CN108529559A - A kind of integral method and device of the useless hydrogen recycling of manufacture of semiconductor - Google Patents
A kind of integral method and device of the useless hydrogen recycling of manufacture of semiconductor Download PDFInfo
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
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Abstract
The invention discloses the integral methods and device of a kind of useless hydrogen recycling of manufacture of semiconductor, integrated treatment process includes that processes, the integrated treatment units such as catalysis burning, spray washing, aqueous vapor separation, adsorption cleaning, pressure-variable adsorption and hydrogen purification include the structures such as catalytic burner, spray jet scrubber, moisture separator, air blower, the first absorber, the second absorber, adsorption cleaning sequencing valve, supercharger, integrated form pressure swing adsorber, pressure-variable adsorption regulating valve/sequencing valve, pressure reducing valve, hydrogen purifier successively.Using a kind of integral method and device of the useless hydrogen recycling of manufacture of semiconductor of the present invention, compensate for the irretrievable weakness of the useless hydrogen of manufacture of semiconductor, it can realize the recycling of useless hydrogen, the electron level hydrogen standard met needed for manufacture of semiconductor can also be purified to, and hydrogen yield is up to 80%, and blank has been filled up with recycling economy development for semiconductor industry green.
Description
Technical field
The present invention relates to the field of environment protection of the useless hydrogen recycling in semiconductor fabrication, and in particular to Yi Zhongban
The integral method and device of the useless hydrogen recycling of conductor processing procedure.
Background technology
Electron level hydrogen (PH2, hydrogen content >=99.99999% (7N) are similar below) is used as a kind of special gas, is existing
For indispensable one of the important chemical raw material of electronics industry, and semiconductor industry is the core of modern electronics industry, system
Journey is roughly divided into the wafer manufacture of upstream, IC (integrated circuit) manufactures in middle reaches, the relevant light shield of downstream IC package and periphery, sets
Meter, using etc. industries.The basis of semiconductor industry is silicon materials industry, wherein 90% or more semiconductor devices (TFT-LCD
(flat-panel monitor), OLED etc.) and integrated circuit, especially super large-scale integration (ULSI) be all be produced on it is high-purity high-quality
Silicon single-crystal polishing plate and epitaxial wafer on.In recent years, semiconductor industry scale of the whole world based on wafer silicon chip had reached several
Trillion dollars, for example, silicon wafer chip manufacturing and foundry, South Korea, China's Mainland and Taiwan have occupied 60% of the industry or more.In
It is more than 1.8 trillion dollars that state's last decade, which adds up the chip inlet amount of money, has even more reached within 2016 nearly 2,30,000,000,000 dollars,
More than 1 times, become the maximum bulk product of Chinese import volume more than 1,116,000,000,000 dollars of petroleum import volume.
One typical silicon wafer chip production process (processing procedure) has 400~500 procedure steps, wherein taking around use
50~100 multiple gases.For PH2 as a kind of bulk gas, dosage is bigger, is mainly used for the process gas of silicon wafer chip processing procedure
One of, it is doped with gas for example, PH2 is used as, adopts gas, ion implanting gas, etching gas, purge gas, manufacture outside
The inert gas that various equipment use in the process, and wait use.Chemical vapor deposition (CVD) extensions of PH2 in silicon wafer chip
Carrier gas is cleaned with protection gas, plasma gas, and as hydrogen-containing gas such as synthesis similar arsine (AsH3), phosphines (PH3)
In hydrogen molecule source etc., especially chemical vapor deposition (CVD) process in the preparation of silicon wafer chip thin films and epitaxial manufacture process,
The purity of PH2 directly influences the quality of silicon wafer chip.
The useless hydrogen (EH2) for largely containing various impurity compositions is generated while manufacture of semiconductor consumes PH2, including
Silicon wafer chip chemical vapor deposition (CVD)) film preparation and extension process generate reaction product hydrogen, CVD reaction chambers it is clear
It washes hydrogeneous exhaust gas, the hydrogeneous exhaust gas of doping, the hydrogeneous exhaust gas of photoetching, chip and cleans hydrogeneous exhaust gas, and the hydrogeneous exhaust gas that burning generates
Deng, wherein the CVD processes of film preparation and extension are one of useless most important sources hydrogen (EH2) of manufacture of semiconductor electronics,
The quantum of output of EH2 is 1~5 times of fresh PH2 usage amounts in the process, is approximately the 20~60% of the total discharge rate of useless hydrogen (EH2).
Typical CVD exhaust gas groups become, hydrogen (H2) content about 30~95% (volume ratio, similar below), main key impurity
Such as inflammable, explosive, poisonous SiH4, PH3, AsH3, BH3 equal size of component is more than 1~5%, other impurity include TCH, N2,
HCl, NH3, organic exhaust gas (VOCs) equal size are also above 5~10%.Due to EH2 complicated components, especially key impurity group
The presence divided so that the purification recycling of EH2, which again returns in manufacture of semiconductor, becomes extremely difficult.Currently, mostly partly leading
Body manufacturer is all directly to be vented EH2 or conduct by being incorporated to hydrogen discharge system after catalysis burning and acid-alkali washing processing
Combustion gas uses, and causes the significant wastage of resource.
