CN105986243B - A kind of processing method of MOCVD reactors - Google Patents
A kind of processing method of MOCVD reactors Download PDFInfo
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- CN105986243B CN105986243B CN201510083854.5A CN201510083854A CN105986243B CN 105986243 B CN105986243 B CN 105986243B CN 201510083854 A CN201510083854 A CN 201510083854A CN 105986243 B CN105986243 B CN 105986243B
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Abstract
A kind of processing method of MOCVD reactors, the present invention execute metal organic gas reaction by being recycled in pretreatment stage.It the treating method comprises pretreatment process and crystal growth flow, wherein pretreatment process includes metal organic gas reaction step and oxygen-containing gas reaction step, it is alternately performed metal organic gas reaction step and oxygen-containing gas reaction step, until completing the pretreatment to spray head in reaction chamber.Wherein in pretreatment process, there is the first temperature to control spray head by controlling cooling fluid supply system, there is spray head second temperature, the first temperature to be more than second temperature in crystal growth flow.
Description
Technical field
The present invention relates to metal-organic chemical vapor deposition equipment manufacturing technology fields more particularly to a kind of to metallochemistry gas
Phase deposition reactor processing method.
Background technology
As shown in Figure 1, metal organic chemical vapor deposition (MOCVD) reactor includes a reaction chamber 100, in reaction chamber
Including a pallet 14, multiple pending substrates are fixed on pallet, and there are one rotary shafts 10 to drive for 14 lower central of pallet
Pallet high speed rotation during the reaction.Wherein rotary shaft 10 can also be gas bogey, such as drum type structure in crystalline substance
Round tray peripheral support pallet 14.14 lower section of pallet further includes that a heating pallet 14 of heater 12 reaches suitable high temperature, this
A high temperature is usually at 1000 degree or so, to adapt to the crystalline growth of gallium nitride (GaN) crystalline material.In reaction chamber 100 and pallet
Opposite is a gas spray, and gas spray includes the upper cover 20 at top, intermediate gas distributor 22 and is located at bottom
The coldplate 24 in portion forms.Include that at least one gas inlet pipe road 28 is connected to external air source on upper lid.Wherein gas point
Orchestration includes that different types of reaction gas is isolated in different gas expanded chambers by polylith isolation board, and the gas of top expands
It includes that the gas conduit largely extended downwardly passes through the gas diffusion chamber of lower section to reach corresponding ventilation in coldplate 24 to dissipate chamber
Hole or air channel.The gas diffusion chamber of lower section can also include the gas conduit largely extended downwardly, specific gas conduit
Arrangement can need optimization design according to different reaction cavity configuration and crystal growth technique, for example flow through gas containing gallium
The conduit of TMG is arranged alternately in column with the conduit containing ammonia is flowed through.It is evenly distributed on including cooling passage 26 in coldplate 24
In entire plane, venthole or slot between cooling passage make the multiple gases from gas distributor 22 open below into instead
Answer region.Since MOCVD reactions need the high temperature of thousands of degree so entire reaction chamber and the gas spray of top mostly use greatly
Stainless steel is made and is just resistant to this temperature, but needs to be passed through two luxuriant magnesium (CP in MOCVD reaction process2Mg) gas, it is this
Gas easily reacts with stainless steel surface so that the iron of stainless steel surface can reach underlying substrate with air-flow, eventually
The luminescent properties of LED to being formed using MOCVD techniques cause significant impact, so needing strongly to avoid.
The prior art carries out pretreated method there are serious problems to stainless steel, i.e. process cycle is too long.Because of spray
Head temperature, which remains at traditional 50 degree, causes reaction speed very slow, more cycles is needed to can be only achieved to stainless steel surface
Iron carry out saturation displacement.Meanwhile heater is needed to be heated to excessive temperature in preprocessing process to assist accelerating in spray head
The reaction speed for carrying out atomic substitutions, then also needs to naturally cool to room temperature, the two temperature changing processes just need to consume
There is the about several hours in reaction time for being filled with two luxuriant magnesium gas or air one hour after still more reaching predetermined temperature,
Carry out entire pretreatment time after repeatedly recycling and be even up to several weeks often beyond one week, this to the waste of equipment and material very
Seriously.It needs a kind of new method that can realize and saturated process is carried out to the iron of surface of stainless steel, and can be largely at saving
Manage the time.
