CN102251277A - Zinc oxide transparent conductive film and production method thereof - Google Patents

Zinc oxide transparent conductive film and production method thereof Download PDF

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CN102251277A
CN102251277A CN2010102417529A CN201010241752A CN102251277A CN 102251277 A CN102251277 A CN 102251277A CN 2010102417529 A CN2010102417529 A CN 2010102417529A CN 201010241752 A CN201010241752 A CN 201010241752A CN 102251277 A CN102251277 A CN 102251277A
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zinc oxide
oxide transparent
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CN102251277B (en
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王钢
王孟源
童存声
雷秀铮
江灏
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Foshan Zhonghao Photoelectric Technology Co.,Ltd.
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FOSHAN ZHONGHAO PHOTOELECTRIC TECHNOLOGY CO LTD
RESEARCH INSTITUTE OF SUN YAT-SEN UNIVERSITY IN FOSHAN
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Abstract

The invention discloses a zinc oxide transparent conductive film and a production method thereof. The zinc oxide transparent conductive film comprises a ZnO nucleating layer, a ZnO main body layer and a crown nano-cylindrical ZnO layer which are sequentially attached to the surface at one side of a lining material, wherein the crown nano-cylindrical ZnO layer is provided with a plurality of crown nano-cylindrical surfaces; the span of a crown of the crown nano-cylindrical ZnO layer is 10-1000nm; and the distance between the top of the crown to the ZnO main body layer is 10-600nm. The production method comprises the following steps of: pre-treating a growth substrate; pre-depositing; growing the ZnO nucleating layer; growing the ZnO main body layer; and growing the crown nano-cylindrical ZnO layer. ZnOTCL obtained by using the production method of the zinc oxide transparent conductive film can be used for accurately controlling the growth quality and the morphology except for meeting excellent conductive and transparent characteristics and has the surface morphology of the photonic crystal characteristic and higher optical extraction efficiency; and the LED (Light Emitting Diode) external quantum efficiency can be greatly improved, the considerable development of the LED industry is promoted and the realization on the purposes of environment friendliness, energy saving and sustainable development is facilitated.

