CN104659166A - Wet-oxygen oxidation method of GaAs-based light emitting diode - Google Patents

Wet-oxygen oxidation method of GaAs-based light emitting diode Download PDF

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Publication number
CN104659166A
CN104659166A CN201510072029.5A CN201510072029A CN104659166A CN 104659166 A CN104659166 A CN 104659166A CN 201510072029 A CN201510072029 A CN 201510072029A CN 104659166 A CN104659166 A CN 104659166A
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gaas
wet
epitaxial wafer
oxygen
oxygen oxidation
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CN104659166B (en
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彭璐
黄博
吴向龙
徐现刚
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Shandong Inspur Huaguang Optoelectronics Co Ltd
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Shandong Inspur Huaguang Optoelectronics Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/10—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a light reflecting structure, e.g. semiconductor Bragg reflector

Abstract

The invention discloses a wet-oxygen oxidation method of a GaAs-based light emitting diode. The wet-oxygen oxidation method comprises the following steps: (1) manufacturing a layer of SiO2 film as a protecting layer on the surface of a GaAs-based epitaxial wafer; (2) performing semi-cutting operation on the GaAs-based epitaxial wafer; (3) introducing nitrogen into an annealing furnace after passing through a bubble generator, horizontally placing the GaAs-based epitaxial wafer facing the direction of the nitrogen flow in the annealing furnace, wherein the liquid in the bubble generator is deionized water containing H2O2, the mass percentage of H2O2 is 0.5-2%, the temperature of the annealing furnace is set to be 350-400 DEG C, and the oxidation time is 20-30 minutes; (4) corroding SiO2 on the surface of the GaAs-based epitaxial wafer by using hydrofluoric acid, so as to complete wet-oxygen oxidation. According to the wet-oxygen oxidation method, hydrogen peroxide is additionally used in the conventional wet-oxygen oxidation process, so that the oxidation property of the aluminum component can be improved; meanwhile when being in contact with the wafer, hydrogen peroxide can be explosively decomposed into water and oxygen, so that oxygen partial pressure on the surface of the wafer is improved, and the aluminum component can be sufficiently oxidized into A12O3 with a low refractive index.

