CN102553588A - Catalyst for zinc oxide nanowire growth, and application of catalyst - Google Patents
Catalyst for zinc oxide nanowire growth, and application of catalyst Download PDFInfo
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- CN102553588A CN102553588A CN2012100082290A CN201210008229A CN102553588A CN 102553588 A CN102553588 A CN 102553588A CN 2012100082290 A CN2012100082290 A CN 2012100082290A CN 201210008229 A CN201210008229 A CN 201210008229A CN 102553588 A CN102553588 A CN 102553588A
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- zinc oxide
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Abstract
The invention discloses a catalyst for a zinc oxide nanowire and application of the catalyst in growth of the zinc oxide nanowire. The catalyst for the zinc oxide nanowire is an Au/M multilayer film or an Au-M alloy film formed by metal Au and metal M with a mass ratio of 0.2 to 5:1, wherein M is a metal, the eutectic point of which and Zn is below 500 DEG C, preferably, M is a metal, the eutectic point of which and Zn is below 300 DEG C. Compared with gold as a catalyst under similar conditions, the catalyst is used for the growth of the zinc oxide nanowire, and the higher growth rate of the zinc oxide nanowire can be obviously obtained, the density of arrays of the prepared zinc oxide nanowire is larger, the diameter and the length of the nanowire are more uniform, and the grown zinc oxide nanowire has higher crystalline quality.
Description
Technical field
The present invention relates to the preparation field of nano material, used catalyst and the application thereof of particularly a kind of zinc oxide nanowire orthogonal array growth.
Background technology
One dimension oxidisability nano wire has big draw ratio, and big exciton bind energy at room temperature has big energy gap.Therefore have the excellent photoelectric characteristic, having broad application prospects aspect nano laser, field emitting electronic source, solar cell and the gas sensitive device.And controllably the synthesizing zinc oxide nano wire is the basis of its device application.
Chemical vapour deposition technique is to prepare one of the most frequently used method of zinc oxide nanowire, and this method is compared with other method, and the zinc oxide nanowire of being grown has best crystalline quality and orientation.But chemical vapour deposition technique needs very high synthesis temperature (＞500 ℃) usually; Simultaneously; Is diameter, length, the uneven problem of Density Distribution that the Preparation of Catalyst zinc oxide nanowire also exists nano wire with the gold, this gives, and device is integrated to have caused great difficulty.
The present invention intends and in traditional Au catalyst film, mixes low-melting metal, does catalyst film with the Au-M alloy, makes the zinc oxide nanowire of preparation have better Density Distribution and pattern.In the solid method growth course of nano wire gas-liquid; Catalyst and reactant need form the catalyst drop of congruent melting, and the drip gauge mask has higher coefficient of viscosity, help adsorbing vapor-phase reactant; When the reactant of absorption is in hypersaturated state in drop after; Will from drop, separate out, because reactant is constantly separated out deposition, nano wire is constantly growth just.The eutectic point of gold-zinc is more than 400 ℃, so the temperature of zinc oxide nanowire growth is usually all than higher, this big limitations the practical application of nano-material.And in gold thin film, sneak into low melting point and can form the metal of eutectic point with zinc, can reduce the synthesis temperature of zinc oxide nanowire greatly.
Summary of the invention
To the objective of the invention is in order addressing the above problem, to provide a kind of zinc oxide nanowire growth used catalyst
2 o'clock of the object of the invention provide the above-mentioned used application of catalyst aspect the zinc oxide nanowire growth of a kind of zinc oxide nanowire growth.
Adopt new catalyst formulation, it can effectively control its density and pattern in the growth course of preparation zinc oxide nanowire.
Technical scheme of the present invention
The catalyst that the growth of a kind of zinc oxide (ZnO) nano wire is used; For being that Au:M is the formed Au/M multilayer film of 0.2～5:1, Au-M alloy firm by mass ratio by metal A u and metal M; Wherein M is and the eutectic point of the Zn metal below 500 degree; Be preferably and the eutectic point of the Zn metal below 300 degree, like gallium.
