CN1818610A - System and method for measurement and/or analysis of particles in gas stream - Google Patents
System and method for measurement and/or analysis of particles in gas stream Download PDFInfo
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- CN1818610A CN1818610A CN 200610059229 CN200610059229A CN1818610A CN 1818610 A CN1818610 A CN 1818610A CN 200610059229 CN200610059229 CN 200610059229 CN 200610059229 A CN200610059229 A CN 200610059229A CN 1818610 A CN1818610 A CN 1818610A
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Abstract
A system and method for measuring and analyzing particles within a gas feed stream. In one aspect, the system comprises a particle counter and a particle capture filter that are arranged in parallel. In another aspect, the system comprises a purifying device to remove trace molecular impurities from a gas feed stream to reduce the presence of impurities.
Description
The cross reference of related application
The application require according to the application in 3 days February in 2005 of 35U.S.C. § 119 (e) regulation at first to file U.S. patent application serial number No.60/649,490 and on October 4th, 2005 application at first to file U.S. patent application serial number No.60/723,619 right of priority, its disclosure is quoted in this merging.
Technical field
The present invention relates in being used for the sample gas incoming flow to determine the system and method with characteristic of existing of the dirty right thing of this gas stream particle.Especially, the present invention relates in the system that comprises particle collector and particle capture filtrator, wherein useful is that this particle capture filtrator and particle collector are arranged in parallel.
Background technology
The user of many special gas such as manufacturers of semiconductor devices, requires suspended particle content in the low gas.For example, in manufactured materials, particulate pollutant causes low yield in the device fabrication and the integrity problem in the finished product semiconductor devices.Therefore, usually to following but be not restricted to its gas and the strict cleanliness factor of many other gases, such as Ar, He, N
2, Xe, Kr, Ne, SiH
4, SiH
2Cl
2, NH
3, BCl
3, CO
2, CO, N
2O, O
2, H
2, SiHCl
3, PH
3, AsH
3, BF
3, B
2H
6, Si
2H
6, SiCl
4
Particle level in the gas feed stream can change between following two kinds of situations: or relatively evenly and be stable stream, or, for example, when near utensil interface (tool interface), in the time cycle, change.Variation in the gas feed stream can be the form of breaking out attitude (peak), being (up or down) and/or step change (up or down) that drift about over time.In dynamic system, fill (transfill) system and utensil (tool) feeding line such as fluid transfer, circulate normal good mixing and uniform particles of this gas feed distributes.Yet in static system, such as gas bottle and gas supply container, fine grain level spatially changes with the order of magnitude.This particle changes owing to gravity settling and is diffused into the inside surface effect.These effects produce non-homogeneous Particle Distribution in supply container, comprise layering.
Before entering gas feed stream, reduce the pressure of bottled gas and gas in bulk through automatic regulating apparatus commonly used.For example, the decompression of gas feed stream can produce the formation of the particle level, impurity nucleation and the cohesion droplet that pass through adjusting gear " outflow " of increase.In some situation, can form the non-volatile residue of suspension.
Except the problems referred to above, if gas feed stream comprises reacting gas, such as silane, reacting gas can combine with air pollution and form the solid material (particle) that suspends.Silane and oxygen or oxidant reaction produce the silicon dioxide (SiO of particle form
2) powder.Think that in silane storage/induction system the moisture or the oxygen of any trace can produce a large amount of silicon dioxide microparticles.These solid reaction products can cause tangible inexactness in the measurement of any suspended particle content.This particulate continues to produce up to having exhausted oxygen or oxygenant and eliminated this oxidizer source in this system.Because the problem of these and other, for the feed gas stream that comprises reacting gas, perhaps careful attention detects and removes air pollution is necessary.
It is general because the existence of molecular impurity causes the formation of particle in the gas feed.Many semiconductor process gases are supplied in the container of pressurization.Generally comprise the molecular impurity of trace for these highly purified gases, such as the hydrocarbon in the nitrogen, in the silane siloxane and according to the impurity of other gas of high-pure gas composition.These impurity can by in pressurizing vessel, be used to make, the processing of conveying and stored-gas produces.The internal pressure of gas storage container and temperature are usually on the critical-point pressure and critical point temperature of this gas.For example, when being transported to the user, the temperature and pressure in the gas storage container surpasses N usually
2Critical point (492psia ,-232) and SiH
4Critical point (703psia, 26).As everyone knows, supercritical fluid is for the material such as the hydrocarbon of higher molecular weight, and it exists as surface contamination in gas delivery, storage and transfer system, has the high solvent ability.These dissolved impurities generally can increase the molecular impurity that exists in the gas.
In order to control state-variable that causes the particle contamination in the gas and the quality of guaranteeing gas, pressurized-gas source is carried out particle sizing accurately.Need to measure the particles suspended concentration in the gas-pressurized.Yet because the pressure limitation of available instrument, it is unpractical measuring granule content under the total head of storage container.Therefore, for gaseous tension being reduced to and the consistent level of available instrument that is used for actual measurement, can pass through reliever, for example automatic pressure adjuster, valve, throttling orifice plate etc. are carried gaseous sample.Can flow online or off-line measurement with respect to gas feed.
When step-down, contain the increase that the particle of the gas of trace molecular impurity can produce granule content, this is known in the particle sizing field.This deterioration is because the molecular aggregates of trace impurity causes forming the suspended particle of stable (promptly persistent).These particles can not be by heating evaporation easily.In addition, in some cases, frequent reduced pressure treatment produces undercritical conditions in gas.In this, along with pressure descends, subcritical gas has been lost its high solvent ability, and therefore any dissolved impurity tends to form the stable suspersion particle in sample gas stream.It is known forming particle during reducing pressure, and produces greater than 10 for the gas greater than 0.02 micron the every standard cubic foot of particle
6Particle level.This level is well beyond the actual particle level in the pressurizing vessel.Fig. 1 provides by flowing the example of the representative gases incoming flow 1 of reliever such as the valve 2 that 1 fluid is communicated with gas feed.Although gas feed stream initially comprises low-level gas and carries particle 3,, flow particle 4 increases of 1 grain amount that contains or " nucleation " at gas feed by behind the valve 2.The particle 4 of these nucleation is carried to the particle collector (not shown) in downstream in lower pressure gas stream 5.From measure, can not be identified in the actual granule density in the container.Therefore, decompression technology greatly reduces the accuracy of particle sizing.