Description

A kind of zinc oxide transparent conductive film and manufacture method thereof
Technical field
The present invention relates to technical field of semiconductors, be specifically related to a kind of transparent conductive film and manufacture method thereof, particularly a kind of zinc oxide transparent conducting film and manufacture method thereof.
Background technology
Gallium nitride light-emitting diode (GaN-LED) is as the core devices of realizing solid-state illumination, and external quantum efficiency is low to be its major obstacle that further develops.For improving the external quantum efficiency of GaN-LED, people have made number of research projects for many years, use TCL(Transparent Conductive Layer, transparency conducting layer) be to improve the most effective a kind of method of external quantum efficiency known at present.
The TCL of GaN-LED mainly adopts Ni/Au(nickel au-alloy at present) or ITO(Indium Tin is Oxides, tin-doped indium oxide) material, film coating method is an electron beam evaporation.Ni/AuTCL evenly spreads in order to ensure electric current, require TCL that certain thickness is arranged, and ensureing that electric current spreads under the uniform situation, only up to 76%, this has greatly limited the application of Ni/Au TCL in fields such as backlight, high-power illuminations to Ni/Au at the light transmission rate of visible light wave range.And for ITO TCL, has high visible transmittance and lower resistivity though proved it, and widely applied in the photoelectric device industry, yet diffusion easily under the middle high temperature heavy atom In(indium among the ITO), thereby the degradation that causes ITO TCL makes it be restricted in the high-power applications field.Simultaneously In still is valuable rare metal, under following solid-state illumination generally uses, will face resource exhaustion and the problem that can not maintain.
ZnO(zinc oxide) material not only has the lattice that almost completely mates with GaN, also has very high visible light transmissivity, lower characteristics such as resistivity, but also have characteristics such as cost of material is cheap, material non-toxic environmental protection, be following Ni/Au of replacement and ITO, become the main optional material of TCL of new generation.But the growth of ZnO TCL great majority use sputtering technology at present, can not precisely control the film quality and the appearance structure of extension, only can satisfy basic conduction and transparent characteristic.
In sum, existing ZnO TCL and manufacturing technology thereof are still waiting to improve.
Summary of the invention
One of technical problem to be solved by this invention provides a kind of zinc oxide transparent conductive film, and zinc oxide transparent conductive film can not precisely be controlled the film quality of extension and the problem of appearance structure in the solution prior art.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of zinc oxide transparent conducting film, it comprises ZnO nucleating layer, ZnO body layer and the circle hat nanometer column ZnO layer of order attached to substrate material one side surface, described circle hat nanometer column ZnO layer is attached to described ZnO body layer outer surface; The span length of the circle hat of described circle hat nanometer column ZnO layer is 10 to 1000nm, circle be preced with the top apart from ZnO body layer 10 to 600nm.
Two of technical problem to be solved by this invention is manufacture method that a kind of zinc oxide transparent conductive film is provided accordingly.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of manufacture method of zinc oxide transparent conducting film comprises the steps:
S1), growth substrates pre-treatment: to carrying out matting as the surface of the epitaxial wafer of growth substrates material and furnace high-temperature is handled;
S2), pre-deposition: at epitaxial wafer one side surface pre-deposition Zn, Mg, Ga, the perhaps oxide compound of Zn, Mg, Ga;
S3), ZnO nucleating layer growth: form the ZnO nucleating layer on GaN-LED epitaxial wafer surface;
S4), ZnO body layer growth: utilize the layer growth pattern to build crystalline substance, obtain stratiform ZnO body layer fine and close, surface smoothing;
S5), circle hat nanometer column ZnO layer growth: utilizing the mixed growth pattern to grow some diameters in the ZnO body layer outside is 10 to 1000nm, has the circle hat nanometer column ZnO layer of the circle hat nanometer column surface topography of photonic crystal characteristic.
The invention has the beneficial effects as follows:
The ZnO TCL that the manufacture method of employing zinc oxide transparent conducting film of the present invention obtains, except satisfying good conduction and transparent characteristic, precisely the control growing quality and control pattern, utilize the specific refractory power of ZnO and the difference and the surface topography characteristics of air, can form surface topography, thereby make it reach higher characteristic the optical extraction efficiency with photonic crystal characteristic; Thereby use the ZnO TCL of the manufacture method manufacturing of ZnO TCL of the present invention, have high reliability, low-resistivity, high light transmittance and light extraction efficiency efficiently, can improve the LED external quantum efficiency greatly, can promote the tremendous development of LED industry, help realizing the target of environmental protection and energy saving, Sustainable development.
Description of drawings
Fig. 1 is the structural representation of GaN LED epitaxial wafer and ZnO TCL in the specific embodiment of the invention.
Fig. 2 is the epitaxially grown schematic flow sheet of ZnO TCL in the specific embodiment of the invention.
Fig. 3 is to the resistivity measurement figure of ZnO TCL sample in the specific embodiment of the invention.
Fig. 4 is to the light transparent transmission rate test pattern of ZnO TCL sample in the specific embodiment of the invention.
Fig. 5 is to the sem photograph of ZnO TCL sample laminate structure in the specific embodiment of the invention.
