CN102051593A - Method and device for epitaxially growing metal oxide transparent conductive film - Google Patents
Method and device for epitaxially growing metal oxide transparent conductive film Download PDFInfo
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- CN102051593A CN102051593A CN 201010562233 CN201010562233A CN102051593A CN 102051593 A CN102051593 A CN 102051593A CN 201010562233 CN201010562233 CN 201010562233 CN 201010562233 A CN201010562233 A CN 201010562233A CN 102051593 A CN102051593 A CN 102051593A
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Abstract
The invention discloses a method and a device for epitaxially growing a metal oxide transparent conductive film. The device comprises a controlled gas supply system, a growth reaction chamber and a tail gas treatment system which are connected in turn, wherein the growth reaction chamber comprises a reaction chamber body, a gas homogenizing unit and a slide glass unit; the reaction chamber body is provided with a closed reaction cavity; the gas homogenizing unit is positioned at the upper end of the reaction cavity and connected with the controlled gas supply unit; the glass slide unit is arranged in the reaction chamber, and a substrate is borne on the glass slide unit; and the bottom of the reaction chamber is connected with the tail gas treatment system. Through the technical scheme, a scientific and reasonable gas homogenizing unit is arranged in the device for epitaxially growing the metal oxide transparent conductive film, so that an oxygen source, a metal source and auxiliary gas transversely flow respectively, are uniformly diffused and flow downwards to a reaction zone to realize the uniformity of epitaxial growth, and a plurality of high-quality metal oxide conductive films can be epitaxially grown at one time to meet the requirement of industrial production.
Description
Technical field
The present invention relates to technical field of semiconductors, be specifically related to a kind of method and used MOCVD device of this method of transparent conductive metal oxide thin film epitaxial growth.
Background technology
The technical development of photodiode (LED) aspect is very fast in recent years.From existing situation, gallium nitride light-emitting diode (GaN LED) will become the core devices of solid-state illumination, in order to promote the application of LED fast, need increase substantially the performance, particularly light extraction efficiency under high-power condition and job stability of LED again in the solid-state illumination field.Be applied in photoelectric fields such as LED and the transparent conductive metal oxide film can be used as transparency electrode, the performance of LED is had great effect.ITO(Indium Tin Oxides nano indium tin metal oxide) replacing the Ni/Au transparency conducting layer is the major progress of LED industry, yet along with the development of LED to the large power solid-state illumination field, because of ITO contains the rare metal indium and has toxicity, unfriendly to environment, more not ideal enough owing to its thermostability, so the transparency electrode of gallium nitride light-emitting diode still needs to improve.
Zinc oxide (ZnO) nesa coating has high visible light transmissivity, low resistivity, and more significantly itself and GaN lattice almost completely mate, and make it have the characteristics of high high-temp stability, thereby are the transparent conductive films of future generation of tool potentiality.The growth of ZnO transparent conductive film at present has several different methods, such as: hydrothermal method, method of evaporation, sputtering method, pulsed laser deposition, molecular beam epitaxy and organo-metallic vapour deposition (MOCVD, Metal-organic Chemical Vapor DePosition) method etc., but wherein everybody generally acknowledges may commercially produce, the organo-metallic vapour deposition is only arranged, big area is even, the ZnO transparent conductive film of better quality because this method may obtain within a short period of time, and may the repeatability growth.But do not see the method for suitable industrialization growing metal oxidic transparent conductive film and the report of device now, the MOCVD device that searching appropriate amount pan belongs to the oxidic transparent conductive film is urgent expectation in the industry with the processing method that matches.
Summary of the invention
One of technical problem to be solved by this invention provides a kind of transparent conductive metal oxide thin film epitaxial growth device that is fit to industrialization.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of transparent conductive metal oxide thin film epitaxial growth device comprises being linked in sequence: be used for the controllable respectively controlled airing system that the auxiliary source of the gas of oxygen source, organometallic sources and growth is provided; Be used to carry out the epitaxially grown growth response of organo-metallic vapour deposition chamber; Be used for exhaust treatment system that the epitaxy reacted tail gas is handled; Described growth response chamber comprises: reaction chamber body, even gas unit, and the slide glass unit that is used to carry epitaxial growth substrate; Described reaction chamber body has the reaction chamber of sealing, and described even gas unit is arranged on the upper end of described reaction chamber, and is connected with described controlled airing system; Described slide glass unit is arranged in the reaction chamber, is used for epitaxially grown substrate supporting thereon, and substrate place near zone is the reaction zone of growth reaction chamber; The bottom of reaction chamber is connected with described exhaust treatment system.