Invention content
Problems solved by the invention is to prevent the gas shower head material in MOCVD reactors from causing the pending wafer in lower section
Pollution, to solve this problem the present invention propose a kind of processing method of MOCVD reactors, including：One reactor is provided,
The reactor includes a reaction chamber, and a gas spray is fixed at the top of the reaction chamber, and the gas spray includes a gas
Body distributor and the coldplate below gas distributor, the coldplate is interior to be connected to outside including a plurality of cooling pipe
For cooling fluid supply system to control the temperature of coldplate, an air extractor is arranged for being discharged in reaction chamber in the reaction chamber bottom
Gas, a support device is used to support pending wafer tray, and a heating device is located at below the wafer tray；Institute
It includes pretreatment process and crystal growth flow to state processing method, and wherein pretreatment process includes metal organic gas reaction step
Rapid and oxygen-containing gas reaction step, in the metal organic gas reaction step, in placement wafer tray to the support device,
Controlling the cooling fluid supply system makes gas spray have the first temperature, and the first power is supplied to the heating device, to
The first Organometallic Reac- tion gas is passed through in reaction chamber, until completing metal organic gas reaction step；The oxygen-containing gas is anti-
It answers in step, stops supplying the first Organometallic Reac- tion gas, while supplying oxygen-containing gas into reaction chamber, until completing
Oxygen-containing gas reaction step；Cycle executes the metal organic gas reaction step and oxygen-containing gas reaction step, until completing
Pretreatment process enters crystal growth flow；In the crystal growth flow, places and carry the pallet of wafer to be handled to institute
It states in support device, controlling the cooling fluid supply system makes gas spray have second temperature, is supplied to the heater
Second power is passed through the second Organometallic Reac- tion gas into reaction chamber；It is characterized in that the first temperature is more than second temperature, the
One power is less than the second power.
Content of magnesium in wherein the first metal organic gas is higher than the second metal organic gas, so that reaction speed is more
The flow of trimethyl gallium is less than the stream of trimethyl gallium in second metal organic gas soon or in the first metal organic gas
Amount.And cost containing magnesium gas is relatively low with respect to the cost of trimethyl gallium, and Organometallic Reac- tion gas of the invention can be reduced into
This improves reaction speed simultaneously.
Wherein the first temperature is 70-200 degree, and second temperature is 45-55 degree, and higher is used in Organometallic Reac- tion step
Temperature can significantly improve reaction speed, shorten processing time.Wherein the metal gas reaction step duration is 2-3 hours.
Oxygen-containing gas is air or water vapour, and the oxygen-containing gas reaction step time is 20-40 minutes.Pretreatment process includes at least 10
The cycle of a the metal organic gas reaction step and oxygen-containing gas reaction step.
Wherein the second power makes the temperature of wafer tray between 600-1200 degree, is heated described in the first power input
Device so that temperature of tray is less than 500 degree.
Description of the drawings
Fig. 1 is prior art MOCVD reactor overall structure diagrams；
Specific implementation mode
Pollution problem the invention solves the iron in the gas flow pipe road of MOCVD reactors to epitaxial growth chip.
Heater 12 needs to heat wafer tray 14 in crystal growing process, and pending wafer is placed in wafer tray 14.Together
The coolant liquid with suitable temperature is passed through in coolant duct in the spray head of Shi Shangfang makes the temperature of coldplate 24 stablize
At 50 degrees Celsius, such temperature can ensure that gas spray will not deform, and also just prevent the gas of the spray head caused by deformation
The sealing mechanism of body pipeline enclosure is destroyed and causes gas leakage.Metal organic gas source is all to flow through liquid by carrier gas such as nitrogen
Then metallo-organic compound container takes metallo-organic compound molecule out of, the molecule that these are brought out by carrier gas is in pipeline
Can be different with temperature in interior flow process and be saturated and be precipitated to get off as liquid precipitation again, in order to prevent these molecules into
It is precipitated before entering reactor, the temperature for controlling gas pipeline is needed to stablize at 30 degree or more.Keep the higher temperature of gas spray
Degree such as can ensure that gas molecule will not be precipitated for 100 degree, but can cause prodigious burden to coolant circulation system in this way：It needs
Want liquid at higher temperature, higher pressure in coolant duct, higher pressure needs all parts in pipeline to need more again
High pressure resistance is broken if the long-term pressure for bearing high-temp liquid of rubber interconnecting piece especially between different metal pipeline can exist
The danger split causes prodigious harm to entire MOCVD reactors.So considering by each design factor, in the industry
The temperature of coldplate is all usually set in 50 degree, not only can guarantee that reactant is not precipitated in advance but also does not need additional transformation cooling
Liquid supply line.
