CN102172458B - Method and equipment for processing tail gas containing ammonium chloride - Google Patents
Method and equipment for processing tail gas containing ammonium chloride Download PDFInfo
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- CN102172458B CN102172458B CN 201010617738 CN201010617738A CN102172458B CN 102172458 B CN102172458 B CN 102172458B CN 201010617738 CN201010617738 CN 201010617738 CN 201010617738 A CN201010617738 A CN 201010617738A CN 102172458 B CN102172458 B CN 102172458B
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Abstract
The invention provides a method for processing tail gas containing ammonium chloride and designs tail gas processing equipment. In the method, a mode of heating and cooling mixed gas reaction is adopted to control a place for generating and depositing NH4Cl dust, and cooling and depositing equipment is designed to effectively filter the ammonium chloride dust in the tail gas after reaction. The problem that ammonium chloride generated in a reaction cavity is difficult to clean in the process that GaN grows in a semiconductor material, especially in HVPE (High Voltage Paper Electrophoresis) is solved, tail gas does not contain dust, the subsequent cavity and pipeline of main reaction can be prevented from being blocked, the effective service life of the equipment is longer than the semiconductor material growth as long as possible, the use ratio of the equipment is improved, and the material growth cost is lowered.
Description
Technical field
The present invention relates to gallium nitride (GaN) semiconductor material growing and hardware system thereof, being specifically related to is a kind ofly having hydrogen chloride (HCL) and ammonia (NH
3) chemical reaction that participates in and the chemical reaction that has ammonium chloride to generate.
Background technology
Third generation semiconductor emerges at present, and third generation semi-conducting material is that GaN sill simultaneously is otherwise known as based on the III-V group nitride material of GaN, AlN, InGaN and AlGaN etc.Wherein GaN, AlN have that the forbidden band is wide, electron saturation velocities is high, breakdown voltage is high, dielectric constant is little, advantage such as Heat stability is good and stable chemical performance.And the GaN sill is the direct band gap semiconductor material with wide forbidden band, and its direct band gap can cover 1.9-6.2eV, is the good equipment of making devices such as backlight, blue-ray LED, purple LED, white light LEDs, blue light LD and purple light LD.
GaN is the representative of GaN sill, and its preparation method is varied, such as gas phase epitaxy of metal organic compound method (MOCVD), high temperature and high pressure synthesis, molecular beam epitaxy (MBE) and hydride vapour phase epitaxy method etc.But satisfy the demand of industry to quality and quantity, the HVPE method gains great popularity.The main advantage of HVPE is that equipment is simple, and control is convenient in growth, the thick film of can growing, and also the thick film dislocation density of growth is little, obtains superior in quality self-standing gan substrate after peeling off easily.
Use hydride gas-phase epitaxy (HVPE) legal system to be equipped with GaN, its main reaction equation is as follows:
1、2Ga+2HCl＝2GaCl+H
2
2、GaCl+NH
3＝GaN+H
2+HCl
Be these two reactions in theory, take place but in real process, have subsidiary reaction, especially in order to improve the GaN growth rate, at HCL and NH
3The feeding amount on all be at double increase, so do not have the NH that has reacted
3Will react with the HCL that feeds or the HCL of generation, generate NH
4Cl, reaction equation is as follows:
HCl+NH
3＝NH
4Cl
When temperature drops to below 337.8 ℃, just have solid and generate, dust is just arranged, in the gas under inside cavity and pipe interior deposition.
Present in the preparation process of GaN, NH
4The generation of Cl is difficult to avoid, and does not yet have good method to remove NH
4Cl.So solid NH in the system
4The generation of Cl has had a strong impact on the growth of GaN material, and the maintenance period of equipment sharply shortens, and frequency of maintenance increases, consume the plenty of time, GaN equipment is in the maintenance for a long time, and utilization rate of equipment and installations reduces, the GaN production cost increases considerably, and is unfavorable for the commercialization growth of GaN.
Many insiders are seeking a kind of method and apparatus, under the situation that does not influence main reaction, and the NH in can the minimizing system
4The growing amount of Cl, or effectively clear up NH on reaction chamber and the inner-walls of duct
4Cl.
The design obtains a cover thinking, and designs a kind of effective ammonium chloride depositing device just according to the physical characteristic and the chemical characteristic of reaction condition and ammonium chloride.