Electronics give up on hydrogen (EH2) recovery and reuse technology exist it is following difficult：
First, EH2 complicated components：The useless hydrogen component of electronics to be recycled is more multiple than the unstripped gas for preparing fresh electronics hydrogen
It is miscellaneous, can be introduced into generated other impurity in manufacture of semiconductor, including oxide, organic matter volatile materials, inorganic matter (such as
Inorganic acid, hydrogen peroxide, sulfide, chloride etc.) and its toxic inflammable and explosive key impurity composition (SiH4, PH3, AsH3,
BH3) etc..Therefore, the fluctuation of impurity influences subsequent hydrogen purification technique (palladium film or metal getter) very big；
Second, EH2 complicated components influence the selection of recovery technology：Contain inflammable and explosive silicon (oxygen) alkane in unstripped gas
(SiH4), phosphine (PH3), the stronger hydrochloric acid of corrosivity (HCl) and ammonia (NH3/NH4OH), the effumability being more toxic are organic
Steam (VOCs), oxygen (O2), CO, CH4 and water etc., it is necessary first to by toxic component in useless hydrogen and explosive inflammable miscellaneous
Matter, which is first handled, is converted into harmless components or micro harmful constituent, feeds standard according still further to hydrogen purification process, selects imurity-removal
Purification recycling technique.Harmful constituent content height, directly affects the selection of purification recycling technique, and then certainly
Whether whether the hydrogen recycled surely, which can return to hydrogen purification process, uses, can finally return in manufacture of semiconductor and realize profit again
With.Wherein, most sensitive is SiH4, PH3, AsH3, BH3 with critical impurities component, and acid (HCl etc.), alkaline (NH3 etc.),
Other impurity compositions such as chlorine-containing compound (BCl3, PCl3 etc.), VOCs, photoresist；
Third, the sources EH2 are complicated：The useless hydrogen component that semiconductor manufacturing difference process generates is different, such as chemical gaseous phase
Useless hydrogen silane-containing, phosphine, the borine amount generated in deposition (CVD) and extension process is more, also, useless amounts of hydrogen is larger；Deng
VOCs, water, organic impurities (especially photoetching colloid in ion hydrogen etch and the useless hydrogen of cleaning (PEC/PC) process discharge
Residual) equal size is more；It is then desired to for hydrogen type and the quantity of giving up caused by different semiconductor fabrication sequences, carry
Go out corresponding comprehensive technological scheme；
The front-end processing of 4th, EH2：Semiconductor factory all configures special various electronics emission-control equipments, such as removes
The acid-alkali washing device of soda acid exhaust gas, flammable or poisonous fume catalytic combustion burner etc., the front-end processing work that each factory is configured
Skill is different, how using communication front-end equipment, pre- purifying technique can it is effectively coupled thereto/matching, formed one makeup
Set etc., and purify recycling technique and design considered one of key factor；
5th, treatment scale miniaturization integration：Existing manufacture of semiconductor waste gas treatment equipment is mostly burning and washes
It washs, only plays the role of reaching discharge standard after removing harmful substance, do not recycle the active principles such as hydrogen therein, and advise
Mould is small, in-situ processing.And the device economic scale of existing recycling hydrogen is big, can not realize one with processing equipments such as burning, washings
Body；
6th, existing fresh PH2 absorption purification technique is difficult to handle EH2, such as Cyroadsorption method, palladium embrane method, metal
Getter method, pressure-variable adsorption or temp.-change adsorptive process, chemiadsorption etc. have removing energy only for certain trace impurities in EH2
Power, and the impurity composition of Various Complex in EH2 is difficult to remove totally, therefore, EH2 can only be purified and commercial-grade hydrogen be made,
It can not return in manufacture of semiconductor and recycle；
7th, EH2 recycling still need to handle standard by toxic inflammable and explosive hazardous chemical, and standard height executes stringent；
8th, the maximum difficult point of the useless hydrogen of recycling electronics is that purification recycling technique should be limited by the front end of EH2
Treatment process is limited by rear end hydrogen purification process again, but front-end processing influences maximum.Semiconductor factory is often existing
The hydrogen purification process of front-end processing exhaust gas and rear end is substantially stationary, therefore, hydrogen purification recycling of giving up is arranged to centre
Technological requirement it is harsher.
Invention content
The present invention provides a kind of integral method and device of the useless hydrogen recycling of manufacture of semiconductor, existing to solve
Technology influences very big technical problem because of the fluctuation of impurity on subsequent hydrogen purification technique (palladium film or metal getter).
The technical solution adopted by the present invention is as follows：
A kind of integral method of the useless hydrogen recycling of manufacture of semiconductor, the unstripped gas of processing is from semiconductor system
Chemical vapor deposition CVD in journey, or doping diffusion and ion implanting or the useless hydrogen of photoetching or other process direct emission,
Its major impurity group is divided into nitrogen N 2, methane CH4, ammonia NH3, a small amount of silane and more siloxanes SiH4, phosphine and more phosphines
PH3, arsine and more arsine AsH3, borine and more borine BH3, acidic components, basic component, organic matter and volatile components
VOCs, metal oxide and particle, water and oxygenatedchemicals and other impurities, pressure is normal pressure or is less than 0.3MPa, temperature
It it is 20~90 DEG C, integral method includes following process：
(1) catalysis burning, by manufacture of semiconductor chemical vapor deposition or doping or photoetching direct emission it is useless
Hydrogen feed is mixed with the high-temperature fuel gas ejected from the fuel gas jets of heating, at a high temperature of 800~1200 DEG C, into
Toxic ignitable components in unstripped gas are oxidized to harmless component by row catalyst combustion reaction, form burning mixed pyrolysis gas, combustion
It burns mixed pyrolysis gas bag and includes silica SiO2, arsenic and oxide and other metal oxide particles and inert component：H2、
N2, carbon monoxide CO, carbon dioxide CO2, water and other components；
(2) spray washing, the burning mixed pyrolysis gas from catalytic combustion process, is washed by spray washing unit
It washs, water-soluble component in burning mixed pyrolysis gas is dissolved, and solid particle therein is washed away to spray washing unit
Bottom emits together with aqueous solution, and the saturation gaseous mixture that temperature is less than 100 DEG C is formed after spray washing；
(3) aqueous vapor detaches, the saturation gaseous mixture from spray washing, into moisture separator, mixing of the water droplet from rising
It is disengaged in gas, adsorbed and formed big water droplet and be discharged by the filler loaded in moisture separator, disengage the gaseous mixture of moisture