The present invention proposes one kind and being adapted for the pretreated method of gas spray, is carrying out formal crystal growth mistake
Before journey, pretreatment process is carried out first, and pretreatment process includes metal organic gas reaction step and oxygen-containing gas reaction step
Suddenly.
In metal organic gas reaction step, it is placed with wafer tray 14 in rotary shaft 10, but is not put on pallet 14
Set pending wafer.The cooling plate temperature that the coolant liquid with higher temperature makes gas spray is passed through in cooling passage 26
It can stablize between 70-90 degree.Pretreatment gas is passed into gas spray by steam line 28 simultaneously, flows through spray head
Interior all inner surfaces finally reach the conversion zone of 14 top of wafer tray.The air extractor of lower section is extracted out from exhaust outlet 16
Reaction gas in reaction compartment and byproduct of reaction so that the low pressure of vacuum is maintained close in reactor.Due to gas
Spray head is, typically as stainless steel is made, so itself has good heat conductivility, to pass through cooling passage 26 by metal
In coolant temperature and flow-rate adjustment can be such as above-mentioned so that entire spray head has whole consistent pretreatment temperature
70-250 degree, best is 75-90 degree.In order to make spray head faster reach suitable temperature, the heater 12 of lower section can be same
The upward radiations heat energies of Shi Kaitong are to wafer tray 14, further upward spray head radiations heat energy after pallet is warmed, still
Its temperature can be far below the required temperature of crystal growth, for example be less than 500 degree.Due to that need not held in the palm in pretreatment process
Semiconductor layer of the growth with good crystalline structure on disk, so the temperature of pallet need not also be protected as crystal growth phase
The high temperature in thousands of degree left and right is held, as long as can ensure that the temperature of spray head reaches above-mentioned pretreatment temperature.Due to this hair
The bright coolant liquid using higher temperatures controls the temperature of gas spray, so high temperature coolant uses low temperature cold more in the prior art
But water is taken away the energy of heat and can be declined, so if the heat that lower section heater radiates upwards is crossed is taken away heat more than cooling water
Ability temperature limiting on spray head can be caused higher, and will produce temperature gradient between spray head different parts and lead to spray head
Deformed damaged.So the present invention using high temperature coolant (such as water or oil) while below heater wattage output need
Lower numerical value is selected, or even directly closes heater 12.Side can cover down on the heaters for the unloaded setting of pallet 14
The heater of side prevents the particle generated in preprocessing process or other solid deposits from adhering to above heater, in turn
Seriously affect the Temperature Distribution of subsequent crystallographic growth phase.The present invention can also place wafer in pretreatment stage on pallet,
Although at this time since the semiconductor structure of suitable LED component can not be grown on the too low wafer of temperature.The present invention is in the organic gas of metal
The reaction gas being passed through in precursor reactant step is similar with the gas that crystal growth phase is passed through, such as metal organic gas trimethyl gallium
(TMG), trimethyl aluminium (TMAL), two luxuriant magnesium (MgCP2) and the alternative a small amount of ammonia or nitrogen added.Due to this hair
It is bright to solve be after iron in gas spray is replaced the pending wafer of pollution lower section the technical issues of, as long as so energy
Ensure the iron atom of spray head interior conduit inner wall exposure by replacements energy such as active metal gallium, magnesium, aluminium in metal organic gas
Realize prevents the generation again of above-mentioned replacement phenomenon in formal crystal growth phase.Due to the magnesium in above-mentioned metal organic gas
Active highest reduces other metal organic gas so its content can be improved in the selection of metal organic gas ingredient
The content of ingredient such as TMG.After completing metal organic gas reaction step and executing such as 2-3 hour for a long time enough, you can cut
Swap-in enters reacted step.