In the optimized technical scheme, described reaction chamber body is a barrel shaped structure, comprising: sidewall, be closed in the upper flange plate of sidewall upper opening part, and the lower flange that is closed in the side wall lower ends opening part; Described even gas unit is arranged on the upper flange plate, and described slide glass unit is arranged on the lower flange.
Further in the optimized technical scheme, described even gas unit comprises three kinds of spouts and two-layer steel mesh; Three kinds of spouts are respectively: the source metal gas circuit spout that is connected with organometallic sources in the controlled airing system, the oxygen source gas circuit spout that is connected with oxygen source in the controlled airing system, the auxiliary gas gas circuit spout that is connected with the auxiliary source of the gas of growth in the controlled airing system; Two-layer steel mesh is respectively to go up steel mesh and following steel mesh, parallel interval setting between described upward steel mesh, following steel mesh and the upper flange plate three; Described auxiliary gas gas circuit spout runs through upper flange plate, and extends between upper flange plate and the last steel mesh; Described source metal gas circuit spout and oxygen source gas circuit spout run through upper flange plate, and extend between the steel mesh and between the following steel mesh.
Further in the optimized technical scheme, described even gas unit also comprises three layers of isolation mount, the first layer isolation mount is arranged between upper flange plate and the last steel mesh, and second layer isolation mount is arranged between steel mesh and the following steel mesh, and the 3rd layer of isolation mount is arranged on down the lower surface of steel mesh.
Further in the optimized technical scheme, described source metal gas circuit spout, oxygen source gas circuit spout, auxiliary gas gas circuit spout all have a plurality of; Described even gas unit comprises that also described division board is arranged on the upper flange plate inboard with the individual separately division board that leaves of described spout.
In the optimized technical scheme, described slide glass unit comprises: be used to carry the slide glass dish of substrate, be used to drive the slide glass dish driving mechanism of described slide glass disc spins, and be used for the heating unit to the reaction chamber heating; Described slide glass dish driving mechanism is arranged on the lower flange; Described slide glass dish is connected with slide glass dish driving mechanism power, rotates under the driving of slide glass dish driving mechanism; Described heating unit and slide glass dish parallel interval are provided with, to the substrate even heating on the slide glass dish.
Further in the optimized technical scheme, described slide glass dish driving mechanism comprises rotation supporting disk, rotating shaft and rotary electric machine; Described rotating shaft is rotating to be arranged on the lower flange, and its lower end passes lower flange and is connected with described rotary electric machine power, then fixedlys connected with described rotation supporting disk in its upper end, under the driving of rotary electric machine, and the rotation of driven rotary supporting disk; Described slide glass dish is arranged on the rotation supporting disk; Described heating unit comprises heating wire and heating wire pallet, and the heating wire pallet is fixedly installed in the rotating shaft and is positioned at rotation supporting disk below, becomes spiral to amplify the distribution of shapes heating wire and is fixedly installed on the heating wire pallet.
Further in the optimized technical scheme, described slide glass unit also comprises sealing bearing, and described sealing bearing is arranged on the lower flange central position, and described rotating shaft is arranged on the lower flange by sealing bearing is rotating.
Further in the optimized technical scheme, described slide glass unit also comprises the heat spacer sleeve, and described heat spacer sleeve is arranged on heater strip pallet below.
Two of technical problem to be solved by this invention is corresponding epitaxial growth methods that a kind of industrialization growing metal oxidic transparent conductive film is provided.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of method of transparent conductive metal oxide thin film epitaxial growth comprises the steps:
S1), growth substrates pre-treatment:, carry out matting and furnace high-temperature and handle, for subsequent epitaxial growth is prepared to pre-epitaxially grown substrate;
S2), pre-deposition: with pretreated substrate, use aforesaid a kind of transparent conductive metal oxide thin film epitaxial growth device, in substrate one side surface deposition one deck organo-metallic;
S3), nucleating layer growth: use aforesaid a kind of transparent conductive metal oxide thin film epitaxial growth device, have on the organometallic substrate of one deck at pre-deposition, epitaxy goes out the metal oxide nucleating layer, for subsequent epitaxial growth is done the basis;
S4), body layer growth: use aforesaid a kind of transparent conductive metal oxide thin film epitaxial growth device, go out in epitaxy on the substrate of metal oxide nucleating layer, further growth goes out layer of metal oxide compound body layer;
S5), anneal: use aforesaid a kind of transparent conductive metal oxide thin film epitaxial growth device, to growing the substrate of metal oxide body layer, under protective atmosphere, keep temperature be 400 to 900 degrees centigrade 1 to 60 minute.
