CN109461682A - A kind of wet oxidation devices and methods therefor - Google Patents

A kind of wet oxidation devices and methods therefor Download PDF

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Publication number
CN109461682A
CN109461682A CN201811284776.5A CN201811284776A CN109461682A CN 109461682 A CN109461682 A CN 109461682A CN 201811284776 A CN201811284776 A CN 201811284776A CN 109461682 A CN109461682 A CN 109461682A
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control valve
closed shell
flow control
heating dish
wafer
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CN109461682B (en
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王冲
魏子尧
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Ningbo Moisten Core Microelectronic Equipment Co Ltd
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Ningbo Moisten Core Microelectronic Equipment Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005Apparatus not specifically provided for elsewhere
    • H01L21/67011Apparatus for manufacture or treatment
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02518Deposited layers
    • H01L21/02521Materials
    • H01L21/02551Group 12/16 materials
    • H01L21/02554Oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02614Transformation of metal, e.g. oxidation, nitridation

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Formation Of Insulating Films (AREA)

Abstract

The present invention provides a kind of wet oxidation device, including closed shell, heating dish, wafer, water bath with thermostatic control, porous steam generator, first flow control valve, second flow control valve, CCD camera and computer;The heating dish is mounted in the closed housing body;The wafer is arranged in the heating dish;The porous steam generator is arranged in the water bath with thermostatic control.Quality of the present invention is stablized, and manufacturing cost is low, avoids the addition of the corrosive liquids such as acidity, and improving device security and service life expands device oxide layer constantly, improves the range of work;The processing efficiency of device is improved, operation is simpler, and undesired impurities is effectively prevent to interfere;Have many advantages, such as that small in size, round output facula, single longitudinal mode output, threshold current are small, cheap, easy of integration for large area array.

