CN103668115A - Vapor phase epitaxy reaction tube with cavity wall temperature set by growth program in real time - Google Patents

Vapor phase epitaxy reaction tube with cavity wall temperature set by growth program in real time Download PDF

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Publication number
CN103668115A
CN103668115A CN201210353647.3A CN201210353647A CN103668115A CN 103668115 A CN103668115 A CN 103668115A CN 201210353647 A CN201210353647 A CN 201210353647A CN 103668115 A CN103668115 A CN 103668115A
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China
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reaction chamber
circulatory mediator
temperature
circulating medium
chamber
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CN201210353647.3A
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Chinese (zh)
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江风益
刘军林
方文卿
蒲勇
徐龙权
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Nanchang Huanglv Lighting Co., Ltd.
Nanchang University
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NANCHANG HUANGLV LIGHTING CO Ltd
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Abstract

The invention discloses a vapor phase epitaxy reaction tube with cavity wall temperature set by a growth program in real time. The vapor phase epitaxy reaction tube comprises a reaction chamber and a control system, wherein a graphite substrate base and an epitaxy substrate are mounted on an MOCVD (metal organic chemical vapor deposition) heater in the reaction chamber; and an MOCVD spray head is mounted above the epitaxy substrate. The vapor phase epitaxy reaction tube is characterized in that circulating medium channels are arranged on the top, bottom and four side walls of the inner wall of the reaction chamber; and the circulating medium channel is connected with a thermostat circulating medium outlet of a thermostat at a reaction chamber circulating medium inlet on the left side wall, and the circulating medium channel is connected with a thermostat circulating medium inlet of the thermostat at a reaction chamber circulating medium outlet on the right side wall so that the circulating medium circulates between the circulating medium channels of the reaction chamber and the thermostat. In conclusion, the vapor phase epitaxy reaction tube disclosed by the invention has the advantages that the controllability of the epitaxy process is improved, the energy is saved and the like by performing real-time online temperature change of the cavity wall, accelerating desorption of foreign gases on the cavity wall, improving the quality of epitaxy material and reducing the growth cost.