The trial formerly that addresses this problem comprises the measuring body particle collector of structure.The feasible pressure that needn't reduce this instrument upstream sample gas of this kind instrument.Yet these instruments can not provide the composition of measurement particle and the information of form.
Similarly be that low-voltage instrument can be arranged in the compression chamber of customization (for example, excess air pressure chamber) and operate under near the source atmospheric pressure.Yet this scheme is expensive and is difficult to improve for the design of instrument, therefore produces practical problems.
Under the situation that need not state decompression, also can use pressure filter to catch from the particle in the sample flow.Then making ins all sorts of ways detects the particle of these seizure, such as optical microscope method, scanning electron microscope method, or in liquid medium with its digestion or dissolving, carry out the constituent analysis of liquid etc. subsequently.Yet, the false particle that these detection methods can not be distinguished the primary particles in gas supply source and form in sample system.
Before decompression, use various absorbing agents, adsorbent, catalytic cleaner and other purification plant well known in the art, can remove the molecular impurity that leaves a question open in the gas-pressurized.During reducing pressure, this method is known for fully reducing or eliminating particle formation.Yet this clarifier is that feed gas stream is operated by bed granular or ball shape purification medium.This bed also tends to as filtrator to remove the actual particle that flows out from pressurizing vessel or new particle can be incorporated into this air-flow from purification medium.Therefore, in the downstream of bed type clarifier, can not accurately be determined at the actual granule content in the pressurizing vessel.
During reducing pressure, attempt using heated air stream or heating reliever to stop impurity nucleation.In the gas stream that expands, this method is generally invalid for the formation that stops into nuclear particle.
Therefore, need in the art improved, reliably be used to measure and/system of particle in the analytical gas incoming flow, it was removed these molecular impurities before molecular impurity causes false impurity measurement effectively.
Summary of the invention
In one aspect, the invention provides a kind of measurement and/or endocorpuscular system of analytical gas incoming flow of being used for, this system comprises particle collector and particle capture filtrator, and wherein particle capture filtrator and particle collector are arranged in parallel.
In yet another aspect, the invention provides a kind of system that is used to measure lower pressure gas incoming flow endoparticle content, this system comprises in order to remove the purification plant that gas feed flows interior impurity and the gas feed stream of purification is provided, the reliever that is communicated with the purification plant fluid, the gas feed stream that wherein purifies flows with the gas feed that lower pressure is provided by reliever, measure the particle collector of the granule content in the lower pressure gas incoming flow, with the particle capture filtrator, wherein particle capture filtrator and particle collector are arranged in parallel.
In yet another aspect, the invention provides a kind of method that is used to measure lower pressure gas incoming flow endoparticle content, this method comprises the step that gas feed stream is flowed with the gas feed that purification is provided by purification plant, wherein purification plant is not removed the particle that comprises in the gas feed stream that purifies basically, and wherein gas feed stream is in first pressure.This method comprises that also the Purge gas incoming flow with a part imports reliever, be reduced to the pressure that is lower than first pressure and the Purge gas incoming flow by will being in this part under the pressure that is lower than first pressure by particle collector with the Purge gas incoming flow of another part is measured the step of the granule content that comprises in the gas feed stream of purification by the particle capture filtrator with pressure with the Purge gas incoming flow of this part.Particle capture filtrator and particle collector are arranged in parallel.
Description of drawings
By the accompanying drawing of the present invention (wherein same numbers representative similar elements) of reference disproportional, those skilled in the art will be better appreciated by a plurality of advantage of the present invention, wherein:
Fig. 1 is the synoptic diagram by the general gas feed stream of reliever;
Fig. 2 is the sketch map according to the system of one embodiment of the invention, is described to the system of off-line sampling system at this;
Fig. 3 is the sketch map according to the system of another embodiment of the invention, is described to the system of off-line sampling system at this;
Fig. 4 A-C is the synoptic diagram of several embodiments of one aspect of the present invention; With
Fig. 5 is SEM microphoto and the EDS spectrum by the particle of system of the present invention seizure.
Embodiment
The system and method that can be used for measuring and/or analyzing the particle in gas feed stream in this description.This system and method can be used for determining for example number of particles or grain count; The concentration and density of the particle in the gas feed stream; Particle size distribution, particle shape; And/or particle is formed.Detectable particle mean size scope can be from 0.02 micron (μ m) to 10 μ m in this gas feed stream, or from .05 μ m to 1 μ m, or from 0.1 μ m to 1 μ m.Detectable average grain number can be scope from 1/sq.ft. (sq.ft.) to 10,000,000/sq.ft., or from 1/sq.ft. to 10,000/sq.ft., or, 000/sq.ft from 1/sq.ft. to 1.
This system and method can be used for all gases and supercritical fluid incoming flow, comprises pyrophorus, fire goods, oxygenant, mordant and inert gas.The example of analyzable gas feed stream includes but not limited to: electronics special gas (" ESG "), such as, inert gas (for example, Ar, He, N
2, Xe, Kr, Ne etc.), SiH
4, CF
4, WF
6, SiH
2Cl
2, NH
3, NF
3, Cl
2, BCl
3, C
2F
6, CO
2, CO, F
2, N
2O, CHF
3, O
2, H
2, HBr, HCl, HF, CH
4, SiHCl
3, SF
6, PH
3, AsH
3, BF
3, B
2H
6, Si
2H
6, SiCl
4, SiF
4And many other gases.Term " gas " comprises steam, supersaturated gas and supercritical fluid.The example of concrete supercritical fluid provides in the disclosed U.S. application 2004/0144399 of pending trial, and it is incorporated herein in full and is for reference.For example, this system can be used for measuring and/or analyzing various particles, and it can comprise, for example, and molecular cluster, drop, metallic suspended solids, organic or other material and various other contamination particle.
