AD Sep Nozzle

8/2/2019 AD Sep Nozzle

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(US)Correspondence Address:THOMPSON HINE L.L.P.Intel lectual Property GroupP.O. BOX 8801DAYTON, OH 45401-8801 (US)

(73) Assignee: TENOROC, LLC, Orlando, FL(US)

(21) Appl. No.: 12/249,779(22) Filed: Oct. 10, 2008

Related U.S. Application Data(60) Provisional application No. 61/080,672, filed on luI.

14,2008.

(51) Int. Cl.BOlD 29/00 (2006.01)

(52) U.S. Cl. 55/315.1; 55/392; 55/315(57) ABSTRACTMultiple designs and methods for aerodynamic separationnozzles and systems for integrating multiple aerodynamicseparation nozzles into a single system are disclosed herein.These aerodynamic separation nozzles utilize a combinationof aerodynamic forces and separation nozzle structure toinduce large centrifugal forces on the gases that in combina-tion with the structure of the nozzle are used to separateheavier constituents of the process gas from lighter constitu-ents. In some embodiments a number of separation nozzlesare combined into a single system suitable for dynamic pro-cessing of a process gas. In other embodiments the separationnozzles are temperature controlled to condition the incominggas to a temperature in order to encourage a phase change incertain constituents of the gas to occur within the nozzle tofurther enhance separation.

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AERODYNAMIC SEPARATION NOZZLECROSS-REFERENCE TO RELATED

APPLICATIONS[0001] This application claims the benefit of U.S. Applica-tion No. 61/080,672.

TECHNICAL FIELD[0002] The subject matter described herein relates todevices, systems, and methods related to the separation andconcentration or depletion of various constituents of a flow orgas, including gas species, particles, and so forth.

BACKGROUND[0003] Aerodynamic separation of gas constituents is use-ful for a number of industrial and commercial applications.Anaerodynamic separation nozzle, or, as used herein, a sepa-ration nozzle, uses aerodynamic effects and forces generatedby high speed flow through structures to apply large centrifu-gal and aerodynamic forces to gases flowing through thosestructures to urge the various gas species that comprise aseparation gas to be separated (i.e. process gas) apart therebyenabling separation of the gas species. The combination ofthe centrifugal forces and the design of the structure areadapted to the type of gas species being separated. In particu-lar, the invention disclosed herein in its various embodimentspreferentially separates and isolates the constituents of a pro-cess gas into heavier and lighter species that are suitable forconcentration and collection. In one aspect the aerodynamicseparation nozzle utilizes temperature control of the nozzle toenhance separation efficiency. In another aspect, the aerody-namic separation nozzle utilizes pre-conditioning of theincoming gas stream to enhance separation efficiency. In stillother aspects combinations of the foregoing are used toenhance separation efficiency.

1 INDUSTRIAL APPLICABILITY[0004] The system and method has potential applicabilityto a wide range of different industrial and commercial appli-cations. The following brief synopsis is intended only toprovide background on some exemplary applications to assista person of ordinary skill in the art in understanding thisdisclosure more fully.1.1 Natural Gas Processing[0005] Natural gas provides more than one-fifth of all theprimary energy used in the United States. Much of the rawnatural gas is sub-quality and exceeds pipeline specificationsfor carbon dioxide, hydrogen sulfide, and nitrogen content,and much of this low-quality natural gas cannot be producedeconomically with present processing technology.[0006] A number of industry trends are affecting the naturalgas industry. Despite the current high price of natural gas,long-term demand is expected to overcome supply, requiringnew gas fields to be developed, including gas fields not beingused because of their low-quality products. In the future, theproportion of the gas supply that must be treated to removecontaminants before introduction into the pipelines willmcrease.[0007] Amine gas treating, or acid gas removal, refers to agroup of processes that use aqueous solutions of variousamines to remove carbon dioxide (C02) and hydrogen sulfide

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(H2S) from gases. Itis a common unit process used in refin-eries, petrochemical plants, gas-processing plants, and gas-ification plants. Gases containing carbon dioxide and/orhydrogen sulfide are commonly referred to as acid gases orsour gases in the hydrocarbon processing industries.[0008] A typical amine gas treating process includes anabsorber unit and a regenerator unit in addition to other ancil-lary equipment. In the absorber unit, the down-flowing aminesolution absorbs CO2 and H2S from the up- flowing sour natu-ral gas to produce a gas that meets specifications for CO2 andH2S content that exits the absorber unit . The resultant 'rich'amine is then routed into a regenerator (a stripper with areboiler) to produce regenerated or 'lean' amine that isrecycled for reuse in the absorber.[0009] A similar process is used in the steam reformingprocess of hydrocarbons to produce gaseous hydrogen forsubsequent use in the industrial synthesis of ammonia. Aminetreating is one of the commonly used processes for removingexcess carbon dioxide in the final purification of the gaseoushydrogen.[0010] Problems associated with amine treating include theenergy expense of the process, the chemical expense of theprocess (due to evaporative loss of amine), the inability toprocess highly contaminated CO2 gases, and the emission ofgases during the regeneration stage to the atmosphere.[0011] As of2005, according to the EPA there are 287 acidgas removal ("AGR") units operating inthe natural gas indus-try in the United States. These AGR units collectively emit634 million cubic feet (MMcf) of methane to the atmosphereannually, averaging 6 thousand cubic feet per day (Mcf/day)of methane per individual AGR unit. Methane is a knowngreenhouse gas, collectively less in quantity in the atmo-sphere when compared to carbon dioxide, but having about 20times the heat insulation properties than carbon dioxide, andhas a life-span in the atmosphere of 12 years on average.[0012] One need in industry today and for the future, is anacid-gas removal technology that can process high-levels ofcontaminants efficiently and does not require chemicals forabsorption, and does not emit contaminants to the atmo-sphere. The present system and method is capable of separat-ing CO2 and H2S from a sour natural gas stream without theneed to use an amine based process thereby eliminating theneed for costly, polluting AGR units.1.2 Carbon Dioxide Capture[0013] Extensive efforts have recently been directed towardcapturing CO2 emitted from large point sources such as fossilfuel power plants and other fossil fuel powered thermal gen-eration units. There are a number of processes that have beenposited for commercial use at large point sources of CO2including the same amine process described above for remov-ing CO2 from sour natural gas. However, the same limitationscaused by the operation ofAGR units are present when usingthe process to capture carbon being emitted from a large pointsource. Further, additional technologies such as scrubbers,electrostat ic precipitators and flue gas de-sulfurization isneeded to remove sulfur dioxide (S02) and particulate matterfrom the flue gas. In the case oflarge point source emitters, aseparation nozzle can be employed to remove all of the con-taminants in the exhaust stream, thereby allowing the con-centration of the various gases and part iculates in separate