Description

A kind of wet oxidation devices and methods therefor
Technical field
The present invention relates in technical field of semiconductors more particularly to a kind of wet oxidation devices and methods therefor.
Background technique
K.Holonyalk of University of Illinois, the nineteen ninety U.S. et al. has found high Al contents in an experiment first AlxGa1-xAs reacts with vapor in higher temperature and generates the stable good oxide layer of insulation performance of chemical property.In turn The AlAs wet oxidation technology of appearance becomes most extensive in VCSEL (vertical cavity surface emitting laser) and its array development and closes The technique of key, key technology are, limit the high aluminium layer in VCSEL resonant cavity, well suited Yu Yu little by oxidation reaction Size, the VCSEL of low threshold current.Wet oxidation method refers in VCSEL active layer and upper and lower distributed bragg reflector mirror (DBR) it is inserted into the AlGaAs oxide layer containing high aluminium component between layer, generates aluminium oxide from lateral oxidation using water vapour, is formed High value restricted area can make the extremely low threshold value of VCSEL realize continuous transmitting for carrying out electricity limitation and light limitation.Oxide-aperture Precision and oxidation technology thermal stability, to improve VCSEL output power and photoelectric conversion efficiency it is most important.Wet process oxygen Chemical industry skill is exactly to control oxidation depth by oxidization time by certain oxidation rate, realizes oxidation limiting aperture and light hole diameter Precisely align.
Simple wet etching technique: laterally limiting carrier, and simplest method is exactly by the resonance of device Chamber and upper DBR are etched into columnar structures.Etch air column type wet process wet processing corrosion depth it is more difficult to control, after etching The bottom of column is fluted, and which has limited further decreasing for device diameters;The repeatability of technique is poor, the proportion of corrosive liquid, Etching time and corrosion temperature can all influence the quality on surface.
Ion implantation: ion implantation technology be exactly with energetic ion injection set it is each the charged particle with certain energy It is incorporated into semiconductor material, to change the electrical properties and optical property of semiconductor material.Ion injects from upper DBR, It collides with brilliant intracorporal electronics and atomic nucleus, generates lattice vacancy, and formed around by the compensation of free carrier High resistance area can thus be such that Injection Current concentration is injected into active area.The production efficiency of ion implanting is low, and high temperature will cause Dopant redistribution increases junction depth and lateral doping effect;Sub- injection device system complex, it is careful and expensive that operation needs.
Summary of the invention
Technical problems to be solved
The problem to be solved in the present invention is to provide a kind of wet oxidation devices and methods therefors, to overcome technique in the prior art Complexity, unstable quality, the high defect of manufacturing cost.
Technical solution
To solve the technical problem, the present invention provides a kind of wet oxidation device, including closed shell, heating dish, crystalline substance Circle, water bath with thermostatic control, porous steam generator, first flow control valve, second flow control valve, CCD camera and computer;Institute Heating dish is stated to be mounted in the closed housing body;The wafer is arranged in the heating dish;The porous steam generator It is arranged in the water bath with thermostatic control;The closed shell is connected to by pipeline with the porous steam generator;Described first One end of flow control valve is connected to by pipeline with the porous steam generator, the other end of the first flow control valve It is connected to by pipeline with the first gas tank, is filled with nitrogen;One end of the second flow control valve passes through pipeline and the closed housing The other end of body connection, the second flow control valve is connected to by pipeline with the second gas tank, and the mixing of nitrogen and hydrogen is filled with Gas;The surface of the wafer is arranged in the CCD camera, and the CCD camera is connect with the computer.
Preferably, the wet oxidation device further includes drier, and the drier is arranged in the closed shell and institute It states on the pipeline between porous steam generator.
Preferably, the closed shell side is provided with gas vent.
A kind of wet oxidizing process, which comprises the steps of:
S01, place: the wafer for carrying out device is put into heating dish, it is ensured that after placing, shuts closed shell;
S02, clean air: being filled with nitrogen, and the air in closed shell is discharged;
S03, preheating: heating dish can heat, heating and temperature control is at 100-600 degrees Celsius in close encapsulating housing;
S04 keeps water temperature: control water bath with thermostatic control temperature is at 80 DEG C -90 degrees Celsius;
S05, inflation: carrying water vapour by nitrogen and a certain proportion of hydrogen enter closed shell, by dry water vapour Also close encapsulating housing, the oxidation rate of control device are filled with;Hydrogen is as reducing agent;
S06, pressure regulation: adjusting first flow control valve and second flow control valve, changes the flow for being filled with gas, Jin Ergai Become air pressure in sealing dress housing chamber and changes oxidizing reaction rate;
