CN112111727A - Method for rapidly recovering MOCVD upper cover after maintenance - Google Patents
Method for rapidly recovering MOCVD upper cover after maintenance Download PDFInfo
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- CN112111727A CN112111727A CN201910542292.4A CN201910542292A CN112111727A CN 112111727 A CN112111727 A CN 112111727A CN 201910542292 A CN201910542292 A CN 201910542292A CN 112111727 A CN112111727 A CN 112111727A
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- 238000000034 method Methods 0.000 title claims abstract description 70
- 238000012423 maintenance Methods 0.000 title claims abstract description 26
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 title claims abstract 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 117
- 238000006243 chemical reaction Methods 0.000 claims abstract description 95
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000001301 oxygen Substances 0.000 claims abstract description 48
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 48
- 230000008569 process Effects 0.000 claims abstract description 27
- 238000011084 recovery Methods 0.000 claims abstract description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 60
- 238000004140 cleaning Methods 0.000 claims description 56
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 30
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 25
- 239000012459 cleaning agent Substances 0.000 claims description 24
- 238000001514 detection method Methods 0.000 claims description 24
- 239000010935 stainless steel Substances 0.000 claims description 24
- 229910001220 stainless steel Inorganic materials 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 13
- CTNCAPKYOBYQCX-UHFFFAOYSA-N [P].[As] Chemical compound [P].[As] CTNCAPKYOBYQCX-UHFFFAOYSA-N 0.000 claims description 12
- 230000007797 corrosion Effects 0.000 claims description 12
- 238000005260 corrosion Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000010926 purge Methods 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 229910052785 arsenic Inorganic materials 0.000 claims 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 10
- 230000008901 benefit Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910002601 GaN Inorganic materials 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
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- 238000007689 inspection Methods 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 1
- 229910000070 arsenic hydride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
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- 239000012495 reaction gas Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a method for quickly recovering an MOCVD upper cover after maintenance, wherein in the first scheme, an oven is used for baking the upper cover, the water and oxygen removal efficiency is high, the time is short, but other impurities are easily introduced during operation because the oven belongs to external equipment; in the second scheme, high-temperature water circulation of an external circulating water pipeline is utilized, the working efficiency of removing water and oxygen is lower compared with that of the first scheme, but the water and oxygen in the reaction chamber are removed more thoroughly because the high-temperature water circularly flows in the upper cover and the lower cover; the third scheme combines the first scheme and the second scheme, so that the water oxygen removal efficiency in the reaction chamber is effectively improved, and the water oxygen in the reaction chamber can be effectively and thoroughly removed; the technical scheme greatly accelerates the removal of residual water and oxygen in the maintenance process, accelerates the recovery of the growth environment of the reaction chamber cavity, improves the equipment utilization rate, indirectly improves the equipment yield and has better practicability.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for quickly recovering an MOCVD upper cover after maintenance.
Background
Along with the development of modern society, energy and environmental problems become more and more important to the problems to which the people are facing at present, and sustainable development and ecological environment protection become the key points of work attention of the people increasingly. How to find better energy substitutes or reduce energy consumption without delaying the existing productivity has become the focus of our work gradually.
In this case, then, it is widely used based on the characteristics of the LED. The inherent characteristics of the LED determine that the LED is the most ideal light source to replace the traditional light source so as to achieve the purposes of energy conservation and consumption reduction.