Description

A kind of wet-oxygen oxidation method of GaAs based light-emitting diode
Technical field
The present invention relates to a kind of wet-oxygen oxidation method of GaAs based light-emitting diode, belong to photoelectron technical field.
Background technology
LED (light-emitting diode) is first commercial compound semiconductor come into the market, and has had the development course of more than 40 year.LED the earliest adopts the ruddiness GaAsP LED that makes of LPE (rheotaxial growth) technology, but the performance of these LED is relative to lower current.1970, add the method proposition of nitrogen in GaP and GaAsP after, improve the performance of LED and produced the LED component such as the green glow except ruddiness, orange coloured light.Early 1980s, the AlGaAs LED utilizing liquid phase deposition technology to make has good performance.After the nineties in 20th century, because new material and new epitaxy technology are incorporated in the research of red-light LED, the GaAs base AlGaInP LED utilizing MOCVD method (MOCVD) to make substantially improves LED performance that is red and yellow spectrum district.
The research of present stage GaAs base LED has obtained larger achievement, particularly internal quantum efficiency is more than 90% present stage, AlGaInP quaternary series LED generally uses GaAs substrate, for GaAs substrate, its energy gap is the change with al composition of 1.424ev, AlGaInP, and energy gap is from 1.9 to 2.3ev, so the photon down launched that active area produces will be predominantly absorbed, luminous efficiency is significantly reduced.For avoiding substrate extinction, between substrate and active layer, usually adding one deck distributed Bragg reflecting layer (DBR), to reflect the light of directive substrate, reducing the absorption of GaAs.Light energy usable reflection due to DBR reflector only to (usual qDBR < 20 °) in normal direction smaller angle, other light overwhelming majority away from normal incidence is all absorbed by GaAs substrate, thus promotes the limited efficiency of light efficiency.
In order to solve the extinction phenomenon of GaAs, improve luminous efficiency, people take a lot of method:
1. replace GaAs to absorb substrate with other substrate.Wherein a kind of method is exactly replace GaAs substrate (TS) with to the GaP substrate of visible transparent, namely there is the epitaxial layer structure of thick GaP Window layer on a gap substrate bonding with bonding techniques by long, and erode GaAs substrate, its luminous efficiency can be enhanced about more than once, and the transparent characteristic of GaP makes light-emitting area increase simultaneously.But there is the shortcoming that qualification rate is low, use equipment complicated, manufacturing cost is high in this technique.
2. upside-down mounting substrate.The thermal conductivity of silicon is better than GaAs, generally chooses the carrier of silicon substrate as flip-chip, makes speculum, make the light of directive substrate reflex to surface, from the outgoing of N district at silicon face.
Because above-mentioned two kinds of methods all need to increase repeatedly photoetching, corrosion, even use the equipment that price is high, product cost is improved.In IC (Integrated Circuit, integrated circuit) technique, wet-oxygen oxidation technique is extensively adopted to make SiO 2, first allow oxygen by bubble generator, make containing a certain amount of steam in oxygen, moisture content number depend on bath temperature and bleed pressure, then oxygen is imported into high temperature furnace pipe, makes Si and O 2reaction, forms SiO 2.Wet oxygen technique has the fast advantage of oxidation rate, but oxide layer short texture, exists the cavity of Pinhole-shaped, quality is not as dry oxygen technique, therefore generally take dry oxygen, wet oxygen in actual use, technique that dry oxygen replaces, not only ensure film performance but also take into account oxidation rate.
At VCSEL (Vertical Cavity Surface Emitting Laser, vertical cavity surface emitting laser) in technique, wet-oxygen oxidation technique also progressively arrives, utilize wet oxygen process oxidizes AlAs/AlGaAs, by the high Al layer oxidation in DBR, the oxide layer formed can play the effect of electricity restriction and refractive-index-guiding, lowers threshold current, improves conversion efficiency.
The structure bottom because of GaAs base chip is the dbr structure of high aluminium component, said method can be applied in the wet-oxygen oxidation process of GaAs based light-emitting diode equally, al composition is oxidized to Al2O3 film in actual applications, this film is attached to material surface and reaction can be caused to stagnate, have impact on the continuation reaction of side direction, DBR is oxidized insufficient, refractive index promotes not obvious, the unduplicated problem of result occurred in the wet-oxygen oxidation technique of namely existing GaAs based light-emitting diode.
Summary of the invention
Insufficient problem is oxidized for DBR in existing GaAs base light emitting diode chip wet-oxygen oxidation process, the present invention proposes a kind of process simplification, is beneficial to the wet-oxygen oxidation method of the GaAs based light-emitting diode of operation, to improve lateral oxidation, promote proceeding of reaction.
The wet-oxygen oxidation method of GaAs based light-emitting diode of the present invention, comprises the following steps:
(1) one deck SiO is made on GaAs base epitaxial wafer surface 2film is as protective layer;
(2) carry out hemisection operation to GaAs base epitaxial wafer, cutting-in reaches between Bragg reflecting layer (DBR) and substrate;
Depending on different epitaxial structure, the degree of depth is 10-15 μm.
(3) carry out wet oxygen operation, nitrogen is entered annealing furnace after bubble generator, the liquid in bubble generator is for containing H 2o 2deionized water, H 2o 2mass fraction be 0.5%-2%, fluid temperature 60-85 DEG C, keeps flat GaAs base epitaxial wafer in annealing furnace, towards nitrogen flow path direction place, annealing furnace temperature setting 350-400 DEG C, oxidization time 20 minutes-30 minutes;
(4) hydrofluoric acid is utilized to erode the SiO on GaAs base epitaxial wafer surface 2, complete the wet-oxygen oxidation of GaAs based light-emitting diode.
SiO in step (1) 2the thickness of film is 0.3 μm-0.6 μm.
Gas piping end in step (3) in annealing furnace and the distance of GaAs base epitaxial wafer are 10cm-30cm, to avoid H 2o 2do not contact GaAs base epitaxial wafer after access arrangement just to decompose, malleation cannot be formed around GaAs base epitaxial wafer.
Process of the present invention is simple, be beneficial to operation, and improve lateral oxidation, in the process of traditional wet-oxygen oxidation, increase hydrogen peroxide, hydrogen peroxide has strong oxidizing property, can acutely decompose more than 150 DEG C, and form water and oxygen, this can improve the oxidation of al composition; Hydrogen peroxide is when contacting GaAs base epitaxial wafer, because the substrate temperature in annealing furnace is more than 150 DEG C, now hydrogen peroxide volatilely can be decomposed into water and oxygen, improves partial pressure of oxygen on GaAs base epitaxial wafer surface, can by fully oxidized for al composition be the Al of low-refraction 2o 3.
Accompanying drawing explanation
Fig. 1 be GaAs base epitaxial wafer and on SiO 2the schematic diagram of film.
Fig. 2 is hemisection operation schematic diagram.
Fig. 3 is wet-oxygen oxidation operation process schematic diagram.
In figure: 1, SiO 2protective layer, 2, GaP layer, 3, P type limiting layer, 4, MQW, 5, DBR; 6, GaAs substrate layer, 7, N-type limiting layer, 8, resilient coating, 9, half cutting depth, 10, nitrogen; 11, bubble generator, 12, carry the nitrogen of steam, 13, RTA equipment, 14, GaAs base epitaxial wafer.
Embodiment
The wet-oxygen oxidation method of GaAs based light-emitting diode of the present invention, comprises the following steps:
(1) PECVD is utilized to make one deck SiO on GaAs base epitaxial wafer surface 2film as protective layer, SiO 2the thickness of film is about 0.3-0.6 μm.As shown in Figure 1, the structure of GaAs base epitaxial wafer comprises GaAs substrate layer 6, resilient coating 8, DBR layer 5, N-type limiting layer 7, mqw layer (multiple quantum well layer) 4, P type limiting layer 3 and GaP layer 2, SiO from bottom to top successively 2protective layer 1 is produced on GaP layer 2.
(2) as shown in Figure 2, carry out hemisection operation to the wafer (GaAs base epitaxial wafer) of step (1), half cutting depth 9 reaches between Bragg reflecting layer (DBR) and substrate.Depending on different epitaxial structure, the degree of depth can more than 10 μm.
(3) wafer of step 2 is carried out wet oxygen operation.As shown in Figure 3, nitrogen 10 is entered after bubble generator 11 annealing furnace (RTA equipment) 13, the liquid in bubble generator 11 is for containing H 2o 2deionized water, H 2o 2mass fraction be 0.5%-2%, fluid temperature 60-85 DEG C, keeps flat GaAs base epitaxial wafer 14 in annealing furnace, towards nitrogen flow path direction place, annealing furnace temperature setting 350-400 DEG C, oxidization time 20 minutes-30 minutes, take out epitaxial wafer.
In the lehr, the distance controlling of gas piping end and GaAs base epitaxial wafer, at 10-30cm, avoids H 2o 2malleation cannot be formed around GaAs base epitaxial wafer after premature decomposition.
(4) hydrofluoric acid is utilized to remove the SiO on GaAs base epitaxial wafer surface 2, complete the wet-oxygen oxidation of GaAs based light-emitting diode.