The invention has the beneficial effects as follows:
Adopted a kind of transparent conductive metal oxide thin film epitaxial growth method of a kind of transparent conductive metal oxide thin film epitaxial growth of technical solution of the present invention device, owing to be provided with scientific and reasonable even gas unit, make oxygen source, source metal and auxiliary gas transverse flow and flow to reaction zone after spreading evenly downwards respectively, to realize epitaxially grown homogeneity, can the high-quality metal conductive oxide film of disposable epitaxy place multi-disc, thus satisfy the requirement that industrialization is produced.
Description of drawings
Fig. 1 is the structural representation of a kind of transparent conductive metal oxide thin film epitaxial growth of the specific embodiment of the invention with the MOCVD device.
Fig. 2 is the structural representation of growth response chamber in the specific embodiment of the invention.
Fig. 3 is an even air chamber structure synoptic diagram in the specific embodiment of the invention.
Fig. 4 is an organometallic sources gas circuit spout distribution schematic diagram in the specific embodiment of the invention.
Fig. 5 is a growth raw material gas gas circuit spout distribution schematic diagram in the specific embodiment of the invention.
Fig. 6 is a growth assist gas gas circuit spout distribution schematic diagram in the specific embodiment of the invention.
Go up the steel mesh space in Fig. 7 specific embodiment of the invention and settle synoptic diagram.
Synoptic diagram is settled in the steel mesh space under in Fig. 8 specific embodiment of the invention.
The 3rd layer of rack space settled synoptic diagram in Fig. 9 specific embodiment of the invention.
Figure 10 is a structural representation of going up steel mesh in the specific embodiment of the invention
Figure 11.It is the structural representation of following steel mesh in the specific embodiment of the invention.
Figure 12 is the structural representation of gas spout in the specific embodiment of the invention.
Figure 13 is the structural representation of heating unit in the specific embodiment of the invention.
Figure 14 is the transmittance test pattern of the transparent conductive metal oxide membrane sample that grows of the specific embodiment of the invention.
Figure 15 is the resistivity measurement figure of the ZnO electrically conducting transparent membrane sample that grows of the specific embodiment of the invention.
Figure 16 is the luminous working drawing after ZnO electrically conducting transparent membrane sample that the specific embodiment of the invention grows is made chip.
Figure 17 is the ZnO electrically conducting transparent membrane sample that the specific embodiment of the invention grows, with ITO, Ni/Au TCL in conjunction with identical GaN-LED epitaxial wafer, the optical output power correlation data figure of made chip.
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment
The purpose of this embodiment is to provide a kind of and can be fit to epitaxially grown method of zinc oxide (ZnO) transparent conductive film and the corresponding M OCVD device that industrialization is produced, this method and MOCVD device, use high purity oxygen gas (O
2) as the source of oxygen in the zinc oxide (O) element, purity is the source of other organo-metallic zinc (Zn) of extension level as the zinc in zinc oxide element, high-purity argon gas (Ar) is as carrier gas and growth assist gas, high pure nitrogen (N
2) drive and vacuum aided gas as device.Certainly, can also in organo-metallic zinc, mix organometallic aluminium (Al), gallium (Ga), indium (In) in case of necessity, as the conductiving doping source.
We studies show that, why the ZnO transparent conductive film is difficult to extensive epitaxy, and its major cause is that the reaction between organo-metallic zinc and the oxygen is too violent, restive.For solving the problems of the technologies described above, the present invention adopts following technical scheme:
As shown in Figure 1, the MOCVD device of this embodiment roughly comprises three parts that are linked in sequence, and is respectively: controlled airing system, growth response chamber and exhaust treatment system.
