach 0.03 MPa to passing into high purity oxygen gas to pressure in stove in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is normal pressure, by described substrate at normal pressure, 1000 DEG C of insulation 10min, after soaking time expires, substrate is taken out and is naturally cooled to room temperature, 3. furnace temperature is down to 600 DEG C, by step 2. substrate after treatment put into stove, during to reach-0.095MPa of stove evacuation to furnace pressure, stop vacuumizing, then to passing into high purity oxygen gas in stove to reach-0.092Pa of pressure in stove, then on one side discharge furnace gas on one side to passing into high purity oxygen gas in stove, keeping the pressure in stove is 3000Pa, by described substrate at 3000Pa, 600 DEG C of insulation 30min, after soaking time expires, take out substrate, in substrate, grow orthogonal array ZnO nano-wire.The SEM photo of orthogonal array ZnO nano-wire prepared by the present embodiment is similar to Fig. 1 ~ Fig. 3.
Claims (3)
1. a preparation method for orthogonal array ZnO nano-wire, is characterized in that processing step is as follows:
(1) prepare precursor aqueous solution
In reaction vessel, add deionized water, then add zinc salt and polymine, under room temperature, normal pressure, stir 0.5～3h, obtain 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 zinc salt, deionized water, polymine and is limited;
Described zinc salt is zinc nitrate, zinc acetate or zinc chloride, purity >=99%; The molecular weight of described polymine is 1000, and purity is 99%;
(2) ultra-filtration
Step (1) gained precursor aqueous solution is carried out to ultra-filtration, and the ultra-filtration time is limited can not separate liquid;
(3) spin coating
Step (2) is held back to gained solution and under the rotating speed of 200～1000rpm, be added drop-wise in substrate, then with rotating speed gluing 10～60s of 500～3000rpm;
(4) thermal treatment
1. by the substrate after step (3) gained gluing at normal pressure, oxygen atmosphere, 400～600 DEG C of insulation 30～120min, soaking time at the expiration after, substrate is naturally cooled to room temperature,
2. by step 1. substrate after treatment at normal pressure, oxygen atmosphere, 800～1000 DEG C, be incubated 1～10min, soaking time at the expiration after, described substrate is naturally cooled to room temperature,
3. by step 2. substrate after treatment under 100～3000Pa, oxygen atmosphere, the condition of 400～600 DEG C, be incubated 5～30min.
2. the preparation method of orthogonal array ZnO nano-wire according to claim 1, is characterized in that the molecular weight cut-off that described ultra-filtration operates the ultra-filtration membrane using is 400～10000.
3. according to the preparation method of orthogonal array ZnO nano-wire described in claim 1 or 2, it is characterized in that described substrate for (0001) sapphire substrates, (
) sapphire substrates, (
) sapphire substrates, (
) any in sapphire substrates, (111) silicon base.
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| CN103183373B (en) * | 2013-04-18 | 2014-09-03 | 四川大学 | Horizontal array ZnO nano-wire and preparation method thereof |
| 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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| CN102531031A (en) * | 2010-12-08 | 2012-07-04 | 吉林师范大学 | Dimension and position controllable growth process of ZnO nano-wire array being vertical to substrate |
| CN102765743A (en) * | 2012-07-16 | 2012-11-07 | 四川大学 | Preparation of corn-shaped multilevel structure zinc oxide nanorod array film on zinc sheet substrate |
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| US20110052896A1 (en) * | 2009-08-27 | 2011-03-03 | Shrisudersan Jayaraman | Zinc Oxide and Cobalt Oxide Nanostructures and Methods of Making Thereof |
| US20120282645A1 (en) * | 2011-04-27 | 2012-11-08 | Natural History Museum | Nanoparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102531031A (en) * | 2010-12-08 | 2012-07-04 | 吉林师范大学 | Dimension and position controllable growth process of ZnO nano-wire array being vertical to substrate |
| CN102765743A (en) * | 2012-07-16 | 2012-11-07 | 四川大学 | Preparation of corn-shaped multilevel structure zinc oxide nanorod array film on zinc sheet substrate |
Non-Patent Citations (6)
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| "Preferential Growth of Long ZnO Nanowire Array and Its Application in Dye-Sensitized Solar Cells";Chengkun Xu et al.;《J. Phys. Chem. C》;20091216;第114卷(第1期);第125-129页 * |
| "Solution-Grown Zinc Oxide Nanowires";Lori E. Greene et al.;《Inorg. Chem》;20061231;第45卷(第19期);第7535-7543页 * |
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