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streams for final processing and in the case of carbon captureplants, sequestration of the CO2,1.3 Oxygen Concentration[0014] Many persons having diminished lung capacityneed to breath either pure or enriched oxygen as part of theirtherapy. Traditionally, when persons need continuous oxygentherapy, they use an oxygen concentrator that use typically amolecular sieve, such as a zeolite, to remove nitrogen fromambient air, thereby concentrating oxygen for use in thetherapy. These oxygen concentrators are typically less expen-sive than liquid oxygen canisters, and thus are more com-monly used for home administration of oxygen therapy. How-ever, oxygen concentrators capable of supplying more than1-2 li ters per minute of oxygen are typically larger, bulkierunits that are not suitable for portable use and require largequantities of energy to operate. Thus, most patients whorequire oxygen therapy when outside the home must usetraditional liquid oxygen bottles that are heavy and poten-tially dangerous. The present separation nozzle can providethe performance of an oxygen concentrator by separatingambient air into its constituent gases, thus concentrating theoxygen present in ambient air to a level suitable for oxygentherapy, without the need for bulky, power-intensive molecu-lar sieves.

2 BACKGROUND OF THE INVENTION[0015] An alternative separation process using aerody-namic techniques in conjunction with a specified nozzlegeometry was developed E. W. Becker for uranium isotopicenrichment. Separation nozzles of this type are generallyreferred to as a Becker process nozzle for isotopic enrich-ment. This Becker process nozzle depends upon diffusiondriven by pressure gradient effect, similar to the gas centri-fuge in order to separate gas constituents. In order to achieveeffective separation of isotopes, the centrifugal forces gener-ated in a Becker process nozzle must be increased. The cen-trifugal forces are typically increased by including a cut gas orseparation enhancing gas that allows the process gas to accel-erate faster within the Becker process nozzle and thus gener-ate greater centrifugal forces to enhance separation. In aBecker process nozzle, the gas mixture of the process gas andthe carrier gas is compressed and then directed along a curvedwall at high velocity through a convergent-divergent nozzle.The heavier molecules move preferentially out toward thewall relative to those containing the lighter molecules. At theend ofthe curved wall, a skimmer splits the overall gasjet intoa light enriched fraction and a light depleted fraction, whichare withdrawn separately. By nature of the Becker processnozzle design process, the use of a balance gas to acceleratethe velocity of the process gas and the gas to be separated, andfocus on isotope separation, the expansion of the process gasis quite large as the expansion gas exits the relatively shortconvergent -divergent nozzle and the gaseous expansion of theprocess gas is controlled by suction control rather than geo-metric expansion ration control.[0016] Generally the curved nozzle wall of the Becker pro-cess nozzle may have a radius of curvature as small as 0.0004inch. Production of these tiny nozzles by manufacturing istechnically demanding, and the overall process typicallyincludes stages having multiple vessels containing hundredsof separation elements, gas distribution manifolds, gas cool-

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ers to remove the heat of compression, and centrifugal com-pressors to pressurize the flow.[0017] Diffusion across a streamline, used by a Beckerprocess nozzle, is analogous to the diffusion against a gravi-tational or centrifugal force. So all separation processes in thegas occur in directions perpendicular to the streamlinesbecause no net material transport takes place across thestreamline. If a streamline is curved, this implies that the gasis being accelerated, and that a pressure gradient or force mustexist perpendicular to the streamline.[0018] The Becker process nozzle is typically adapted foruse in the separation of isotopes of heavier atomic weight. Inthis application, it is important for the designers to maintainhigher speeds. One approach to this is to introduce a balanceor separation gas to the process gas passing through theBecker process nozzle. The balance gas is typically l ightergas such as hydrogen or helium. The purpose of the balancegas istwo fold. First the lighter balance gas lowers the overallmolecular weight of the process gas thereby allowing theprocess gas to accelerate faster. Second, the lighter balancegas exerts a differential drag force on the heavier and lighterisotopes. This differential drag force is used to enhance theseparation of the isotopes.[0019] The use of a balance gas, however, requires theBecker process nozzle to adopt a characteristic form, namelya relatively short expansion nozzle that exits into a stagnationzone. Thus it is necessary for those of ordinary skil l in the artwhen using a Becker process nozzle to maintain a relativelyshort expansion nozzle length in order to separate isotopes ina relatively short flight time through the nozzle since a longernozzle would have a tendency to separate out all of the iso-topes from the balance gas as opposed to separating isotopes,thus changing isotope enrichment to a gas process.[0020] As a result of these requirements and design con-straints, the Beckerprocess nozzle has a number of significantlimitations that have reduced its applicability to general pur-pose gas separation including:[0021] 1. The small size of the curvature wall requiresthat the nozzle and skimmer components are also minutein size, requiring the components be made of foil mate-rial and bonded to assemble even one nozzle. Nano-fabrication is required to form the nozzles, with specifi-cations to the 0.001 mm tolerance.

[0022] 2. The operating pressure of the separation gas isat several bar, usually below 6 bar. The addition of spe-cialized compressors in the cascade add energy to theoperating costs to maintain the process at separationpressure.

[0023] 3. The flow stream along the curvature wall haslittle if any centrifugal force acting on that streamline, sothe 95/5 mixture along the curvature wall dilutes theconcentrating heavy isotope stream at extraction,thereby reducing the separation factor by dilution.

[0024] 4.To reduce the cost of the processing, the add-inhydrogen gas must be cleaned at the end of the processfor reflux back into the system, adding another separa-tion process to the cascade.