Description

The vapour phase epitaxy reaction tubes that chamber wall temperature can be arranged in real time by growth procedure
Technical field
The present invention relates to semiconductor material producing apparatus, relate in particular to the vapour phase epitaxy reaction tubes that a kind of chamber wall temperature can be arranged in real time by growth procedure.
background technology:
Current, large-scale energy-saving and emission-reduction campaign is just being risen in the whole world, and (be photodiode, be LED) a kind of effective measure wherein to semiconductor lighting, still, if will come into Chinese huge numbers of families, also will greatly reduce costs, and continue to improve electro-optical efficiency.The manufacturer of current metal organic chemical vapor deposition equipment (MOCVD) only has three, the VEECO of German AIXTRON, the U.S. and Britain Thomasswan company (being called for short TS).At present, the chamber wall temperature of the reaction tubes of three kinds of MOVCD of these three productions is all constant, cannot, in process of growth, by epitaxy program, be set in real time and be controlled.And through applicant research, the real-time control of chamber wall temperature is precipitous to doping, interface, the wavelength homogeneity of epitaxial wafer, MOCVD itself are energy-conservation etc., all benefit, by real-time control chamber wall temperature, can produce the LED that electro-optical efficiency is higher.
The epitaxial film of LED is comprised of tens layers epitaxial material, and the growth temperature of every layer, composition form, dopant species may be all different.Generally all wish that the material composition of these layers is strictly controlled, but in LED outer layer growth process, the growth raw material of front one deck and dopant can be adsorbed in the wall of chamber, and slow release always, thereby affect Material growth quality, finally affect the electro-optical efficiency of LED.At present, the chamber wall temperature of Britain Thomasswan company is to carry out constant setting by the temperature of water coolant, and operated by rotary motion is at 50-60 ℃, once set, in process of growth, just no longer change, more can not be controlled by extent of growth.Other MOCVD equipment of two is also like this.
When reaction tubes blow-on load or while getting sheet, airborne oxygen and water also can be adsorbed onto reaction tube wall, and the quality control that these external gases externally prolong material all has impact, the stability that also impact is produced.The impact of the external gas for reducing dress, while getting sheet, generally will be placed in reaction tubes nitrogen environment (glove box) or all by Robot actions, the cost of these devices is also very high, and operates extremely inconvenient.Although use these measures can reduce the impact of external gas, but during maintenance, reaction tubes still will be exposed in atmosphere, often, after maintenance, reaction tubes will be grown several stoves and could recover, sometimes just normal, take again reaction tubes apart, move in circles like this, maintain epitaxial growth very painful, also cause great waste.
To in process of growth, remove last layer in time and (or which floor be gone up, or even former stoves) be adsorbed on the foreign gas of chamber wall, will allow the chamber wall energy of reaction tubes heat and the online temperature by extent of growth control chamber wall, by heating, allow impurity desorption, but when key stratum is grown, can reduce chamber wall temperature again, thereby minimizing in time even finishes impurity from the desorption of chamber wall.
summary of the invention:
The vapour phase epitaxy reaction tubes that the object of the present invention is to provide a kind of chamber wall temperature to be arranged in real time by growth procedure, this vapour phase epitaxy reaction tubes is by the real-time online alternating temperature to chamber wall, the desorption of accelerating cavity wall foreign gas, the impact of the foreign gas of control chamber wall absorption on epitaxial film materials, thereby improve the quality of epitaxial substrate, improve the controllability of electro-optical efficiency and epitaxial growth equipment, reduce growth cost.
The object of the present invention is achieved like this:
The vapour phase epitaxy reaction tubes that a kind of chamber wall temperature can be arranged in real time by growth procedure, comprise reaction chamber and Controlling System, MOCVD well heater is installed in reaction chamber, graphite substrate pedestal and epitaxial substrate are installed from bottom to up successively on MOCVD well heater, MOCVD well heater carries out heated for controlling temperature to graphite base, graphite base heats epitaxial substrate, in reaction chamber, the top of epitaxial substrate is provided with over against epitaxial substrate and the MOCVD shower nozzle placed with epitaxial substrate interval, in the middle of the top board of reaction chamber, be provided with an air inlet port, on the base plate both sides of reaction chamber, be respectively provided with a venting hole, feature is: at the top of reaction chamber wall, bottom and surrounding sidewall are provided with the circulatory mediator passage of sealing, on the left side wall of reaction chamber and right side wall, be respectively equipped with reaction chamber circulatory mediator entrance and the outlet of reaction chamber circulatory mediator, reaction chamber circulatory mediator entrance links together the constant temperature machine circulatory mediator outlet of circulatory mediator passage and constant temperature machine, the outlet of reaction chamber circulatory mediator links together the constant temperature machine circulatory mediator entrance of circulatory mediator passage and constant temperature machine, make circulatory mediator circulation between the circulatory mediator passage of reaction chamber and constant temperature machine, the controlled system of reaction chamber and constant temperature machine is controlled.
Circulatory mediator is a kind of in thermal oil, water or Liquid Sodium, and the temperature of circulatory mediator is at 20-600 ℃.The temperature of thermal oil is 20-350 ℃, and the temperature of Liquid Sodium is 100-600 ℃.
The present invention is owing to being provided with the circulatory mediator passage of sealing on the top at reaction chamber wall, surrounding sidewall, and be communicated with constant temperature machine, circulatory mediator just can be between the circulatory mediator passage of reaction chamber and constant temperature machine circulation. circulatory mediator, except maintaining the wall temperature of chamber, also plays the effect of cooling reaction chamber.Reaction chamber keeps the Heating temperature of the MOCVD well heater in reaction chamber under the control of Controlling System, and constant temperature machine keeps the temperature of the circulatory mediator in constant temperature machine under the control of Controlling System.