LEDs have a wide range of uses and irreplaceable advantages: one, small, LED is basically a very small chip encapsulated in epoxy, so it is very small and very light; secondly, the power consumption is low, the power consumption of the LED is quite low, and generally, the working voltage of the LED is 2-3.6V. The working current is 0.02-0.03A. That is to say: the consumed electric energy does not exceed 0.1W, so that guiding significance is provided for work of people in the aspect of energy; the service life is long, the LED light source solid cold light source is packaged by epoxy resin, no loose part exists in the lamp body, the defects of easy burning, thermal deposition, light decay and the like of filament luminescence do not exist, and the service life can reach 6 to 10 ten thousand hours under proper current and voltage and is longer than the service life of the traditional light source by more than 10 times; fourthly, the LED lamp has high brightness and low heat, uses a cold light emitting technology, and has much lower heat productivity than a common lighting lamp; the LED lamp has the advantages that the LED lamp is environment-friendly, better environmental-friendly benefit is achieved, ultraviolet rays and infrared rays are not contained in a spectrum, heat and radiation are not generated, glare is small, waste can be recycled, pollution is avoided, mercury is not contained, a cold light source can be touched safely, the LED lamp belongs to a typical green lighting source and is made of non-toxic materials, pollution is not caused by mercury contained in a fluorescent lamp, and meanwhile the LED lamp can be recycled; and sixthly, the LED is firm and durable, is completely encapsulated in epoxy resin, and is firmer than a bulb and a fluorescent tube. The lamp body has no loose part, and the characteristics ensure that the LED is not easy to damage; seventhly, high energy conservation: energy conservation and no pollution are the environmental protection. Direct current driving, the electro-optical power conversion of ultra-low power consumption (0.03-0.06 watt of single tube) is close to 100%, and the same illumination effect saves more than 80% of energy compared with the traditional light source; eight, changeable, the LED light source can utilize the three primary colors principle of red, green, blue, make three kinds of colors have 256-level gray scale and arbitrary mix under the control of computer technology, can produce 256 x 256 ═ 16777216 kinds of colors, form the combination change multiterminal of different photochromic, realize the dynamic change effect and various pictures of the rich and varied.
Because of the advantages of LED, it is important to produce a product with high brightness and meeting our requirements. Metal Organic Chemical Vapor Deposition (MOCVD) equipment is a mature technology for growing all semiconductor compounds worldwide.
The MOCVD technology has been proposed since the sixties of the twentieth century, and through the development of the seventies to the eighties, the ninety years has become a core growth technology for preparing epitaxial wafers of optoelectronic materials such as gallium arsenide and indium phosphide. At present, the method is widely applied to the production of photoelectronic materials such as gallium arsenide, indium phosphide and the like. The japanese scientist Nakamura applied MOCVD to gallium nitride material preparation, and utilized his own developed MOCVD equipment (a very special reaction chamber structure), firstly produced high-brightness blue and green light emitting diodes in 1994, and realized continuous lasing at room temperature for 10,000 hours in 1998, which made epoch-making progress. With the progress of semiconductor materials and device processes, particularly with the increasing maturity of epitaxial processes such as MOCVD, in the early nineties of the last century, japanese sub-chemical company (Nichia) and krey (Cree) company in the united states successfully grow GaN-based LED epitaxial wafers with device structures on sapphire and SiC substrates by MOCVD technology, respectively, and produce blue, green and violet LED devices with very high brightness. The second characteristic of the ultra-high brightness LED is the expansion of the light emitting wavelength, the appearance of InGaAlP device expands the light emitting wave band to the yellow green light region of 570nm towards the short wave, and the GaN-based device further expands the light emitting length to the green, blue and purple wave bands and gradually expands to the light color of the wide wave band.
The epitaxial technology and equipment are the key points of the epitaxial wafer manufacturing technology, and the Metal-Organic Chemical vapor deposition (MOCVD) technology is the main method for growing thin layer single crystals of III-V group, II-VI group compounds and alloys. II. The group III metal organic compound is typically a methyl or ethyl compound, such as: ga (CH3)3, In (CH3)3, Al (CH3)3, Ga (C2H5)3, Zn (C2H5)3, etc., most of which are high vapor pressure liquids or solids. Introducing hydrogen or nitrogen as carrier gas into liquid to carry out vapor, mixing with hydride of V group (such as NH3, PH3, AsH3), introducing into reaction chamber, reacting on the surface of heated substrate, and epitaxially growing compound crystal film.