Summary of the invention
The objective of the invention is in order to solve in hydride gas-phase epitaxy (HVPE) process, because the generation of ammonium chloride accessory substance contains a large amount of ammonium chloride (NH in the tail gas
4Cl) dust, stop up follow-up pipeline, make frequency of maintenance high, the problem that idleness of equipment overlong time, utilization rate of equipment and installations are low excessively, one cover gallium nitride growth vent gas treatment thinking is provided, and design processing one cover tail gas treatment device, be to add hot exhaust gas, cooled exhaust gas then earlier, deposit main by-product ammonium chloride, filter tail gas; Hardware design has gone out a kind of cooling depositing device.
For reaching above-mentioned purpose, a kind of processing method that contains ammonium chloride tail gas of the present invention, adopt following technical scheme:
A kind of processing method that contains ammonium chloride tail gas is that ammonium chloride dust sedimentary condition is controlled, and described method comprises the steps:
1., adopt HVPE modes such as (all can) vertical and person are horizontal growing GaN in the A district, main reaction place that GaN generates, the main reaction chamber is the A district, main reaction place of GaN generation, reacted mist is mist a: contain HCl, NH simultaneously
3And NH
4The mixture of Cl;
2., the mist a in A district is through the transition region B district between main reaction place and the depositing device, heat with heating facility in transition region B district between main reaction place and depositing device, and the temperature that makes the transition region B district interior extremity between main reaction place and the depositing device is a little more than 400 ℃;
3., mist a cools off through the inner inclination cooling device and the cooling device of the deposition of the one-level in the chopped-off head C1 district of depositing device, by cooling fluid the C1 district lowered the temperature, the C1 district becomes solid state N H
4Cl major sedimentary place; Through the gas diverter and the cooling device of the deposition of the secondary in the secondary C2 district of depositing device, to the cooling of C2 district, C2 has only in the district a little solid state N H by cooling fluid successively
4Cl major sedimentary place; C1 district level and level space, C2 district are done greatlyyer than transition region B district, can prolong the normal working hours of depositing device, also can reduce the plant maintenance frequency to a certain extent; Cooling fluid adopts water as cooling fluid, and big because specific heat of water holds, flow velocity is guaranteed cooling effect greater than 4L/min;
4., the final stage small-bore filters the C3 district and is provided with the small-bore screen pack, the small-bore screen pack is selected 0.1 micron model for use, the small-bore screen pack is to NH in the mist
4The Cl powder filters, and effectively reduces mist cooling back NH
4The content of Cl powder, tail end connected system follow-up equipment D district, C3 district, gained mist b:HCl and NH
3Can not exist simultaneously in theory, actual have the extremely existence of low concentration, but can ignore NH
4Cl has the extremely existence of low concentration, but can ignore.
Further, described step 2. in, and plane of vision body that a D district top horizontal positioned area equal terminal in the B district so that contrast is done in the back, when
Situation one: the heating facility in the transition region B district between main reaction place and the depositing device does not heat, and by pre-set growth rate growth a period of time, the time, effect was apparent in view more preferably greater than one day, detected NH on the plane of vision
4The thickness of Cl;
Situation two: heating facility 1 heating in B district, use the growth pattern identical with situation one, the time of the same length of growth, detect the plane of vision in B district and D district in the accompanying drawing 1 then.
A kind of ammonium chloride tail gas processing device that contains of the present invention, adopt following technical scheme:
A kind of ammonium chloride tail gas processing device that contains, include the A district, main reaction place that GaN generates, the back, A district, main reaction place that GaN generates connects transition region B district, transition region B between main reaction place and the depositing device is provided with heating facility, transition region B tail end back is provided with the chopped-off head C1 district of depositing device successively, the secondary C2 district of depositing device, the C3 district is filtered in the final stage small-bore, the chopped-off head C1 district of depositing device is provided with the inner inclination cooling device and the cooling device of one-level deposition, the secondary C2 district of depositing device is provided with the gas diverter and the cooling device of secondary deposition, the final stage small-bore is filtered the C3 district and is provided with the small-bore screen pack, the small-bore screen pack is selected 0.1 micron model for use, tail end connected system follow-up equipment D district, C3 district.
Classification thought of the present invention be because divide multistage after, can adopt repeatedly cooling, different ranks is used different streamer modes, after the classification, the amount of the ammonium chloride of arrival filter core is very little, and filter core is not easy to stop up, prolong the normal service time that crosses filter core greatly, reduced frequency of maintenance.The present invention deposits to main dust by-product ammonium chloride in the tail gas in the designated equipment by cooling and the control exhaust gas flow direction of heating up, and has reached dust removing effects.And tail gas is cooled off, follow-up equipment has been played protective effect.Prolong the normal growth time of equipment, prolonged maintenance period.