S07, temperature adjustment: observation heating dish temperature, and according to perfect condition heating and cooling, reaction rate is controlled with this and reaches ideal It is horizontal;
Observation: the picture of the oxidization condition of wafer by CCD camera, is uploaded to computer in real time, computer passes through by S08 The mode of image comparison confirms oxidation effectiveness;
S09 stops gas supply: after reaching oxidation effectiveness, stopping injecting steam to close encapsulating housing;
S10, cooling: closing heating dish, and close encapsulating housing is made to restore room temperature;
S11, exhaust: close encapsulating housing gas and impurity, recovery room wet pressure is discharged in exhaust outlet effect;
Pickup: S12 after othermohygrometer is restored, takes out wafer.
Preferably, in the S05, the ratio of hydrogen is controlled in the range of 0.1%-10%.
Preferably, in the S03, preferred 400-500 degrees Celsius of heating temperature.
Preferably, in the S04, preferably 80 degrees Celsius of water bath with thermostatic control temperature are controlled.
Have the beneficial effect that wet oxidation devices and methods therefor of the invention, quality is stablized, and manufacturing cost is low, avoids acidity The addition of equal corrosive liquids, improving device security and service life expands device oxide layer constantly, improves the range of work;It mentions The processing efficiency of high device, operation is simpler, and undesired impurities is effectively prevent to interfere;With small in size, round output facula, Single longitudinal mode output, threshold current it is small, cheap, easy of integration be large area array the advantages that.
Detailed description of the invention
Fig. 1 is a kind of flow chart of wet oxidizing process of the present invention;
Fig. 2 is a kind of structural schematic diagram of wet oxidation device of the present invention;
Fig. 3 is the structural schematic diagram of wafer and VCESL;
Fig. 4 is the partial enlarged view of A in Fig. 3.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below Example is not intended to limit the scope of the invention for illustrating the present invention.
As shown in Fig. 2, a kind of wet oxidation device of the invention, including closed shell 1, heating dish 2, wafer 3, thermostatted water Bath 5, porous steam generator 6, first flow control valve 7, second flow control valve 8, CCD camera 9 and computer 10;It is described Heating dish 2 is mounted in the closed shell 1;The wafer 3 is arranged in the heating dish 2;The porous water vapour occurs Device 6 is arranged in the water bath with thermostatic control 5;The closed shell 1 is connected to by pipeline with the porous steam generator 6;Institute The one end for stating first flow control valve 7 is connected to by pipeline with the porous steam generator 6, the first flow control valve 7 other end is connected to by pipeline with the first gas tank 13, and nitrogen is filled with;One end of the second flow control valve 8 passes through pipeline It is connected to the closed shell 1, the other end of the second flow control valve 8 is connected to by pipeline with the second gas tank 12, is filled with The mixed gas of nitrogen and hydrogen;The surface of the wafer 3, the CCD camera 9 and institute is arranged in the CCD camera 9 State the connection of computer 10.
The wet oxidation device further includes drier 4, the drier 4 setting the closed shell 1 with it is described more On pipeline between hole steam generator 6.
1 side of closed shell is provided with gas vent 11.Gas vent 11 is connect with on-off valve, allow gas vent 11 into Row opens and closes.
As shown in Figure 1, a kind of wet oxidizing process of wet oxidation device as described in claim 1, which is characterized in that Include the following steps: S01, place: the wafer 3 for carrying out device is put into heating dish 2, it is ensured that after placing, shuts closed shell 1;S02, clean air: being filled with nitrogen, and the air in closed shell 1 is discharged;S03, preheating: heating dish 2, can in close encapsulating housing 1 With heating, heating and temperature control is at 100-600 degrees Celsius, preferably 400 degrees Celsius of the present embodiment;S04 keeps water temperature: control is permanent 5 temperature of tepidarium is at 80 DEG C -90 degrees Celsius, preferably 80 degrees Celsius of the present embodiment;S05, inflation: by nitrogen carry water vapour and A certain proportion of hydrogen enters closed shell 1, and dry water vapour is also filled with close encapsulating housing 1, the oxidation rate of control device; Hydrogen is as reducing agent;S06, pressure regulation: adjusting first flow control valve 7 and second flow control valve 8, changes the stream for being filled with gas Amount, and then change the intracavitary air pressure of close encapsulating housing 1 and change oxidizing reaction rate;S07, temperature adjustment: observation 2 temperature of heating dish, and According to perfect condition heating and cooling, reaction rate is controlled with this and reaches desirable level;S08, observation: by CCD camera 9, in real time The picture of the oxidization condition of wafer 3 is uploaded into computer 10, computer 10 confirms oxidation effectiveness by way of image comparison; S09 stops gas supply: after reaching oxidation effectiveness, stopping injecting steam to close encapsulating housing 1;Cooling: S10 closes heating dish 2, makes Close encapsulating housing 1 restores room temperature;S11, exhaust: exhaust outlet 11 acts on, and close 1 gas of encapsulating housing and impurity is discharged, and restores room temperature Air pressure;Pickup: S12 after othermohygrometer is restored, takes out wafer 3.