In reacted step, stopping is passed through metal organic gas while being passed through the steaming of sky gas and water into reaction chamber
Vapour or other oxygen-containing gas.Oxidizing gas can be passed through by above-mentioned admission line 28 can also be by other controllable pipelines
It is passed through.Gas spray keeps original temperature still through above-mentioned cooling fluid supply system, with the operation of lower section air extractor,
Original metal organic gas is discharged reactor, and subsequent air extractor stops pumping, and oxygen-containing gas is full of empty in entire reaction chamber
Between.Oxygen under the higher temperature that defines of the present invention can quickly with stayed in after displacement the magnesium of stainless steel surface in spray head,
Gallium isoreactivity metal generates reaction and forms stable metal oxide, prevents these active metals from being chemically reacted again by subsequent
It takes away so that internal iron is exposed to spray head inner surface of pipeline again.The duration of reacted step can basis
Reaction speed optimum choice preferably can be 20-40 minutes, and design parameter is by reaction chamber inner space and gas spray
Temperature influences, can realize that the active metal oxidation of stainless steel surface is advisable.
It completes that after first time reacted step above-mentioned pretreatment process can be executed again, again into row metal
Organic gas reaction step and reacted step.So repeatedly cycle carries out pretreatment process and is to ensure that spray head
The iron atom on the surface of Organometallic Reac- tion gas is inside exposed to all by active metal replacement and these active metal quilts
Oxidation is fixed, and specific cycle-index preferably can be able to be 5-20 cycle period, most preferably according to treatment effect optimum choice
It it is 10-15 period, the pretreatment time of summation shortens to about 2 day time.Gas spray after pretreatment process
The wafer of lower section can be polluted to avoid in subsequent crystal growth flow.It then can be by unloaded wafer tray 14
Reaction chamber is removed, reaction chamber is fed again into crystal growth flow after loading pending wafer.
After entering crystal growth flow, enough power is inputted in heater 12 so that the upward spoke of heater downwards
It penetrates heat to be heated to the wafer on pallet 14 and pallet to be suitble to the temperature of crystal growth, which can be 600-1300 degree.
Heater 12 can be metallic resistance silk made of the materials such as tungsten, molybdenum, can also be the multiple high-power lamps in lower section, by high-strength
The heating to 14 back side of wafer tray is realized in the radiation of degree.The cold of coldplate is sent into coolant circulation system by controlling simultaneously
But liquid temperature and flow reduce the temperature of spray head, so that spray head temperature is reduced to conventional 50 degree, can reduce energy in this way
Amount consumption can also ensure that the technological parameter of existing 50 degree of spray head temperature of acquired correspondence still ensures that effectively, a large amount of to save
Debugging cost.
The present invention leads to too small amount of improvement cost, enhances pressure resistance and the temperature resistant capability of cooling fluid supply system, improves
The range of operation of spray head temperature improves spray head temperature in pretreatment process so that and chemical reaction velocity is obviously improved,
The time of pretreatment process needs is greatly reduced, the utilization rate of MOCVD device also greatly improved, reduce cost.In crystalline substance
Lower temperature is reduced in body growth phase to match traditional technological parameter.Since the gas spray after heating can
Substantially shorten than the prior art and gas spray is carried out the pretreated time, caused economic benefit is much larger than cold to increase
But liquid supply system temperature range and the hardware modification cost made, so the present invention can significantly improve the utilization of MOCVD device
Rate reduces the defects of wafer growth process incidence.
Although present disclosure is as above, present invention is not limited to this.Any those skilled in the art are not departing from this
It in the spirit and scope of invention, can make various changes or modifications, therefore protection scope of the present invention should be with claim institute
Subject to the range of restriction.