Working process is as follows: when epitaxial substrate is put into after reaction chamber, the sequence of control of whole temperature is as follows: the temperature in reaction chamber is raised to (as 400 ℃) after moderate temperature, constant temperature machine is set to higher temperatures (as 150 ℃), reaction chamber is carried out to low pressure degasification, now with high-purity gas, carry out pressure changeable flushing on the one hand, on the other hand, high temperature can impel the foreign gas desorption on the wall of chamber.These foreign gases can be the entrap bubbles of a upper stove, can be to be also adsorbed on oxygen and the aqueous vapor on the wall of chamber after opening reaction chamber.
Subsequently, reaction chamber is warmed up to higher temperature and carries out epitaxy, before starting outer layer growth, preferably first reduces the temperature of chamber wall to reduce the impact of the foreign gas of desorption.In a word, when certain layer of epitaxial film insensitive or while artificially suspending Material growth to impurity, the constant temperature machine degasification that just can heat up, otherwise, constant temperature machine will be lowered, to reduce impurity desorption.
In AlGaInN material system, Si is as N-shaped impurity conventionally, and Mg is as p type impurity.In the process of growth of this material, the precipitous control in the interface of quantum well, the doping of Mg, the growth of AlGaN, all can be used and become chamber this measure of wall temperature, now proved that this is conducive to high-quality Material growth.
The suitable raising of chamber wall temperature, (for example also can reduce the temperature difference between epitaxial substrate and chamber wall, underlayer temperature during growth blue light quantum well is generally 720 ℃, with chamber wall be to have the temperature difference), thereby the temperature of the epitaxial substrate that can reduce the turbulent flow of growth gasses and cause due to position deviation is uneven, thereby can improve the temperature homogeneity (conventionally require to be controlled at ± 1 ℃ in) of epitaxial substrate, and then improve the homogeneity (temperature homogeneity and turbulent flow determine the homogeneity of emission wavelength) of the emission wavelength of epitaxial substrate.
After opening reaction chamber and safeguarding, the constant temperature machine that can make reaction chamber be raised to suitable temp (as 400 degree) and cooling this reaction chamber is raised to comparatively high temps (as 200 degree) chamber wall is carried out to vacuum stripping or pressure changeable degasification, can make like this reaction tubes very fast clean, drop into fast normal production.
The raising of chamber wall temperature also helps energy-conservation, and the graphite base temperature of the placement epitaxial substrate in reaction chamber can reach 1100 ℃, reduces the temperature difference of chamber wall and graphite base, both can save energy the life-span that also can extend MOCVD well heater.
In a word, thus the foreign gas that the present invention has desorption by the real-time online alternating temperature on chamber wall, accelerating cavity wall foreign gas, the absorption of control chamber wall on the impact of epitaxial film materials improve epitaxial material quality, improve electro-optical efficiency, improve epitaxial growth equipment controllability, reduce growth cost, reduce time of recovery after maintenance of equipment, improve epitaxy technique controllability, energy-conservation, extend the series of advantages such as MOCVD well heater life-span.
accompanying drawing explanation:
Fig. 1 is block diagram of the present invention;
Fig. 2 is the structural representation of reaction chamber.
embodiment:
Below in conjunction with embodiment and contrast accompanying drawing method of the present invention is further detailed.
The vapour phase epitaxy reaction tubes that a kind of chamber wall temperature can be arranged in real time by growth procedure, comprise reaction chamber 1 and Controlling System 2, MOCVD well heater 4 is installed in reaction chamber, graphite substrate pedestal 5 and epitaxial substrate 6 are installed from bottom to up successively on MOCVD well heater 4, 4 pairs of graphite bases of MOCVD well heater 5 carry out heated for controlling temperature, 5 pairs of epitaxial substrate 6 of graphite base heat, in reaction chamber 1, the top of epitaxial substrate 6 is provided with over against epitaxial substrate 6 and the MOCVD shower nozzle 8 placed with epitaxial substrate 6 intervals, in the middle of the top board 9 of reaction chamber 1, be provided with an air inlet port 10, base plate 11 both sides at reaction chamber 1 are respectively provided with a venting hole 12, top at reaction chamber 1 inwall, bottom and surrounding sidewall are provided with the circulatory mediator passage 13 of sealing, on the left side wall 15 of reaction chamber 1 and right side wall 16, be respectively equipped with reaction chamber circulatory mediator entrance 14 and reaction chamber circulatory mediator outlet 7, reaction chamber circulatory mediator entrance 14 links together the circulatory mediator outlet of circulatory mediator passage 13 and constant temperature machine 3, reaction chamber circulatory mediator outlet 7 links together the circulatory mediator entrance of circulatory mediator passage 13 and constant temperature machine 3, make circulatory mediator circulation between the circulatory mediator passage 13 of reaction chamber 1 and constant temperature machine 3, the controlled system 2 of reaction chamber 1 and constant temperature machine 3 is controlled.
Circulatory mediator is a kind of in thermal oil, water or Liquid Sodium, and the temperature of circulatory mediator is at 20-600 ℃.
The temperature of thermal oil is 20-350 ℃.The temperature of Liquid Sodium is 100--600 ℃.
Reactant gases, from air inlet port 10 is come in, is distributed to the surface of epitaxial substrate 6 through MOCVD shower nozzle 8.Epitaxial substrate 6 is placed on graphite base 5, and graphite base 54 pairs of graphite bases 5 of MOCVD well heater below heat, thereby maintain necessary epitaxial growth temperature.Circulatory mediator, except maintaining the wall temperature of chamber, also plays the effect of cooling reaction chamber 1.Reacted gas is received air-bleed system through venting hole 12, thereby can control the air pressure in reaction chamber 1.
Be to be understood that to be, above-described embodiment is just to explanation of the present invention, rather than limitation of the present invention, any not exceeding within the replacement of the unsubstantiality within the scope of connotation of the present invention or the innovation and creation of modification all fall into protection domain of the present invention.