For dry mixture；
(4) adsorption cleaning, the dry mixture from aqueous vapor separation process, into the suction being made of two concatenated absorbers
Coupon member, loads one or more adsorbents in absorber, dehydration is further dried, removing be not completely burned on a small quantity it is toxic
Gas component and burning are formed by oxynitrides not soluble in water, are purified gaseous mixture；Wherein, the first absorber is
Disposable physical absorption is slightly purified, and water-soluble polar impurity and water are removed；Second absorber carries out for chemisorption
Essence purification removes nonpolarity not soluble in water or the weak impurity composition of polarity；
(5) pressure-variable adsorption, the purification gaseous mixture from adsorption cleaning process, by being pressurized to 1.0~5.0MPa, into change
Adsorption system is pressed, the impurity composition in gaseous mixture will be purified and adsorbed, the gas not adsorbed is formed by fluid phase gas and is
The superelevation pure hydrogen intermediate products that hydrogen purity is 99.999~99.9999%, the adsorbent loaded in pressure swing adsorption system are adopted
With activated alumina, silica gel, activated carbon/load active component activated carbon, molecular sieve/load active component molecular sieve one kind or
It is a variety of, regeneration is rinsed or vacuumized using superelevation pure hydrogen intermediate products when adsorbent reactivation；Rinse gas or evacuation and inverse
Put and be formed by stripping gas, according to gas component, a part or enter catalytic combustion process directly as combustion gas, a part or
Catalytic combustion process, a part or direct emission are returned to as unstripped gas；
(6) hydrogen purification, the superelevation pure hydrogen intermediate products from pressure-variable adsorption process, at a temperature of 50~500 DEG C,
It is decompressed to the pressure needed for manufacture of semiconductor hydrogen directly or by pressure reducing valve, by metal getter or palladium film or palladium film-
The hydrogen purification process of metal getter coupling, operation temperature is 50~500 DEG C, operating pressure is normal pressure to manufacture of semiconductor
It is purified under the pressure condition needed for hydrogen, removes trace impurity, obtain final electron level hydrogen product.Electron level hydrogen
Product purity reaches the product standard of the electron level hydrogen of international semiconductor association SEMI defineds, and hydrogen purity is more than or equal to 7
~8N grades, cool down by heat exchange or be depressured, or be sent into the storage of electron level hydrogen product tank, or passes through hydrogen product surge tank,
It is returned directly in the workshop section that manufacture of semiconductor needs hydrogen, wherein the operation temperature of hydrogen purification process is by used
The technique of metal getter or palladium film determines that the service life of metal getter or palladium film was at least more than 2 years, without regeneration；By
The yield of this obtained electron level hydrogen product is more than 70~80%.
Preferably, the fuel gas used in the catalytic combustion process is fresh hydrogen, natural gas, purified
One kind in the stripping gas of manufacture of semiconductor exhaust gas, clean air and pressure-variable adsorption process containing methane or hydrogen or nitrogen or
A variety of, fuel gas imports reaction chamber again after being preheated using the waste heat of catalytic combustion process catalyst combustion reaction cavity, carries
High heat utilization rate.
Preferably, in the pressure-variable adsorption process, the regeneration carrier gas of adsorbent is using vapor, pressure-variable adsorption process
One kind in the superelevation pure hydrogen intermediate products of generation, the hydrogen product of hydrogen purification process；Regenerate carrier gas and catalysis burner
One kind in the fuel gas of sequence or the hydrogen product of the saturation gaseous mixture of spray washing process or hydrogen purification process, carries out hot friendship
It changes and reaches 100~250 DEG C of regeneration temperature, improve heat utilization rate.
Preferably, the adsorptive pressure of the pressure-variable adsorption process is 2.0~5.0MPa, adsorption and desorption circulate operation
Pressure change in the process is realized by sequence valve and regulating valve on the pipeline that is connected between each sorption channel both ends
It is slow to control, prevent system pressure from changing the absorbent atomizing production of excessive caused airflow scouring sorption channel and its filling
It is raw so that system operatio stability and security.
Preferably, the operation temperature of the hydrogen purification process depend on used palladium film, metal getter with
And palladium film coupling metal getter process choice, palladium film and without activation or medium temperature activated form metal getter operation temperature
It it is 50~100 DEG C, the operation temperature of the metal getter of high-temperature activation is 300~500 DEG C, wherein the operation pressure under high temperature
Power is less than 2.0MPa.
A kind of integrated apparatus of the useless hydrogen recycling of manufacture of semiconductor, including sequentially connected catalytic burner,
Spray jet scrubber, moisture separator, air blower, the first absorber, the second absorber, supercharger, integrated form pressure swing adsorber and
Hydrogen purifier；The catalytic burner is arranged to internal and external casing shape, and the inner tube of catalytic burner is arranged to combustion chamber, institute
Combustion chamber upper end setting gas distributing disc mouth is stated, combustion chamber lower end is connected to the top of spray jet scrubber, catalytic burner
Interlayer inner disc be wound with burning gas coil pipe, air inlet, the upper end for the gas coil pipe that burns and gas is arranged in the burning gas coil pipe lower end
Distributing disc mouth is connected to；The spray jet scrubber includes spray chamber, and nozzle is arranged in the spray chamber inner wall；The aqueous vapor separation
The bottom of device is connected with the bottom of spray jet scrubber with U-shaped connecting tube, wherein U-shaped connection bottom of the tube be equipped with particle suspension liquid with
The collection floss hole of water, moisture separator top escape pipe pass through the sequencing valve on air blower and the first absorber bottoms inlet tube
It is connected, the second absorber is connected up and down with the first absorber, and escape pipe is inhaled by sequencing valve and second on the first absorber top
Adnexa bottom inflow pipe is connected, and escape pipe is by being arranged sequencing valve and supercharger and integrated form pressure-variable adsorption at the top of the second absorber
Regulating valve on device lower inlet pipe is connected, and escape pipe is by setting pressure reducing valve and hydrogen purification at the top of integrated form pressure swing adsorber
The inlet tube of device is connected, outlet conduit and the decompression on escape pipe at the top of integrated form pressure swing adsorber of the hydrogen purifier
Valve is connected, the fuel gas inlet pipe in sequencing valve and catalytic burner in the bypass of integrated form pressure swing adsorber bottom inflow pipe
It is connected.