Wherein, controlled airing system and exhaust treatment system combine by sophisticated city's dealer's parts (outsourcing standardized component), and the growth response chamber is the core technology place of this embodiment.
Controlled airing system is used for controllable for follow-up growth response chamber provides oxygen source, grow auxiliary gas (argon source) and organometallic sources (zinc source).As shown in Figure 1, wherein, behind mass flowmeter, directly flow to the growth response chamber as the oxygen of oxygen source; Argon gas as the argon source then is divided into two-way, and wherein one the tunnel is similar with oxygen, behind mass flowmeter, directly flows to the growth response chamber; Another road is delivered to the zinc source container by behind the mass flowmeter.Store organo-metallic zinc in the zinc source container, argon gas feeds after the organo-metallic zinc, from organo-metallic zinc, overflow, again by a pipe-line transportation to the growth response chamber, and can carry organic metallic zinc and offer the growth response chamber as the zinc source.In addition, on the pipeline between zinc source container and the growth response chamber, be sequentially with manual valve, pressure warning unit and mass flowmeter, control the break-make of this road pipeline, pressure and the flow in the pipeline respectively.
The concrete structure of growth response chamber mainly comprises three parts as shown in Figure 2, is respectively: reaction chamber body, even gas unit and slide glass unit.
In this embodiment, the reaction chamber body is a barrel shaped structure, comprising: upper flange plate 9, reaction chamber sidewall 5 and lower flange 4.Columnar reaction chamber sidewall 5 upper end open places are by described upper flange plate 9 sealings, and the lower ending opening place then seals by described lower flange 4, thereby form the barrel-shaped reaction compartment of a sealing, and space wherein is exactly a reaction chamber.Have tail gas bleeding point 18 on the lower flange 4, tail gas bleeding point 18 is used for being connected with described exhaust treatment system, and reacted tail gas is extracted out and handled, and the principle of work and the structure of exhaust treatment system belong to prior art, and this paper no longer describes in detail.The concrete structure of upper flange plate 9 is distributed with a plurality of apertures on the circular upper flange plate 9 as shown in Figure 3.As shown in Figure 2, all be inserted with a spout in the mixed gas unit in each aperture, described spout has three kinds, is respectively: source metal gas circuit spout 12, oxygen source gas circuit spout 11 and auxiliary gas gas circuit spout 10.
In the aforementioned airing system, having one the tunnel to carry the argon gas of organic metallic zinc, is exactly to be connected with source metal gas circuit spout 12, and the argon gas that is mixed with organo-metallic zinc is injected the growth response chamber.One road oxygen is arranged in the airing system, be connected, for the growth reaction chamber provides oxygen source with described oxygen source gas circuit spout 11.Also have one the tunnel not carry the argon gas of organic metallic zinc in the airing system, be connected, for the growth reaction chamber provides argon gas with described auxiliary gas gas circuit spout 10.It is emphasized that, as shown in Figure 4, source metal gas circuit spout 12 is that center 180 degree are symmetrically distributed on the diameter line of upper flange plate 9 with the initial point, and as shown in Figures 2 and 3, each spout respectively is provided with a division board 19, and the oxygen source gas circuit spout 11 and the auxiliary gas gas circuit spout 10 of source metal gas circuit spout 12 each spouts, both sides are kept apart.And oxygen source gas circuit spout 11 and auxiliary gas gas circuit spout 10 are that center 180 degree are symmetrically distributed on the upper flange plate 9 with the initial point, and are positioned at the both sides of source metal gas circuit spout 12 place diameter lines, shown in accompanying drawing 5,6.Experiment shows that various spouts make organo-metallic raw material and growth gasses raw material independently separately according to the upper type layout, reduce parasitic reaction, are the essential steps of realization scale volume production.Even gas unit is the key of this embodiment, and can the extension elongation be carried out smoothly, and most important factor just is whether the even unitary design of gas is reasonable.Even gas unit is except comprising aforesaid three kinds of spouts, and outside the division board 19, key also comprises steel mesh 8 and following steel mesh 7, as shown in Figure 3.
Shown in Fig. 4,5 and 6, upper flange plate 9 is not the structure of a flat board, but is provided with 5 view ports, 10,12 oxygen source gas circuit spouts 11 of 12 auxiliary gas gas circuit spouts and 10 source metal gas circuit spouts 12 within it.
