CN104894640B - ZnO classifying nanos array and preparation method and application on a kind of graphene substrate - Google Patents
ZnO classifying nanos array and preparation method and application on a kind of graphene substrate Download PDFInfo
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- CN104894640B CN104894640B CN201510245224.3A CN201510245224A CN104894640B CN 104894640 B CN104894640 B CN 104894640B CN 201510245224 A CN201510245224 A CN 201510245224A CN 104894640 B CN104894640 B CN 104894640B
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Abstract
The present invention discloses the classification ZnO nano array on a kind of graphene substrate on ZnO classifying nanos array and preparation method and application, including graphene nanometer sheet substrate and graphene nanometer sheet substrate.Classification ZnO nano array on the graphene nanometer sheet substrate is the classification ZnO nano array without catalytic CVD growth on graphene nanometer sheet substrate.The invention also discloses the preparation method and application of above-mentioned classification ZnO nano array.Compared with prior art, the advantages of present invention is with without Depositing Metal Catalyst and other forming core layers of deposition, and the ZnO nano array prepared can be transferred to flexible substrate and high heat conduction substrate, be advantageous to prepare efficient, flexible, high-performance ZnO base device.
Description
Technical field
The present invention relates to ZnO classifying nano arrays and preparation method thereof, more particularly to grow ZnO points on graphene substrate
Level nano-array and preparation method thereof, application.
Background technology
Zinc oxide ZnO (band gap at room temperature width is 3.37eV) is the direct band-gap semicondictor material of II-VI race's wurtzite structure
Material, bound exciton combination can be up to 60meV, and simultaneous oxidation zinc abundant raw materials are cheap, the advantages that environmental sound, quilt
It is widely used in the fields such as surface acoustic wave device, microelectronics and opto-electronic device.At present, One-Dimensional ZnO nano-array is demonstrate,proved
It is real that there is unique physical characteristic, such as quantum size effect, skin effect etc., it is current international nano photoelectronic devices field
Forward position and focus.One-Dimensional ZnO nano-array is the component of important 1-dimention nano opto-electronic device.Based on the heterogeneous nanometers of ZnO
Structure is widely used to field-effect transistor, gas sensor, photo-detector, solar cell, photocatalysis, Piezoelectric Driving
Device.Graphene has high carrier mobility (230000cm2/Vs), height as most thin monoatomic layer two-dimensional material
Thermal conductivity (3000W/mK) and superior optical characteristics (absorptivity of single-layer graphene be 2.3%) and mechanical characteristic
(tensile strength is up to 130GPa), this explanation graphene for prepare efficiently, flexibility, high performance device provide it is excellent feasible
Property.However, it is difficult to directly in pure graphene film layer Epitaxial growth One-Dimensional ZnO nano-array.This is mostly derived from pure
Graphene film its sp2 hydridization C atomic level surfaces property it is stable, be used to being supplied to metallic atom to carry out without unnecessary dangling bonds anti-
Forming core is answered, so as to cause ZnO nucleation rates low, it is difficult to direct growth ZnO nano array.Therefore growth ZnO receives on graphene substrate
Rice array is always the focus and difficult point studied.
Researcher in the majority employs nucleation rates of the related measure increase ZnO on graphene layer, and conclusion mainly has following two
Kind method：(1) pre-deposition metal Au or Ni etc. on graphene substrate, it is close to increase ZnO forming cores by adding metallic catalyst
Degree, after by VLS methods (Vapor-Liquid-Solid) catalytic growth One-Dimensional ZnO nano-array, still, catalytic growth method easily exists
Metal pollutant is introduced in material.(2) the pre-deposition ZnO seeds forming core layer on graphene substrate.ZnO is previously deposited by insertion
Seed Layer etc. is used as forming core layer, then passes through hydro-thermal method synthesizing one-dimensional ZnO nano array.But hydro-thermal method ZnO Seed Layers can not
It is evenly distributed on graphene substrate, it is therefore desirable in other decorative layer materials of graphene elder generation pre-deposition, such as conducting polymer
Thing so that increase exogenous impurity, and add organic matter and cause the reduction of device temperature in use.