[0025] Another alternative separation technique disclosedin the prior art is the use of a Pitot probe in a supersonic gasmixture, first explained by Fenn and Reis (1963), of the typeexemplified in the following U.S. Patents-U.S. Pat. No.3,465,500 to Fenn (1969) and U.S. Pat. No. 3,616,596 toCampargue (1971). Itwas disclosed that at suitably low Rey-nolds numbers in a free-expansion jet of nitrogen/hydrogen


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gas mixture, the gas entering the probe was enriched in theheavier of the two species due to the stagnation effects at theprobe tip. Ithad previously been considered that gas samplestaken by such probe effect contained the two-molecular com-position of the free-expansion jet that had been separated byradial diffusion effects in the jet upstream of the probe. How-ever, in later experimentation by Rothe (1966), it wasrevealed that the magnitude of the probe-induced separationmeasured by Fenn and Reis was up to 50 times greater thanthat due to radial diffusion in the free jet alone. This determi-nation revealed that itwas the shock front preceding the probethat caused lighter specie to follow streamlines around theprobe, while heavier specie passed into the probe inlet. Thiseffect has been experimentally and theoretically tested for theseparation effect causing minor separation of isotopes, pri-mari ly for the potential use in uranium isotope enrichment.Due to the small degree of separation caused by a singleprobe, the method has not progressed to any commercialdegree.[0026] M. R. Bloom, the present inventor, in the early1990's developed gas-gas separation device using a centri-fuge based method for the separation of lower molar weightgas mixtures commonly found in the energy and chemicalindustry sectors. The mechanical device of his work isdescribed in U.S. Pat. No. 5,902,224 to Bloom (the '224Patent), for a device used for gas mixture separation. In the'224 Patent, a centrifuge device is described for the separationof components of low-molar weight gas mixtures, includingnatural gas, air, and contaminated air. Inthis centrifuge deviceconstruction, a narrow-gap centrifuge is built consisting ofmany individual and stacked plates that are spaced from oneanother to form the centrifuge rotor, and the central area at theaxis of rotation for this centrifuge is an open expansion cham-ber that extends through the height of the centrifuge. The '224Patent discloses a narrow gap centrifuge with a stationaryhousing, a rotor with multiple, stacked, inverted pyramidalplates that form channels between the plates. As lighter con-stituents are separated from the gas mixture they travel downthrough the device for extraction.[0027] Although the embodiments of the present deviceand method are described in combination with and in somecases contrasted to the theory and method of this previous art,this isnot intended to limit the claimed invention inany sense.

3 SUMMARY OF INVENTION[0028] The present aerodynamic separation nozzle (sepa-ration nozzle) has been focused upon optimizing a number ofparameters to tailor the characteristics of the separationnozzle to separate different consti tuents of the process gas.The separation nozzle possesses six main operating or designparameters governing the separation of constituents: (1) ll.Mbeing the difference in mass between gas components andalso in the case of partial condensation of constituents of theprocess gas, differences between phase particles and gas; (2)the development of velocity in the nozzle; (3) the averageinlet temperature of the gas into the nozzle; (4) the length ofgas expansion within the nozzle; (5) the radius of curvature ofthe divergent section ofthe nozzle; and, (6)temperature of theseparation nozzle and the surfaces of the separation nozzlefacing the flow of the process gas through the separationnozzle. There are a number of secondary and operating ordesign parameters that also govern the performance of aseparation nozzle as known to those of ordinary skill in the artinformed by the present disclosure. In the various embodi-

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ments of the present separation nozzle, these six parametersor separation factors, are controlled and used to tailor theseparation nozzle to control the performance of the separationnozzle and overall quality of constituent separation, alsodescribed herein as the separation performance of the sepa-ration nozzle. In one embodiment, the process gas enteringthe separation nozzle is condit ioned to enhance separationperformance by cooling the process gas.[0029] In another embodiment, cooling the body of theseparation nozzle enhances the performance ofthe separationnozzle. In this embodiment, the body or physical structure ofthe separation nozzle is held at a reduced temperature. Reduc-ing the temperature of the separation nozzle body in oneaspect reduces and minimizes shock effects occurring in theseparation nozzle thereby increasing the overall velocity ofthe process gas within the separation nozzle and enhancingthe separation effects. In still another embodiment a combi-nation of a cooled separation nozzle body is combined withpreconditioned or cooled process gas entering the separationnozzle.[0030] In yet another embodiment, the separation factorsare controlled to effect the quality of gas separation throughthe relationship of the gas inlet temperature and the tempera-ture of the nozzle to further reduce the temperature of the gasto phase change of the highest-boiling point component of thegas. The development of the proper separation nozzle geom-etry to effect supersonic cooling and increased temperatureexchange from the gas has evolved where the process gasmaintains supersonic flow for a majority of the distancethrough the curving portion of the separation nozzle. Embodi-ments ofthis separation nozzle design, having a longer super-sonic expansion region, results in a reduction in shock effectsoccurring at the exit of the curving expansion port ion of theseparation nozzle.[0031] This design and development of the separationnozzle geometry and operation, and hence tailoring of theseparation parameters, has been triangulated using CFD tomodel the gas flow characteristics, along with numericallymodeling those gas characteristics, and experimental testingof the separation nozzle to verify the CFD and numericalcalculation for flow rate, pressure, temperature, and separa-tion effect. This allows the creation of a set of design tools anddesign methodology that allows the optimization of variousembodiments of the separation nozzle to provide enhancedseparation performance tailored to the specific requirementsof the process gas and desired constituents to be separated.[0032] Other embodiments of the present separation nozzleare directed to the combination of the separation nozzle withother separation nozzles and other support ing equipment inorder to create a system incorporating the separation nozzle,adapted to achieve desired separation performance withrespect to a particular process gas and desired separationconstituents.[0033] In some embodiments of the separation nozzles, aheat exchanger is integrated into the nozzle design and allowsthe use of a refrigerant to control the temperature of thenozzle, and subsequently the temperature of the gas throughthe supersonic expansion process. In some of these embodi-ments, a system of separation nozzles is created to connect theheat exchanger in the separation nozzle to a vessel that col-lects separated heavy fractions evolving from the separationprocess in the separation nozzle. Thus, in some embodimentsof the separation nozzle with a heat exchanger, temperatureloss through the system is managed by using the heavy frac-