As shown in Figure 7, the described steel mesh 8 of going up is installed in the upper flange plate 9 just by the first layer isolation mount, and wherein the height of 12 auxiliary gas gas circuit spouts 10 is parallel with the first layer isolation mount, isolation mount and last steel mesh are opened assist gas and growth raw material gas and metal organic source gas barrier.
As shown in Figure 8,7 of described steel meshes down pass through second layer isolation mount, are installed in the upper flange plate 9, and be arranged in parallel with last steel mesh 8.Wherein 12 oxygen source gas circuit spouts 11 are parallel with second layer isolation mount with the height of 10 source metal gas circuit spouts 12.Second layer isolation mount and following steel mesh 7 are opened growth raw material gas and metal organic source gas barrier, and have been guaranteed that each spout independently spreads.
As shown in Figure 9, the upper flange plate assembly also comprises the 3rd layer of isolation mount.The 3rd layer of isolation mount be arranged in parallel with following steel mesh 7, plays fastening each assembly and buffer action.
As shown in figure 10, in this embodiment, last steel mesh 8 is wafer architectures of stainless steel, evenly be densely covered with a plurality of mesh on it, mesh diameter is 0.025 ~ 0.1mm, and thickness is 0.1 ~ 0.5mm, thereby the formation reticulated structure, supplied gas is passed through, and gas is produced the mixing effect.In addition, also be provided with a plurality of bigger holes on the last steel mesh 8, source metal gas circuit spout 12 on the position in hole and the upper flange plate 9 and oxygen source gas circuit spout 11 and observation on Growth window are corresponding, pass for source metal gas circuit spout 12 and oxygen source gas circuit spout 11 observation on Growth windows.Two of the important inventive point of this embodiment, just be to use steel mesh 8 and first, second layer isolation mount jointly assist gas gas circuit spout 10 and other two kinds of spouts to be kept apart, make assist gas earlier between last steel mesh 8 and upper flange plate 9, the first layer isolation mount transverse dispersion even, and then flow downward, dredge assist gas to reaction zone thereby reach, to realize the purpose of growth homogeneity control.
As shown in figure 11, in this embodiment, following steel mesh 7 is wafer architectures of stainless steel, evenly be densely covered with a plurality of mesh on it, mesh diameter is 0.1 ~ 2.5mm, and thickness is 0.2 ~ 1.5mm, thereby the formation reticulated structure, supplied gas is passed through, and gas is produced the mixing effect.Also be provided with 5 bigger holes on the last steel mesh, the position in hole is corresponding with the observation on Growth window on the upper flange plate 9, and the observation on Growth window passes.Two of the important inventive point of this embodiment, just be to use down steel mesh 7 and second, third isolation mount that growth raw material gas (oxygen) gas circuit spout 11 and organic metal gas gas circuit spout 12 are kept apart, and make oxygen and organic metal gas by on steel mesh, the space internal diffusion formed of steel mesh and second layer support is even down, then by entering the growth response district and grow from pushing away growth raw material gas and organic metal gas topmost, flowing downward through the uniform assist gas of last steel mesh.Avoid the spout air-flow to be directly injected to growth district and to cause the retention layer instability, thereby effectively guarantee the sedimentary homogeneity of gas-phase chemical reaction.
In this embodiment, assist gas gas circuit spout 10 has 12, and growth raw material (oxygen) gas gas circuit spout 11 has 12, and organic metal gas gas circuit spout 12 has 10, and the structure of all spouts as shown in figure 12.The different flow of input can be controlled by the pairing mass flowmeter in the airing system, thereby the control that air-flow distributes can be realized, and then the homogeneity of control growing speed.
As shown in Figure 2, the slide glass unit comprises: slide glass dish 13, rotation supporting disk 14, rotating shaft 2, rotary electric machine 1 and heat-generating units.The rotating center that is arranged on lower flange 4 of described rotating shaft runs through vertically that to stretch into growth response after the lower flange 4 indoor.Described rotary electric machine 1 is positioned at outdoor of growth response, is connected with described rotating shaft 2 lower end power, drives rotating shaft 2 rotations.Fixedly connected with described rotation supporting disk 14 in rotating shaft 2 upper ends, 14 rotations of driven rotary supporting disk.Described slide glass dish 13 is arranged on the rotation supporting disk 14, together rotates in company with rotation supporting disk 14.Being used for carrying out epitaxially grown substrate then is placed on the described slide glass dish 13.