In the S05, the ratio of hydrogen controls the present embodiment preferably 3% in the range of 0.1%-10%.
Shown in Fig. 4, because wet oxidation at a temperature of 400-500 DEG C has very the AlGaAs of AlAs and high Al contents Strong selectivity, and 15 performance of oxide layer formed is stablized, and electrical insulation capability is good, and refractive index is low, is very suitable for electric current limit System and optical confinement, so before this wet process oxidation technology has well in the preparation of semiconductor devices and photoelectric field Scape.
This technique is for vertical cavity surface emitting laser (VCESL14) research application, and VCESL14 is with gallium arsenide semiconductor material It is developed based on material, is different from the other light sources such as LED (light emitting diode) and LD (laser diode), had small in size, round Output facula, single longitudinal mode output, threshold current it is small, cheap, easy of integration be large area array the advantages that, be widely applied and light The fields such as communication, light network, optical storage.
As shown in Figure 3 and Figure 4, several VCESL14 are evenly arranged on wafer 3.
When the invention works: this technique carries hydrogen and water vapour by N2, on VCESL14 in closed environment AlAs semiconductor material carries out oxidation reaction.The mixed gas of nitrogen and hydrogen is discharged by the second gas tank 12, is filled by pipeline Enter in closed shell 1;The nitrogen gas tank of another the first gas tank 13 discharges, and by pipeline, gas enters porous steam evaporator 6, water vapour is carried by nitrogen, enters closed shell 1 by drier 4.Oxidation because AlAs is easily reacted with water, but at normal temperature Destructive hydrolysis can occur, therefore reaction temperature should be warming up to 300 DEG C~400 DEG C by heating dish.(present apparatus heating dish highest can Be heated to 600 DEG C) AlAs at high temperature, react with water vapour, generate the oxide of Al and the oxide of As, specific chemistry Equation is as follows: 2AlAs+6H2O (g)=Al2O3+As2O3+6H2 ↑, As2O3+3H2=2As+3H2O (g);The high temperature of AlAs Oxidation reaction can material the edge of the circle start to aoxidize, oxidized portion be Al oxide, high resistant, can carry out well current limit and Optical confinement.A microscope CCD camera 9 is placed above wafer 3, is connected to computer 10, observes the oxidation journey of this wafer 3 Degree.Degree of oxidation reflects the aperture constantly reduced for 3 radius of wafer on computer 10, when reaching expected aperture size, stops The release of water vapour.
Flow control valve: control gas flow;Gas tank: storage nitrogen and hydrogen mixer store nitrogen;Porous vapor Generator 6: the water vapour of constant temperature is prepared;Closed shell 1: being that wafer 3 reacts under impregnable confined space;Heating dish 2: Condition is provided for the high temperature of oxidation reaction;Exhaust outlet 11: discharge tail gas and impurity;CCD camera 9: high resistance area on observation device Radius size;The effect of drier 4 is: porous steam generator 6 can carry droplet, and purpose excludes droplet, only retains gaseous state.
The principle of the present invention: destructive hydrolysis can occur for the oxidation because AlAs is easily reacted with water, but at normal temperature, therefore react Temperature should be warming up to 300 DEG C~400 DEG C by heating dish.(present apparatus heating dish highest can be heated to 600 DEG C.) AlAs is in high temperature Under, it reacts with vapor, generates the oxide of Al and the oxide of As, specific chemical equation is as follows: 2AlAs+6H2O (g)=Al2O3+As2O3+6H2 ↑, As2O3+3H2=2As+3H2O (g);The high-temperature oxydation reaction meeting material the edge of the circle of AlAs is held Begin to aoxidize, oxidized portion is the oxide of Al, and high resistant can carry out current limit and optical confinement well, and two sides become to do resistance Value, substantially impervious light plays the role of limiting light.
Movement: changing the flow for being filled with gas by flow control valve, and the first gas tank 13 is that being filled with for N2 tank passes through first Porous steam evaporator 6, purpose carry water vapour and enter closed shell 1.It, can be by adjusting first after required gas is filled with Flow control valve 7, and then the oxidizing reaction rate in control device;2 temperature of heating dish is adjusted, purpose is also for passing through temperature Degree influences reaction rate, and then reaches perfect condition.
Operating path: the second gas tank 12 is that mixed gas tank is filled with closed shell 1, and is adjusted by second flow control valve 8 Section;Porous steam evaporator 6 prepares constant temperature vapor in water bath with thermostatic control 5;What opening was connected with porous steam evaporator 6 First gas tank 13, is charged therein nitrogen, brings water vapour into closed shell 1;In closed shell 1, in the gentle pressing of temperature In the case where reason, water vapour and AlAs react, and the reaction was continued for a small amount of hydrogen being filled with and the oxide of generation, on the one hand Oxidation rate is controlled, useless oxide is on the one hand restored.
In conclusion it is restricted embodiment of the invention, all those skilled in the art that above embodiment, which is not, The modification carried out on the basis of substantive content of the invention or equivalent deformation, in technology scope of the invention.