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tion exiting from the separation nozzle as a refrigerant tocondition the incoming process gas. In these embodiments,this thermal management increases the overall efficiency ofthe separation nozzle system as a whole.[0034] In one aspect, the device and method comprises anaerodynamic separation nozzle that is designed to cause gasvelocity through the curved expansion nozzle element of theseparation nozzle, to be at a supersonic velocity up to theflow-fractioning skimmer plane, by which the gas signifi-cantly drops pressure and temperature through expansion. Inthese embodiments, the expansion ratio of the nozzle extendsthrough the curved geometry of the divergent section of thenozzle through at least 1200 of gas flow travel, and possiblyup to 1800 of gas flow travel. Beyond the expansion exit ofthenozzle throat in these embodiments, the geometry of thedivergent channel gradually expands to two separate super-sonic diffusers, divided by a leading-edge skimmer for over-all flow division, and two separate gas fractions evolve intotheir respective diffuser to be extracted from the nozzle as twoseparated flow streams, separated such that with respect toone constituent gas the one flow stream is enriched while theother flow stream is depleted.[0035] In another aspect of separation nozzle system, thepressurized inlet gas or process gas may be cooled by anexternal heat exchanger from its originating temperatureprior to entering the separation nozzle. In these embodiments,the cooled and pressurized inlet gas entering the nozzlebecomes supersonic in velocity through expansion. Expan-sion ofthe gas decreases the density of the gas and the expan-sion gas results in significant cooling of the moving gasthrough supersonic velocity.[0036] Another embodiment of this device and method istopre-cool the inlet gas to the aerodynamic separation nozzle byan external heat exchanger that is positioned upstream of thenozzle, and the nozzle itself is cooled through the action of arefrigerant that circulates through a heat exchanger thatencompasses the nozzle. In this embodiment, the separationnozzle-body can be regulated in temperature in a range fromabout 1330 R to about 5400 R or more by having the refrig-erant acting on the stagnant temperature of the expansionnozzle. Further, in applications for gas separation where acondensable fraction is tobe separated by phase inthe expan-sion nozzle, generally the inlet gas has a higher temperaturevalue than the separation nozzle body temperature value. Inthis manner, energy is extracted from the inlet process gasthrough the expansion process as the process gas passesthrough the expansion nozzle, and that energy is transferredfrom the gas to the separation nozzle body. The heat in tum isremoved from the separation body via a refrigerant for energyremoval. Still further, the refrigerant can be controlled as to itsflow rate to control the overall temperature of the separationnozzle body, thereby enabling the control of the temperatureratio between the inlet process gas and the separation nozzlebody, which of course modulates the overall heat transferfrom the inlet gas to the separation nozzle body.[0037] As used herein, the stagnation temperature of anexpansion nozzle is calculated as the mean temperature of thegas passing through the expansion nozzle in a sonic-super-sonic state between the nozzle throat 108 and the skimmer112. The stagnation temperature of an expansion nozzle is afnnction of at least the stagnation temperature of the gasentering the nozzle, the nozzle material temperature thedegree of expansion ratio between the nozzle throat 108 and

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the expansion nozzle exit 107 or Type-2 nozzle exit 208depending on the embodiment of the expansion nozzle con-sidered.[0038] Another embodiment of the separation nozzledevice and method is to have the refrigerant provided in theheat exchange component of this invention as either a con-densed gas that has been separated from the gas flow, or as aliquid refrigerant such as liquid nitrogen. In the case of anembodiment using separated condensed gas, that refrigerantmay be drawn from a vessel combined with the separationnozzle using a metering pump and delivered by a fill pipe tothe heat exchanger of the nozzle in a flow-controlled manner.Further, the amonnt of refrigerant flow may be controlled bya control unit that utilizes a sensor signal to increase ordecrease the flow of refrigerant required to maintain thedesired level of temperature of the nozzle.[0039] Another aspect of the device and method is to havethe coolant provided to the heat exchanger component of thenozzle as a cryogenic gas wherein a liquid cryogen or con-densed gas is vaporized to act as the temperature medium. Inthis application, refrigerant as a liquid is stored in a reservoirvessel that has an adjustable resistive heater that vaporizes theliquid refrigerant at a controlled rate and volume of producedrefrigerant gas. The refrigerant gas is then piped through afeed line to the nozzle heat exchanger where the heat transferoccurs between the inlet gas and the nozzle body. Similarly,the flow volume of the cryogenic gas refrigerant can be regu-lated by a control unit that utilizes a sensor signal to increaseor decrease the refrigerant flow required to maintain the levelof nozzle cooling from 1330 R to 5400 R.[0040] Another embodiment ofthis device and method istohave the aerodynamic separation nozzle configured into aseparation cascade arrangement where the inlet gas enters theseparation cascade of successive aerodynamic separationnozzles, and is separated of some of its constituents throughsuccessive inter-cascade flows that produce a product streamand a waste stream. The operation of the various embodi-ments of a cascade system of separation nozzles is specifiedby the type of application, wherein the cascade is at least twosuccessive stages and may be as many as 20 or more stagesselected according to the separation performance of eachseparation nozzle stage and the desired quality of the outletgas products. In some embodiments, the cascade system isoperated from the initial pressure of the inlet gas, wherein thegas pressure of the processing gas is reduced through eachstage as is specified by the separation nozzle geometry. Inother embodiments, an individual stage pump is used torepressurize the gas prior to each successive separationnozzle stage. The stage pump thus recovers the pressure thatis reduced in the expansion process at the prior separationnozzle stage. In other embodiments, the design of the sepa-ration nozzle stages of the cascade varies and is separatelysized from the bottom to the top of the cascade thereby allow-ing the flow volume at each stage to be regulated by eachstage 's nozzle geometry to control the throughput of the gasand adapted to accommodate the residual pressure of theprocess gas exiting the earl ier stage as an inlet to the currentstage and maintain relative pressure ratios across the separa-tion nozzle by adjusting the total volume and physical geom-etry of the separation nozzle.[0041] An embodiment of the present device and method isfabricated to be a supersonic nozzle that is curved in itsdivergent section, whereby process gas is expanded through anozzle throat becoming less dense and achieving supersonic


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velocity. The flow of the process gas through the curveddivergent nozzle results in curved supersonic streamlineswithin the nozzle. This results in a pressure gradient estab-lished within the curved divergent section of the expansionnozzle that is perpendicular to the curved supersonic stream-lines within the curved divergent expansion nozzle section ofthe separation nozzle. The pressure gradient thus urgesheavier, more massive species or constituents of the processgas toward the outer wall of the curved divergent nozzle whilelighter species are urged toward the inner wall of the curveddivergent nozzle. In still other embodiments, the separationnozzle assembly is held or controlled to a temperature that isdifferent compared to the inlet gas temperature. Gas fractionsor constituents of the process gas flow in this curved super-sonic condit ion of flow either release or gain heat throughheat transfer and aerodynamic processes. In one aspect, theseparation nozzle assembly is held at a reduced temperatureto increase the velocity of the process gas flow resulting inincreased separation performance.[0042] In another aspect the heat transfer from the processgas is used to encourage the condensation of at least onespecies or constituents within the process gas. This heat trans-fer allows a different phase state to form in the process gascompared to the remaining gaseous fraction. The condensedconstituents in the curved expansion nozzle effectively crossthe supersonic streamlines in a radial and perpendiculardirection to the supersonic streamlines, thereby moving fromsmaller pressure to larger pressure, and subsequently lessdense gaseous fractions may move from larger pressure tosmaller pressure by radial perpendicular movement. The par-tial condensation of at least one constituent ofthe process gasresults in increased separation performance.[0043] Another aspect of this device and method is to causeseparation of components or constituents of a gas throughpre-conditioning the temperature and pressure of the gasupstream of an aerodynamic separation nozzle, and thencausing a secondary temperature and pressure change tooccur within the nozzle, due to supersonic cooling and havingthe temperature of the nozzle at a different range compared tothe inlet gas temperature. Further, through the geometry ofthe nozzle, causing a separation of the flow within the nozzleyields two separate flows; one being concentrated in thephase-changed fraction, and the other being depleted of thephase-changed fraction.[0044] Finally, the device and method of this invention isconfigured to economically separate a gas of its componentson a continuous operation, so that the device and method canbe used for commercial applications.