Particle in handling the gas stream typical sample is measured and analyzed in this system described here by using particle collector and particle capture filtrator.This system can not add or remove from this gas feed diffluence the particle of significant number.This disturbs and can change the granule density of measuring in this sampled gas feed stream.In certain embodiments, can use the pipeline of electropolishing and/or abrasive bottom valve to reduce the sample deviation.In addition, in the embodiment of these and other, this system makes particle because gravity settling or because the molecular brownian motion effect is diffused into the conveyance loss of the particle that tube wall causes minimizes.
This system described here can or have the tributary or the extraction system of sample flow is used in combination with the continuous processing incoming flow that is described as " off-line sampling " at this.This system described here can be used in combination with a kind of gas sample extraction equipment of the dynamic sampling probe such as so-called grade that inserts this feed gas pipe that comprises as known in the art.In this connected, (that is, the stylostome that is suitable for conveying gas in bulk that is provided with in single integrated unit extract the separated flow of sample in) the processing gas pipeline out, it referred to gas feed stream at this from gas cylinder or ISO cabin.The off-line sampling system may need exhaust or flow through particle collector or other emission control form of the gas feed of particle capture filtrator stream.Gas feed stream comprises reacting gas in embodiments, the off-line sampling system can further comprise the subsystem (promptly using one or more this flues of inert gas purge) that inert purge is provided, discharger (promptly using one or more vacuum pumps to discharge the pipeline of gas), and/or emission control.In other embodiments, for example when gas feed stream comprises the gas of easy condensation (temperature or when being higher than environment temperature gas become liquid), also can accompany heat to the systematic pipeline and/or the system unit that comprise at this.In these embodiments, before introducing gas feed stream in the pipeline.Because gas can with trace residue moisture or the oxidant reaction in the pipe, come dry starter system so companion's heat can be used in combination (promptly use pressure change) with inert gas purge and/or pressure cycling.
Fig. 2 provides the example according to an embodiment of the off-line sampling system of the particle that is used for measuring and analyze the gas stream that contains silane of the present invention.In certain embodiments, such as depicted in figure 2, system 10 is placed in the exit casing and in environment temperature.Can provide gas feed stream 25 from source of supply 20 such as hold-up vessel, pressurized cylinder, transfer filling pipeline (transfill line), gas service pipes line or other device (not shown).Source of supply 20 can be big or little volume.Removal flows 25 from the portion gas at least of source of supply 20 so that the gas feed that adds by sampling system 10 to be provided.General according to for example source of supply volume, the characteristic of gas feed stream 25, whether the gas that wherein comprises in supercriticality etc., from 4psia to 10,000psig, or from 0psig to 3,000psig, or from 100psig to 1, the pressure limit of 600psig is incorporated into system 10 with gas feed stream 25.System 10 further comprises inert gas source 30, and itself and system's 10 fluid connected sums are used for inert gas purge and others.Inert gas purge device 35 is connected to be provided for the purification inert gas of purge/flushing operation with inert gas source 30 fluids.
In the embodiment of the gas feed stream 25 that contains silane, before introducing gas feed stream, implement the inert gas purge, carry out one or more discharge circulations thereafter.Still with reference to Fig. 2, by shut-off valve V9 and V19 with open valve V7 and V8 implements the inert gas purge.After analytical gas incoming flow 25, move the inert gas purge in a similar fashion to remove any residual silane from this system.By shut-off valve V8, V9 and V19 with open valve V7 and implement to discharge circulation.
The embodiment described among Fig. 2 use particle collector 50 and/or such as the particle capture filtrator 60 of membranous type filtrator with measure and the detected gas incoming flow in particle.Can connect particle collector 50 to the gas feed source by a plurality of pressure governors.Regulate flow velocity by flow control valve and dense-phase flow amount meter by device.In certain embodiments, system is working near under the atmospheric pressure.The pressure of the gas feed stream 25 that in these embodiments, between source of supply 20 and particle collector 50, may need to reduce to introduce.Shown in figure 2 in the system, use two pressure governors 52 and 54 that are arranged in series to carry out decompression with two steps.This multistep die-offs to press and makes tendency takes place during reduced pressure treatment particle flow out gentle body condensation to minimize.In other embodiments of the present invention, can use the single stage decompression.In other embodiments, the gas feed that does not perhaps need to be lowered into particle collector 50 because pressure is enough low flows 25 pressure.
In other embodiment preferred of the present invention, particle collector 50 is measuring body or is encapsulated in (not shown among Fig. 2) in the compressive sealed container.When instrument or airtight container can be kept out whole pressure of gas source 20, do not need the sample flow that reduces pressure.In this embodiment, do not need pressure governor 52 and 54 accurate measurements with the suspended particle content that obtains gas stream.
The example that is fit to the suitable particle collector 50 of using system 10 is the particle sizing system (PMS) that is made by Boulder company.The PMS of Model Micro LPC-HS company can detect has the little particle to 50nm of equivalent light scattering diameter, and the HeNe laser instrument that uses 633nm is at 80nm counting efficiency＞80%.The sample flow speed of appliance requires per minute 0.1 standard cubic foot (SCFM) or per minute 2.8 standard liters (SLPM).Micro LPC-HS has＜2/ft
3, perhaps＜0.2/ minute zero count level can be measured up to 80 000/ft
3Granule density.Instrument has the channel that threshold value is 8 sizes of 50,100,150,200,300,500,700 and 1,000 nanometer (nm).Sampling interval can be provided with in 1 second to 100 hours scope.
In some preferred embodiment, particle collector 50 is optical particle counter (OPC), and it allows grain count in real time automatically and allows the spurious counts of direct, real-time identification by for example silane and residual moisture and oxygen reaction generation.These reactions may be caused by the insufficient purge/drying of sampling system during the sampling process startup.After reaching the steady state (SS) particle level of system, may resist this by the real-time counting ability of using OPC and break out state.