Claims (8)
1. a kind of processing method of MOCVD reactors, including：
A reactor is provided, the reactor includes a reaction chamber, and a gas spray, the gas are fixed at the top of the reaction chamber
Body spray head includes a gas distributor and the coldplate below gas distributor, includes a plurality of cooling in the coldplate
Pipeline is connected to external cooling fluid supply system to control the temperature of coldplate, and an air extractor is arranged in the reaction chamber bottom
Gas for being discharged in reaction chamber, a support device are used to support pending wafer tray, and a heating device is located at institute
It states below wafer tray；
Pretreatment process and crystal growth flow are the treating method comprises, wherein pretreatment process includes metal organic gas
Reaction step and oxygen-containing gas reaction step,
It in the metal organic gas reaction step, places in wafer tray to the support device, controls the coolant liquid and supply
It answers system to make gas spray that there is the first temperature, supplies the first power to the heating device, first is passed through into reaction chamber
Organometallic Reac- tion gas, until completing metal organic gas reaction step；
In the oxygen-containing gas reaction step, stop supplying the first Organometallic Reac- tion gas, while supplying into reaction chamber
Oxygen-containing gas is answered, until completing oxygen-containing gas reaction step；
Cycle executes the metal organic gas reaction step and oxygen-containing gas reaction step, enters until completing pretreatment process
Crystal growth flow；
In the crystal growth flow, place on the pallet to the support device for carrying wafer to be handled, control is described cold
But liquid supply system makes gas spray have second temperature, supplies the second power to the heater, is passed through into reaction chamber
Second Organometallic Reac- tion gas；
It is characterized in that the first temperature is more than second temperature, the first power is less than the second power, and first temperature is 70-200
Degree, second temperature are 45-55 degree.
2. processing method as described in claim 1, which is characterized in that the content of magnesium in first metal organic gas is higher than
Second metal organic gas.
3. processing method as described in claim 1, which is characterized in that the metal gas reaction step duration is that 2-3 is small
When.
4. processing method as described in claim 1, which is characterized in that the oxygen-containing gas be air or water vapour, it is oxygen-containing
Gas reaction Step Time is 20-40 minutes.
5. processing method as claimed in claim 2, which is characterized in that the stream of trimethyl gallium in first metal organic gas
Flow of the amount less than trimethyl gallium in second metal organic gas.
6. processing method as described in claim 1, which is characterized in that the pretreatment process includes metal described at least ten
The cycle of organic gas reaction step and oxygen-containing gas reaction step.
7. processing method as described in claim 1, which is characterized in that second power makes the temperature of wafer tray exist
Between 600-1200 degree, heater described in the first power input so that temperature of tray is less than 500 degree.
8. processing method as described in claim 1, which is characterized in that the gas spray is made of stainless steel.
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| CN106702348B (en) * | 2016-12-29 | 2019-06-18 | 圆融光电科技股份有限公司 | The method for eliminating water oxygen molecular impurity in MOCVD device reaction chamber |
| CN107881487B (en) * | 2017-11-09 | 2019-12-03 | 上海华力微电子有限公司 | A kind of edge-protected coil structures, reaction chamber and chemical vapor depsotition equipment |
| CN113699509B (en) * | 2021-10-27 | 2022-02-01 | 苏州长光华芯光电技术股份有限公司 | Semiconductor growth equipment and working method thereof |
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| US5647945A (en) * | 1993-08-25 | 1997-07-15 | Tokyo Electron Limited | Vacuum processing apparatus |
| CN102409318B (en) * | 2011-12-08 | 2013-08-21 | 中微半导体设备(上海)有限公司 | Thermochemical vapor deposition reactor and method for improving thermal radiance in reactor |
| CN103074601A (en) * | 2012-01-21 | 2013-05-01 | 光达光电设备科技（嘉兴）有限公司 | Spray head used in chemical vapor deposition process |
| CN103794459B (en) * | 2012-10-29 | 2016-04-06 | 中微半导体设备(上海)有限公司 | For gas spray and the coating shaping method thereof of plasma treatment chamber |
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Address after: 201201 No. 188 Taihua Road, Jinqiao Export Processing Zone, Pudong New Area, Shanghai Patentee after: Medium and Micro Semiconductor Equipment (Shanghai) Co., Ltd. Address before: 201201 No. 188 Taihua Road, Jinqiao Export Processing Zone, Pudong New Area, Shanghai Patentee before: Advanced Micro-Fabrication Equipment (Shanghai) Inc. |
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Effective date of registration: 20190724 Address after: 201201 Shanghai City Jingqiao export processing zone of Pudong New Area (South) Taihua Road No. 188 Co-patentee after: Nanchang Medium and Micro Semiconductor Equipment Co., Ltd. Patentee after: Medium and Micro Semiconductor Equipment (Shanghai) Co., Ltd. Address before: 201201 Shanghai City Jingqiao export processing zone of Pudong New Area (South) Taihua Road No. 188 Patentee before: Medium and Micro Semiconductor Equipment (Shanghai) Co., Ltd. |