Description of drawings
Figure 1 shows that the device schematic diagram of the embodiment of the invention.
The dependency structure part description is as follows among the figure:
The main reaction place that A district: GaN generates;
B district: the transition region between main reaction place and the depositing device;
The C district: the chopped-off head of C1 depositing device, C2 are the secondary of depositing device, and C3 is a final stage small-bore screen pack.C1 district level and level space, C2 district are done more greatly, can prolong the normal working hours of depositing device, also can reduce the plant maintenance frequency to a certain extent;
D district: system's follow-up equipment;
Mist a: contain HCl, NH simultaneously
3And NH
4Mixtures such as Cl;
Mist b:HCl and NH
3Can not exist simultaneously in theory, actual have the extremely existence of low concentration, but can ignore NH
4Cl has the extremely existence of low concentration, but can ignore;
1: heating facility;
2: the inner inclination cooling device of one-level deposition, prevent that gas from directly passing through, strengthen cooling effect.Surface roughness is had relatively high expectations, the NH that adheres to
4Cl arrives a bit and will drop automatically after amount;
3: the gas diverter of secondary deposition because the secondary cooling externally, allows gas flow with the depositing device inner surface;
4: cooling device;
5: the small-bore screen pack;
6: solid state N H
4Cl major sedimentary place.
The specific embodiment
For further understanding feature of the present invention, technological means and the specific purposes that reached, function, resolve the advantages and spirit of the present invention, and by below in conjunction with the accompanying drawing and the specific embodiment detailed description of the present invention being further understood.
Technical problem underlying solved by the invention: a, to NH
4The Cl sedimentary condition is controlled; B, to NH
4The design of Cl precipitation equipment.
The proposition of first problem: because hydrogen chloride (HCl) and ammonia (NH
3) reaction generation ammonium chloride (NH
4Cl) be a reversible reaction, can control the carrying out of reaction by the conditions such as amount (gas mainly is concentration control), pressure and temperature of control reactant.In order to improve the growth rate of GaN, ammonia (NH
3) and hydrogen chloride (HCl) concentration be not easy to adjust easily, so control reactant concentration infeasible.The pressure in entire reaction chamber is controlled by main reaction, can not change.That can change is exactly ammonia (NH
3) and after hydrogen chloride (HCl) mixes, through the temperature of the different sections of cavity.After temperature is lower than 337.8 ℃, will the adularescent powder deposition, so how to control ammonia (NH
3) and hydrogen chloride (HCl) mix the back until before the precipitation equipment their temperature all to be higher than 337.8 ℃ (in order to ensure do not produce the ammonium chloride white powder before arriving depositing device, the temperature that mist is arrived between the depositing device is controlled at a little more than 400 ℃ in fact) be first problem.And behind the arrival depositing device it is cooled fast, make NH
4Cl is deposited in the depositing device as much as possible.
Solution has two kinds: because main reaction gallium chloride (GaCl) and ammonia (NH
3) reaction temperature about 1040 ℃, first method is exactly the distance that shortens between depositing device and the main reaction place, makes ammonia (NH
3) and hydrogen chloride (HCl) after mixing, arrive depositing device before temperature all be higher than 400 ℃.Method two is the system that has because other reasons, and the main reaction place is bigger to the distance between the depositing device, and before mist arrived depositing device, temperature had been reduced to the adularescent powder production and has deposited.In this case, just need between main reaction place and depositing device, use the mode of heating, to guarantee to mix the ammonium chloride (NH that the back generates
4Cl) before arriving depositing device, do not deposit as far as possible.
The proposition of second problem: under the prerequisite that first problem has solved, the mist temperature that arrives depositing device should be higher than 400 ℃.The designing requirement of depositing device should be simple in structure, is convenient to again safeguard, must effectively deposit NH
4Cl, this just needs the design that structure is good.
Solution: aspect in the design of depositing device, mainly considering two: hydrodynamics and deposition classification.
From hydrodynamics, when the gas of certain volume, the pipeline by certain distance in the regular hour, as long as pipeline is big more, it is slow more then to put up a guest for the night, if dust is arranged in the gas, what then the dust deposition was maximum is the pipeline thickness, the basic principle that Here it is adopts.The internal cavity of depositing device is done to such an extent that be the bigger the better, but unconfined doing is greatly impossible, specifically do much, must be with reference to the gas flow size of whole system.Also having an exquisite part, is exactly in one-level equipment, and the cooling water plane of use is to be inclined to the engagement shape to arrange, and it is the effect of the similar eddy current of meeting that gas flows through, and helps mist and contacts with cooling body, reaches the good cooling effect.