When not using particle collector 50, can itself and system be isolated by shut-off valve V1 and V2.This allows particle collector 50 to keep avoiding polluting, otherwise it can enter into system.
In a preferred embodiment of the invention, when removing these sections counting from system, particle collector 50 combines so that assay method to be provided with capture filter device 60.In this embodiment of the present invention, can simultaneously or in a sequence gas feed stream introduction particle collector 50 and capture filter device 60 be measured.Such as, at first gas feed stream 25 is introduced particle collector 50, then the part of gas feed stream 25 is introduced capture filter device 60, with the result who confirms that particle collector 50 observes, and further characterizing particles as described below.The capture filter device of only isolating in these embodiments, the gas feed stream 25 that is exposed to introducing then.
In a preferred embodiment of the invention, capture filter device 60 has two devices 71,72, and its permission is removed capture filter device 60 from system.When shut-off valve V3, V4, V17 and V18, can easily capture filter device 60 be removed by installing 71,72.
In case remove the particle that capture filter device 60 is collected from system 10, it just can be by the methods analyst below using.At first, preferably separate in capture filter device 60 lip-deep background impurities (promptly being exposed to the pollutant that exists on capture filter device 60 surfaces before the gas feed stream 25) with sample contaminant.Typically during filtrator manufacturing and processing procedure, produce background impurities.In this, must detect and estimate the superficial density of the background impurities on the filtrator 60 with the particle capture method.Microscopy is used for determining the quantity of the background particle on non-exposure filtrator.This can be realized by the part of only checking filter surfaces.Check the part A in filter surfaces zone
B, to obtain the quantity N of background particle in that zone
BBehind exposed sample gas or supercritical fluid, check surperficial area part A
P, to determine in that zone the total quantity N of background and seizure particle
PAt the total quantity N of the whole lip-deep seizure particle that exposes filtrator, following drawing:
N＝A(N
P/A
P-N
B/A
B)，
Wherein A is the total surface area of filtrator.If V is sample gas or the volume that passes through the supercritical fluid of exposure filtrator, following the drawing of per unit volume granule density C of sample so:
C＝N/V.
In some embodiments of the present invention, vacuum pump 70 is used for from low pressure source draw samples fluid.Sample fluid enters emission control 80 then by particle collector 50 or capture filter device 60 before by vacuum pump 70.Emission control 80 and one or more burner 90 can comprise for example gas recovery system, combustion system, blowdown system, air-washing system, adsorption system, absorption system, or purification and storage system.These systems are known in emptying stream exhaust control field.
In certain embodiments of the invention, capture filter device 60 can be track etching filtrator (tracketch filter) or Woelm Alumina filtrator.Be different from OPC, do not have the upper limit at capture filter device aspect measurable granule density.Polycarbonate track etching filter film can obtain in little aperture as 15nm.The aluminium oxide filter film can obtain in little aperture as 20nm.The more high density holes of aluminium oxide filtrator provides minimum fluid resistance in high flow rate.High fluid rate in minimum time is of value to a large amount of gases of sampling.Particle capture filtrator 60 can be encapsulated in the housing of resistance to compression filtrator such as the Bedford by Milliore company, the xx4502500 25mm stainless steel filter housing that MA makes.Filter body comprises filter film, wherein uses various elastomeric materials such as teflon
TMO encircles sealing.This filter film is used for comprising at different gases at high pressure as seizure the particle of silane.On filtrator, catch after the particle in the gas feed stream, can use various technology such as, but be not limited to, light microscopy, SEM and EDS come analysing particulates.
In a preferred embodiment of the invention, particle capture filtrator 60 can be that the chemically-resistant filter media is such as teflon
TMMicroporous barrier.Because their thick surface structure, this film are not suitable for EDS or displaing microparticle check.Yet, by analyzing particulate component and total seizure amount of on this filtrator, catching in digestion in various acid or the solvent or dissolving.Comprise that by various known methods liquid chromatography analyzes described acid or solvent then.
Generally by the working pressure meter for example membranometer measure the pressure of the gas feed stream of in system 10, introducing 25.In the system of in Fig. 2, describing, the sample incoming flow is sent in combustion in situ device or 90.Yet, characteristic according to feed gas stream 25, also the sample feed gas can be discharged, regained or send into (not shown) in emission control 80 or adsorber, absorber (absorper), scrubber, clarifier and the storage system, perhaps be circulated to main gas feed supply (not shown).
Usually the speed of the sample gas stream of passing through particle collector or particle capture filtrator is controlled and monitored to use traffic controller 120 in test process.Flow controller 120 can comprise manual flowrate control valve and flowmeter such as mass flowmeter, and perhaps flow controller 120 can comprise that the flow controller that starts automatically is such as mass flow controller.The sample gas downstream that comes from flow controller 120 can be discharged by fluid line 140, and it also is communicated with vacuum pump 70 fluids.
In a preferred embodiment of the invention, air operated valve can be isolated with the clean internal member of system when not using.Before each sampling operation, use processing logic controller (PLC) (not shown) automatic sequence to carry out circulation purge and sampling operation.PLC receives input from pressure transmitter and the hot temperature controller of companion to guarantee that vacuum pressure circulates in the restriction of appointment during operation.In certain embodiments, heat tracing pipe remains on 100 ℃ during the circulation purge.During the circulation purge with system evacuation to＜50 the holder and turn back to atmospheric pressure at least 150 times.
With before getting rid of atmosphere and after any residual gas of sampling removal, use the inert gas rinse-system that purifies at the circulation purge.According to the characteristic of gas to be sampled, such as when sample gas comprises silane, flush cycle can be sent into these gas such as recovery system, burner or scrubber.In other embodiments, flush cycle can be discharged to atmosphere with gas.When system is connected with the gas feed source, with afterwards, carry out purge operation before the sampling process.The sample source valve cuts out during the inert gas flushing operation.Comprise in the embodiment of silane at sample gas, purge gas is sent into silicone hydride combustion device, recovery system or scrubber.The purging process also can be used for purge and goes out (purge-out) silane source coupling arrangement when system and silane source disconnect.Purge is to be used for stoping pollutant to enter into open sampling system.Inert gas will be discharged to atmosphere by the silane inlet tube.