Fig. 6 is to the sem photograph of ZnO TCL sample surfaces structure in the specific embodiment of the invention.
Fig. 7 is to the XRD diffractogram of ZnO TCL sample in the specific embodiment of the invention.
Fig. 8 is the spontaneous sharp spectrogram of penetrating of the PL of ZnO TCL sample in the specific embodiment of the invention.
Fig. 9 is that ZnO TCL is applied in work illuminated diagram on the led chip in the specific embodiment of the invention.
Figure 10 is that ZnO TCL and ITOTCL, Ni/AuTCL are applied in electric current and optical output power figure on the led chip in the specific embodiment of the invention.
The invention will be further described below in conjunction with accompanying drawing.
Embodiment
Embodiment one
The purpose of this embodiment provides the method for a kind of ZnO of manufacturing TCL, produces a kind of novel ZnO TCL.The ZnO TCL that this method produces comprises ZnO nucleating layer, ZnO body layer and the circle hat nanometer column ZnO layer of order attached to GaN-LED epitaxial wafer one side as shown in Figure 1.Through test, this ZnO TCL has lower resistivity, higher visible light penetration coefficient, and film surface appearance can center on the photonic crystal size control, with GaN very high lattice match degree is arranged; When this method is applied to GaN-LED, can obviously improve the efficient of the outer quantum of GaN-LED chip.
For obtaining above-mentioned ZnO TCL, the preliminary thinking of the present invention is:
Utilize existing industrial production type MOCVD(Metal-organic Chemieal Vapor DePosition, the organometallics chemical vapor deposition) or MBE(Molecular Beam Epitaxy molecular beam epitaxy) etc. equipment, with organo-metallic DEZn(zinc ethyl) as the Zn source, organo-metallic TMAl(trimethyl aluminium), the TEGa(triethyl-gallium), the TMIn(trimethyl indium), Cp2Mg cyclopentadienyl magnesium is the doping metals source, purity is the O more than 99.9999% 2As oxygen source, purity is the Ar(argon gas more than 99.999%), the He(helium) as carrier gas and epitaxy protective atmosphere, progressively epitaxy goes out ZnO TCL on substrate material.
As shown in Figure 2, the concrete steps that prepare the above ZnO TCL are:
1, growth substrates pre-treatment
The growth substrates pre-treatment mainly comprises: handle carry out matting and furnace high-temperature as the epitaxial wafer surface of growth substrates material, for subsequent epitaxial growth is prepared.
Get the GaN-LED epitaxial wafer and carry out surface acid alkalization and learn the processing of removing contamination at this place, MOCVD being grown, temperature is controlled at 400 to 900 degrees centigrade in the stove again, pressure-controlling is at 3 to 100torr(Bristols, 1torr is equivalent to 1 mmhg), thermal treatment 1 to 60 minute is as the substrate of subsequently epitaxial growing ZnO TCL.
The temperature that this place particularly controls in the MOCVD growth stove is 650 degrees centigrade, and pressure is 10torr, and the treatment time is 20 minutes.
2, pre-deposition
Pre-deposition is meant in MOCVD, MBE homepitaxy equipment; under the protective atmosphere of Ar or He; temperature is controlled at 200 to 450 degrees centigrade; pressure-controlling 2 to 20torr; 5 to 120 seconds hold-times; flow with 8.6E-6 to 2.1E-4 moles/min feeds the DEZn(zinc ethyl), thereby at the certain organo-metallic Zn of epitaxial wafer one side surface deposition.
Originally be under the Ar atmosphere, adjust in the MOCVD stove temperature to 350 degree centigrade, pressure-controlling is 8.4torr, feeds organo-metallic DEZn, the flow of DEZn is 4.9E -5Moles/min, the feeding time is 30 seconds, makes the side surface as the GaN-LED epitaxial wafer of epitaxial growth substrate form rich Zn attitude, for subsequent epitaxial growth provides good basis.
3, ZnO nucleating layer growth
The growth of ZnO nucleating layer is meant, in epitaxial device, under the protective atmosphere, adjusts growth temperature and remains on 200 to 900 degrees centigrade, feeds organo-metallic DEZn then, and the flow control of DEZn is at 1.36E -5To 1.1E -4Moles/min also feeds O 2, O 2Flow control at 4.5E -3To 2.7E -2Moles/min, pressure-controlling goes out 3 to 30nm ZnO nucleating layer in the surface epitaxy of GaN-LED epitaxial wafer, for subsequent epitaxial growth is done the basis 3 to 100torr.
This place specifically under Ar atmosphere, adjusts growth temperature and remains on 250 degrees centigrade, feeds organo-metallic DEZn then, and feeds O 2, pressure-controlling is carried out epitaxy at 30torr, makes the surface of GaN-LED epitaxial wafer form the 10nm(nanometer) and the ZnO nucleating layer of thickness.
4, ZnO body layer growth
The ZnO body layer is grown, and in epitaxial device, under the protective atmosphere, growth temperature is controlled at 300 to 900 degrees centigrade, and Reaktionsofen pressure 3 mixes doping metals source TEGa to 100torr, and flow is 2.18E -6To 8.4E -4Moles/min will feed O then 2Speed bring up to 4.5E -3 Extremely2.7E -2Moles/min, the speed that will feed organo-metallic DEZn is simultaneously brought up to 2.73E -5To 1.09E -3Moles/min, thus the speed of growth accelerated, grow thickness and be 50 to 5000nm ZnO body layer.
Utilize stratiform (F-M, Frank-van der Merwe) growth pattern to build crystalline substance in this step, obtain stratiform ZnO body layer fine and close, surface smoothing, this layer reduces light propagation loss mainly as optical waveguide layers.During growth ZnO body layer, need to use three-group metal such as TEGa, TMAl, TMIn etc. to mix, realize the n type conduction of film; Described doping metals source be among TEGa, TMAl, the TMIn a kind of, two kinds or three kinds.
This place specifically is under Ar atmosphere, adjusts growth temperature to 850 degree centigrade, mixes organo-metallic TEGa, and molar flow is 4.36E -5Moles/min improves feeding organo-metallic DEZn and O then 2Molar weight respectively to 1.3E -4Moles/min and 6.7E -2Moles/min grows compact structure, surfacing, and thickness is the stratiform ZnO body layer of 700nm, and next the N type ZnO layer of the Ga that promptly mixes interrupts the feeding of metal organic raw material, but keeps O 2Flow stop growing.