BRIEF DESCRIPTION OF THE DRAWINGS[0045] The accompanying figures depict multiple embodi-ments of a device and method for the separation of constitu-ents from a flow. A brief description of each figure is providedbelow. Elements with the same reference numbers in eachfigure indicate identical or fnnctionally similar elements.[0046] FIG. 1 is a perspective view of a Type-l separationnozzle.[0047] FIG. 2a is a perspective view of a Type-2 separationnozzle.[0048] FIG. 2b is a perspective view of another embodi-ment of a Type-2 separation nozzle incorporating a dual skim-mer configuration.

Jan. 14,20105

[0049] FIG. 3a is a perspective view of a single Type-2separation nozzle confided into an embodiment of a nozzleplate.[0050] FIG. 3b is a perspective view of a pair of the Type-lseparation nozzles configured into an embodiment nozzleplate.[0051] FIG. 4a is a perspective side-view of an embodimentof a separation nozzle module.[0052] FIG. 4b is a perspective top-side view of an embodi-ment of the elements of a separation nozzle module assemblyincorporating a Type-2 separation nozzle.[0053] FIG. 5 is a view of the results of ComputationalFluid Dynamics (CFD) analysis of gas flow mach velocitythrough an embodiment of a Type-l nozzle with ambientprocess gas and ambient nozzle.[0054] FIG. 6 is a view of a CFD portrayal of gas tempera-ture through an embodiment of a Type-l nozzle with ambientprocess gas and ambient nozzle.[0055] FIG. 7a is a view of the results of ComputationalFluid Dynamics (CFD) analysis of gas flow mach velocitythrough an embodiment of a Type-2 nozzle with ambientprocess gas and ambient nozzle.[0056] FIG. 7b is a view of the results of ComputationalFluid Dynamics (CFD) analysis of gas flow mach velocitythrough an embodiment of a Type-2 nozzle with coolednozzle and ambient process gas.[0057] FIG. 7c is a view of the results of ComputationalFluid Dynamics (CFD) analysis of gas flow mach velocitythrough an embodiment of a Type-2 nozzle with heated pro-cess gas and cooled nozzle.[0058] FIG. 7d is a view ofCFD results of gas flow machvelocity through an embodiment of a Type-2 nozzle withcooled process gas and cooled nozzle.[0059] FIG. 8a is a three-dimensional CFD depiction oftemperature through an embodiment of a Type-2 nozzle withambient process gas and ambient nozzle.[0060] FIG. 8b is a view of CFD estimates of gas tempera-ture through an embodiment of a Type-2 nozzle with cooledprocess gas and cooled nozzle.[0061] FIG. 9 is a schematic view of an embodiment of aType-2 nozzle assembly that is formed of several bondednozzle plates.[0062] FIG. 10 is a schematic view ofa nozzle module thathas an integrated heat exchanger element.[0063] FIG. 11 is a view of an embodiment of a nozzlemodule/heat exchanger.[0064] FIG. 12 is a profile view of an embodiment of aseparation nozzle assembled into a phase tube assembly.[0065] FIG. 13 is a top view of an embodiment of a phasetube assembly.[0066] FIG. 14a is an assembly view of embodiments of anozzle module and heat exchanger adapted to join with aninlet distribution tube for mounting on a phase tube assembly.[0067] FIG. 14b is a view of a distribution manifold withintegral orifice plate.[0068] FIG. 15 is a phase diagram ofa methane (CH4) andcarbon dioxide (C02) gas mixture.[0069] FIG. 16 isa depiction ofa cascade using anembodi-ment of a separation nozzle.[0070] FIG. 17 is a second embodiment of a three-stageseparation nozzle cascade configured to a central phase tube.[0071] FIG. 18 is a depiction of an embodiment of an indi-vidual swirl generation unit for the phase tube.


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[0072] FIG. 19 is a depiction of another embodiment of anindividual swirl generation unit for the phase tube with detailsof intemal features provided.[0073] FIG. 20 is a basic process flow path for acid gasremoval.[0074] FIG. 21 is a schematic of an embodiment ofa sepa-ration stage.[0075] FIG. 22 is a schematic depict ion of an embodimentof a twelve stage separation system.[0076] FIG. 23 is a detailed schematic depiction of a secondembodiment of a twelve stage separation system.[0077] FIG. 24 is a depiction of an embodiment of a nucle-ate generation conditioning system.

DETAILED DESCRIPTION[0078] Multiple embodiments of a system, device, andmethod for the separation of constituents of a flow are pre-sented herein. Those of ordinary skill inthe art can readily usethis disclosure to create alternative embodiments using theteaching contained herein.Vernacular[0079] The following terms used herein are defined as fol-lows.[0080] The term "gas" or "process gas" as used herein isused as a general term to refer to any gas that is input to anaerodynamic nozzle for separation, including enriched ordepleted gas that has previously exited a prior separationnozzle. In some embodiments, a gas contains particulate mat-ter or condensed vapor (i.e. liquid phase) that are substantiallyentrained in the flow or vapor creating a multi -phase flow. Inother embodiments, the gas contains a mixture of gases andisotopes suitable for enrichment. In one embodiment, the gascomprises a process gas and a balance gas, wherein the pro-cess gas istargeted for either enrichment or depletion and thebalance gas is used to enhance the aerodynamic effects of theseparation system. Enriched or depleted gas indicates that thegas contains, respectively, either a greater concentration ofthe indicated gas species or a reduced concentration of theindicated gas species.[0081] As used herein, the term "oblique shock wave" is aflow structure created by flow through a curved duct or nozzlewhereby a flow that is substantial ly uniform and parallel isturned by action of the duct walls into another flow that is alsosubstantially parallel but is compressed and has a differentdirection. To achieve the oblique shock wave, the walls of anozzle are formed in such a way to form the desired stream-line such that there is only a single expansion wave, where the"reflected" wave drops out and is canceled due to interactionswith the incoming wave. See e.g., Applied MathematicalSciences, Vol. 21, Supersonic Flow and Shock Waves, R.Courant, K. O. Friedrichs, Chap. lYB, pg. 282-286.[0082] When discussing the present application and theseparation nozzle and separation nozzle system, the readerwill note that in some circumstances the term separationnozzle is used independently and in other circumstances isused in conjunction with the adjective Type-n where n is aninteger number. The Type-n adjectives are used to highlightfeatures that characterize specific embodiments of what isgenerally described as a separation nozzle. Thus the termseparation nozzle refers to features common between allembodiments of the described separation nozzles that areapparent to those of ordinary skill in the art, while discussions