Claims (3)

1. a chamber wall temperature can be by the real-time vapour phase epitaxy reaction tubes arranging of growth procedure, comprise reaction chamber and Controlling System, MOCVD well heater is installed in reaction chamber, graphite substrate pedestal and epitaxial substrate are installed from bottom to up successively on MOCVD well heater, MOCVD well heater carries out heated for controlling temperature to graphite base, graphite base heats epitaxial substrate, in reaction chamber, the top of epitaxial substrate is provided with over against epitaxial substrate and the MOCVD shower nozzle placed with epitaxial substrate interval, in the middle of the top board of reaction chamber, be provided with an air inlet port, on the base plate both sides of reaction chamber, be respectively provided with a venting hole, feature is: at the top of reaction chamber wall, surrounding sidewall is provided with the circulatory mediator passage of sealing, on the left side wall of reaction chamber and right side wall, be respectively equipped with reaction chamber circulatory mediator entrance and the outlet of reaction chamber circulatory mediator, reaction chamber circulatory mediator entrance links together the constant temperature machine circulatory mediator outlet of circulatory mediator passage and constant temperature machine, the outlet of reaction chamber circulatory mediator links together the constant temperature machine circulatory mediator entrance of circulatory mediator passage and constant temperature machine, make circulatory mediator circulation between the circulatory mediator passage of reaction chamber and constant temperature machine, the controlled system of reaction chamber and constant temperature machine is controlled.
2. the vapour phase epitaxy reaction tubes that chamber according to claim 1 wall temperature can be arranged in real time by growth procedure, is characterized in that: circulatory mediator is a kind of in thermal oil, water or sodium liquid, and the temperature of circulatory mediator is at 20-600 ℃.
3. the vapour phase epitaxy reaction tubes that chamber according to claim 2 wall temperature can be arranged in real time by growth procedure, is characterized in that: the temperature of thermal oil is 20-350 ℃, the temperature of Liquid Sodium is 100--600 ℃.
CN201210353647.3A 2012-09-21 2012-09-21 Vapor phase epitaxy reaction tube with cavity wall temperature set by growth program in real time Pending CN103668115A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104952710A (en) * 2015-06-12 2015-09-30 湘能华磊光电股份有限公司 LED (Light-emitting Diode) epitaxial layer growing method
CN107895102A (en) * 2017-11-23 2018-04-10 苏州矩阵光电有限公司 One kind growth instruction checking method and device
CN114486543A (en) * 2022-01-04 2022-05-13 浙江大学 System and method for testing influence of trace gas impurities on high-pressure hydrogen embrittlement of material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101748391A (en) * 2008-12-12 2010-06-23 东京毅力科创株式会社 Film deposition apparatus and film deposition method
CN102127757A (en) * 2011-01-14 2011-07-20 映瑞光电科技(上海)有限公司 Metal organic chemical vapor deposition (MOCVD) reaction system

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101748391A (en) * 2008-12-12 2010-06-23 东京毅力科创株式会社 Film deposition apparatus and film deposition method
CN102127757A (en) * 2011-01-14 2011-07-20 映瑞光电科技(上海)有限公司 Metal organic chemical vapor deposition (MOCVD) reaction system

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104952710A (en) * 2015-06-12 2015-09-30 湘能华磊光电股份有限公司 LED (Light-emitting Diode) epitaxial layer growing method
CN104952710B (en) * 2015-06-12 2018-01-30 湘能华磊光电股份有限公司 A kind of LED outer layer growths method
CN107895102A (en) * 2017-11-23 2018-04-10 苏州矩阵光电有限公司 One kind growth instruction checking method and device
CN107895102B (en) * 2017-11-23 2021-08-17 苏州矩阵光电有限公司 Growth instruction checking method and device
CN114486543A (en) * 2022-01-04 2022-05-13 浙江大学 System and method for testing influence of trace gas impurities on high-pressure hydrogen embrittlement of material
CN114486543B (en) * 2022-01-04 2024-06-07 浙江大学 System and method for testing influence of trace gas impurities on high-pressure hydrogen embrittlement of material

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Application publication date: 20140326