MOCVD has the following advantages: firstly, all components and doping agents for growing compound crystals can be introduced into a reaction chamber in a gaseous state, and the characteristics of components, conductivity types, carrier concentrations, thicknesses and the like of an epitaxial layer can be controlled by controlling the flow of various gases, so that the difficulty of work of people is reduced in the aspect of growth component control; secondly, due to the air extractor, the flow rate of gas in the reaction chamber is high, and the reaction gas is switched quickly for heterogeneous epitaxy, so that a steep interface can be obtained; and thirdly, epitaxy occurs on the surface of the heated substrate, the reaction process can be controlled by monitoring the temperature of the substrate, and good monitoring conditions provide a powerful guarantee for the growth of equipment, and under certain conditions, the growth speed of the epitaxial layer is in direct proportion to the supply of the metal organic source.
The MOCVD equipment is roughly composed of six systems: the system comprises a gas conveying system, a source supply system, a reaction chamber, a heating system, a tail gas treatment system, a safety control system and a computer control system. In the field of AsP (arsenic phosphorus) materials, MOCVD equipment is widely used in research and development and large-scale mass production of red and yellow light emitting diodes, laser diodes, and thin film solar cells.
MOCVD produced by VEECO has the characteristics of high production efficiency and low maintenance frequency, and is popular with wide users.
The existing VEECO turbine MOCVD reaction chamber maintenance method commonly adopts an ammonia water hydrogen peroxide wet cleaning method, and AlGaInP materials with the red light growth function are difficult to dissolve in organic solvents such as ethanol and the like, but can quickly react with ammonia water hydrogen peroxide chemical reagents to achieve the cleaning effect. After the maintenance by ammonia water and hydrogen peroxide is carried out, the removal of water and oxygen is slow due to the limitation of the conditions of the reaction chamber, the growth conditions of the reaction chamber cannot be met, the recovery period of equipment is long, and the utilization rate of the equipment is reduced.
The existing reaction chamber maintenance mode is mainly characterized in that the chemical characteristics of materials are met, the materials are corroded by a wet method, after the materials are cleaned, residual ammonia water and hydrogen peroxide are cleaned by water, then the materials are dehydrated by an organic solvent, water and oxygen are removed through high-temperature treatment of equipment in the later stage, the temperature of the cavity wall of the reaction chamber is influenced, the water and oxygen removal rate is low, and the recovery period of the equipment is long.
Aiming at the problems, a method for rapidly recovering the MOCVD upper cover after maintenance is designed, so that the loss of water in contact with the upper cover and the cavity wall of the reaction chamber can be effectively accelerated, the utilization rate of equipment is improved, and the method is one of the problems to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for quickly recovering an MOCVD upper cover after maintenance, which aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for fast recovery of an MOCVD upper cover after maintenance comprises the following steps:
1) preparing work and preliminary examination;
2) cleaning the upper cover;
3) removing water and oxygen on the upper cover at high temperature;
4) and finishing the operation.
Preferably, the method comprises the following steps:
1) preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device;
2) cleaning an upper cover:
a) preparing a cleaning agent, and performing corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; according to the technical scheme, firstly, ammonia water and hydrogen peroxide are matched to remove residual AlGaInP materials on an upper cover;
b) then cleaning the upper cover by using sufficient deionized water; the step b) is mainly used for removing residual ammonia water and hydrogen peroxide and preventing the pollution to a reaction chamber equipment system after the later recovery;
3) removing water and oxygen on the upper cover at high temperature:
a) taking the upper cover cleaned in the step 2), dismantling pipelines of the upper cover and spare parts which do not resist high temperature, and protecting the pipelines by using tools; in the step a), an upper cover pipeline and non-high temperature resistant spare parts are dismantled and protected by a proper tool (such as a plug), so that the service life of the component is prolonged and the subsequent use is not influenced;
b) taking out the oven, and cleaning the inside of the oven; cleaning the oven in the step b), ensuring that the oven is clean and dustless, and avoiding secondary pollution to a baked piece in the using process;
c) taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface;
d) adjusting the temperature of the oven, and baking;
e) after baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber; in the step e), the absolute ethyl alcohol is used for removing impurities generated by baking the upper cover, so that the upper cover is clean and convenient for subsequent treatment;
f) then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed; and f), vacuumizing the cavity of the reaction chamber to ensure that the reaction chamber is in low-pressure vacuum, so as to accelerate the removal of water and oxygen.