Preferably, the nozzle setting of the spray jet scrubber circularizes or semi-circular, nozzle direction obliquely and with
Spray chamber inner wall is in 40~90 ° of angle, facilitates water mist that the solid particle of generation is washed away discharge.
Preferably, the water droplet that the collection floss hole for connecting U-shaped connection bottom of the tube is equipped in the moisture separator returns
Baffle or return duct are flowed, drip discharge is conducive to.
Preferably, first absorber and the second absorber integrated setting, are arranged to a geometry module
The integrated form temperature swing adsorbers that unit is formed by stacking, there is at least four sorption channel in integrated form temperature swing adsorbers, in sorption channel
Load adsorbent.
Preferably, the integrated form pressure swing adsorber is formed by stacking by a solid modular unit, and integrated form becomes
There is at least two sorption channel in pressure absorber, adsorbent is loaded in sorption channel.
The present invention is according to complete warm journey pressure-variable adsorption (full name in English：Full Temperature Range-Pressure
Swing Adsorption, referred to as：FTrPSA), it is one kind based on pressure-variable adsorption (PSA) and can be detached and instead with various
Answer the method that technology is coupled, using different material component itself different pressures at a temperature of adsorbing separation coefficient and physics
The otherness of chemical property takes adsorption and desorption in room temperature/medium temperature pressure-swing absorption process to be easy to the cycle behaviour for matching and balancing
Make the method to detach and purify various low-boiling point gas (being purified containing ultra-pure hydrogen, purity >=6 H2~7N).According to manufacture of semiconductor
The electronics of middle generation give up the physicochemical characteristics of plurality of impurities component, relative separation coefficient contained by hydrogen (EH2), corresponding point
From purification method and corresponding operating condition (temperature and pressure), will catalysis burning, spray washing, physics and chemisorption,
The various technologies such as pressure-variable adsorption, UF membrane are coupled, and realize a kind of useless hydrogen recycling of manufacture of semiconductor, and formed
A kind of integrated device.
Compared to the prior art, the beneficial effects of the invention are as follows：
(1) solve because electronics to be recycled give up hydrogen can be introduced into manufacture of semiconductor caused by other impurity, including
Oxide, organic matter volatile materials, inorganic matter (such as inorganic acid, hydrogen peroxide, sulfide, chloride etc.) and its toxic inflammable
Explosive key impurity composition (SiH4, PH3, AsH3, BH3) etc. is to subsequent hydrogen purification technique (palladium film or metal getter
Agent) it influences very big and can not recycle and return in manufacture of semiconductor the problem of recycling；
(2) it is especially applicable to toxic inflammable and explosive key impurity composition contained in EH2 (SiH4, PH3,
AsH3, BH3) there is larger fluctuation operating mode, while in view of the safety issue of process, using catalysis burning, spraying
Washing, the coupling of two-stage adsorption cleaning, pressure-variable adsorption and/or hydrogen purification technique, by key impurity composition and other impurity
Component removes the feeding gas requirement for totally meeting last hydrogen purification process defined one by one, finally obtains qualified PH2 productions
Product, and may return in manufacture of semiconductor and recycle, the product gas yield of PH2 is more than 70~80%；
(3) solving the problems, such as in-situ processing unit scale can not minimize and integrated：Existing manufacture of semiconductor is useless
Gas field processing equipment is mostly burning and washing, only plays the role of reaching discharge standard after removing harmful substance, not return
Receive the active principles such as hydrogen therein, and small scale, in-situ processing.And the device economic scale of existing recycling hydrogen is big, nothing
Method with burning, washing etc. processing equipments realization it is integrated；
(4) present invention passes through the rational heat exchange system of arrangement using the otherness of the operation temperature of each process so that
The heat of whole operation system is fully utilized；
(5) present invention passes through the two-stage series connection of adsorption cleaning and the coupling with integrated form pressure swing adsorber so that separation carries
The device miniaturization integration of pure hydrogen becomes a reality, and can easily be spliced with existing live emission-control equipment,
So that whole recycling becomes a reality；
(6) present invention is adsorbed to key impurity composition and easily and is solved according to the feature of various adsorption methods in system
The polar impurity component for inhaling relative difficulty, two-stage one is replaced using reproducible temp.-changing adsorption and the series system of chemisorption
The absorber of secondary property adsorption cleaning, and the regeneration carrier gas that subsequent step can be used is regenerated so that the yield of hydrogen product and
Used sorbent life further increases；
(7) present invention uses high voltage bearing integrated form pressure swing adsorber and slow equal transformation side in pressure-variable adsorption step
Formula carries out deep purifying to the hydrogeneous unstripped gas after essence is de- and removes various micro or even trace impurity composition, avoid because
Adsorbing contaminant component it is too low because dividing due to can not deep removal, meanwhile, avoid because micro- using traditional temp.-changing adsorption (TSA) removing
Amount or trace impurity component and cause to hydrogen purification process may introduce hot nitrogen regeneration or heat carrier be formed by new impurity group
The problem of dividing, and absorption are formed by circulate operation problem with difficult for regeneration to match, and both ensure that the original of hydrogen purification step
Expect gas feed needs, and the adsorbent service life of pressure-variable adsorption step can be extended so that integrated method and device is more
Add stability and security；
(8) present invention solves the maximum technological difficulties during EH2 purification recyclings：Purify recycling work
Skill should be limited by the front-end processing technique (burner, washer or moisture separator) of EH2, and it is pure to be limited by rear end hydrogen again
Chemical industry sequence, and then the hydrogen purification process of semiconductor factory's existing front-end processing exhaust gas and rear end can be made full use of, it saves
Investment and occupation of land；
(9) present invention compensates for the blank in manufacture of semiconductor normal pressure EH2 recyclings field, opens semicon industry
Interior circular economy new route, while solving the environmental problem of air discharge.