Jan. 14,20106

relating to embodiments of the separation nozzle, describedas Type-n separation nozzles, discuss features that are uniqueto that particular embodiment as well as common features ofall embodiments of the separation nozzle.[0083] As used herein, the term "state" when used in refer-ence to a physical object is intended to define the variousparameters of that particular physical object or dynamic sys-tem. For example, when referring to a gas, the state of the gasincludes various parameters or states associated with the gassuch as pressure, temperature, composition or constituentratios, density, enthalpy, entropy, velocity, and acceleration.[0084] The following terms and definitions are used todescribe the flow of a gas or fluid, or mixture of a gas, liquid,and/or solids: mean velocity vector at a location means themean or average of the instantaneous velocity vectors asso-ciated with the flow at a given location. For example, in achannel with fully developed flow, the mean velocity vectoracross the channel would integrate the velocity vectors of theflow from both the free stream portion of the flow as well asthe relatively slower contributions from the boundary layer.The magnitude of the velocity vector is the total velocity ofthe velocity vector at a given location.

4 SEPARATION NOZZLE[0085] Various embodiments of the separation nozzle aredescribed below. These embodiments are variously adaptedbased on the characteristics ofthe process gas that is inlet intothe separation nozzle, and the nozzle parameters are selectedin order to enhance the desired separation performance toallow a portion of the process gas to be separated into a flowthat is enriched with a constituent of the process gas and aflow that is depleted with respect to a constituent of theprocess gas. In this manner the separation nozzle allows theselective concentration or depletion of desired gas species.4.1 Type-l Separation Nozzle[0086] FIG. 1 is a perspective view of an embodiment of aType- I separation nozzle, or as referred to herein a Type-lnozzle 100. In FIG. 1, the basic geometry ofthe Type-l nozzle100 can be seen; with the inlet gas reservoir 106 beingupstream of the nozzle throat 108. The inlet gas reservoir 106is adapted to receive the process gas entering the separationnozzle. As with all of the various embodiments discussedherein, the term flow path isused when referring to the flow ofthe process gas through a given separation nozzle from theinlet gas reservoir 106 until the flow exits the extents of theseparation nozzle at the various diffusers and the upstreamdirection is generally against the mean velocity of the flow(i .e. toward the inlet gas reservoir 106) while downstream isgenerally inthe direction of the mean velocity ofthe flow (i.e.toward the diffusers).[0087] The Type-l nozzle 100 comprises a divergentexpansion nozzle, or simply an expansion nozzle 102 that isf1uidicly coupled to the nozzle throat 108 to accept the flow ofthe process gas and an expansion nozzle exit 107. As usedherein, the term f1uidicly coupled indicates that a connectionismade between the recited elements that are adapted to allowthe transport of a fluid (including gases and multi-phase flowswithout limitation) between the recited elements. The lengthof the expansion nozzle 102 along the flow path is definedbetween the nozzle throat 108 to the expansion nozzle exit107. The expansion nozzle exit 107 exhausts the flow into anover-expanded region 118 that in the embodiment depicted in


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FIG. 1 is a portion of the expansion diffuser 105. The flowpath of the process gas through Type-l nozzle 100 after enter-ing the nozzle throat 108 is generally along the separationflow path 130 that is defined along the nominal flow path fromthe nozzle throat 108 through the expansion nozzle 102 andthe expansion nozzle exit 107 to the skimmer 112, which inthe embodiment shown passes through the over-expandedregion 118.[0088] When describing the various embodiments of theseparation nozzle, an angle (a) is used to describe and iden-tify the location of various features and characteristics of theseparation nozzle. This angle, denoted using the symbol (a),shown in FIG. 1 and common to all depictions of the variousembodiments of the separation nozzle detailed herein, is cal-culated from an arbitrary nozzle midpoint 111. The nozzlemidpoint 111 is defined along a phantom or construction linedrawn between a perpendicular drawn from at a first point 122to a second point 126, which in the embodiment depicted isco-located atthe tip 124 of the skimmer. The first point 122 ofthe construction line is located at the interior wall of thenozzle throat 108 at the point where the nozzle throat 108transitions to the expansion wall 109. In cases where theskimmer 112 is shifted above or below the (a) equals 180degrees, the second point 126 is defined as the intersectionbetween the construction line and a perpendicular l ine thatintersects the tip 124 of the skimmer 112 where the construc-tion line intersects the deflection wall 101 as the deflectionwall 101 crosses about 180 degrees. In the embodimentdepicted, the second point 126 of the construction line iscoincident with the tip 124 of the separation skimmer 1 12.The angle (a)=O degrees is defined along the radius (rll)between the nozzle midpoint 111 and the first point 122. Theangle (a) has a positive sense defined in the direction of theflow path. Those of ordinary skil l in the art wil l note that thenozzle midpoint 111 is not the actual midpoint of the separa-tion nozzle, rather it is an arbitrary construct used to providea reference or fiducial indicator for establishing locations ofspecific elements in the figure.[0089] The embodiment of the expansion nozzle exit 107,depicted in FIG. 1, is oriented with a nozzle exit angle (aexit)about 1200 downstream of the nozzle throat 108. The radiusr l2is drawn from the nozzle midpoint 111 to the intersectionofthe expansion nozzle exit 107. Inthe embodiment depicted,the deflection wall 101 has a substantially constant radius,while the expansion wall 109 has a slight helical profile thatexpands the total volume of the separation flow path 130 asthe angle (a) increases along the flow path in order to allowthe flow to expand and accelerate within the expansion nozzle102. In other embodiments, those of ordinary skil l in the artwill use a variable radius deflection wall 101 and variableradius expansion wall 109, or other generally curvilinearprofiles or combinations thereof in order to achieve thedesired flow characteristics for the process gas when itreaches the expansion nozzle exit 107.[0090] Continuing with the embodiment of the Type-lnozzle 100 depicted in FIG. 1, the deflection diffuser 104 isalso oriented downstream of the expansion nozzle exit 107,and is downstream of the separator skimmer 112. The skim-mer 112 separates the process gas into two separate flows, afirst flow that passes into the deflection diffuser 104 and asecond flow that passes into the expansion diffuser. In theembodiment of the Type-l nozzle 100 depicted in FIG. 1, thefirst flow passing into the deflection diffuser is urged by the