In the preferred embodiment that the present invention such as Fig. 2 describes, comprise that companion's heat is with the traces of moisture in the minimization system.In these embodiments, all system components (referring to thick line among Fig. 2) of preferred particulates counter and particle capture filtrator upstream are companion's heat.Companion's heat comprises the resistance heated parts that can be fixed to such as the outer surface of system pipes, valve, filter body, pressure governor and miscellaneous part.Companion's heat comprises temperature sensor, such as providing Temperature Feedback to temperature indicator (TI) with such as the thermopair of the temperature controller of processing controller or temperature relay.Temperature controller comprises and is designed for the circuit of regulating heater block power, to be used for design temperature in the maintenance system.This heating is used for eliminating fast the traces of moisture from system's inside surface absorption, after checkout procedure, allows to remove the trace residue sample fluid from system.In certain embodiments, system 10 can use the water analysis instrument 100 of the residual moisture that can detect in the pipeline, and if for example in the gas feed stream moisture exceeded the expection level and can drive various valves.In this or other embodiment, system 10 can use lambda sensor, works in a similar fashion with the water analysis instrument aspect the oxygen that it exists in the detected gas incoming flow.
In other preferred embodiment of the present invention, can use method and system described here to be reduced to the lower pressure gas incoming flow and can not form particle subsequently with gas feed stream that purification is provided and the pressure that flows with the gas feed that will purify by under elevated pressures, using one or more clarifiers to remove trace impurity from the gas feed diffluence.The Purge gas incoming flow of having passed through reliever described in term " lower pressure gas incoming flow " as used herein, such as hard-core, and automatic pressure controller, valve, throttling orifice plate or analog.Pressure with the initial gas incoming flow after purifying is reduced to the level consistent with the instrument that is used for particle sizing.For example, in one embodiment of the invention, gas feed stream can be scope from 150 to 10, the original pressure of 000psig.The pressure of the dropping equipment nearly materials flow of gas that reduces to purify is to from 0 to 150psig pressure limit then.Can change pressure limit described here according to type, granulometer and/or its dependent variable of the dropping equipment of the original pressure of gas feed stream, use.
Term " Purge gas incoming flow " is described by the gas feed stream with the one or more purification plants that remove the various impurity that wherein comprise as used herein.The system and method for describing does not influence unfriendly such as causing that the granule content of gas feed stream increases by dropping equipment.In certain embodiments, the granule content of Purge gas incoming flow is with basic identical by the granule content of the stream of the gas feed before the purification plant.
Refer to be present in the fraction of the polluter in the initial gas incoming flow at this term " impurity ", according to gas feed stream composition, for example but be not restricted to siloxane, hydrocarbon, moisture and other pollutants.In certain embodiments, being present in impurity in the gas feed stream is siloxane in the silane gas incoming flow or the hydrocarbon in nitrogen and/or the silane gas incoming flow.As used herein purification plant be a kind of remove fully be included in gas feed stream (such as volume about 5% and below, perhaps volume about 1% and below, perhaps volume about 0.01% and following) in all impurity and the chemical composition of gas is not had the instrument of adverse effect.In certain embodiments, purification plant is the granule content of materially affect gas not, does not perhaps have removal basically or adds particle to the gas feed stream that purifies.In these embodiments, the granule content of the granule content of Purge gas incoming flow and initial gas incoming flow (just 10% of amounts of particles with interior or 5% with in interior or 1%) basic identical.The Purge gas incoming flow is flowed with the gas feed that lower pressure is provided through dropping equipment then.Gas feed stream with lower pressure is sent to particle collector then.
Referring now to Fig. 3, another preferred embodiment of system of the present invention has been described.The system of Fig. 3 is except comprising that the system of Fig. 3 is similar with the system of Fig. 2 (wherein identical numeral refers to identical parts) with the impurity purification plant 700 such as molecular impurity in the removal gas feed stream 25.The purification plant 700 that the system and method for this description uses can be for example diffusion type gas-solid phase separator, cold-trap, or both.Also diffusion type gas-solid phase separator and downstream dropping equipment are not used in combination in the prior art with as the device that purifies the dedicated processes gas of under elevated pressure, operating, and/or during the gas expansion process, are used to stop trace molecular impurity nucleation.Similarly, to be known conduct remove the device of impurity from streaming flow to cold-trap in gas technology, and cold-trap generally is not used in as the device of removing impurity from pressurized stream before decompression, during reducing pressure also not as stoping granuloplastic device.
In one of preferred embodiment of the invention, purification plant 700 is diffused gas-solid phase separators, central gas-solid phase separator 710, annular air solid phase separation vessel 720 and the fin-shaped gas-solid phase separator 730 that settle dropping equipment 52 upstreams of describing respectively such as Fig. 4 A, 4B, 4C.In certain embodiments, then can use lower pressure gas incoming flow 25b to flow to Fig. 2 and Fig. 3 mesolow grain count instrument 50 with sampling.
In impurity and particle detection field, diffused gas-solid phase separator refers to that here " diffusion type gas-solid phase separator " is known.This quasi-instrument generally is used for atmospheric sampling or other do not change airborne particulates content and the application of needs removal molecular impurity.They are also gone up to be used for the facility of later analysis as the trace molecular impurity is collected the surface from air sample.This quasi-instrument generally is designed to use under the situation of atmospheric pressure and temperature, and the gas that proof can be removed more than 99% carries impurity.Diffusion type gas-solid phase separator is a tubular type fluid instrument, and it utilizes the higher diffusivity of molecular impurity that impurity is removed from gas feed stream, and the not obvious suspended particle content that influences.Conventional granulates in gas feed stream has the diffusivity lower than conventional molecule.This mainly be since the size of particle basically greater than molecule.For example, 0.02 micron particle only has 0.019cm in nitrogen
2The coefficient of diffusion of/s (because the low mobility of bulky grain in gas itself even have littler coefficient of diffusion).By contrast, the conventional coefficient of diffusion numerical value of molecular impurity is bigger.For example, water has 0.22cm in air
2The coefficient of diffusion of/s.Therefore, the suspended particle trend is followed flowing gas, and the easier surface that is diffused into of molecular impurity trend.