The above-mentioned used catalyst of a kind of ZnO nano wire growth, promptly the preparation method of Au/M multilayer film, Au-M alloy firm adopts electron-beam vapor deposition method, specifically comprises the steps:
The preparation of Au/M multilayer film:
With simple metal Au and simple metal Ga is evaporation source, at a-face Al
2O
3Or c-face Al
2O
3Deposit one deck Ga on the backing material earlier, and then the deposition layer of Au, so hocket, topmost one deck is the Au metallic film, finally obtains the catalyst A u/M multilayer film of zinc oxide nanowire; Above-mentioned deposition process control beam power is 5 kW, and sedimentation rate is 0.01A/s, and gross thickness is 1.5-10nm, and thickness in monolayer is adjustable, and the proportion control of Au and Ga is between 0.2～5:1;
The preparation of Au-M alloy firm:
With pure Au and pure Ga metal is evaporation source, adopts the method preparation of codeposition, promptly simultaneously Au and Ga thin film deposition is arrived a-face Al
2O
3Or c-face Al
2O
3On the backing material, thickness is 1.5-10nm, and the ratio between Au and the Ga is regulated through regulating Au film and Ga thin film evaporation speed, and ultimate constituent proportioning is between 0.2～5:1, and the evaporation rate of Au film and Ga film is regulated through regulating beam power.
In addition, catalyst A u/M multilayer film, the Au-M alloy firm of above-mentioned zinc oxide nanowire can also adopt ionic-implantation, promptly control accelerating potential 30kV, and the line size is 0.19nA, and the time is 70ms.
Utilize the above-mentioned used catalyst of a kind of ZnO nano wire growth to carry out the growth of ZnO nano wire, step is following:
(1), will wait the zinc oxide nano powder of mass ratio and graphite powder fully to grind, in the quartz boat of packing into;
Described graphite powder is preferably crossed 300 mesh sieves;
(2), will be coated with the a-face Al of Au/M multilayer film or Au-M alloy firm catalyst
2O
3Or c-face Al
2O
3Backing material is put on the powder of quartz boat;
(3), quartz boat is put in the quartz glass tube, again quartz glass tube is put into tube furnace, and make quartz boat
Aim at the tube furnace centre;
(4), the control heating rate is after 10-60 ℃/min is warming up to 880-1200 ℃, feeds 10-120 Sccm Ar gas, keeps 1-60min, stops Ar, naturally cools to room temperature, the a-face Al of gained
2O
3Or c-face Al
2O
3The grey matter of substrate surface is the ZnO nano wire.
The used catalyst of above-mentioned a kind of ZnO nano wire growth is applicable to the growing and preparing of all kinds of zinc oxide nanowires based on gas-liquid-solid principle.
Beneficial effect of the present invention
The used catalyst of a kind of ZnO nano wire growth of the present invention; Owing to contain the M metal; Like gallium, make it when being used for the growth of ZnO nano wire, make the growth rate of ZnO nano wire greatly improve; In a preferred embodiment of the present invention, the growth rate of the growth rate of ZnO nano wire when using pure Au as the used catalyst of ZnO nano wire growth provides 4 times.
In addition, because the used catalyst of a kind of ZnO nano wire growth of the present invention, owing to contain the M metal; Make it when being used for the growth of ZnO nano wire, the ZnO number of nanowires of growing on the unit are is more, and promptly stand density is big; In a preferred embodiment of the present invention; The stand density of the ZnO nano wire stand density when using pure Au as the used catalyst of ZnO nano wire growth has improved 33.3%, and the diameter Distribution narrow range, generally all about 100nm.
Description of drawings
The photo of the ESEM of the ZnO nano wire of Fig. 1, embodiment 1 gained;
The photo of the ESEM of the ZnO nano wire of Fig. 2, comparative example's 1 gained;
The surface is coated with the a-face Al of Au/Ga alloy firm catalyst among Fig. 3, the embodiment 2
2O
3The EDX of backing material
Power spectrum;
The stereoscan photograph of the ZnO nano wire top view of Fig. 4, embodiment 2 gained under low power lens (4500 times);
The ZnO nano wire side view of Fig. 5, embodiment 2 gained is at the stereoscan photograph of high power lens (40000 times);
The ZnO nano wire top view of Fig. 6, embodiment 2 gained is at the stereoscan photograph of high power lens (40000 times);
The curve map of the diameter Distribution of the ZnO nano wire of Fig. 7, embodiment 2 gained;
The ZnO nano wire side view of Fig. 8, embodiment 3 gained is at the stereoscan photograph of high power lens (12000 times);
The ZnO nano wire top view of Fig. 9, embodiment 3 gained is at the stereoscan photograph of high power lens (8000 times).