5, circle hat nanometer column ZnO layer growth
Circle hat nanometer column ZnO layer growth is to utilize to mix (S-K, Stranski-Krastanov) growth pattern, grow some circle hat span lengths in the ZnO body layer outside and be 10 to 1000nm, circle hat top is 10 to 600nm apart from the distance of laminar film, has the circle hat nanometer column ZnO layer of the circle hat nanometer column surface topography of photonic crystal characteristic.Circle hat nanometer column ZnO layer makes the long-pending increase of light output surface, and can also play lensing, thereby can make the outgoing efficient of light higher.
This step by the growth online treatment, is reduced to 2 to 50torr with the pressure of MOCVD epitaxial furnace under Ar atmosphere, temperature is reduced to 250 to 650 degrees centigrade, keeps doping metals Ga to continue to feed 10 seconds to 10 minutes, next stops to feed O 2With organo-metallic DEZn, keep the interface to stop growth 1 to 20 minute, feed then as the raw-material O of growth 2With organo-metallic DEZn, TEGa, the induced growth pattern changes the mixed growth pattern into by layer growth before, growth with circle hat nanometer column ZnO upper layer of photonic crystal characteristic, promptly on ZnO body layer surface, grow circle hat span length and be 10 to 1000nm, circle hat top is apart from the circle hat nanometer column ZnO layer of the distance 10 to 600nm of laminar film, so far complete ZnO TCL.
This place particularly by the growth online treatment, is reduced to 30torr with the pressure of MOCVD epitaxial furnace under Ar atmosphere, temperature is reduced to 550 degrees centigrade, keeps doping metals Ga to continue to feed 2 minutes, next stops to feed O 2With organo-metallic DEZn, keep the interface to stop growth 10 minutes, feed then as the raw-material O of growth 2With organo-metallic DEZn, TEGa, the induced growth pattern changes the mixed growth pattern into by layer growth before, growth with circle hat nanometer column ZnO upper layer of photonic crystal characteristic, promptly growing circle hat span length on ZnO body layer surface is 300nm, circle hat top is apart from the circle hat nanometer column ZnO layer apart from 46nm of laminar film, so far complete ZnO TCL.
6, anneal
In order to make the ZnO TCL that grows have better optics and electrical stability, ZnO TCL need be under Ar, He atmosphere, and keeping temperature is 400 to 900 degrees centigrade, through 1 to 60 fen clock time, has promptly finished anneal.
This place particularly under Ar atmosphere, is elevated to 900 degrees centigrade with temperature and kept 10 minutes, thereby carry out high temperature annealing in the MOCVD growth furnace after finishing circle hat nanometer column ZnO layer growth.
Figure 3 shows that the resistivity of using the Hall55 survey meter to record the ZnO TCL sample that is generated, the resistivity of this ZnO TCL sample is lower than 5E-4 Ω cm as seen from the figure.Figure 4 shows that the ZnO TCL sample that uses the UV2550 spectral investigator to record to be generated transmitance to visible light, as seen from the figure, this ZnO TCL sample for the transmitance of the visible light of 460nm up to 94%.
Fig. 5 and Figure 6 shows that the ZnO TCL sample that is generated SEM(scanning electronic microscope) lower surface pattern.As seen from the figure, ZnO TCL sample comprises stratiform ZnO body layer and the circle hat nanometer column ZnO upper layer with photonic crystal characteristic.ZnO TCL sample surfaces presents the circle hat island structure that self-assembly generates, and circle hat span length reaches 600nm, circle hat top apart from laminar film apart from 150nm.
Figure 7 shows that the diffractogram that uses Brooker D8 high resolution XRD to record ZnO TCL sample.Figure 8 shows that and use PL(photoluminescence spectra measuring system) observe the self-excitation frequency spectrum of ZnO TCL.By being of high quality of the visible gained sample of specimen material analytical data among Fig. 7 and Fig. 8.Figure 9 shows that ZnO TCL is applied in the work illuminated diagram on the led chip, it is controlled to use SEM to observe membrane structure, and favorable working performance, whole uniformly light-emitting.Figure 10 shows that the correlation data of ZnO, ITO, Ni/Au TCL chip photoelectricity test, particularly be that GaN LED epitaxial wafer with same quality uses Ni/Au, ITO and ZnO as the TCL layer respectively, be processed into the chip crystal grain of 200um*250um then, pass to electric current then, measure the optical output power data of three kinds of chips then.Through calculating as can be known, to use ZnO TCL of the present invention and be processed into the led chip element, the led chip element that it is processed into than the Ni/Au TCL under the same terms and ITO TCL is that light extraction efficiency under the 20mA promotes 120% and 57% respectively at received current.
In sum, the ZnO TCL that the present invention utilizes MOCVD, PECVD, MBE homepitaxy deposition growing technology to obtain, except satisfying good conduction and transparent characteristic, precisely the control growing quality and control pattern, utilize the specific refractory power of ZnO and the difference and the surface topography characteristics of air, can form surface topography, thereby make it reach higher characteristic the optical extraction efficiency with photonic crystal characteristic; Thereby use the ZnO TCL of the manufacture method manufacturing of ZnO TCL of the present invention, have high reliability, low-resistivity, high light transmittance and light extraction efficiency efficiently, can improve the LED external quantum efficiency greatly, can promote the tremendous development of LED industry, help realizing the target of environmental protection and energy saving, Sustainable development.
Need to prove, use the material that technical solution of the present invention grows transparent conductive film, comprise ZnO, but be not limited only to ZnO, also comprise binary or multivariant oxide with close character.
 