Claims (7)

1. a kind of wet oxidation device, it is characterised in that: including closed shell (1), heating dish (2), wafer (3), water bath with thermostatic control (5), porous steam generator (6), first flow control valve (7), second flow control valve (8), CCD camera (9) and electricity Brain (10);The heating dish (2) is mounted in the closed shell (1);The wafer (3) is arranged on the heating dish (2); Porous steam generator (6) setting is in the water bath with thermostatic control (5);The closed shell (1) by pipeline with it is described Porous steam generator (6) connection;It is sent out by pipeline and the porous water vapour one end of the first flow control valve (7) The other end of raw device (6) connection, the first flow control valve (7) is connected to by pipeline with the first gas tank (13), and nitrogen is filled with; One end of the second flow control valve (8) is connected to by pipeline with the closed shell (1), the second flow control valve (8) the other end is connected to by pipeline with the second gas tank (12), and the mixed gas of nitrogen and hydrogen is filled with;The CCD camera (9) it is arranged in the surface of the wafer (3), the CCD camera (9) connect with the computer (10).
2. wet oxidation device according to claim 1, it is characterised in that: the wet oxidation device further includes drier (4), on the pipeline that the drier (4) is arranged between the closed shell (1) and the porous steam generator (6).
3. wet oxidation device according to claim 1, it is characterised in that: closed shell (1) side is provided with row Stomata (11).
4. a kind of wet oxidizing process of wet oxidation device as described in claim 1, which is characterized in that including walking as follows It is rapid:
S01, place: the wafer (3) for carrying out device is put on heating dish (2), it is ensured that after placing, shuts closed shell (1);
S02, clean air: being filled with nitrogen, and the air in closed shell (1) is discharged;
S03, preheating: heating dish (2) can heat, heating and temperature control is at 100-600 degrees Celsius in close encapsulating housing (1);
S04 keeps water temperature: control water bath with thermostatic control (5) temperature is at 80 DEG C -90 degrees Celsius;
S05, inflation: carrying water vapour by nitrogen and a certain proportion of hydrogen enter closed shell (1), by dry water vapour It is filled with close encapsulating housing (1), the oxidation rate of control device;Hydrogen is as reducing agent;
S06, pressure regulation: adjusting first flow control valve (7) and second flow control valve (8), changes the flow for being filled with gas, in turn Change the intracavitary air pressure of close encapsulating housing (1) and changes oxidizing reaction rate;
S07, temperature adjustment: observation heating dish (2) temperature, and according to perfect condition heating and cooling, reaction rate is controlled with this and reaches ideal It is horizontal;
S08, observation: by CCD camera (9), in real time uploading to the picture of the oxidization condition of wafer (3) computer (10), electricity Brain (10) confirms oxidation effectiveness by way of image comparison;
S09 stops gas supply: after reaching oxidation effectiveness, stopping injecting steam to close encapsulating housing (1);
S10, cooling: closing heating dish (2), and close encapsulating housing (1) is made to restore room temperature;
S11, exhaust: close encapsulating housing (1) gas and impurity, recovery room wet pressure is discharged in exhaust outlet (11) effect;
Pickup: S12 after othermohygrometer is restored, takes out wafer (3).
5. wet oxidizing process according to claim 4, it is characterised in that: in the S05, the ratio control of hydrogen exists In the range of 0.1%-10%.
6. wet oxidizing process according to claim 4, it is characterised in that: in the S03, the preferred 400- of heating temperature 500 degrees Celsius.
7. wet oxidizing process according to claim 4, it is characterised in that: in the S04, control water bath with thermostatic control (5) temperature Preferably 80 degrees Celsius of degree.
CN201811284776.5A 2018-10-31 2018-10-31 Wet oxidation device and application method thereof Active CN109461682B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110994359A (en) * 2019-12-13 2020-04-10 武汉光安伦光电技术有限公司 Wet oxidation process for improving oxidation uniformity of vertical cavity surface emitting laser
CN111162452A (en) * 2020-01-02 2020-05-15 深亮智能技术(中山)有限公司 Method and device for improving uniformity of wet oxidation process of vertical cavity surface emitting laser
CN113904215A (en) * 2021-10-09 2022-01-07 苏州长瑞光电有限公司 Wet oxidation method for vertical cavity surface emitting laser and vertical cavity surface emitting laser

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JPH0897196A (en) * 1994-09-26 1996-04-12 Sony Corp Heat treating furnace
US6221791B1 (en) * 1999-06-02 2001-04-24 Taiwan Semiconductor Manufacturing Company, Ltd Apparatus and method for oxidizing silicon substrates
CN101623661A (en) * 2009-08-05 2010-01-13 山东电力研究院 Metal material high temperature water vapor oxidation experiment device
CN104729979A (en) * 2015-03-27 2015-06-24 华电电力科学研究院 High temperature water vapor oxidation experiment device capable of accurately controlling oxygen content
CN108461564A (en) * 2018-05-19 2018-08-28 江苏东鋆光伏科技有限公司 Anti- PID performances photovoltaic cell and preparation method thereof

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Publication number Priority date Publication date Assignee Title
JPH0897196A (en) * 1994-09-26 1996-04-12 Sony Corp Heat treating furnace
US6221791B1 (en) * 1999-06-02 2001-04-24 Taiwan Semiconductor Manufacturing Company, Ltd Apparatus and method for oxidizing silicon substrates
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CN104729979A (en) * 2015-03-27 2015-06-24 华电电力科学研究院 High temperature water vapor oxidation experiment device capable of accurately controlling oxygen content
CN108461564A (en) * 2018-05-19 2018-08-28 江苏东鋆光伏科技有限公司 Anti- PID performances photovoltaic cell and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110994359A (en) * 2019-12-13 2020-04-10 武汉光安伦光电技术有限公司 Wet oxidation process for improving oxidation uniformity of vertical cavity surface emitting laser
CN111162452A (en) * 2020-01-02 2020-05-15 深亮智能技术(中山)有限公司 Method and device for improving uniformity of wet oxidation process of vertical cavity surface emitting laser
CN113904215A (en) * 2021-10-09 2022-01-07 苏州长瑞光电有限公司 Wet oxidation method for vertical cavity surface emitting laser and vertical cavity surface emitting laser

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