The specific embodiment
Below through embodiment and combine accompanying drawing that the present invention is further set forth, but do not limit the present invention.
The used nanowire deposition of the present invention is used the Lindberg tube furnace, and manufacturer is a U.S. Thermo Scientific company;
ESEM adopts Quanta FEG type field emission scanning electron microscope, and manufacturer is FEI Co.;
Focused-ion-beam lithography adopts DualBeamFEI company;
Electron beam evaporation deposition adopts Explorer 14 type electron beam evaporation deposition appearance, and the manufacturer is the U.S.
Denton company.
Embodiment 1
The catalyst that the growth of a kind of zinc oxide nanowire is used is for being that Au:Ga is the formed Au/Ga duplicature of 1.5:1 by metal A u and metal Ga by mass ratio;
The preparation method of the catalyst A u/Ga duplicature that above-mentioned a kind of zinc oxide nanowire growth is used is following:
Adopt a-face Al
2O
3As backing material, the deposited by electron beam evaporation method plates the gallium layer of 1nm on substrate, evaporation rate be 0.01A/s again on substrate the deposited by electron beam evaporation method plate the gold layer of 1.5nm, evaporation rate is 0.01A/s.
The a-face Al that handled with above-mentioned employing electron evaporation method
2O
3Be backing material, with chemical vapour deposition technique growth of zinc oxide nano line, detailed process is following:
(1), will wait the zinc oxide nano powder of mass ratio and the graphite powder of mistake 300 mesh sieves fully to grind, in the quartz boat of packing into;
The a-face Al that is coated with the used catalyst A u/Ga duplicature of zinc oxide nanowire growth that (2), will adopt electron-beam vapor deposition method to obtain
2O
3Backing material is put on the powder of quartz boat;
(3), quartz boat is put in the quartz glass tube, again quartz glass tube is put into tube furnace, and make quartz boat aim at the stove centre;
(4), the control heating rate is after 50 ℃/min is warming up to 910 ℃, feeds 12 Sccm Ar gas, keeps 5min, stops to naturally cool to room temperature with like Ar gas, the substrate surface grey matter that finally obtains is the ZnO nano wire.
The comparative example 1
As a comparison, with the same chemical vapor deposition method condition of embodiment 1 under, the simple metal Au that with thickness is 2.5nm is as the catalyst ZnO nano wire of also having grown.
With ESEM two ZnO nano wire samples of embodiment 1 and comparative example's 1 gained are observed sign, result such as Fig. 3 and shown in Figure 4 respectively.From Fig. 3 and Fig. 4, can find out, under identical growth technique condition, be that the Au/Ga multilayer film is that the ZnO nano wire of catalyst growth is very long with the Au/M multilayer film among the embodiment 1, to such an extent as to twine each other.And the ZnO nano wire sample length of growing when making catalyst with pure Au among the comparative example 1 is short a lot, explains that when there is gallium in the surface of growth substrate the growth rate of ZnO nano wire greatly improves.
Under identical preparation process condition, be that the ZnO nano wire sample average density that catalyst is grown is 9/um with Au-Ga
2With Au is that the ZnO nano wire sample average density that catalyst is grown is 6/um
2, density has improved 33.3%.The growth rate that with Au-Ga is the ZnO nano wire of catalyst growth is 2um/min, and Au be the growth rate of the ZnO nano wire of catalyst growth is 500nm/min, and growth rate has improved 4 times.
Embodiment 2
At first the deposited by electron beam evaporation method is at a-face Al
2O
3The thick Au film of plating one deck 1.5nm on the substrate; Use focused-ion-beam lithography (FIB) method to carry out the implantation of local Ga ion then, the ion beam milling condition is: accelerating potential 30kV, and the line size is 0.19nA; Etching period is 70ms, and the etch areas size is the circle of 20um for diameter.The Au thin film electronic energy dispersive spectrum (EDS) that the Ga+ of focused-ion-beam lithography rear region implants is as shown in Figure 3, as can be seen from Figure 3, the peak of Ga in the EDS collection of illustrative plates, occurred, explains that Ga successfully is implanted in the Au film.