Embodiment two
Present embodiment is the same with the basic step of embodiment one, and just correlation parameter is not quite alike, and the correlation parameter of the last ZnO film sample that generates also has some difference, particularly, when nucleating layer is grown, generates the ZnO nucleating layer of 15nm thickness.
After tested, the transmitance of the ZnO TCL sample 454nm visible light that is generated is up to 93.1%, and resistivity is lower than 3.4E-4 Ω cm, and surface topography presents self-assembly and generates circle hat island structure, circle hat span length reaches 560nm, circle hat top apart from laminar film apart from 80nm.
 
Embodiment three
The difference of present embodiment and embodiment one is:
During the nucleating layer growth, temperature is controlled at 250 degrees centigrade, and pressure-controlling is at 80torr, and the ZnO nucleating layer thickness that grows is 22nm.
In the stratiform ZnO body layer process of growth, gold doping belongs to Ga when carrying out N type ZnO layer growth, and temperature is 450 degrees centigrade, and the thickness of the N type ZnO layer that is generated is 600nm.
Under other condition is constant, feed organo-metallic Al then, and the molar weight of control organo-metallic Al is higher 5 times than the molar weight of metal Ga, continued growth 200nm.
After tested, up to 92.1%, and resistivity is lower than 7.4E-4 Ω cm to gained ZnO TCL sample to the transmitance of 468nm visible light, and surface topography presents self-assembly and generates circle hat island structure, circle hat span length reaches 150nm, circle hat top apart from laminar film apart from 28nm.
 