Adopt HVPE modes such as (all can) vertical and person are horizontal mode growing GaN, the main reaction chamber is the main reaction place of the A district in the accompanying drawing 1: GaN generation, and reacted mist is the mist a in the accompanying drawing: contain HCl, NH simultaneously
3And NH
4Mixtures such as Cl.The mist a in A district (contains HCl, NH simultaneously
3And NH
4Mixtures such as Cl) through the transition region B district between main reaction place and the depositing device, heat with heating facility 1 in transition region B district between main reaction place and depositing device, the temperature that makes the transition region B district interior extremity between main reaction place and the depositing device is a little more than 400 ℃, if too high rapid cooling effect to the back has considerable influence.Make water as cooling fluid, big because specific heat of water holds, flow velocity is guaranteed cooling effect greater than 4L/min.Small-bore screen pack 5 is selected 0.1 micron model for use.The plane of vision body terminal in the B district and top horizontal positioned area in D district equates is so that contrast is done in the back.In two kinds of situation:
Situation one: the heating facility 1 in the transition region B district between main reaction place and the depositing device does not heat, and by pre-set growth rate growth a period of time, the time, effect was apparent in view more preferably greater than one day, detected NH on the plane of vision
4The thickness of Cl.
Situation two: heating facility 1 heating in transition region B district, use the growth pattern identical with situation one, the time of the same length of growth, detect the plane of vision in B district and D district then.
Found that, use this depositing device after, can ignore at the thick base written or printed documents of D district deposition.This equipment of explanation can effectively reduce mist cooling back NH
4The content of Cl powder, and the back screen pack can use for a long time like this, clogging can not occur.
C divides into: the C3 district is filtered in the chopped-off head C1 district of depositing device, the secondary C2 district of depositing device, final stage small-bore.The C1 district is provided with the inner inclination cooling device 2 and cooling device 4 of one-level deposition, and to the cooling of C1 district, the C1 district becomes solid state N H by cooling fluid
4Cl major sedimentary place 6; C2 is provided with the gas diverter 3 and cooling device 4 of region two-stage deposition, and to the cooling of C2 district, C2 has only in the district a little solid state N H by cooling fluid
4Cl major sedimentary place 6; C1 district level and level space, C2 district are done more greatly, can prolong the normal working hours of depositing device, also can reduce the plant maintenance frequency to a certain extent; The C3 district is provided with small-bore screen pack 5, NH in 5 pairs of mists of small-bore screen pack
4The Cl powder filters, back, C3 district connected system follow-up equipment D district, gained mist b:HCl and NH
3Can not exist simultaneously in theory, actual have the extremely existence of low concentration, but can ignore NH
4Cl has the extremely existence of low concentration, but can ignore.
The present invention proposes a kind of processing method that contains ammonium chloride tail gas, and designed a cover tail gas treatment device.Adopted in the invention reacting back mist heating and temperature reduction way, control NH
4The place that the Cl dust generates and deposits, and design a kind of cooling and depositing device, effectively filtered out the ammonium chloride dust in the tail gas of reaction back.Solve in semiconductor material growing, especially the HVPE growing GaN process, generate the difficult problem that chloride solid is difficult to clear up in the reaction chamber.Reaching does not have dust in the tail gas, guarantee that main reaction follow-up cavity and pipeline are not blocked, makes long as far as possible being on the semiconductor material growing of effective life time of equipment, improves utilization rate of equipment and installations, reduces the cost of material growth.
The above embodiment has only expressed part embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as limitation of the scope of the invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention, protection scope of the present invention should be as the criterion with claims.