Description of the drawings
Fig. 1 is 1 flow diagram of the embodiment of the present invention；
Fig. 2 is 5 schematic device of the embodiment of the present invention；
Figure label is respectively：1, catalytic burner；2, spray jet scrubber；3, moisture separator；4, air blower；5, first
Absorber；6, the second absorber；7, sequencing valve；8, supercharger；9, regulating valve；10, integrated form pressure swing adsorber；11, pressure reducing valve；
12, hydrogen purifier.
Specific implementation mode
In order to make those skilled in the art more fully understand the present invention, following will be combined with the drawings in the embodiments of the present invention
Technical solution in the embodiment of the present invention carries out clear, complete description.
Embodiment 1
The integral method of hydrogen recycling as shown in Figure 1, a kind of manufacture of semiconductor gives up, specific implementation step packet
It includes,
Step 1. unstripped gas：The useless hydrogen of chemical vapor deposition (CVD) in manufacture of semiconductor, flow 50Nm3/
H, key component are：H2 is 56% (volume ratio, similar below), the silane as key impurity composition and more (oxygen) silane
(SiH4) 5.3%, phosphine and more phosphines (PH3) 0.1%, arsine and more arsines (AsH3) 0.1%, borine and more borines (BH3)
0.1%, acidic components (in terms of HCl) 0.1%, basic component (in terms of NH4OH) 5.1%, organic matter and volatile components
(VOCs) 0.1%, mist of oil 0.1%, particle 0.01% (mass ratio), methane (CH4) 10.5%, total hydrocarbon (TCH) 0.2%, water
(H2O) 0.1%, carbon dioxide (CO2) 0.05%, low-boiling carbon monoxide (CO) 1%, nitrogen (N2) 17.8%, oxygen
(O2) 3ppm, nitrogen oxides (NOx) 10ppm, other impurity≤1~2%；It is room temperature that pressure, which is less than 0.1MPa, temperature, directly
Enter step 2；
Step 2. catalysis burning：Unstripped gas from step 1 is led through catalyst combustion reaction chamber (room) gas distributing disc mouth
Enter, is mixed with from the fresh hydrogen for entering preheating coil pipe and from step 6 stripping gas, as combustion gas from the nozzle of combustion gas
The high-temperature fuel gas mixing ejected carries out catalyst combustion reaction, by the key in unstripped gas at a high temperature of 800~900 DEG C
Property impurity and ignitable components be oxidized to harmless component, including silica (SiO2), arsenic and oxide and the oxidation of other metals
Composition granule and a large amount of inert component, including H2, N2, carbon monoxide (CO), carbon dioxide (CO2), water and other components,
The burning mixed pyrolysis gas after catalysis burning is formed, 3, i.e. spray washing are entered step；
Step 3. spray washing：Burning mixed pyrolysis gas from step 2, by being sprayed as the water mist built in reaction lumen wall
The spray washing unit that head is constituted is washed, and water-soluble component in burning mixed pyrolysis gas is dissolved, and washes away
Solid particle therein is emitted to spray washing unit bottom together with aqueous solution.Meanwhile it being formed after spray washing
Saturation gaseous mixture, temperature is down to 100 DEG C hereinafter, entering step 4, i.e., aqueous vapor detaches；
Step 4. aqueous vapor detaches：Saturation gaseous mixture from step 3 is caused by the relief valve of moisture separator
Being saturated mixed airflow becomes supersaturated vapor pressure, and water droplet is disengaged from the gaseous mixture of rising, loaded in moisture separator
Stainless steel ring packing adsorbs and forms big water droplet and be discharged, and the gaseous mixture for disengaging moisture is dry mixture, enters step 5,
That is adsorption cleaning；
Step 5. adsorption cleaning：Dry mixture from step 4, into being connected by two and be filled with activated carbon, three oxygen
Change two aluminium, the composite adsorption that the activated carbon of load active component, the molecular sieve of load active component and a small amount of silica gel are formed
Dehydration is further dried, the toxic gas components that removing is not completely burned on a small quantity in the absorbing unit of the absorber composition of agent, with
And burning is formed by oxynitrides not soluble in water and other trace impurity components, is purified gaseous mixture, enters step
6, i.e. pressure-variable adsorption；Wherein, the first absorber is that disposable physical absorption is slightly purified, and removes water-soluble polar impurity
And water；Second absorber is that chemisorption carries out smart purification, removes nonpolarity not soluble in water or weaker key miscellaneous of polarity
Matter component；
Step 6. pressure-variable adsorption：Purification gaseous mixture from step 5, by being pressurized to 3.0~4.0MPa, by one
The pressure-variable adsorption step that pressure-variable adsorption (PSA) device of packaging type is constituted will purify the impurity composition in gaseous mixture and adsorb, do not inhaled
It is superelevation pure hydrogen intermediate products that attached gas, which is formed by fluid phase gas, hydrogen purity is 99.999~
99.9999% (being denoted as 5~6N), remaining impurity content are satisfied by next process and limit requirement to its feeding gas quality, enter
Next step.Wherein, integrated form pressure swing adsorber is formed by stacking by a hexahedron module unit, inside has 6 absorption logical
Road, the built-in carrying active charcoal in channel, silica gel, molecular sieve and selective absorption N2/CO compound adsorbent, to meet each absorption
It is carried out while passage adsorbent, desorption process, ensures consecutive production.One sorption channel is being adsorbed, remaining 5 channel carries out
Desorption.When adsorbent reactivation, it is rinsed+evacuates combination using superelevation pure hydrogen intermediate products and desorbed；Flushing gas,
It evacuates and inverse put is formed by stripping gas, a part enters step 2 directly as combustion gas, and a part is returned to as unstripped gas
Step 2, a part or direct emission；
Step 7. hydrogen purification：Superelevation pure hydrogen intermediate products from step 6, by being fired with the preheating in step 2
The heat exchange for burning gas is decompressed to the pressure needed for manufacture of semiconductor hydrogen at a temperature of 450~500 DEG C by pressure reducing valve
1.0MPa, into the hydrogen purification process being made of metal getter, operation temperature is 450~500 DEG C, operating pressure is
It is purified under conditions of 1.0MPa, removes trace impurity, obtain final electron level hydrogen product, purity reaches international and partly leads
The product standard of the electron level hydrogen of body association (SEMI) defined, hydrogen purity are more than or equal to 7~8N grades, extremely by heat exchange
Room temperature or the required temperature of manufacture of semiconductor CVD processes, by hydrogen product surge tank, being returned directly to manufacture of semiconductor needs
In the workshop section for wanting hydrogen, wherein the service life of metal getter was at least more than 2 years, without regeneration；Thus obtained electron level
The yield of hydrogen product is more than 70~80%.