In a preferred embodiment of the invention, purification plant 700 is diffusion type gas-solid phase separators, and it removes all molecular impurities and particulate that not obvious removal wherein comprises basically from gas feed stream.The variable that is used for influencing the gas feed stream endoparticle clearance before the step-down comprises the hydraulic radius of gas flow rate, gas-solid phase separator length and instrument.In diffusion type gas-solid phase separator, the impurity in the gas feed stream is exposed to chemical reaction surface, comprises absorbing agent or other purification mediums behind sieve formula or the porous barrier.Baffle design becomes physically to comprise purification medium granular or the ball shape, directly passes through dielectric layer to stop gas stream.As a result, impurity be retained in the purification medium and the remaining feed gas that pass through medium as the feed gas of purification.It is used for removing moisture impurity from air in an object lesson of diffusion type gas-solid phase separator, and the purification medium in diffusion type gas-solid phase separator is made up of drying material, for example Drierite
TM, this drying material is round the gas feed stream that comprises air and by tubulose stainless steel sift and air insulated.Drierite around moisture is diffused into from air by sieve
TMAnd with its removal.In another example of traditional gas-solid phase separator of removing ammonia impurity from aeriferous gas feed stream, purification plant is a glass flow, and its inside applies with absorption of N H from gas feed stream with oxalic acid
3Impurity and do not influence its granule content.
In a preferred embodiment of the invention, can form by various known adsorbents, absorbing agent or catalyst material, such as acticarbon, drying agent (Driefite for example such as the purification medium in the purification plant of gas-solid phase separator
TM), phenol resin (Ambersorb for example
TM), Raney nickel, copper catalyst etc., it becomes to assign to select according to dopant type to be removed and/or gas feed stream.In the example of system described here, by Ambersorb
TMThe purification medium that ball is formed is contained in the big envelope of being made up of sealed at both ends stainless steel screen casing, and gas feed stream flows through around it.For example, in the embodiment that Fig. 4 A (with respect to Fig. 2 and Fig. 3, identical numeral refers to identical parts) illustrates, contain the gas feed stream 25 of particle 430, under 1400psig pressure, comprise SiH such as a kind of
4Gas feed stream, for example, by before the dropping equipment 52 by central gas-solid phase separator 710.In this specific embodiment, for example, central gas-solid phase separator 710 can be from initial SiH
4Remove impurity such as siloxane and trace amounts of carbon hydrogen compound in the gas feed stream, allow the actual particle of initial generation in pressurization reservoir vessel (not shown) unhinderedly to pass through simultaneously.For example, central gas-solid phase separator 710 can comprise the tube screen of 1/4 inch diameter or several tube screens that this type of is connected and vertically arranges of scheme as an alternative in the pressurized gas lines of 1/2 inch diameter.Use high-purity automatic pressure controller (not shown), SiH
4The pressure of gas feed stream can be reduced to lower pressure gas incoming flow 25b, such as, 80psig.The SiH that contains particle 430
4The lower pressure gas incoming flow of 25b can flow into conventional low pressure grain count instrument (not shown).
In another preferred embodiment of the present invention, the purification medium of being made up of granular activated charcoal comprises the restraining barrier that the tubulose stainless steel sift is formed such as annular air solid phase separation vessel 720, and this stainless steel sift is flow through in the initial gas incoming flow.For example, in a specific embodiment, as shown in Fig. 4 B, under 2000psig pressure, comprise that the initial gas incoming flow 25 of nitrogen can be passed through annular air solid phase separation vessel 720 before by dropping equipment 52.In this embodiment, annular air solid phase separation vessel 720 is from initial N
2The gas feed diffluence removes the impurity that leaves a question open, and such as moisture and trace amounts of carbon hydrogen compound, allows the actual particle of original formation in pressurization reservoir vessel 20 to pass through in the clear simultaneously.In a specific embodiment, annular air solid phase separation vessel 720 can comprise the tube screen of 1/4 inch diameter or several this type of tube screens that series connection is vertically arranged in the pressurized gas lines of 1/2 inch diameter of scheme as an alternative.Working pressure dropping equipment 52 is such as the fluid throttling orifice plate, then the N of Jing Huaing
2The pressure of gas feed stream can be reduced to 0psig.The lower pressure gas incoming flow 25b that contains particle 430 can flow into conventional low pressure grain count instrument (not shown).
Being included in the purification medium that comprises behind the porous restraining barrier and other similar solids that are positioned at suitable dropping equipment upstream can be used among the system and method described here.For example these solids can be made up of the flat bag that the purification medium that comprises in sieve type or porous restraining barrier is formed, and are inserted within the gas line upstream of decompression instrument.
In the another one embodiment, in order to be provided for exposing the facility of gas feed stream 25, purification plant comprises the granular or ball shape purification medium that is fixed to the surface that exposes in the pressurized gas lines, for example the annular air solid phase separation vessel 720 as describing among Fig. 4 B.Use the adhesives mounting medium that is fit to.In this embodiment, do not need the restraining barrier with from the gas feed flow point from described medium.The example of another embodiment has been shown in Fig. 4 C, wherein purification plant is a fin-shaped gas-solid phase separator 730, wherein purification medium is fixed to the inwall of gas line or other inside surface of scheme as an alternative, such as flat fin, baffle plate, container etc., providing high surface area to be used for Impurity removal, do not hinder the conveying of the airborne particulates 430 that wherein comprise simultaneously or before decompression to guarantee accurate particle sizing.