Described heat-generating units comprises heating wire 15 and heating wire pallet 16.Heating wire pallet 16 is arranged in the rotating shaft 2 and is positioned at rotation appropriate position, supporting disk 14 below.15 of heating wires are arranged on the heating wire pallet 16.As shown in figure 13,15 one-tenth spirals of heating wire amplify distribution of shapes, can realize the uniform high-temperature temperature of big area height field.And the material of heating wire 15 is an iron: chromium: manganese alloy, the atomic ratio of each component is: 74%:24%:2%, this kind heating wire 15 have very excellent thermally-stabilised and oxidation-resistance.When carrying out epitaxy, drive the substrate that is placed on the slide glass dish 13 with certain speed Rotating with Uniform by rotary electric machine 1, can be so that reaction be more even.
In the preferred scheme, also be provided with sealing bearing 3, described sealing bearing is arranged on lower flange 4 central positions, and described rotating shaft 2 is by sealing bearing 3 rotating being arranged on the lower flange 4.
Further in the scheme, also be provided with heat spacer sleeve 17 in rotating shaft 2, described heat spacer sleeve 17 is arranged on heater strip pallet 16 belows, stops the heat radiation downwards that heat-generating units sent.
The transparent conductive metal oxide thin film epitaxial growth device of this embodiment, its exhaust treatment system comprises: dust filter unit, vacuum system and the spray thrower of acid, alkali lye is housed.Because vent gas treatment is not the core place of this embodiment innovative point, this paper no longer describes in detail.
The method of a kind of transparent conductive metal oxide thin film epitaxial growth that this embodiment provides comprises the steps:
1, growth substrates pre-treatment.
Growth substrates can be 1 to 8 inch sapphire sheet, quartz glass plate, silicon chip, or the GaN-LED epitaxial wafer etc.
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, and pressure-controlling is 2 to 20torr, and 5 to 120 seconds hold-times are with 8.6E
-6To 2.1E
-4The flow of 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 300 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 exists
1.36E -5 To 1.1E -4 Moles/min also feeds O
2, O
2Flow control exist
4.5E -3 To 2.7E -2 Moles/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.
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, 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.
Experiment showed, the method and the used MOCVD device of this method that use a kind of transparent conductive metal oxide thin film epitaxial growth, can obtain high-quality ZnO transparent conductive film.Use the MOCVD device of manufacturing of the present invention and the material behavior of the ZnO TCL that mixes Ga that above technology is made on GaN-LED, Sapphire Substrate and quartz glass plate:
1) visible light transmissivity of measuring on the quartz plate is 94%, and peak wavelength is 460.4nm, sees accompanying drawing 14.
2) the ZnO material Hall electrical characteristic on the measurement sapphire, resistivity is lower than 5E-4 Ω cm, sees accompanying drawing 15.
3) the last growth of GaN-LED ZnO transparency electrode is made the luminous working drawing behind the chip, sees Appendix 16.
4) make optical output power correlation data behind ZnO, ITO and the Ni/Au TCL electrode on the identical GaN-LED epitaxial wafer, chip size is 200um*250um, is that light extraction efficiency under the 20mA promotes 120% and 57% respectively at received current, sees accompanying drawing 17.
Adopt the method and the used MOCVD device of this method of a kind of transparent conductive metal oxide thin film epitaxial growth of this embodiment, the disposable 38 even high-quality ZnO transparent conductive films of can growing particularly are applied in ZnO transparent conductive film on the GaN base blue-ray LED as transparency electrode.The ZnO film of being grown has high electric conductivity, visible light transmissivity and thermostability, more can obtain the ZnO nanometer columnar structure that the surface has the photonic crystal characteristic by growth technology, improves the light extraction efficiency of GaN-LED.
Show through the experimental result of repeated growth repeatedly: the MOCVD device that uses a kind of transparent conductive metal oxide thin film epitaxial growth of this embodiment method, has rational structure, easy growth technique control and good repeatability, it is desired to meet suitability for industrialized production: high quality, low cost, can repeat volume production.