4) And finishing the operation.
Preferably, the method comprises the following steps:
1) preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device;
2) cleaning an upper cover:
a) preparing a cleaning agent, and performing corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1;
b) then cleaning the upper cover by using sufficient deionized water;
3) removing water and oxygen on the upper cover at high temperature:
a) taking the upper cover cleaned in the step 2), wiping and cleaning the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber; wiping the upper cover by using absolute ethyl alcohol in the step a), and removing residual water in the upper cover;
b) preparing an external circulator, adjusting the water temperature of the external circulator, and connecting circulating water of the external circulator to an original circulating water pipeline in the reaction chamber; in the step b), an external circulator is utilized to enable high-temperature water to circularly flow in the upper cover and the lower cover, so that the temperature of the whole reaction chamber is increased, and the removal speed of water oxygen of the upper cover is increased;
c) then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed;
4) and finishing the operation.
Preferably, the method comprises the following steps:
1) preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device;
2) cleaning an upper cover:
a) preparing a cleaning agent, and performing corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1;
b) then cleaning the upper cover by using sufficient deionized water;
3) removing water and oxygen on the upper cover at high temperature:
a) taking the upper cover cleaned in the step 2), dismantling pipelines of the upper cover and spare parts which do not resist high temperature, and protecting the pipelines by using tools;
b) taking out the oven, and cleaning the inside of the oven;
c) taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface;
d) adjusting the temperature of the oven, and baking;
e) after baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber;
f) preparing an external circulator, adjusting the water temperature of the external circulator, and connecting circulating water of the external circulator to an original circulating water pipeline in the reaction chamber;
g) then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed;
4) and finishing the operation.
Preferably, in the step 3), the temperature of the oven is 100-150 ℃, and the baking time is 1-2 h.
Preferably, in the step 3), the upper cover is in a nitrogen purging environment during baking to accelerate gas flow in the baking environment, and the upper cover is in a low-pressure environment during baking.
Let upper cover nitrogen gas purge environment during toasting among this technical scheme, can accelerate the gas flow of toasting the environment.
Preferably, in the step 3), the water temperature of the external circulator is 40-50 ℃.
In the technical scheme, the water temperature of the external circulator is 40-50 ℃, the original water pipeline of the reaction chamber is easily damaged when the water temperature is too high, and the water oxygen removal efficiency is reduced when the water temperature is too low, so that the time is long.
Compared with the prior art, the invention has the beneficial effects that:
the technical scheme discloses a method for rapidly recovering an MOCVD upper cover after maintenance, which comprises three schemes:
the first scheme is as follows: in the first scheme, the upper cover is baked by using an oven, the temperature of the upper cover is increased, wherein the temperature of the oven is adjusted to be 100-150 ℃, the upper cover is arranged back to the circular growth chamber equipment after baking, residual water and oxygen on the upper cover are removed by using the oven, and the water and oxygen removal efficiency in the reaction chamber is further increased by using the temperature of the upper cover;
scheme II: in the second scheme, an external circulating water pipeline is connected with an internal circulating water pipeline of the reaction chamber, the temperature of the external circulating water pipeline is adjusted to be 40-50 ℃, and high-temperature water is circulated in the upper cover and the lower cover to increase the temperature of the reaction chamber, so that water and oxygen in the reaction chamber are removed;
the third scheme is as follows: and the third scheme combines the first scheme and the second scheme, not only utilizes the oven to bake the upper cover, but also is connected with the internal circulation water path of the reaction chamber through an external circulation water pipeline, so that the temperature of the reaction chamber is effectively improved, and the water oxygen in the reaction chamber is removed.
In the first scheme, the upper cover is baked by using the oven, the water and oxygen removal efficiency is high, the time is short, but other impurities are easily introduced during operation because the oven belongs to external equipment; in the second scheme, high-temperature water circulation of an external circulating water pipeline is utilized, the working efficiency of removing water and oxygen is lower compared with that of the first scheme, but the water and oxygen in the reaction chamber are removed more thoroughly because the high-temperature water circularly flows in the upper cover and the lower cover; and the third scheme combines the first scheme and the second scheme, so that the water and oxygen removal efficiency in the reaction chamber is effectively improved, and the water and oxygen in the reaction chamber can be effectively and thoroughly removed.