As can be seen here, to make on graphene zno-based efficiently, flexible, high performance device really realize extensive use, most at all
Method be exactly to solve the problems, such as One-Dimensional ZnO nano-array forming core difficulty on graphene substrate, realize on graphene layer without catalysis
With not introducing impurity direct growth One-Dimensional ZnO nano-array.
The content of the invention
In order to overcome the disadvantages mentioned above of prior art and deficiency, an object of the present invention is that providing one kind is grown in stone
Classification ZnO nano array on black alkene nanometer sheet substrate, have the advantages that forming core is simple, high quality, flexibility, high heat conduction, and make
Standby cost is cheap.The second object of the present invention is to provide the classification ZnO nano array system on above-mentioned graphene nanometer sheet substrate
Preparation Method.The third object of the present invention is the application for providing the classification ZnO nano array on above-mentioned graphene nanometer sheet substrate.
The purpose of the present invention is achieved through the following technical solutions：
ZnO nano array, including graphene nanometer sheet substrate and graphene nanometer sheet are classified on a kind of graphene substrate
The classification ZnO nano array without catalytic CVD growth, described graphene nanometer sheet are spun on Si or Sapphire Substrate on substrate
On.
The preparation method of ZnO nano array is classified on a kind of graphene substrate, is comprised the following steps：
(1) use graphene nanometer sheet that the graphene nanometer sheet of preparation is spun on Si or Sapphire Substrate for substrate,
Spin coating 1-3 times for several times, spin speed 1000-6000rmp；
(2) substrate by graphene nanometer sheet spin coating in step (1) is put into CVD horizontal pipe furnaces, using chemical gaseous phase
Deposit CVD without catalytic growth be classified ZnO nano array, by control tubular type furnace technology parameter atmosphere flow oxygen flow,
Argon flow amount；Growth temperature；Growth time, graphene substrate placement location in 1-3cm diameter quartz tubes, urge by final directly nothing
Change grows classification ZnO nano array with no damage.
Further, the preparation method of ZnO nano array is classified on described graphene substrate, is prepared in step (1)
Graphene nanometer sheet a diameter of 5-100um, thickness 0.5-2nm, concentration 0.1-1mg/ml.
Further, the preparation method of ZnO nano array is classified on described graphene substrate, control pipe in step (2)
Formula furnace technology parameter is as follows, atmosphere flow：Oxygen flow is 40-200sccm, argon gas 40-200sccm；Growth temperature：600-
800℃；Growth time：30-120min.
Further, the preparation method of ZnO nano array, control tubular type furnace technology ginseng are classified on described graphene substrate
As follows, the atmosphere flow of number：Oxygen flow is 100sccm, argon gas 100sccm；Growth temperature：700℃；Growth time：
60min, graphene substrate are positioned in 2cm diameter quartz tubes.
Further, the application of ZnO nano array is classified on described graphene substrate, the classification ZnO nano array is used
In preparing zno-based UV photodetector.
Further, the application of ZnO nano array is classified on described graphene substrate, the classification ZnO nano array is used
In preparing zno-based LED component.
Further, the application of ZnO nano array is classified on described graphene substrate, the classification ZnO nano array is used
In preparation ZnO hybrid solar cell devices.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) present invention uses graphene nanometer sheet as substrate, without catalyst and other forming core Seed Layers.Using graphite
Alkene nanometer sheet, which makees substrate, can be greatly enhanced the nucleation rate of semi-conducting material, this mainly due to：Graphene nanometer sheet has in itself
There is substantial amounts of seamed edge step, dangling bonds more than needed, forming core of the increase nano material on graphene substrate can be provided for reaction forming core
Point, so as to form the constituency of nano material without catalytic growth pattern.This is both without pre-deposition metallic catalyst and other shape seeds
Stratum nucleare, reaches the effect for avoiding bringing the pollutions such as exogenous impurity, solves the problems, such as forming core difficulty again.This is on current graphene substrate
The phenomenon ignored in growth ZnO nano material research.