Claims (3)
1. a processing method that contains ammonium chloride tail gas is that ammonium chloride dust sedimentary condition is controlled, and it is characterized in that described method comprises the steps:
1., adopt vertical or horizontal mode growing GaN, the main reaction chamber is the A district, main reaction place of GaN generation, and reacted mist is mist a: contain HCl, NH simultaneously in the A district, main reaction place that GaN generates
3And NH
4The mixture of Cl;
2., the mist a in A district is through the transition region B district between main reaction place and the depositing device, heat with heating facility (1) in transition region B district between main reaction place and depositing device, and the temperature that makes the transition region B district interior extremity between main reaction place and the depositing device is a little more than 400 ° of C;
The plane of vision body terminal in the B district and top horizontal positioned area in D district equates, so that contrast is done in the back, when
Situation one: the heating facility (1) in the transition region B district between main reaction place and the depositing device does not heat, should be by pre-set growth rate growth a period of time, and the time is greater than one day, detects NH on the plane of vision again
4The thickness of Cl;
Situation two: the heating facility in transition region B district (1) heating, use the growth pattern identical with situation one, the time of the same length of growth, detect the plane of vision in transition region B district and D district then;
3., mist a cools off with cooling device (4) through the inner inclination cooling device (2) of the deposition of the one-level in the chopped-off head C1 district of depositing device, by cooling fluid the C1 district lowered the temperature, the C1 district becomes solid state N H
4Cl major sedimentary place (6); Through the gas diverter (3) and cooling device (4) of the deposition of the secondary in the secondary C2 district of depositing device, to the cooling of C2 district, the C2 district is less important solid-state NH by cooling fluid successively
4Cl major sedimentary place (6);
Cooling fluid adopts water as cooling fluid, and flow velocity is greater than 4L/min, and C1 district level and level space, C2 district are done greatlyyer than transition region B district;
4., the final stage small-bore filters the C3 district and is provided with small-bore screen pack (5), small-bore screen pack (5) is to NH in the mist
4The Cl powder filters, and reduces mist cooling back NH
4The content of Cl powder, tail end connected system follow-up equipment D district, C3 district.
2. treatment facility that contains the processing method of ammonium chloride tail gas as claimed in claim 1, include: the A district, main reaction place that GaN generates, it is characterized in that: the back, A district, main reaction place that described GaN generates connects transition region B district, transition region B between main reaction place and the depositing device is provided with heating facility (1), transition region B tail end back is provided with the chopped-off head C1 district of depositing device successively, the secondary C2 district of depositing device, the C3 district is filtered in the final stage small-bore, the chopped-off head C1 district of depositing device is provided with the inner inclination cooling device (2) and cooling device (4) of one-level deposition, the secondary C2 district of depositing device is provided with the gas diverter (3) and cooling device (4) of secondary deposition, the final stage small-bore is filtered the C3 district and is provided with small-bore screen pack (5), tail end connected system follow-up equipment D district, C3 district.
3. treatment facility according to claim 2 is characterized in that: described small-bore screen pack (5) is selected 0.1 micron model for use.
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|---|---|---|---|
| CN 201010617738 CN102172458B (en) | 2010-12-31 | 2010-12-31 | Method and equipment for processing tail gas containing ammonium chloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102797034B (en) * | 2012-08-27 | 2015-05-20 | 东莞市中镓半导体科技有限公司 | Support boat for GaN material epitaxy industrialization |
| CN106367733B (en) * | 2015-07-24 | 2019-02-22 | 东莞市中镓半导体科技有限公司 | A kind of device and method for removing HVPE equipment pipe tail gas deposit |
| CN109205643B (en) * | 2018-07-11 | 2023-12-19 | 连云港市福源德邦科技发展有限公司 | Dry ammonium chloride tail gas comprehensive utilization device and method in soda production process |
| CN112588060A (en) * | 2020-11-26 | 2021-04-02 | 山东大学 | Novel hydride vapor phase epitaxy tail gas treatment device and method |
| CN113521953B (en) * | 2021-07-21 | 2023-06-02 | 苏州纳维科技有限公司 | Gallium source recovery device in tail gas, tail gas treatment device and HVPE reactor |
| DE102022105526A1 (en) | 2022-03-09 | 2023-09-14 | Aixtron Se | CVD device and method for cleaning a process chamber of a CVD device |
| CN115287456A (en) * | 2022-07-11 | 2022-11-04 | 默特瑞(武汉)科技有限公司 | Method for recovering metal gallium from gallium nitride waste |
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| CN1589951A (en) * | 2003-08-27 | 2005-03-09 | 天津渤海化工有限责任公司天津碱厂 | Ammonium chloride dry dusting method |
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| CN101069804A (en) * | 2005-11-21 | 2007-11-14 | 株式会社科特拉 | Method of processing alkali-activation exhaust gas |
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| JP2001248827A (en) * | 2000-03-08 | 2001-09-14 | Hitachi Zosen Corp | Equipment for treatment of incineration waste gas for obtaining clean incineration fly ash |
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| CN1589951A (en) * | 2003-08-27 | 2005-03-09 | 天津渤海化工有限责任公司天津碱厂 | Ammonium chloride dry dusting method |
| CN101069804A (en) * | 2005-11-21 | 2007-11-14 | 株式会社科特拉 | Method of processing alkali-activation exhaust gas |
| CN1843565A (en) * | 2006-03-27 | 2006-10-11 | 张锡麟 | Low pressure double flow spray method and system for high temperature fume quenching and tempering and dust processing |
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