The technical scheme is that the temperature of the upper cover is directly optimized on the basis of MOCVD equipment, and additional equipment modification is not needed. According to the technical scheme, after the equipment is recovered, the removal of residual water and oxygen in the maintenance process is greatly accelerated, the recovery of the growth environment of the cavity of the reaction chamber is accelerated, the equipment utilization rate is improved, the equipment yield is indirectly improved, and the equipment has better practicability.
Drawings
In order that the present invention may be more readily and clearly understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments that are illustrated in the appended drawings.
FIG. 1 is a diagram showing a usage state of an external circulator of a method for rapid recovery after maintenance of an MOCVD upper cover according to the present invention;
fig. 2 is a diagram of the baking usage state of the oven of the method for rapidly recovering the MOCVD upper cover after maintenance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the method comprises the following specific steps:
firstly, preparing work and preliminary inspection, preparing an upper cover and each device assembly, and inspecting the running condition of the device; preparing a cleaning agent, and carrying out corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; then cleaning the upper cover by using sufficient deionized water;
then taking the cleaned upper cover, dismantling the pipeline of the upper cover and the spare parts which do not resist high temperature, and protecting the pipeline by using a tool; taking out the oven, and cleaning the inside of the oven; taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface; and (3) adjusting the temperature of the oven, wherein the temperature of the oven is 100 ℃, baking is carried out for 1h, the upper cover is in a nitrogen purging environment during baking, the gas flow of the baking environment is accelerated, and the upper cover is in a low-pressure environment during baking.
After baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber; and then leak detection is carried out on the reaction chamber, the original circulating water pipeline in the reaction chamber is connected back to the system after leak detection, the reaction chamber is vacuumized, the low-pressure environment is kept, water and oxygen are removed, and the operation is finished.
Example 2:
the method comprises the following specific steps:
firstly, preparing work and preliminary inspection, preparing an upper cover and each device assembly, and inspecting the running condition of the device; preparing a cleaning agent, and carrying out corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; then cleaning the upper cover by using sufficient deionized water;
then taking the cleaned upper cover, dismantling the pipeline of the upper cover and the spare parts which do not resist high temperature, and protecting the pipeline by using a tool; taking out the oven, and cleaning the inside of the oven; taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface; and (3) adjusting the temperature of the oven to 130 ℃, baking for 1.5h, wherein the upper cover is in a nitrogen purging environment during baking to accelerate the gas flow of the baking environment, and the upper cover is in a low-pressure environment during baking.
After baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber; and then leak detection is carried out on the reaction chamber, the original circulating water pipeline in the reaction chamber is connected back to the system after leak detection, the reaction chamber is vacuumized, the low-pressure environment is kept, water and oxygen are removed, and the operation is finished.
Example 3:
the method comprises the following specific steps:
firstly, preparing work and preliminary inspection, preparing an upper cover and each device assembly, and inspecting the running condition of the device; preparing a cleaning agent, and carrying out corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; then cleaning the upper cover by using sufficient deionized water;
then taking the cleaned upper cover, dismantling the pipeline of the upper cover and the spare parts which do not resist high temperature, and protecting the pipeline by using a tool; taking out the oven, and cleaning the inside of the oven; taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface; and (3) adjusting the temperature of the oven to 150 ℃, baking for 2h, wherein the upper cover is in a nitrogen purging environment during baking to accelerate the gas flow of the baking environment, and the upper cover is in a low-pressure environment during baking.
After baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber; and then leak detection is carried out on the reaction chamber, the original circulating water pipeline in the reaction chamber is connected back to the system after leak detection, the reaction chamber is vacuumized, the low-pressure environment is kept, water and oxygen are removed, and the operation is finished.