(2) what the present invention was obtained is classification ZnO nano array.Graphene nanometer sheet can provide selective area growth, so as to
Classification nanostructure is obtained, its pattern has close relationship with deposition process parameters, can grown by adjusting process parameter
It is classified ZnO nano-wire/post array.
(3) classification ZnO nano-wire/post array is prepared, its defect concentration is low, higher than surface, can increase substantially nitridation
The sundries part such as efficiency of semiconductor laser, light emitting diode and solar cell.
(4) use graphene nanometer sheet to be readily available as substrate, it is cheap, and can be transferred to flexible substrate with
And on high heat conduction substrate, be advantageous to prepare efficient, flexible, high-performance ZnO base device.
Brief description of the drawings
Fig. 1 is the schematic cross-section that ZnO nano array is classified on graphene nanometer sheet substrate prepared by the present invention.
Fig. 2 is the XRD test charts that ZnO nano array is classified on graphene nanometer sheet substrate prepared by the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph that ZnO nano array is classified on graphene nanometer sheet substrate prepared by the present invention.
Fig. 4 is to be classified ZnO nano array photoresponse test chart on graphene nanometer sheet substrate prepared by the present invention.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not
It is limited to this.
Embodiment 1
The present embodiment is grown in the preparation method that ZnO nano array is classified on graphene nanometer sheet substrate, including following step
Suddenly：
(1) graphene nanometer sheet is used as substrate：By the graphene nanometer sheet of preparation, (a diameter of 5-15um, thickness are
0.5nm, concentration 0.1mg/ml) typical substrates such as n-Si substrates are spun on, the spin coating number of plies is 3 times for several times, spin speed
1000rmp；
(2) CVD is classified ZnO nano array without catalytic growth：The substrate of above-mentioned graphene nanometer sheet spin coating is put into CVD
In horizontal pipe furnace, CVD is vapor-deposited without catalytic growth classification ZnO nano array using general chemical.By controlling tubular type
Furnace technology parameter：Atmosphere flow (oxygen flow 40sccm, argon gas 40sccm), 600 DEG C of growth temperature, growth time
120min, graphene substrate placement location finally directly grow classification with no damage in 1cm diameter quartz tubes without catalysis
ZnO nano array.
As shown in figure 1, ZnO nano array is classified on growth graphene nanometer sheet substrate prepared by the present invention, including Si linings
Bottom 11, spin coating different parameters graphene nanometer sheet 12, growth graphene nanometer sheet substrate on be classified ZnO nano array 13.
Fig. 2 is the XRD test charts that ZnO nano array is classified on graphene nanometer sheet substrate prepared by the present invention.Test
To ZnO (0002) and (0004) face, show that ZnO nano array prepared by the present invention has extraordinary crystalline quality.
Fig. 3 is the scanning electron microscope (SEM) photograph that ZnO nano array is classified on graphene nanometer sheet substrate prepared by the present invention.Can by figure
Know, the classification ZnO of graphene nanometer sheet Grown receives to grow diameter 150nm, hexagonal column and monocrystalline buergerite ZnO
Rice array, while the region for not covering graphene nanometer sheet does not form ZnO nano array then.
Fig. 4 is to be classified ZnO nano array photoresponse test chart on graphene nanometer sheet substrate prepared by the present invention.Can by figure
Know, obtain good I-V characteristic and response characteristics to light, due to the insertion of graphene nanometer sheet, photoresponse is rapid, illustrates carrier
Injection rate is fast.Show to be classified ZnO nano array either electrical properties also on graphene nanometer sheet substrate prepared by the present invention
It is on optical properties, all with extraordinary performance.Using being classified ZnO on graphene nanometer sheet substrate manufactured in the present embodiment
It is as follows that nano-array prepares the step of zno-based UV photodetector：Received in the Si substrate spin coating graphenes that above-mentioned steps obtain
Classification ZnO nano array is grown after rice piece, then Ohmic contact is formed through electron beam evaporation Au/Pt；Finally by N2Atmosphere
Lower annealing.The length for being wherein classified ZnO nano array is about 5 μm, diameter about 100nm.N-Si/Graphene nanometers are prepared
Piece/classification ZnO nano array/Au/Pt photo-detectors.