Embodiment 2
As shown in Figure 1, on the basis of embodiment 1, the metal getter in step 7 is changed to palladium film (shell and tube), is come from
The superelevation pure hydrogen intermediate products of step 6, need not move through heat exchange and pressure reducing valve, are directly entered step 7, less than 100 DEG C
At a temperature of, be directly entered the hydrogen purification process being made of palladium film, operation temperature be 50~100 DEG C, operating pressure be 3.0~
It is purified under the conditions of 4.0MPa, removes trace impurity, final electron level hydrogen product is obtained from palladium-membrane hydrogen per-meate side, it is pure
Degree reaches the product standard of the electron level hydrogen of international semiconductor association (SEMI) defined, and hydrogen purity is more than or equal to 7~8N
Grade, pressure 1.0MPa, by heat exchange to room temperature or the required temperature of manufacture of semiconductor CVD processes, by hydrogen product
Surge tank is returned directly in the workshop section that manufacture of semiconductor needs hydrogen, wherein the service life of palladium film was at least more than 2 years, nothing
It needs to regenerate；The yield of thus obtained electron level hydrogen product is more than 70~80%.
Embodiment 3
As shown in Figure 1, on the basis of embodiment 1, there is ready-made hydrogen purification process in manufacture of semiconductor, then the present embodiment
By the superelevation pure hydrogen intermediate products from step 6, it is passed directly into existing hydrogen purification process, alternative steps 7.
Embodiment 4
On the basis of embodiment 1, the first absorber of the step 5 and the second absorber are merged by a hexahedron
The integrated form temperature swing adsorbers that modular unit is formed by stacking inside have 4 sorption channels, activated alumina are loaded in 2 channels
And active carbon compound adsorbent, load active component activated carbon and molecular sieve compound adsorbent in another 2 channels, to meet
It is carried out while each sorption channel Adsorption and desorption process, ensures consecutive production.Wherein, corresponding sorption channel is two-by-two
It connects and is in adsorbed state, corresponding channels in series is desorbed two-by-two for remaining；When adsorbent reactivation, using from step 6
Stripping gas as regeneration carrier gas, with step 7 hydrogen product carry out heat exchange, reach 180~200 DEG C of regeneration temperature.
Embodiment 5
As shown in Fig. 2, on the basis of embodiment 1, unstripped gas enters from 1 top feed gas distribution plate mouth of catalytic burner,
With the fresh hydrogen from the pre-add hot coil built in entrance 1 tube wall of catalytic burner and the solution from integrated form pressure swing adsorber 10
Air-breathing mixes, and the high-temperature fuel gas ejected from the combustion gas nozzle ring at 1 top of catalytic burner as combustion gas mixes,
At a high temperature of 800~900 DEG C, catalyst combustion reaction is carried out in the reaction chamber in catalytic burner 1, catalysis is formed by and splits
The spray jet scrubber 2 being directly over positioned at 1 lower part of catalytic burner of venting one's spleen is washed, and high pressure water is from 2 tube wall of spray jet scrubber
Built-in semicircular and spray water mist with the nozzle of the axial angle at 45 ° of spray jet scrubber 2, to the catalytic pyrolysis gas that flows through into
Row washing, water-soluble impurity composition and particulate matter in gas are washed away, by being arranged in 2 bottom of spray jet scrubber and water
The particle suspension liquid of the connected U-shaped pipe in 3 bottom of gas separating device and the collection floss hole of water discharge, by the catalysis of spray washing
Cracked gas forms saturation gaseous mixture, and temperature is down to 100 DEG C hereinafter, releasing by 3 bottom of moisture separator of the U-tube other side
Valve is put, causes to be saturated mixed airflow as supersaturated vapor pressure, water droplet is disengaged from the gaseous mixture of rising, by moisture separator
The stainless steel ring packing loaded in 3 adsorbs and is formed big water droplet, by set in moisture separator 3 water droplet reverse flow baffle and
The particle suspension liquid of connected U-shaped pipe and the collection floss hole of water discharge；The mixing of moisture is disengaged from 3 top of moisture separator
Gas is dry mixture, and entering the first absorber 5 through the defeated adsorption cleaning sequencing valve 7 through 5 bottom of the first absorber of air blower 4 carries out
Thick purification absorption is inhaled by the first absorber 5 with positioned at the second of 5 top of the first absorber from the 5 top outflow of the first absorber
Purifying program control valve 7 between adnexa 6 is again introduced into the second absorber 6 and carries out deep purifying absorption, from 6 top of the second absorber
Outflow purification gaseous mixture adsorbs sequencing valve 7 and supercharger 8 and collection by the purification on 6 top outflow pipeline of the second absorber
The connected pipeline of pressure-variable adsorption regulating valve/sequencing valve of 10 lower part of accepted way of doing sth pressure swing adsorber, into integrated form pressure swing adsorber 10
Pressure-variable adsorption is carried out, it is production among superelevation pure hydrogen that the gas that outflow is not adsorbed from top, which is formed by fluid phase gas,
Product, hydrogen purity are 99.999~99.9999% to be denoted as 5~6N, wherein 10 top and bottom institute of integrated form pressure swing adsorber
The pressure-variable adsorption regulating valve 9 of setting combines, and ensures to carry out slowly pressing with along putting in pressure-swing absorption process, prevents from becoming under high pressure
It presses through the too fast caused air flow method unevenness of journey, caused absorbent atomizing and leakage etc. is washed away to adsorbent and regulating valve 9
Phenomenon；Integrated form pressure swing adsorber 10 is formed by stacking by a hexahedron module unit, inside there is 6 sorption channels, channel
The compound adsorbent of built-in carrying active charcoal, silica gel, molecular sieve and selective absorption N2/CO is inhaled with meeting each sorption channel
It is carried out while attached, desorption process, ensures consecutive production.One sorption channel is being adsorbed, remaining 5 channel is desorbed.