The a face Al that handled with FIB
2O
3Be backing material, use the chemical vapour deposition technique growing ZnO nano-wire, concrete growth course is following:
(1), will wait the zinc oxide nano powder of mass ratio and the graphite powder of mistake 300 mesh sieves fully to grind, in the quartz boat of packing into;
The a-face Al that is coated with the used catalyst A u/Ga alloy firm of zinc oxide nanowire growth that (2), will adopt ionic-implantation to obtain
2O
3Substrate is put on the powder of quartz boat;
(3), quartz boat is put in the quartz glass, again quartz glass tube is put into tube furnace, and make quartz boat aim at the stove centre;
(4), the control heating rate is after 50 ℃/min is warming up to 910 ℃, feeds 12 Sccm Ar gas, keeps 2min, stops Ar, naturally cools to room temperature, the substrate surface grey matter that finally obtains is the ZnO nano wire.
The stereoscan photograph of the ZnO nano wire of gained under low power lens is 4500 times seen Fig. 4, as can be seen from Figure 4, and in the zone that ion beam etching is crossed; The ZnO nano wire is fine and close and even; The orientation that preferred growth is arranged, and around etch areas, the growth of ZnO nano wire is suppressed greatly; The ZnO nano wire of growth is carefully lacked, and density is low.The doping of this explanation Ga makes the ZnO nano wire that the preferential growth trend arranged.
Fig. 5,6 is respectively the side view and the stereoscan photograph of top view under high power lens is 40000 times of the ZnO nano wire of gained.From Fig. 5, Fig. 6, can find out the zone of handling at FIB, ZnO nano wire preferred growth, ZnO nanowire length and diameter uniformity are all better.
Fig. 7 is the curve map of diameter Distribution of the ZnO nano wire of gained.As can be seen from Figure 7, the regional ZnO nano wire of handling through FIB has good uniformity, and the diameter Distribution narrow range is generally all about 100nm.
Embodiment 3
With c face Al
2O
3Be substrate, 1.5nm Au film is a catalyst, carries out the implantation of local Ga ion with FIB technology Local treatment catalyst film; The ion beam milling condition is accelerating potential 30kV; The line size is 0.19nA, and etching period is 70ms, and the etch areas size is the circle of 20um for diameter.
The c face Al that handled with FIB
2O
3Be backing material, use the chemical vapour deposition technique growing ZnO nano-wire, concrete growth course is following:
(1), will wait the zinc oxide nano powder of mass ratio and the graphite powder of mistake 300 mesh sieves fully to grind, in the quartz boat of packing into;
The c face Al that is coated with the used catalyst A u/Ga alloy firm of zinc oxide nanowire growth that (2), will adopt ionic-implantation to obtain
2O
3Substrate is put on the powder of quartz boat;
(3), quartz boat is put in the quartz glass tube, again quartz glass tube is put into tube furnace, and make quartz boat aim at the stove centre;
(4), the control heating rate is after 50 ℃/min is warming up to 910 ℃, feeds 12 Sccm Ar gas, keeps 1min, stops Ar, naturally cools to room temperature, the substrate surface grey matter that finally obtains is the ZnO nano wire.The side view of the ZnO nano-wire array of gained growth and the top view stereoscan photograph under low power lens is 12000 times and 8000 times, respectively like Fig. 8, shown in Figure 9.Can find out from Fig. 8 and Fig. 9,, promptly contain the zone of metal Ga, ZnO nano wire vertical-growth in the zone that FIB handled; And, promptly not containing the zone of metal Ga in the zone of unprocessed mistake, the direction of growth of ZnO nano wire is disorderly and unsystematic orientation.After explaining that substrate is implanted Ga, the direction of growth of ZnO nano wire also can change.
Foregoing is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (9)
1. the used catalyst of zinc oxide nanowire growth, the catalyst that it is characterized in that described zinc oxide nanowire is for being that Au:M is formed Au/M multilayer film of 0.2～5:1 or Au-M alloy firm by metal A u and metal M by mass ratio;
Wherein M is and the metal of eutectic point below 500 degree of Zn, is preferably the metal of eutectic point below 300 degree with Zn.
2. the used catalyst of a kind of zinc oxide nanowire growth as claimed in claim 1, it is characterized in that described metal M for the metal of eutectic point below 300 degree of Zn.
3. the used catalyst of a kind of zinc oxide nanowire growth as claimed in claim 1 is characterized in that described metal M is preferably gallium.
4. the used catalyst of a kind of zinc oxide nanowire growth as claimed in claim 3 is characterized in that described metal A u and metal M are that Au:M is preferably 1.5:1 by mass ratio.
