CN1271966A - Production method of high-brightness LED chip using zinc oxide as its window layer - Google Patents

Production method of high-brightness LED chip using zinc oxide as its window layer Download PDF

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Publication number
CN1271966A
CN1271966A CN00111112A CN00111112A CN1271966A CN 1271966 A CN1271966 A CN 1271966A CN 00111112 A CN00111112 A CN 00111112A CN 00111112 A CN00111112 A CN 00111112A CN 1271966 A CN1271966 A CN 1271966A
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China
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growth
flow
window layer
zinc
layer
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CN00111112A
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CN1149685C (en
Inventor
黄柏标
张兆春
于永芹
崔得良
秦晓燕
潘教青
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Shandong University
Shandong Huaguang Optoelectronics Co Ltd
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Shandong University
Shandong Huaguang Optoelectronics Co Ltd
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Priority to CNB001111124A priority Critical patent/CN1149685C/en
Publication of CN1271966A publication Critical patent/CN1271966A/en
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Publication of CN1149685C publication Critical patent/CN1149685C/en
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Abstract

When a metallic organic compound vapour phase deposition (MOCVD) method is used for epitaxial growth of diode material, the MOCVD epitaxy growth technology in continuously used after the growth of upper limitation layer is finished for low-temp. growth of N-type doped zinc oxide film as the window layer of LED while controlling the thickness of window layer less than 2 microns. Its advantages are simple growth process, short period, low cost and optimal current expansion and optical transmission effect.

Description

A kind of with the growing method of zinc oxide as window layer of high-brightness LED chip
The present invention relates to the growing method of a kind of zinc oxide (ZnO), belong to the photoelectron technology field as high brightness LED.
1992, Toshiba Corp developed the high brightness AlGaInP green LED (LED) that has Bragg reflecting layer and current isolating layer first, and the external quantum efficiency during this light-emitting diode 573nm is 0.7%, and luminous intensity is 2 candelas.Between double heterojunction and substrate GaAs, add Bragg reflecting layer, the light of directive substrate is reflected back again, thereby improve luminous efficiency.
1994, hewlette-packard was developed the AlGaInP light-emitting diode that has gallium phosphide (GaP) transparent substrates again, and the luminous efficiency of this light-emitting diode surpasses the light-emitting diode of other structure at that time at 560~650nm wave band.Under 20mA direct current injection condition, the luminous efficiency of 604nm is up to 41.51m/W.The unique distinction of this LED chip construction is original GaAs substrate is carried out selective corrosion, and selects for use the gallium phosphide transparent substrates to be replaced.Yet current extending still adopts the gallium phosphide material of 50 μ m of gas-phase deposition method growth.
The development trend of current led technology is to high brightness, short wavelength, long-life, the development of low-cost aspect.An importance of LED core structural design is to reduce the again absorption of tube core to the radiation photon, and makes full use of the photon that the active layer radiation recombination produces.Light-emitting diode window layer structural design is a pith that directly influences its luminous efficiency, light-emitting diode is owing to adopted quantum well structure, bragg structure, the design of new structure such as barrier layer and barrier layer, its photoelectric properties increase substantially, yet have still kept thick window layer structure so far.Therefore, prior art still exists shortcomings such as growth technique complexity, the cycle is long, cost is high, production efficiency is low.
Purpose of the present invention in order to solve the deficiencies in the prior art, reduces the thickness of light-emitting diode chip for backlight unit Window layer exactly, and has proposed a kind of with the growing method of zinc oxide as window layer of high-brightness LED chip.Of the present inventionly to the effect that follow these steps to carry out:
(1) after finishing the upper limiting layer growth, sample is put into the special-purpose MOCVD equipment of ZnO, the control growing temperature is 330~450 ℃, the flow of reaction source diethyl zinc is 10~30ml/min, or the zinc methide flow is 1~5ml/min, reaction source oxolane flow is 100~300ml/min, N type doped source trimethyl aluminium flow is 1~15ml/min, with reaction source diethyl zinc or zinc methide and oxolane, and the doped source trimethyl aluminium changes 20~60 minutes N type doping zinc-oxide (ZnO) materials of growth line growth over to as Window layer, then by drop out line
(2) change reaction source diethyl zinc or zinc methide and oxolane and doped source trimethyl aluminium over to drop out line by growth line, growth temperature is reduced to 0~30 ℃ simultaneously, the flow of diethyl zinc is reduced to 0~5ml/min, or the flow of zinc methide transfers to 0~1ml/min, reaction source oxolane flow is reduced to 0~50ml/min, and the flow of N type doped source trimethyl aluminium is reduced to 0~2ml/min, so far, the growth ending of zinc oxide Window layer, the thickness of zinc oxide Window layer≤2 μ m.
Utilize double beam spectrophotometer to ZnO film, light transmission rate at visible light wave range is tested, ZnO film surpasses 80% at the light transmission rate of visible light wave range as a result, according to the print voltammetric characteristic measuring, as can be known between ZnO Window layer and the lower limit layer owing to the generation of wearing effect then forms forward conduction.As seen, adopt the thick ZnO material substitution GaP of 1~2 μ m, can make Window layer when direct current injects, have better current expansion and translucent effect.Utilize vanderburg (Vander Pauw) method to measure the electronic property of ZnO film, its film resiativity is 10 -3Ω/cm the order of magnitude shows that electric conductivity is good, its carrier concentration 10 19~10 20/ cm 2
The present invention has that growth technique is simple, growth cycle is short, cost is low, the productivity ratio advantages of higher.
The invention will be further described below in conjunction with embodiment:
Embodiment 1:
After finishing the upper limiting layer growth, sample is put into the special-purpose MOCVD equipment of ZnO, carry out the growth of ZnO Window layer according to the following steps:
The control growing temperature is 350 ℃, reaction source diethyl zinc (DEZ) flow is 12ml/min, reaction source oxolane (THF) flow is 100ml/min, N type doped source trimethyl aluminium (TMA) flow is 5ml/min, with reaction source DEZ and THF, and doped source TMA changes 40 minutes N type doping ZnO materials of growth line (RUN) growth over to as Window layer by drop out line (VENT); When finishing growth, immediately with reaction source DEZ and THF, and doped source TMA changes the VENT line over to by the RUN line, simultaneously growth temperature is transferred to 20 ℃ by 350 ℃, the DEZ flow transfers to 2ml/min, and the THF flow transfers to 50ml/min, and trimethyl aluminium (TMA) flow is 0ml/min, so far ZnO Window layer epitaxial growth finishes, Window layer thickness≤2 μ m.
Embodiment 2:
After finishing the upper limiting layer growth, sample is put into the special-purpose MOCVD equipment of ZnO, carry out the growth of ZnO Window layer according to the following steps:
The control growing temperature is 370 ℃, reaction source DEZ flow is 25ml/min, reaction source THF flow is 100ml/min, N type doped source TMA flow is 3ml/min, with reaction source DEZ and THF, and doped source TMA changes 60 minutes N type doping ZnO materials of growth line (RUN) growth over to as Window layer by drop out line (VENT); When finishing growth, immediately with reaction source DEZ and THF, and doped source TMA changes the VENT line over to by the RUN line, simultaneously growth temperature is transferred to 20 ℃ by 370 ℃, the DEZ flow transfers to 2ml/min, and the THF flow transfers to 50ml/min, and the TMA flow is 0ml/min, so far ZnO Window layer epitaxial growth finishes, Window layer thickness≤2 μ m.