Embodiment four
The difference of present embodiment and embodiment three is, in the stratiform ZnO body layer process of growth, gold doping belongs to Ga when carrying out N type ZnO layer growth, and temperature is 850 degrees centigrade, and the thickness of the N type ZnO layer that is generated is 400nm.
Under other condition is constant, feed organo-metallic In then, and the molar weight of control organo-metallic In is higher 3.5 times than the molar weight of metal Ga, continued growth 200nm.
After tested, up to 94.2%, resistivity is lower than 2.6E-4 Ω cm to gained ZnO TCL sample in the transmitance of visible light 528nm, and surface topography presents self-assembly and generates circle hat island structure, and circle hat span length reaches 350nm, circle hat top apart from laminar film apart from 54nm.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.

Claims (10)

1. zinc oxide transparent conducting film, it comprises ZnO nucleating layer and the ZnO body layer of order attached to substrate material one side surface, it is characterized in that, described zinc oxide transparent conducting film also comprises circle hat nanometer column ZnO layer, and described circle hat nanometer column ZnO layer is attached to described ZnO body layer outer surface; The span length of the circle hat of described circle hat nanometer column ZnO layer is 10 to 1000nm, circle be preced with the top apart from ZnO body layer 10 to 600nm.
2. a kind of zinc oxide transparent conducting film as claimed in claim 1 is characterized in that, described ZnO body layer be mix among organic metal A l, Ga, the In a kind of, two kinds or three kinds, and the stratiform N type ZnO layer that generates.
3. the manufacture method of a zinc oxide transparent conducting film comprises the steps:
S1), growth substrates pre-treatment: to carrying out matting as the surface of the epitaxial wafer of growth substrates material and furnace high-temperature is handled;
S2), pre-deposition: at epitaxial wafer one side surface pre-deposition Zn, Mg, Ga, the perhaps oxide compound of Zn, Mg, Ga;
S3), ZnO nucleating layer growth: form the ZnO nucleating layer on GaN-LED epitaxial wafer surface;
S4), ZnO body layer growth: utilize the layer growth pattern to build crystalline substance, obtain stratiform ZnO body layer fine and close, surface smoothing;
S5), circle hat nanometer column ZnO layer growth: utilizing the mixed growth pattern to grow some diameters in the ZnO body layer outside is 10 to 1000nm, has the circle hat nanometer column ZnO layer of the circle hat nanometer column surface topography of photonic crystal characteristic.
4. the manufacture method of a kind of zinc oxide transparent conducting film as claimed in claim 3, it is characterized in that, step S1) pre-treatment of growth substrates described in is specially, get the GaN-LED epitaxial wafer and carry out surface acid alkalization and learn processings of removing contamination, keeping temperature again in epitaxial device is that 400 to 900 degrees centigrade, pressure are 3 to 100torr furnace high-temperatures processing 1 to 60 minute.
5. the manufacture method of a kind of zinc oxide transparent conducting film as claimed in claim 3 is characterized in that, step S2) described in pre-deposition be specially; under protective atmosphere; adjust the epitaxial device parameter, feed organo-metallic Zn then, make a side surface form rich Zn attitude as epitaxial growth substrate.
6. the manufacture method of a kind of zinc oxide transparent conducting film as claimed in claim 3; it is characterized in that; step S3) growth of the nucleating layer of ZnO described in is specially; in epitaxial device; under the protective atmosphere; adjust growth temperature and remain on 200 to 900 degrees centigrade, feed organo-metallic DEZn then, and feed O 2, pressure-controlling is 3 to 100torr, and epitaxy goes out 3 to 30nm ZnO nucleating layer.
7. the manufacture method of a kind of zinc oxide transparent conducting film as claimed in claim 3 is characterized in that, step S4) described in ZnO body layer growth be specially; in epitaxial device, under the protective atmosphere, growth temperature is controlled at 300 to 900 degrees centigrade; mix the doping metals source, improve feeding O then 2And the speed of organo-metallic DEZn; Described doping metals source be among TEGa, TMAl, the TMIn a kind of, two kinds or three kinds.
8. as the manufacture method of any described a kind of zinc oxide transparent conducting film in the claim 3 to 7; it is characterized in that; described step S5) also comprise step S6 after) anneal; described anneal is meant in epitaxial device; under the protective atmosphere, with temperature remain on 400 to 900 degrees centigrade 1 to 60 minute.
9. the manufacture method of a kind of zinc oxide transparent conducting film as claimed in claim 8 is characterized in that, described epitaxial device is a kind of among MOCVD, the MBE.
10. as the manufacture method of any described a kind of zinc oxide transparent conducting film in the claim 4 to 7, it is characterized in that described epitaxial device is a kind of among MOCVD, the MBE.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104409600A (en) * 2014-11-14 2015-03-11 浙江大学 Near-infrared light-emitting device and preparation method thereof
CN105190914A (en) * 2012-12-26 2015-12-23 首尔半导体株式会社 Process for depositing epitaxial ZnO on iii-nitride-based light emitting diode and light emitting diode including epitaxial ZnO
CN107394023A (en) * 2016-08-17 2017-11-24 佛山市中山大学研究院 A kind of preparation method of crystallized nano structure zinc oxide transparent conductive film
CN109994629A (en) * 2017-12-29 2019-07-09 Tcl集团股份有限公司 Laminated film and its preparation method and application
CN113130716A (en) * 2021-04-21 2021-07-16 京东方科技集团股份有限公司 Light emitting diode device, preparation method thereof and display device