It is emphasized that at last, use the method and the used MOCVD device of this method of a kind of transparent conductive metal oxide thin film epitaxial growth of the present invention, not only can be used for the epitaxy of ZnO transparent conductive film, can also be used for the epitaxy of other transparent conductive metal oxide films such as gallium oxide, aluminum oxide, Indium sesquioxide.
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. transparent conductive metal oxide thin film epitaxial growth device comprises being linked in sequence: be used for the controllable respectively controlled airing system that the auxiliary source of the gas of oxygen source, organometallic sources and growth is provided; Be used to carry out the epitaxially grown growth response of organo-metallic vapour deposition chamber; Be used for exhaust treatment system that the epitaxy reacted tail gas is handled, it is characterized in that described growth response chamber comprises: reaction chamber body, even gas unit, and the slide glass unit that is used to carry epitaxial growth substrate; Described reaction chamber body has the reaction chamber of sealing, and described even gas unit is arranged on the upper end of described reaction chamber, and is connected with described controlled airing system; Described slide glass unit is arranged in the reaction chamber, is used for epitaxially grown substrate supporting thereon; The bottom of reaction chamber is connected with described exhaust treatment system.
2. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 1, it is characterized in that described reaction chamber body is a barrel shaped structure, comprising: sidewall, be closed in the upper flange plate of sidewall upper opening part, and the lower flange that is closed in the side wall lower ends opening part; Described even gas unit is arranged on the upper flange plate, and described slide glass unit is arranged on the lower flange.
3. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 2 is characterized in that described even gas unit comprises three kinds of spouts and two-layer steel mesh; Three kinds of spouts are respectively: the source metal gas circuit spout that is connected with organometallic sources in the controlled airing system, the oxygen source gas circuit spout that is connected with oxygen source in the controlled airing system, the auxiliary gas gas circuit spout that is connected with the auxiliary source of the gas of growth in the controlled airing system; Two-layer steel mesh is respectively to go up steel mesh and following steel mesh, parallel interval setting between described upward steel mesh, following steel mesh and the upper flange plate three; Described auxiliary gas gas circuit spout runs through upper flange plate, and extends between upper flange plate and the last steel mesh; Described source metal gas circuit spout and oxygen source gas circuit spout run through upper flange plate, and extend between the steel mesh and between the following steel mesh.
4. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 3, it is characterized in that, described even gas unit also comprises three layers of isolation mount, the first layer isolation mount is arranged between upper flange plate and the last steel mesh, second layer isolation mount is arranged between steel mesh and the following steel mesh, and the 3rd layer of isolation mount is arranged on down the lower surface of steel mesh.
5. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 3 is characterized in that, described source metal gas circuit spout, oxygen source gas circuit spout, auxiliary gas gas circuit spout all have a plurality of; Described even gas unit comprises that also described division board is arranged on the upper flange plate inboard with the individual separately division board that leaves of described spout.
6. as any described a kind of transparent conductive metal oxide thin film epitaxial growth device in the claim 1 to 5, it is characterized in that, described slide glass unit comprises: the slide glass dish that is used to carry substrate, be used to drive the slide glass dish driving mechanism of described slide glass disc spins, and be used for heating unit to the reaction chamber heating; Described slide glass dish driving mechanism is arranged on the lower flange; Described slide glass dish is connected with slide glass dish driving mechanism power, rotates under the driving of slide glass dish driving mechanism; Described heating unit and slide glass dish parallel interval are provided with, to the substrate even heating on the slide glass dish.
7. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 6 is characterized in that, described slide glass dish driving mechanism comprises rotation supporting disk, rotating shaft and rotary electric machine; Described rotating shaft is rotating to be arranged on the lower flange, and its lower end passes lower flange and is connected with described rotary electric machine power, then fixedlys connected with described rotation supporting disk in its upper end, under the driving of rotary electric machine, and the rotation of driven rotary supporting disk; Described slide glass dish is arranged on the rotation supporting disk; Described heating unit comprises heating wire and heating wire pallet, and the heating wire pallet is fixedly installed in the rotating shaft and is positioned at rotation supporting disk below, becomes spiral to amplify the distribution of shapes heating wire and is fixedly installed on the heating wire pallet.
8. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 7, it is characterized in that, described slide glass unit also comprises sealing bearing, and described sealing bearing is arranged on the lower flange central position, and described rotating shaft is arranged on the lower flange by sealing bearing is rotating.