In certain embodiments, system and method described here can allow the replacement or the regeneration of purification medium.Can use in gas purification field known method and realize regeneration, such as, but be not restricted to, be exposed to high-purity inertia regeneration gas at elevated temperatures.Realize replacing by remove gas-solid phase separator material or whole central gas-solid phase separator from gas line.
In another embodiment, purification plant can comprise that the sub-cooled trap of higher congealing point/solidifying point impurity does not influence the granule content in the fluid to remove impurity before decompression.
With reference to Fig. 2 and 3, system 10 can use a computer 110, for example, and itself and particle collector 50, PLC or other system element electric connection.Computing machine 110 can be operated some valve with parameter (that is, granule density, pressure, temperature, moisture, the oxygen content etc.) automatic operation system in flowing based on some gas feed in system.In preferred embodiments, system 10 also can use the sensor (not shown) of the grain amount in the measurement gas incoming flow, with the controller (not shown) that is communicated with sensor electrical, if sensor surpasses the point of setting at the grain amount of certain point measurement like this, sensor indication sample flow inlet valve cuts out so.
According to the present invention, the method for optimizing of measurement gas incoming flow endoparticle content comprises a plurality of steps that purification plant flows with the gas feed that purification is provided of passing through with the gas feed stream of at least a portion, wherein this gas feed stream is under first pressure, the particle that the gas feed stream that purification plant remove to purify basically includes.Then, for example, the Purge gas incoming flow of a part is incorporated in the dropping equipment with the pressure with the Purge gas incoming flow of this part is reduced to the pressure lower than first pressure.Then, the Purge gas incoming flow that pressure is lower than this part of first pressure is introduced particle collector and the particle capture filtrator is introduced in the Purge gas incoming flow of another part measured the granule content that the gas feed stream of purification includes, and is arranged in parallel at this particle capture filtrator and particle collector.
Based on the checking of following embodiment, other purposes of the present invention, advantage and novel characteristics are conspicuous for those skilled in the art, but the invention is not restricted to these embodiment.
Embodiment
Embodiment 1
The particle collector system of type shown in Fig. 2 and Fig. 3 is connected to various compressed gas cylinders.In native system, use compressive resistance and corrosion particle collector [particle sizing system (PMS), Inc.Modol CylinderGas System (CGS) M100].Therefore, the instrument upstream does not need to reduce sample strain.This apparatus measures is little in gaseous sample stream to be 0.16 micron suspended particle to size.With 19 actual cm
3The low rate of/min is extracted sample gas from each bottle, and by this instrument.In these tests, do not use the particle capture filtrator.The instrument upstream is not carried out sample gas and is filtered.Usually companion's heat of using 50 ℃ of sample lines is with the formation that minimizes droplet in the condensable gases and keep low moisture content in the sample hose.In the decompression of instrument downstream sampling gas, flow speed control, slow down and discharge facility.Before sampling, sampling system is circulated pressurization and heating to remove atmospheric impurities.At circulation pressurization back gas at least 57 standard liters (the 2 standard ft that from each test bottle, sample
3) gas.Test result is as shown in table 1.
Use the present invention, do not have the interference in external contamination thing, particle formation or other out of true sources during the low granule density under each kind situation has proved and measured.
Table 1 is measured the concentration of 〉=0.16 micron particles in pressurized cylinder
| Gas | Bottle is pressed | Particle/standard liter |
| CHF 3 | 580 | 0 |
| C 2F 6 | 590 | 0 |
| He | 2640 | 0 |
| H 2 | 2525 | 0 |
| HCl | 632 | 0.18 |
| N 2 | 2100 | 0 |
| N 2O | 400 | 0.13 |
| SF 6 | 274 | 13 |
| CF 4 | 1770 | 3.7 |
| Ar | 2655 | 0.25 |
| Cl 2 | 96 | 0.33 |
| NF 3 | 1450 | 0.044 |
| NH 3 | 135 | 0.030 |
| O 2 | 2651 | 2.2 |
| SiH 4 | 766 | 0.047 |
Embodiment 2
To be connected to compression SiH in the grain count system of type described in the present patent application
4(silane) gas cylinder.The filtration of sample gas is not carried out in the upstream of instrument or particle capture filtrator.Usually companion's heat of using 50 ℃ of sample lines is to keep low moisture content in the sample hose.In the control of the downstream sampling gas stream of particle collector and particle capture filtrator with slow down.Before sampling, sampling system is circulated pressurization and heating to remove atmospheric impurities.
In this system, use compressive resistance particle collector [particle sizing system (PMS), Inc.ModolCylinder Gas System (CGS) M100, Cylinder Gas System, Inc., Boulder Co].Therefore, instrument upstream sample pressure does not need to reduce.This apparatus measures is little in gaseous sample stream to be 0.16 micron suspended particle to size.With 19 actual cm
3The low rate of/min is from 776psig SiH
4Extract sample gas in the bottle, and it is passed through this instrument.In gas, only measure the granule density of every standard liters 0.047.Use the present invention, this low granule density proof does not have the interference in external contamination thing, particle formation or other out of true sources in test macro.
In test macro, also use the particle capture filtrator external member of compressive resistance and corrosion.The capture filter device is made up of the Whatman polycarbonate trace-etching-film of the 3.8cm diameter with 0.1 micron hole.Sample SiH
4Flow through from bottle with approximate 1 standard liters of per minute.Sampling was approximately carried out 362 minutes.So SiH of about 362 standard liters
4The gross sample volume by the particle capture filtrator.
Then under field emission SEM (FESEM) with 50,000 * magnification particle tested capture filter device.Carry out the SEM test by check point in the manual propelling raster pattern by filtrator.Detect totally 901 points at filter surfaces.Total area of detection is about 0.0015% of the filter surfaces that exposes.Use X-ray energy spectrum analyser (EDS) to determine four kinds of components of the surface particles of observation.SEM figure and the EDS spectrum of surface particles are shown in Figure 5.Data showed that before SEM and EDS detect the coating by the platinum of capture filter device causes surface particles.In detection, do not find other grain type.