When adsorbent reactivation, it is rinsed+evacuates combination using superelevation pure hydrogen intermediate products and desorbed；It rinses gas, evacuate
And inverse put is formed by stripping gas, a part enters the combustion gas feed pipe in catalytic burner 1 directly as combustion gas, one
It is allocated as being mixed with unstripped gas back to catalytic burner 1 for unstripped gas and enter into charging gas distribution plate mouth, a part is straight
Run in and puts；Superelevation pure hydrogen intermediate products pass through the decompression being arranged between integrated form pressure swing adsorber 10 and hydrogen purifier 12
Valve 11 enters hydrogen purifier 12, final electron level hydrogen product is flowed out from outlet end, purity reaches international semiconductor association
The product standard of the electron level hydrogen of SEMI defineds, hydrogen purity are more than or equal to 7~8N grades, wherein a part of hydrogen product
The regeneration carrier gas that adsorbent reactivation is carried out as integrated form pressure swing adsorber 10, by 10 top duct of integrated form pressure swing adsorber
On pressure-variable adsorption pressure reducing valve 11 enter regenerated, from 10 bottom pipe of integrated form pressure swing adsorber pressure-variable adsorption adjust
Valve 9 flows out regeneration gas, is connected with 1 combustion gas of catalytic burner and unstripped gas entrance by 10 bottom of integrated form pressure swing adsorber
The pipeline connect correspondingly enters catalytic burner 1 and carries out catalyst combustion reaction.
It will be apparent that embodiment described above is only the part in the embodiment of the present invention, rather than all.Base
In the embodiment that the present invention records, other all realities that those skilled in the art obtain without creative efforts
Example is applied, or the structure change made under the inspiration of the present invention, the technical schemes that are same or similar to the present invention,
It falls under the scope of the present invention.
Claims (10)
- The integral method of hydrogen recycling 1. a kind of manufacture of semiconductor gives up, which is characterized in that including following process：(1) catalysis burning, by the chemical vapor deposition or the useless hydrogen of doping or photoetching direct emission in manufacture of semiconductor Raw material is mixed with the high-temperature fuel gas ejected from the fuel gas jets of heating, at a high temperature of 800~1200 DEG C, is urged Change combustion reaction, the toxic ignitable components in unstripped gas are oxidized to harmless component, forms burning mixed pyrolysis gas；(2) spray washing, the burning mixed pyrolysis gas from catalytic combustion process, is washed by spray washing unit, will Water-soluble component dissolving in burning mixed pyrolysis gas, and solid particle therein is washed away to spray washing unit bottom, It is emitted with together with aqueous solution, forms the saturation gaseous mixture that temperature is less than 100 DEG C after spray washing；(3) aqueous vapor detaches, and the saturation gaseous mixture from spray washing, into moisture separator, water droplet is from the gaseous mixture of rising It disengages, adsorbed and formed big water droplet and be discharged by the filler loaded in moisture separator, the gaseous mixture for disengaging moisture is dry Gaseous mixture；(4) adsorption cleaning, the dry mixture from aqueous vapor separation process, into the absorption list being made of two concatenated absorbers Member loads one or more adsorbents in absorber, dehydration is further dried, the toxic gas that removing is not completely burned on a small quantity Component and burning are formed by oxynitrides not soluble in water, are purified gaseous mixture；Wherein, the first absorber is primary Property physical absorption is slightly purified, and water-soluble polar impurity and water are removed；Second absorber is that chemisorption carries out essence only Change, removes nonpolarity not soluble in water or the weak impurity composition of polarity；(5) pressure-variable adsorption, the purification gaseous mixture from adsorption cleaning process are inhaled by being pressurized to 1.0~5.0MPa into transformation Attached system will purify the impurity composition in gaseous mixture and adsorb, and it is hydrogen that the gas not adsorbed, which is formed by fluid phase gas, The superelevation pure hydrogen intermediate products that purity is 99.999~99.9999%, the adsorbent loaded in pressure swing adsorption system is using living One kind or more of property aluminium oxide, silica gel, activated carbon/load active component activated carbon, molecular sieve/load active component molecular sieve Kind, regeneration is rinsed or vacuumized using superelevation pure hydrogen intermediate products when adsorbent reactivation；Rinse gas or evacuation and inverse put It is formed by stripping gas, catalytic combustion process, a part or work are entered according to gas component, a part or directly as combustion gas Catalytic combustion process, a part or direct emission are returned to for unstripped gas；(6) hydrogen purification, the superelevation pure hydrogen intermediate products from pressure-variable adsorption process, at a temperature of 50~500 DEG C, directly Or the pressure needed for manufacture of semiconductor hydrogen is decompressed to by pressure reducing valve, by metal getter or palladium film or palladium film-metal The hydrogen purification process of getter coupling, operation temperature is 50~500 DEG C, operating pressure is normal pressure to manufacture of semiconductor hydrogen It is purified under required pressure condition, removes trace impurity, obtain final electron level hydrogen product.
- The integral method of hydrogen recycling 2. a kind of manufacture of semiconductor as described in claim 1 gives up, it is characterised in that： The fuel gas used in the catalytic combustion process is fresh hydrogen, natural gas, purified containing methane or hydrogen or nitrogen Manufacture of semiconductor exhaust gas, clean air and pressure-variable adsorption process stripping gas in it is one or more, fuel gas is using urging The waste heat of change burning process catalyst combustion reaction cavity imports reaction chamber again after being preheated.