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009069785A1 (en) * 2007-11-29 2009-06-04 Kyocera Corporation Light emitting element and illuminating apparatus
US20100025673A1 (en) * 2005-11-25 2010-02-04 Qiu-Hong Hu Light Emitting Diode and Method for Manufacturing the Same
US20100117070A1 (en) * 2008-09-18 2010-05-13 Lumenz Llc Textured semiconductor light-emitting devices

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100025673A1 (en) * 2005-11-25 2010-02-04 Qiu-Hong Hu Light Emitting Diode and Method for Manufacturing the Same
WO2009069785A1 (en) * 2007-11-29 2009-06-04 Kyocera Corporation Light emitting element and illuminating apparatus
US20100117070A1 (en) * 2008-09-18 2010-05-13 Lumenz Llc Textured semiconductor light-emitting devices

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
J.ZHONG ET AL: "Integrated ZnO nanotips on GaN light emitting diodes for enhanced emission efficiency", 《APPLIED PHYSICS LETTERS》, vol. 90, 18 May 2007 (2007-05-18), XP012094899, DOI: doi:10.1063/1.2741052 *

Cited By (9)

* Cited by examiner, † Cited by third party
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CN105190914A (en) * 2012-12-26 2015-12-23 首尔半导体株式会社 Process for depositing epitaxial ZnO on iii-nitride-based light emitting diode and light emitting diode including epitaxial ZnO
CN105190914B (en) * 2012-12-26 2018-01-26 首尔半导体株式会社 For depositing extension ZnO technique on III group-III nitride based light-emitting diode and including extension ZnO light emitting diode
CN104409600A (en) * 2014-11-14 2015-03-11 浙江大学 Near-infrared light-emitting device and preparation method thereof
CN107394023A (en) * 2016-08-17 2017-11-24 佛山市中山大学研究院 A kind of preparation method of crystallized nano structure zinc oxide transparent conductive film
CN107394023B (en) * 2016-08-17 2019-08-20 中山大学 A kind of preparation method of crystallized nano structure zinc oxide transparent conductive film
CN109994629A (en) * 2017-12-29 2019-07-09 Tcl集团股份有限公司 Laminated film and its preparation method and application
CN109994629B (en) * 2017-12-29 2021-01-29 Tcl科技集团股份有限公司 Composite film and preparation method and application thereof
CN113130716A (en) * 2021-04-21 2021-07-16 京东方科技集团股份有限公司 Light emitting diode device, preparation method thereof and display device
CN113130716B (en) * 2021-04-21 2023-02-28 京东方科技集团股份有限公司 Light emitting diode device, preparation method thereof and display device

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