5. like claim 1,2, the used catalyst of 3 or 4 described a kind of zinc oxide nanowires growths, it is characterized in that catalyst is that the gross thickness of Au/M multilayer film or Au-M alloy firm is 1.5-10nm.
6. utilize the method for carrying out the growth of zinc oxide nanowire, it is characterized in that step is following like claim 1,2, the used catalyst of 3 or 4 described a kind of zinc oxide nanowire growths:
(1), Preparation of catalysts;
Adopt electron-beam vapor deposition method or magnetron sputtering method, at a-face Al
2O
3Or c-face Al
2O
3Preparation thickness is Au/M multilayer film or the Au-M alloy firm catalyst film of 1.5-10nm on the backing material, and film deposition rate is 0.01-0.05A/s;
(2), the growth of zinc oxide nanowire
1., will wait the zinc oxide nano powder of mass ratio and graphite powder fully to grind, in the quartz boat of packing into;
2., step (1) is coated with the a-face Al of Au/M multilayer film or Au-M alloy firm catalyst
2O
3Or c-face Al
2O
3Backing material is put on the powder of quartz boat;
3., quartz boat is put in the quartz glass tube, again quartz glass tube is put into tube furnace, and make quartz boat
Aim at the tube furnace centre;
4., the control heating rate is after 10-60 ℃/min is warming up to 880-1200 ℃, feeds 10-120 Sccm Ar gas, keeps 1-60min, stops Ar, naturally cools to room temperature, the a-face Al of gained
2O
3Or c-face Al
2O
3The grey matter on the surface of backing material is zinc oxide nanowire.
7. the method for utilizing the used catalyst of a kind of zinc oxide nanowire growth to carry out the growth of zinc oxide nanowire as claimed in claim 6; It is characterized in that the catalyst A u/M multilayer film of the described zinc oxide nanowire in the step (1) or the preparation employing ionic-implantation of Au-M alloy firm; Control accelerating potential 30kV in the preparation process; The line size is 0.19nA, and the time is 70ms.
8. as the method for utilizing the used catalyst of a kind of zinc oxide nanowire growth to carry out the growth of zinc oxide nanowire as claimed in claim 6, it is characterized in that in the step (2) 1. described in graphite powder preferably cross 300 mesh sieves.
As claim 1,2, the used catalyst of 3 or 4 said growth of zinc oxide nano lines growth be applicable to
The growing and preparing of gas-liquid-solid principle synthesizing zinc oxide nano wire.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020159952A1 (en) * | 2019-01-28 | 2020-08-06 | Global Graphene Group, Inc. | Production of metal nanowires directly from metal particles |
| US10829605B2 (en) | 2015-07-02 | 2020-11-10 | Sabic Global Technologies B.V. | Process and material for growth of adsorbed compound via nanoscale-controlled resistive heating and uses thereof |
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| US7208094B2 (en) * | 2003-12-17 | 2007-04-24 | Hewlett-Packard Development Company, L.P. | Methods of bridging lateral nanowires and device using same |
| CN101407335A (en) * | 2008-08-27 | 2009-04-15 | 上海理工大学 | Method for preparing zinc oxide nano-wire by using zinc nano-particle |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7208094B2 (en) * | 2003-12-17 | 2007-04-24 | Hewlett-Packard Development Company, L.P. | Methods of bridging lateral nanowires and device using same |
| CN101407335A (en) * | 2008-08-27 | 2009-04-15 | 上海理工大学 | Method for preparing zinc oxide nano-wire by using zinc nano-particle |
Non-Patent Citations (2)
| Title |
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| 《功能材料与器件学报》 20081031 彭英才等 "气-液-固法在半导体纳米线生长中的应用" 第867页最后一段 1-5，9 第14卷, 第5期 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10829605B2 (en) | 2015-07-02 | 2020-11-10 | Sabic Global Technologies B.V. | Process and material for growth of adsorbed compound via nanoscale-controlled resistive heating and uses thereof |
| WO2020159952A1 (en) * | 2019-01-28 | 2020-08-06 | Global Graphene Group, Inc. | Production of metal nanowires directly from metal particles |
| US11370023B2 (en) | 2019-01-28 | 2022-06-28 | Global Graphene Group, Inc. | Production of metal nanowires directly from metal particles |
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