Example 4:
the method comprises the following specific steps:
first, preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device; preparing a cleaning agent, and carrying out corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; then cleaning the upper cover by using sufficient deionized water;
cleaning the cleaned upper cover with absolute ethyl alcohol, and then loading the upper cover back to the reaction chamber; preparing an external circulator, adjusting the water temperature of the external circulator to 40 ℃, and connecting the circulating water of the external circulator to an original circulating water pipeline in the reaction chamber; then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed; and finishing the operation.
Example 5:
the method comprises the following specific steps:
first, preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device; preparing a cleaning agent, and carrying out corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; then cleaning the upper cover by using sufficient deionized water;
cleaning the cleaned upper cover with absolute ethyl alcohol, and then loading the upper cover back to the reaction chamber; preparing an external circulator, adjusting the water temperature of the external circulator to 50 ℃, and connecting the circulating water of the external circulator to an original circulating water pipeline in the reaction chamber; then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed; and finishing the operation.
Example 6
The method comprises the following specific steps:
first, preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device; preparing a cleaning agent, and carrying out corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1; then cleaning the upper cover by using sufficient deionized water;
then taking the cleaned upper cover, dismantling the pipeline of the upper cover and the spare parts which do not resist high temperature, and protecting the pipeline by using a tool; taking out the oven, and cleaning the inside of the oven; taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface; and (3) adjusting the temperature of the oven to 130 ℃, baking for 1.5h, wherein the upper cover is in a nitrogen purging environment during baking to accelerate the gas flow of the baking environment, and the upper cover is in a low-pressure environment during baking.
After baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber; preparing an external circulator, adjusting the water temperature of the external circulator to 45 ℃, and connecting the circulating water of the external circulator to an original circulating water pipeline in the reaction chamber; then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed; and finishing the operation.
And (4) conclusion: in the embodiment 1-3, the upper cover is baked by using the oven, so that the water and oxygen removal efficiency is high, and the time is short; in the examples 4-5, the working efficiency of removing water and oxygen is lower in the external circulating water pipeline high-temperature water circulation compared with the examples 1-3, but the water and oxygen in the reaction chamber are removed more completely; embodiment 6 can also ensure that the water and oxygen in the reaction chamber are effectively and thoroughly removed while improving the water and oxygen removal efficiency in the reaction chamber.
The technical scheme is that the temperature of the upper cover is directly optimized on the basis of MOCVD equipment, and additional equipment modification is not needed. According to the technical scheme, after the equipment is recovered, the removal of residual water and oxygen in the maintenance process is greatly accelerated, the recovery of the growth environment of the cavity of the reaction chamber is accelerated, the equipment utilization rate is improved, the equipment yield is indirectly improved, and the equipment has better practicability.
The terms mentioned in the present technical solution are to be interpreted:
1. MOCVD: metalorganic chemical vapor deposition, MOCVD, is a common technique for the growth of semiconductor compounds. The MOCVD equipment mainly comprises six systems: the system comprises a gas conveying system, a source supply system, a reaction chamber, a heating system, a tail gas treatment system, a safety control system and a computer control system. MOCVD equipment is a common equipment in the field of semiconductor technology.
2. PM: production Maintenance generally refers to the periodic Maintenance of equipment after the equipment is quantitatively produced for a period of time.
3. VCR connector: the metal surface sealing joint is generally applied to the connection of Tube pipes. The sealing element is a metal gasket and is in a metal-to-metal sealing mode. The joint assembly is subjected to the processes of electropolishing, cleaning and the like, and is particularly suitable for ultrahigh pure systems, ultrahigh vacuum systems and positive pressure systems which require no leakage.
4. FlowFlange: the upper cover of the equipment growth cavity is mainly used for controlling the distribution of airflow entering the reaction chamber and is replaced by the upper cover later.
5. A reaction chamber: the MOCVD mainly comprises a component, and provides a material growth cavity according to the requirements of a front-end control system.
6. LED: the short term led has the advantages of low voltage, high efficiency, no pollution, etc.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. A method for fast recovery after maintenance of an MOCVD upper cover is characterized by comprising the following steps: the method comprises the following steps:
1) preparing work and preliminary examination;
2) cleaning the upper cover;
3) removing water and oxygen on the upper cover at high temperature;
4) and finishing the operation.