- The integral method of hydrogen recycling 3. a kind of manufacture of semiconductor as described in claim 1 gives up, it is characterised in that： In the pressure-variable adsorption process, the regeneration carrier gas of adsorbent uses in the superelevation pure hydrogen that vapor, pressure-variable adsorption process generate Between product, hydrogen purification process hydrogen product in one kind；The fuel gas or spraying of regeneration carrier gas and catalytic combustion process are washed One kind in the saturation gaseous mixture of process or the hydrogen product of hydrogen purification process is washed, heat exchange is carried out and reaches 100~250 DEG C Regeneration temperature.
- The integral method of hydrogen recycling 4. a kind of manufacture of semiconductor as described in claim 1 gives up, it is characterised in that： The adsorptive pressure of the pressure-variable adsorption process is 2.0~5.0MPa, and the pressure change during adsorption and desorption circulate operation is led to Sequence valve and regulating valve on the pipeline connected between each sorption channel both ends are crossed, realization is slow to be controlled.
- The integral method of hydrogen recycling 5. a kind of manufacture of semiconductor as described in claim 1 gives up, it is characterised in that： The operation temperature of the hydrogen purification process depends on used palladium film, metal getter and palladium film and couples metal getter Process choice, palladium film and without activation or medium temperature activated form metal getter operation temperature be 50~100 DEG C, high-temperature activation The operation temperature of the metal getter of type is 300~500 DEG C, wherein the operating pressure under high temperature is less than 2.0MPa.
- The integrated apparatus of hydrogen recycling 6. a kind of manufacture of semiconductor gives up, it is characterised in that：It is urged including sequentially connected Change burner (1), spray jet scrubber (2), moisture separator (3), air blower (4), the first absorber (5), the second absorber (6), supercharger (8), integrated form pressure swing adsorber (10) and hydrogen purifier (12)；In the catalytic burner (1) is arranged to The inner tube of housing tube shape, catalytic burner (1) is arranged to combustion chamber, and gas distributing disc is arranged in the combustion chamber upper end Mouthful, combustion chamber lower end is connected to the top of spray jet scrubber (2), and the interlayer inner disc of catalytic burner (1) is wound with combustion gas disk Air inlet is arranged in pipe, the burning gas coil pipe lower end, and the upper end for the gas coil pipe that burns is connected to gas distributing disc mouth；The spraying is washed It includes spray chamber to wash device (2), and nozzle is arranged in the spray chamber inner wall；The bottom of the moisture separator (3) is washed with spraying The bottom for washing device (2) is connected with U-shaped connecting tube, wherein U-shaped connection bottom of the tube is equipped with particle suspension liquid and the collection of water is discharged Mouthful, escape pipe passes through the sequencing valve (7) on air blower (4) and the first absorber (5) bottom inlet pipe at the top of moisture separator (3) It is connected, the second absorber (6) is connected up and down with the first absorber (5), and escape pipe passes through sequencing valve on the first absorber (5) top (7) it is connected with the second absorber (6) bottom inflow pipe, escape pipe is by being arranged sequencing valve (7) and increasing at the top of the second absorber (6) Press (8) is connected with the regulating valve (9) on integrated form pressure swing adsorber (10) lower inlet pipe, integrated form pressure swing adsorber (10) Top escape pipe is connected by setting pressure reducing valve (11) with the inlet tube of hydrogen purifier (12), the hydrogen purifier (12) Outlet conduit and integrated form pressure swing adsorber (10) at the top of pressure reducing valve (11) on escape pipe be connected, integrated form pressure-variable adsorption Sequencing valve (9) in the bypass of device (10) bottom inflow pipe is connected with the fuel gas inlet pipe in catalytic burner (1).
- The integrated apparatus of hydrogen recycling 7. a kind of manufacture of semiconductor as claimed in claim 6 gives up, it is characterised in that： The nozzle setting of the spray jet scrubber (2) circularizes or semi-circular, and nozzle direction is in 40 obliquely and with spray chamber inner wall ~90 ° of angle.
- The integrated apparatus of hydrogen recycling 8. a kind of manufacture of semiconductor as claimed in claim 6 gives up, it is characterised in that： The water droplet reverse flow baffle or return duct of the collection floss hole for connecting U-shaped connection bottom of the tube are equipped in the moisture separator (3).
- The integrated apparatus of hydrogen recycling 9. a kind of manufacture of semiconductor as claimed in claim 6 gives up, it is characterised in that： First absorber (5) and the second absorber (6) integrated setting, are arranged to what a solid modular unit was formed by stacking Integrated form temperature swing adsorbers have at least four sorption channel in integrated form temperature swing adsorbers, adsorbent are loaded in sorption channel.
- The integrated apparatus of hydrogen recycling 10. a kind of manufacture of semiconductor as claimed in claim 6 gives up, feature exist In：The integrated form pressure swing adsorber (10) is formed by stacking by a solid modular unit, integrated form pressure swing adsorber (10) Inside there is at least two sorption channel, adsorbent is loaded in sorption channel.
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| JP2022501306A (en) * | 2018-09-29 | 2022-01-06 | 鼎佳能源股▲ふん▼有限公司 | Hydrogen recovery and regeneration system |
| JP7284530B2 (en) | 2018-09-29 | 2023-05-31 | 鼎佳能源股▲ふん▼有限公司 | Hydrogen recovery regeneration system |
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| CN112316713A (en) * | 2020-10-08 | 2021-02-05 | 中船重工（邯郸）派瑞特种气体有限公司 | System and method for stripping hydrogen from cathode tail gas in nitrogen trifluoride preparation process |
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| CN112827319B (en) * | 2020-12-23 | 2023-03-03 | 四川天采科技有限责任公司 | Chlorine-based SiC-CVD epitaxial tail gas full-temperature-range pressure swing adsorption hydrogen extraction and recycling method containing low-concentration silane and light hydrocarbons above carbon two |
| CN113233420A (en) * | 2021-07-02 | 2021-08-10 | 江苏鑫华半导体材料科技有限公司 | Method for purifying hydrogen for producing electronic grade polycrystalline silicon |
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