Embodiment 2
The present embodiment is grown in the preparation method that ZnO nano array is classified on graphene nanometer sheet substrate, including following step
Suddenly：
(1) graphene nanometer sheet is used as substrate：By the graphene nanometer sheet of preparation, (a diameter of 50-100um, thickness are
2nm, concentration 1mg/ml) it is spun on other substrates, the typical substrate such as Si substrates, Sapphire Substrate, the spin coating number of plies for several times 1
It is secondary, spin speed 6000rmp；
(2) CVD is classified ZnO nano array without catalytic growth：The substrate of above-mentioned graphene nanometer sheet spin coating is put into CVD
In horizontal pipe furnace, CVD is vapor-deposited without catalytic growth classification ZnO nano array using general chemical.By controlling tubular type
Furnace technology parameter：Atmosphere flow (oxygen flow 200sccm, argon gas 200sccm), 800 DEG C of growth temperature, growth time
30min, graphene substrate placement location finally directly grow classification ZnO with no damage in 3cm diameter quartz tubes without catalysis
Nano-array.
Zno-based LED component is prepared using ZnO nano array is classified on graphene nanometer sheet substrate manufactured in the present embodiment
Step is as follows：Grow the p-type classification GaN nanometers of column Mg doping successively in the classification ZnO nano array that above-mentioned steps obtain
Array；Again Au/Pt Ohmic contacts and schottky junction are formed through electron beam evaporation；Finally by N2Annealed under atmosphere, to improve p
The carrier concentration and mobility of type GaN nano-arrays.The length for being wherein classified ZnO nano array is about 2 μm, and diameter is about
500nm；The length of the p-type classification GaN of Mg doping nano-array is about 500nm, diameter about 500nm.Si/ is prepared
Graphene nanometer sheets/classification ZnO nano array/graded p GaN nano-arrays/Au/Pt hetero-junctions LED component.
Embodiment 3
The present embodiment is grown in the preparation method that ZnO nano array is classified on graphene nanometer sheet substrate, including following step
Suddenly：
(1) graphene nanometer sheet is used as substrate：By the graphene nanometer sheet of preparation, (a diameter of 15-50um, thickness are
1nm, concentration 0.5mg/ml) it is spun on other substrates, the typical substrate such as n-Si and Sapphire Substrate, the spin coating number of plies for several times 2
It is secondary, spin speed 3000rmp；
(2) CVD is classified ZnO nano array without catalytic growth：The substrate of above-mentioned graphene nanometer sheet spin coating is put into CVD
In horizontal pipe furnace, CVD is vapor-deposited without catalytic growth classification ZnO nano array using general chemical.By controlling tubular type
Furnace technology parameter：Atmosphere flow (oxygen flow 100sccm, argon gas 100sccm), 700 DEG C of growth temperature, growth time
60min, graphene substrate placement location finally directly grow classification ZnO with no damage in 2cm diameter quartz tubes without catalysis
Nano-array.