2. The method for fast recovery after maintenance of an MOCVD upper cover according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
1) preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device;
2) cleaning an upper cover:
a) preparing a cleaning agent, and performing corrosion cleaning on arsenic and phosphorus materials formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1;
b) then cleaning the upper cover by using sufficient deionized water;
3) removing water and oxygen on the upper cover at high temperature:
a) taking the upper cover cleaned in the step 2), dismantling pipelines of the upper cover and spare parts which do not resist high temperature, and protecting the pipelines by using tools;
b) taking out the oven, and cleaning the inside of the oven;
c) taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface;
d) adjusting the temperature of the oven, and baking;
e) after baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber;
f) preparing an external circulator, adjusting the water temperature of the external circulator, and connecting circulating water of the external circulator to an original circulating water pipeline in the reaction chamber;
g) then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed;
4) and finishing the operation.
3. The method for fast recovery after maintenance of an MOCVD upper cover according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
1) preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device;
2) cleaning an upper cover:
a) preparing a cleaning agent, and performing corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1;
b) then cleaning the upper cover by using sufficient deionized water;
3) removing water and oxygen on the upper cover at high temperature:
a) taking the upper cover cleaned in the step 2), dismantling pipelines of the upper cover and spare parts which do not resist high temperature, and protecting the pipelines by using tools;
b) taking out the oven, and cleaning the inside of the oven;
c) taking out the special stainless steel bracket, cleaning, placing the cleaned special stainless steel bracket in an oven, placing the upper cover on the special stainless steel bracket, and paying attention to the protection of the sealing flange surface of the upper cover in the placing process to prevent the damage of the sealing surface;
d) adjusting the temperature of the oven, and baking;
e) after baking, wiping the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber;
f) then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed;
4) and finishing the operation.
4. The method for fast recovery after maintenance of an MOCVD upper cover according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
1) preparation work and preliminary examination: preparing an upper cover and each device assembly, and checking the operation condition of the device;
2) cleaning an upper cover:
a) preparing a cleaning agent, and performing corrosion cleaning on the arsenic-phosphorus material formed in the growth process of the upper cover; the cleaning agent comprises ammonia water and hydrogen peroxide, wherein the volume ratio of the ammonia water to the hydrogen peroxide is 1: 1;
b) then cleaning the upper cover by using sufficient deionized water;
3) removing water and oxygen on the upper cover at high temperature:
a) taking the upper cover cleaned in the step 2), wiping and cleaning the upper cover by using absolute ethyl alcohol, and then putting the upper cover back into the reaction chamber;
b) preparing an external circulator, adjusting the water temperature of the external circulator, and connecting circulating water of the external circulator to an original circulating water pipeline in the reaction chamber;
c) then leak detection is carried out on the reaction chamber, after leak detection, the original circulating water pipeline in the reaction chamber is connected back to the system, the reaction chamber is vacuumized, the low-pressure environment is kept, and water and oxygen are removed;
4) and finishing the operation.
5. The method for rapid recovery after maintenance of an MOCVD lid according to any one of claims 2 to 3, wherein the method comprises the following steps: in the step 3), the temperature of the oven is 100-150 ℃, and the baking time is 1-2 h.
6. The method for rapid recovery after maintenance of an MOCVD lid according to any one of claims 2 to 3, wherein the method comprises the following steps: in the step 3), the upper cover is in a nitrogen purging environment during baking to accelerate gas flow in the baking environment, and the upper cover is in a low-pressure environment during baking.
7. The method for rapid recovery after maintenance of an MOCVD lid according to any one of claims 3 to 4, wherein the method comprises the following steps: in the step 3), the water temperature of the external circulator is 40-50 ℃.
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| CN108588681A (en) * | 2018-05-25 | 2018-09-28 | 聚灿光电科技股份有限公司 | MOCVD systems and its method for cleaning |
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| US5176756A (en) * | 1990-08-29 | 1993-01-05 | Fujitsu Limited | Method for fabricating a semiconductor device including a step for cleaning a semiconductor substrate |
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