Claims (3)

1. a wet-oxygen oxidation method for GaAs based light-emitting diode, is characterized in that, comprise the following steps:
(1) one deck SiO is made on GaAs base epitaxial wafer surface 2film is as protective layer;
(2) carry out hemisection operation to GaAs base epitaxial wafer, cutting-in reaches between Bragg reflecting layer and substrate;
(3) carry out wet oxygen operation, nitrogen is entered annealing furnace after bubble generator, the liquid in bubble generator is for containing H 2o 2deionized water, H 2o 2mass fraction be 0.5%-2%, fluid temperature 60-85 DEG C, keeps flat GaAs base epitaxial wafer in annealing furnace, towards nitrogen flow path direction place, annealing furnace temperature setting 350-400 DEG C, oxidization time 20 minutes-30 minutes;
(4) hydrofluoric acid is utilized to erode the SiO on GaAs base epitaxial wafer surface 2, complete the wet-oxygen oxidation of GaAs based light-emitting diode.
2. the wet-oxygen oxidation method of GaAs based light-emitting diode according to claim 1, is characterized in that, SiO in described step (1) 2the thickness of film is 0.3 μm-0.6 μm.
3. the wet-oxygen oxidation method of GaAs based light-emitting diode according to claim 1, is characterized in that, the gas piping end in described step (3) in annealing furnace and the distance of GaAs base epitaxial wafer are 10cm-30cm.
CN201510072029.5A 2015-02-11 2015-02-11 A kind of wet-oxygen oxidation method of GaAs based light-emitting diodes Active CN104659166B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107845710A (en) * 2017-10-30 2018-03-27 江苏新广联半导体有限公司 A kind of gallium nitride base feux rouges epitaxial slice structure and preparation method

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WO2000065700A2 (en) * 1999-04-27 2000-11-02 Gore Enterprise Holdings, Inc. Postgrowth adjustment of cavity spectrum for semiconductor lasers and detectors
CN101005194A (en) * 2006-01-18 2007-07-25 中国科学院半导体研究所 Method for improving aluminum oxide/gallium arsenide distribution Bragg reflector interface quality
CN102376827A (en) * 2010-08-13 2012-03-14 大连美明外延片科技有限公司 Preparation method of AlGaInp light-emitting diode
CN103117339A (en) * 2013-03-15 2013-05-22 南京大学 Patterned sapphire substrate production method based on composite soft template nanometer stamping technique
US20130214294A1 (en) * 2012-02-17 2013-08-22 Epistar Corporation Light emitting device with planar current block structure
CN103489976A (en) * 2012-06-13 2014-01-01 山东浪潮华光光电子股份有限公司 Method for improving luminance of AlGaInP quaternary single-face dual-electrode light-emitting diode with GaAs substrate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000065700A2 (en) * 1999-04-27 2000-11-02 Gore Enterprise Holdings, Inc. Postgrowth adjustment of cavity spectrum for semiconductor lasers and detectors
CN101005194A (en) * 2006-01-18 2007-07-25 中国科学院半导体研究所 Method for improving aluminum oxide/gallium arsenide distribution Bragg reflector interface quality
CN102376827A (en) * 2010-08-13 2012-03-14 大连美明外延片科技有限公司 Preparation method of AlGaInp light-emitting diode
US20130214294A1 (en) * 2012-02-17 2013-08-22 Epistar Corporation Light emitting device with planar current block structure
CN103489976A (en) * 2012-06-13 2014-01-01 山东浪潮华光光电子股份有限公司 Method for improving luminance of AlGaInP quaternary single-face dual-electrode light-emitting diode with GaAs substrate
CN103117339A (en) * 2013-03-15 2013-05-22 南京大学 Patterned sapphire substrate production method based on composite soft template nanometer stamping technique

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107845710A (en) * 2017-10-30 2018-03-27 江苏新广联半导体有限公司 A kind of gallium nitride base feux rouges epitaxial slice structure and preparation method

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