9. a kind of transparent conductive metal oxide thin film epitaxial growth device as claimed in claim 7 is characterized in that described slide glass unit also comprises the heat spacer sleeve, and described heat spacer sleeve is arranged on heater strip pallet below.
10. the method for a transparent conductive metal oxide thin film epitaxial growth is characterized in that, comprises the steps:
S1), growth substrates pre-treatment:, carry out matting and furnace high-temperature and handle, for subsequent epitaxial growth is prepared to pre-epitaxially grown substrate;
S2), pre-deposition: with pretreated substrate, use any described a kind of transparent conductive metal oxide thin film epitaxial growth device in the claim 1 to 9, in substrate one side surface deposition one deck organo-metallic;
S3), nucleating layer growth: use any described a kind of transparent conductive metal oxide thin film epitaxial growth device in the claim 1 to 9, have on the organometallic substrate of one deck at pre-deposition, epitaxy goes out the metal oxide nucleating layer, for subsequent epitaxial growth is done the basis;
S4), body layer growth: use any described a kind of transparent conductive metal oxide thin film epitaxial growth device in the claim 1 to 9, go out in epitaxy on the substrate of metal oxide nucleating layer, further growth goes out layer of metal oxide compound body layer;
S5), anneal: use any described a kind of transparent conductive metal oxide thin film epitaxial growth device in the claim 1 to 9; to growing the substrate of metal oxide body layer; under protective atmosphere, keep temperature be 400 to 900 degrees centigrade 1 to 60 minute.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102400213A (en) * | 2011-11-18 | 2012-04-04 | 安徽康蓝光电股份有限公司 | Method for epitaxially growing alumina single crystal film |
| CN102418086A (en) * | 2011-11-16 | 2012-04-18 | 上海卓锐材料科技有限公司 | Spraying head device for realizing gas isolation and homogenization |
| CN107675142A (en) * | 2017-10-26 | 2018-02-09 | 杨晓艳 | A kind of gallium oxide film based on quartz substrate and preparation method thereof |
| CN111088526A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | Multi-piece loaded silicon carbide epitaxial growth equipment |
| CN114908419A (en) * | 2022-04-29 | 2022-08-16 | 杭州富加镓业科技有限公司 | Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and MOCVD (metal organic chemical vapor deposition) equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377991A (en) * | 2002-01-30 | 2002-11-06 | 吉林大学 | MOCVD equipment and process for growing ZnO film |
| CN1644754A (en) * | 2004-10-19 | 2005-07-27 | 吉林大学 | Low-pressure metal organic chemical vapour phase depositing apparatus for zinc oxide and process thereof |
-
2010
- 2010-11-29 CN CN2010105622332A patent/CN102051593B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377991A (en) * | 2002-01-30 | 2002-11-06 | 吉林大学 | MOCVD equipment and process for growing ZnO film |
| CN1644754A (en) * | 2004-10-19 | 2005-07-27 | 吉林大学 | Low-pressure metal organic chemical vapour phase depositing apparatus for zinc oxide and process thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102418086A (en) * | 2011-11-16 | 2012-04-18 | 上海卓锐材料科技有限公司 | Spraying head device for realizing gas isolation and homogenization |
| CN102400213A (en) * | 2011-11-18 | 2012-04-04 | 安徽康蓝光电股份有限公司 | Method for epitaxially growing alumina single crystal film |
| CN107675142A (en) * | 2017-10-26 | 2018-02-09 | 杨晓艳 | A kind of gallium oxide film based on quartz substrate and preparation method thereof |
| CN111088526A (en) * | 2019-12-27 | 2020-05-01 | 季华实验室 | Multi-piece loaded silicon carbide epitaxial growth equipment |
| CN111088526B (en) * | 2019-12-27 | 2021-05-11 | 季华实验室 | Multi-piece loaded silicon carbide epitaxial growth equipment |
| CN114908419A (en) * | 2022-04-29 | 2022-08-16 | 杭州富加镓业科技有限公司 | Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and MOCVD (metal organic chemical vapor deposition) equipment |
| CN114908419B (en) * | 2022-04-29 | 2024-03-29 | 杭州富加镓业科技有限公司 | Method for preparing homoepitaxial gallium oxide film on high-resistance gallium oxide substrate and MOCVD equipment |
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