Jan. 14,20107

skimmer 112 or the flow is cut into the skimmer throat 103before passing into the deflection diffuser 104.[0091] The Type-l nozzle 100 is configured with a curveddivergent expansion nozzle section, the expansion nozzle102, traversing along the flow path from the nozzle throat 108to the expansion nozzle exit 107. The radius of curvature ofthe separation flow path 130 within the expansion nozzle 102is substantially defined by the curvature of the deflection wall101. The expansion nozzle 102 is constrained in the planardimensions of FIG. 1 by the deflection wall 101 and theexpansion wall 109. The expansion nozzle 102 is definedwithin the extents of the expansion nozzle, namely thatinscribed within the angle (aexit) between the nozzle throat108 and the expansion nozzle exit 107.[0092] The radius of curvature of the deflection wall 101depicted in FIG. 1s generally constant through all angles (a)through the length of the expansion nozzle 102 to the skim-mer 112. The expansion wall 109 in the embodiment of theType-l nozzle 100 depicted in FIG. 1 is a generally helicalcurve that gradually reduces in radius as the angle (a)increases. The separation between the deflection wall 101 andthe expansion wall 109 determines the overall expansion ratio(calculated between the nozzle throat 108 and the expansionnozzle exit 107) and the expansion rate (i.e. the rate ofchangeof the expansion ratio calculated as a function of angle (a) ofthe expansion nozzle). As used herein, the term radius ofcurvature defines the radius of curvature at a given point on acurved line, and the definition thus, in some circumstances,varies continuously along different locations on an arc suchthat different points of the arc defined by the radius of curva-ture have different radius lengths and even different centers. Acurvature ratio (r.) is defined as the ratio of the radius ofcurvature of the expansion wall 109 (re)relative to the radiusof curvature of the deflection wall 101 (rd) where (r.) is givenby Eq. 1:

Eq. 1

[0093] Downstream of the expansion nozzle exit 107 is astagnation zone or over-expanded region 118. That over-expanded region 118 is defined in the embodiment of theType-l nozzle 100 depicted in FIG. 1 as the region betweenthe expansion nozzle exit 107 and a plane coincident with thetip 124 of the skimmer 112 orientated substantial ly perpen-dicular to the flow, or in the embodiment depicted, oriented tointersect both the plane ofthe tip 124 and the arbitrary nozzlemidpoint 111.[0094] Process gas flow in the Type-l separation nozzle100 begins with inlet process gas entering the Type-l sepa-ration nozzle 100 at the inlet gas reservoir 106. The inletprocess gas ispressurized at a desired pressure dictated by thenatural pressure of the process gas supply source, perfor-mance of a pump upstream of the inlet gas reservoir 106, orthe pressure remaining in the process gas after it passesthrough a separation nozzle located upstream of the inlet gasreservoir 106.[0095] The inlet gas reservoir 106 is adapted using the skillsof one of ordinary skill in the art to minimize the gas-flowvelocity while maintaining the inlet gas pressure, or stagna-tion pressure, so that the gas velocity in the inlet gas reservoiris, relative to the nozzle, slight in velocity and is pressurizedby the gas. In some embodiments, not depicted, flow struc-


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tures are used to substantially straighten and orient the flowprior to entry of the process gas into the nozzle throat 108. Inother embodiments, the walls and floor and ceiling (notshown in FIG. 1) that define the inlet gas reservoir 106includes or is thermally connected to one or more heat trans-fer devices allowing, in part, the process gas passing throughthe inlet gas reservoir 106 to be conditioned. In other embodi-ments' the walls and floor and ceiling of the inlet gas reservoir106 are thermally connected to one or more heat transferdevices to allow the temperature of the separation nozzlebody to be held at a desired temperature, which in oneembodiment is a reduced or lower temperature.[0096] The process gas flows from the inlet gas reservoir106 through the nozzle throat 108 into the expansion nozzle102. The velocity of the process gas increases to the velocityof sound in that particular gas state, i.e. greater than or equalto Mach 1 (M>= 1), and as such, the pressure decreases invalue and the gas flow thins in its density as a function of theMach value of the gas. The downstream curved expansionnozzle 102 has an outer boundary wall, or a deflection wall101, that is a constant radius of curvature determined from thenozzle midpoint 111 of the nozzle configuration, and theexpansion nozzle 102 has an inner boundary wall or expan-sion wall 109 that is a decreasingly smaller-radius from thenozzle throat 108 to the expansion nozzle exit 107. Theexpansion nozzle exit 107 in the embodiment depicted islocated at an angle Uexit of about 130 degrees from the nozzlethroat 108. In other embodiments the expansion nozzle exit107 is located at an angle uexit of between about 120 degreesto about 180 degrees. In st ill other embodiments the expan-sion nozzle exit 107 is greater than about 180 degrees. Insome embodiments wherein the expansion nozzle exit 107 isgreater than an angle (uexit) of 180 degrees the skimmer 112is shifted upward greater than an angle (uexit) of about 180degrees.[0097] The radius of the expansion wall 109 to the nozzlemidpoint 111 varies continuously as a function of the angle(o.) in order to achieve the desired expansion ratio for a givenseparation nozzle geometry. For many of the embodimentsdepicted herein, the expansion ratio varies from a minimumof about 1.7 to a maximum of about 4.3. In other embodi-ments the expansion ratio of a given expansion nozzle 102varies from about 1.5to about 4.5, in still other embodimentsthe expansion ratio of a given expansion nozzle 102 is greaterthan about 4.5. The expansion ratio for a given separationnozzle embodiment is a function of many variables known tothose of ordinary skil l in the art. The expansion nozzle 102 isconfigured by those of ordinary skill in the art based on theprocess gas, and the state of the process gas at various pointsin the Type- I nozzle 100 to be about optimally or fullyexpanded, meaning that the separation flow path 130 throughthe expansion nozzle 102 is substantially neither over-ex-panded nor under-expanded. Similarly, since the flow is nei-ther over-expanded nor under-expanded, there is no flowseparation in the flow. This flow condition is also character-ized as a nonseparated flow or a non-recirculating or nonre-circulation region of the flow. In other embodiments, a major-ity of the separation flow path 130 through the expansionnozzle 102 is fully expanded, and only a fraction of theseparation flow path 130 within the expansion nozzle 102 iseither over-expanded or under expanded. In one embodiment,less than about twelve percent (12%) of the separation flowpath 130 within the expansion nozzle 102 is either over-expanded or under expanded. In another embodiment, less