These detections show the composition of the lip-deep particle that can obtain to be exposed to response sample gas, use the present invention can measure sources of particles.The also enhanced granule counter observation of EDS data, this shows at SiH
4A small amount of intrinsic particle is arranged in the sample flow.
Be limited to those of claim definition with the description of previous embodiment and preferred embodiment as an illustration, rather than with the present invention.Should be clear, do not break away from the scope of setting forth in the claim.The present invention can utilize the various variations and the combination of above-mentioned feature.These change does not regard the disengaging the spirit and scope of the present invention as, and all these classes variation intentions are included in the scope of claim subsequently.
Claims (26)
1. measure and/or the endocorpuscular system of analytical gas incoming flow for one kind, this system comprises:
Particle collector; With
The particle capture filtrator, wherein particle capture filtrator and particle collector are arranged in parallel.
2. the system of claim 1, it further comprises the purification plant that the Purge gas incoming flow is provided, wherein purification plant is not removed the particle that the Purge gas incoming flow includes basically.
3. the system in the claim 2, wherein purification plant comprises diffusion type gas-solid phase separator, cold-trap, perhaps the both comprises.
4. the system of claim 1, it further comprises microprocessor, described microprocessor at least with the particle collector electric connection.
5. the system of claim 1, it further comprises vacuum pump.
6. the system of claim 1, it further comprises the sample line tracing system, described tracing system comprise temperature sensor, heating source and with the controller of temperature sensor and controller electric connection.
7. the system of claim 1, it further comprises moisture analyzer.
8. the system of claim 1, it further comprises emission control system.
9. the system of claim 1, it further comprises at least one inert gas entrance system.
10. the system of claim 1, it further comprises the sensor of measurement gas incoming flow endoparticle amount; With
The controller that is communicated with sensor electrical, if so that the sensor measurement grain amount is higher than set amount, sensor indication sample flow inlet valve cuts out so.
11. a system of measuring low-pressure gas incoming flow endoparticle content, described system comprises:
Purification plant is to remove the interior impurity of gas feed stream and to provide the gas feed of purification to flow;
The dropping equipment that is communicated with the purification plant fluid, the gas feed that wherein purifies stream flows so that the gas feed than low pressure to be provided by dropping equipment;
Particle collector, it measures the endocorpuscular content of low-pressure gas incoming flow; With
The particle capture filtrator, wherein particle capture filtrator and particle collector are arranged in parallel.
12. the system of claim 11, wherein purification plant comprises diffusion type gas-solid phase separator, cold-trap, or the both comprises.
13. the system of claim 11, it further comprises at least the microprocessor with the particle collector electric connection.
14. the system of claim 11, it further comprises vacuum pump.
15. the system of claim 11, it further comprises the sample line tracing system, described tracing system comprise temperature sensor, heating source and with the controller of temperature sensor and controller electric connection.
16. the system of claim 11, it further comprises moisture analyzer.
17. the system of claim 11, it further comprises emission control system.
18. the system of claim 11, it further comprises at least one inert gas entrance system.
19. the system of claim 11, it further comprises the sensor of measurement gas incoming flow endoparticle amount; With
The controller that is communicated with sensor electrical, if so that the sensor measurement grain amount is higher than set amount, sensor indication sample flow inlet valve cuts out so.
20. measure and/or the endocorpuscular system of analytical gas incoming flow for one kind, described system comprises:
Particle collector;
The particle capture filtrator, wherein particle capture filtrator and particle collector are arranged in parallel.
At least with the microprocessor of particle collector electric connection;
Vacuum pump;
The water analysis device;
Emission control system;
At least one inert gas entrance system; With
Sample line tracing system, described tracing system comprise temperature sensor, heating source and with the controller of temperature sensor and controller electric connection.
21. the system of claim 20, it further comprises:
The sensor of measurement gas incoming flow endoparticle amount; With the controller that is communicated with sensor electrical, if wherein the sensor measurement grain amount is higher than set amount, sensor indication sample flow inlet valve cuts out so.
22. the system of claim 20, it further comprises purification plant so that the gas feed stream of purification to be provided, and wherein purification plant is not removed the particle that comprises in the gas feed stream that purifies basically.
23. the system of claim 22, wherein purification plant comprises diffusion type gas-solid phase separator, cold-trap, or the both comprises.
24. the method for a measurement gas incoming flow endoparticle content, this method comprises:
The gas feed stream of at least a portion is passed through purification plant, and so that the gas feed stream of purification to be provided, wherein purification plant is not removed the particle that this gas feed stream includes basically, and wherein said gas feed stream is under first pressure;
The gas feed conductance of the purification of a part is gone into dropping equipment, be reduced to the pressure lower than first pressure with pressure with the Purge gas incoming flow of this part; With
To be in than the Purge gas incoming flow of this part under the low pressure of first pressure and measure the granule content that the gas feed stream of purification includes by particle collector and the Purge gas incoming flow that makes another part by the particle capture filtrator, wherein particle capture filtrator and particle collector are arranged in parallel.
25. the method for claim 24, wherein said measuring process comprise will be in simultaneously than the gas feed stream of the purification of this part under the low pressure of first pressure by particle collector and with the gas feed stream of the purification of another part by the particle capture filtrator.
26. the method for claim 24, wherein said purification plant comprise diffusion type gas-solid phase separator, cold-trap, perhaps the both comprises.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US64949005P | 2005-02-03 | 2005-02-03 | |
| US60/649490 | 2005-02-03 | ||
| US11/340641 | 2006-01-27 |
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|---|---|---|---|
| CN 200610059229 Pending CN1818610A (en) | 2005-02-03 | 2006-02-03 | System and method for measurement and/or analysis of particles in gas stream |
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| CN107870139A (en) * | 2016-09-27 | 2018-04-03 | 深圳长城开发科技股份有限公司 | A kind of device and method of Non-Destructive Testing product surface particulate pollutant |
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| CN113984612B (en) * | 2021-10-30 | 2023-08-04 | 福州大学 | Particulate matter detects integrated device in GIS |
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