ZnO solar cells are prepared using ZnO nano array is classified on graphene nanometer sheet substrate manufactured in the present embodiment
The step of device, is as follows：PECVD deposits CH3NH3PbI3 successively in the classification ZnO nano array that above-mentioned steps obtain, then sinks
Product hole transmission layer (HTM), most form Ohmic contact through electron beam evaporation Au/Pt afterwards.Wherein, it is classified the length of ZnO nano array
Spend for 3 μm, CH3NH3PbI3 thickness 500nm, hole transmission layer (HTM) 200nm.Be prepared Si/Graphene nanometer sheets/point
Level ZnO nano array/CH3NH3PbI3/HTM/Au/Pt hybrid solar cells.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (1)
1. the preparation method of ZnO nano array is classified on a kind of graphene substrate, it is characterised in that comprise the following steps：
(1) graphene nanometer sheet is used the graphene nanometer sheet of preparation to be spun on for substrate on Si or Sapphire Substrate, spin coating
Number of plies 1-3 times for several times, spin speed 1000-6000rmp；
(2) substrate by graphene nanometer sheet spin coating in step (1) is put into CVD horizontal pipe furnaces, using chemical vapor deposition
CVD is classified ZnO nano array without catalytic growth, by controlling tubular type furnace technology parameter：Oxygen flow, argon gas stream in atmosphere
Amount, and growth temperature, growth time are controlled, by graphene substrate placement location in 1-3cm diameter quartz tubes, final direct nothing
Catalysis grows classification ZnO nano array with no damage；
The graphene nanometer sheet a diameter of 5-100um, thickness 0.5-2nm, concentration 0.5-1mg/ml prepared in step (1)；
Control tubular type furnace technology parameter is as follows in step (2), atmosphere flow：Oxygen flow is 40-200sccm, argon gas 40-
200sccm；Growth temperature：700℃；Growth time：60-120min.
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| CN105259218B (en) * | 2015-10-28 | 2018-06-05 | 上海交通大学 | A kind of zinc oxide nanowire-graphene gas sensor and preparation method thereof |
| CN106526716B (en) * | 2016-11-22 | 2018-06-22 | 武汉华星光电技术有限公司 | A kind of production method and display device of micro-nano structure antireflective film |
| CN106835265B (en) * | 2017-03-15 | 2019-01-01 | 厦门大学 | A kind of direct method of growth of zinc oxide nano column array on substrate |
| CN107403853B (en) * | 2017-06-16 | 2018-10-23 | 河南大学 | A kind of ZTO-ZnO/CBS-GSs flexible thin-film solar cells and preparation method thereof |
| CN113224186A (en) * | 2021-05-10 | 2021-08-06 | 南京邮电大学 | Flexible self-driven fiber ultraviolet photoelectric detector based on graphene/zinc oxide heterojunction |
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| CN1313377C (en) * | 2005-07-14 | 2007-05-02 | 天津大学 | Method for large scale quick preparation of one-dimension zinc oxide array thin film in aqueous solution |
| CN100494308C (en) * | 2006-12-12 | 2009-06-03 | 天津理工大学 | Preparing process of nano ZnO line array coated with nano TiO2 particles |
| CN100428502C (en) * | 2006-12-27 | 2008-10-22 | 电子科技大学 | Method for preparation of a-b orientated ZnO nanometer linear array |
| CN101845619B (en) * | 2010-05-07 | 2012-12-05 | 西南石油大学 | Method for preparing ZnO nano needle arrays |
| US8878157B2 (en) * | 2011-10-20 | 2014-11-04 | University Of Kansas | Semiconductor-graphene hybrids formed using solution growth |
| CN102623604B (en) * | 2012-04-11 | 2014-06-25 | 中国科学院半导体研究所 | ZnO nanorod light-emitting diode (LED) and producing method thereof |
| CN102903616A (en) * | 2012-10-22 | 2013-01-30 | 西安电子科技大学 | ZnO substrate-based graphene CVD direct epitaxial growth method and manufactured device |
| CN102941079B (en) * | 2012-11-07 | 2014-10-15 | 上海大学 | Method for preparing photoelectric catalyst multilayer ZnO nanowire array |
| CN103258926B (en) * | 2013-04-28 | 2017-02-22 | 西安交通大学 | LED vertical chip structure and manufacturing method |
| CN103346199B (en) * | 2013-07-10 | 2015-09-16 | 合肥工业大学 | Based on the UV photodetector and preparation method thereof of single-layer graphene/nanometic zinc oxide rod array schottky junction |
| CN204271122U (en) * | 2014-12-17 | 2015-04-15 | 广东德力光电有限公司 | A kind of LED chip of composite transparent conductive electrode |
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