Claims (1)

1. one kind with the growing method of zinc oxide as window layer of high-brightness LED chip, its Bragg reflecting layer, lower limit layer, active layer, upper limiting layers etc. are all grown by computer control by existing technology, it is characterized in that after finishing the upper limiting layer growth, sample is put into the special-purpose MOCVD equipment of ZnO, carry out the growth of zinc oxide Window layer according to the following steps: (1) control growing temperature is 330~450 ℃, the flow of reaction source diethyl zinc is 10~30ml/min, or the zinc methide flow is 1~5ml/min, reaction source oxolane flow is 100~300ml/min, N type doped source trimethyl aluminium flow is 1~15ml/min, with reaction source diethyl zinc or zinc methide and oxolane, and the doped source trimethyl aluminium changes 20~60 minutes N type doping ZnO materials of growth line growth over to as Window layer by drop out line, then (2) change reaction source diethyl zinc or zinc methide and oxolane and doped source trimethyl aluminium over to drop out line by growth line, growth temperature is reduced to 0~30 ℃ simultaneously, the flow of diethyl zinc is reduced to 0~5ml/min, or the flow of zinc methide transfers to 0~1ml/min, reaction source oxolane flow is reduced to 0~50ml/min, the flow of N type doped source trimethyl aluminium is reduced to 0~2ml/min, so far, zinc oxide Window layer growth ending, the thickness of zinc oxide Window layer≤2 μ m.
CNB001111124A 2000-05-19 2000-05-19 Production method of high-brightness LED chip using zinc oxide as its window layer Expired - Fee Related CN1149685C (en)

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CN1149685C CN1149685C (en) 2004-05-12

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1309020C (en) * 2005-04-19 2007-04-04 中国科学院物理研究所 A method for preparing high-quality ZnO single crystal film on magnesium aluminate substrate
CN100494486C (en) * 2007-05-08 2009-06-03 中国科学院上海光学精密机械研究所 Method for developing m-face or a-face ZnO film by metal organic chemical vapour deposition
CN101872663A (en) * 2010-06-18 2010-10-27 上海交通大学 Preparation method of gallium-doped zinc oxide nano-particle
CN102117871A (en) * 2009-12-31 2011-07-06 华新丽华股份有限公司 Method for gaining electric injection efficiency and light extraction efficiency of luminescent device
US8513688B2 (en) 2009-12-02 2013-08-20 Walsin Lihwa Corporation Method for enhancing electrical injection efficiency and light extraction efficiency of light-emitting devices

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1309020C (en) * 2005-04-19 2007-04-04 中国科学院物理研究所 A method for preparing high-quality ZnO single crystal film on magnesium aluminate substrate
CN100494486C (en) * 2007-05-08 2009-06-03 中国科学院上海光学精密机械研究所 Method for developing m-face or a-face ZnO film by metal organic chemical vapour deposition
US8513688B2 (en) 2009-12-02 2013-08-20 Walsin Lihwa Corporation Method for enhancing electrical injection efficiency and light extraction efficiency of light-emitting devices
CN102117871A (en) * 2009-12-31 2011-07-06 华新丽华股份有限公司 Method for gaining electric injection efficiency and light extraction efficiency of luminescent device
CN101872663A (en) * 2010-06-18 2010-10-27 上海交通大学 Preparation method of gallium-doped zinc oxide nano-particle

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