Jan. 14,20108

than about twenty-five percent (25%) of the separation flowpath 130 within the expansion nozzle 102 is either over-expanded or under expanded. In another embodiment, lessthan about forty percent (40%) of the separation flow path 130within the expansion nozzle 102 is ei ther over-expanded orunder expanded.[0098] Downstream, in the over-expanded region 118, theflow separates from the expansion wall 109 and forms aseparated layer. Inside the separated layer, it is common for arecirculation zone to form, whereby higher pressure gas fromthe over-expanded region 118 flows upstream against theseparation flow path 130 along the surface of the expansionwall 109 while a portion of the re-circulating gas is entrainedby the main process gas flow along the separation flow path130, causing a characteristic recirculation flow pattern.[0099] Within the expansion nozzle 102, as the process gasis accelerated along the separation flow path 130 by theexpansion nozzle 102, it increases in velocity. In the embodi-ment shown, the velocity of the process gas increased withinthe separation nozzle to be greater than or about equal to thespeed of sound in the medium, Mach= 1.As well known tothose of ordinary skill in the art , the supersonic flow condi-tions within the expansion nozzle 102 results in both a reduc-tion of the process gas pressure and temperature. The expan-sion ratio and length of the expansion nozzle 102 along theseparation flow path 130 are tailored by one of skill in the artwith knowledge of the process gas and by controlling thepressure of the process gas at the inlet gas reservoir 106 andthe pressure at the expansion diffuser 105 and the deflectiondiffuser 104. Inthis manner, one or ordinary skill inthe art hasthe tools to manipulate and control the state (the coupledvariables pressure, temperature and velocity) of the processgas within the separation nozzle.[0100] In this manner of configuration, the expansion ratioof the expansion nozzle 102 from the nozzle throat 108 to theexpansion nozzle exit 107 is developed in the main by thewidening of the expansion-deflection wall separation dis-tance between the expansion wall 109 to the deflection wall101. This dimension, shown on FIG. 1, is called inthe variousembodiments depicted herein the throat dimension 110. Thisincrease in the expansion wall 109 to deflection wall 101, oran increase in the overall separation distance i.e. the throatdimension 110 creates, in part, the expansion ratio at variouspoints of the expansion nozzle 102 being determined as afunction of the angle (ex).[0101] Due, in part, to the expansion ratio changing as afunction of (o.) the expansion nozzle 102 a first pressuredifferential develops across the channel or throat dimension110 whereby a lower pressure ismanifest in the vicinity of theexpansion wall 109 while a region of greater pressure ismanifest in the vicinity of the deflection wall 101. This pres-sure differential across the width of the channel, i.e. along thethroat dimension 110, is further increased, in part, due to thecentripetal acceleration of the process gas as the deflectionwall 101 forces the process gas flowing through the expansionnozzle 102 along the separation flow path 130 to turn alongthe surface of the deflection wall 101. The combination ofcentripetal force caused by the curved nature of the deflectionwall 101 combined with the pressure difference caused by theexpansion of the expansion nozzle 102 by the change incurvature of the expansion wall 109 results in the concentra-tion of heavier constituents of the separation toward thedeflection wall 101 and lighter constituents of the process gastoward the expansion wall 109. Although the process gas state


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and constituents have an impact on separation performance,this combination of reduced pressure on the expansion wallwith deflection occurring along the deflection wall induce theconstituents of the process gas to concentrate across the chan-nel, namely the separation distance or throat dimension 110.[0102] The process gas accelerates at the nozzle throat 108since the nozzle throat 108 is the narrowest point in the gasflow expansion, and the gas continues to accelerate as a func-tion of the angle (o.) as the throat dimension 110 increasesalong the separation nozzle 102 until the process gas reachesthe nozzle exit. As mentioned previously, in some embodi-ments the expansion wall 109 change radius as a function ofthe angle (o.), in other embodiments the expansion wall 109and the deflection wall 101 both change radius, while in stil lother embodiments only the deflection wall 101 increases inorder to increase the throat dimension 110 as a function of theangle (o.).[0103] In embodiments of the Type-l nozzle 100, the pro-cess gas flow near downstream of the expansion nozzle exit107 generates one or more oblique shock waves as the flowenters the over-expanded region 118. The shocks generallydissipate the velocity of the gas to less than sonic conditions,and allow the flow to recover both temperature and pressure.However, the bulk of the process gas flow, i.e. a beam of gas,continues generally along the separation flow path 130 to theskimmer 112. The skimmer 112 divides the process gas intotwo distinct flows separated by the body of the skimmer 112.The first portion of the divided flow continues through theskimmer throat 103 and further diminishes in velocity to beextracted from the Type-l nozzle 100 through the deflectiondiffuser 104. The remainder of the process gas flows on theother side of the skimmer 112 and collects in the expansiondiffuser 105 for extraction from the Type-l nozzle 100.Within the over-expanded region 118, a recirculation regionforms near the expansion nozzle exit 107 on the expansionwall 109. Further details of this aerodynamic effect aredescribed below in the section titled Nozzle Flow.4.2 Type-2 Separation Nozzle[0104] FIG. 2a is a perspective view ofthe nozzle geometryof an embodiment of a Type-2 nozzle 200. The Type-2 nozzle200 reduces the volume of the over-expanded portion of theType-2 nozzle 200 after the expansion nozzle exit 107, tocreate a Type-2 over-expanded region 218. Thus, the Type-2nozzle 200 depicted provides a more gradually tapering tran-sition from the expansion nozzle exit 107 to the Type-2 over-expanded region 218 as compared to the over-expandedregion 118 associated with the embodiments of the Type-lnozzle 100. This extends the overall supersonic condition ofthe process gas further along the flow path through the Type-2over-expanded region 218, shown in FIG. 2a, as highlightedin the flow analysis described in the section on tit led NozzleFlow below. As in the Type-l nozzle 100 described previ-ously, the divergent expansion nozzle, or simply expansionnozzle 102, extends from the nozzle throat 108 to the expan-sion nozzle exit 107 along the separation flow path 130.[0105] The flow of the process gas in the Type-2 nozzle200, depicted in FIG. 2a, is also over-expanded in the Type-2over-expanded region 218 after the expansion nozzle exit107. This means that the flow of the process gas within theover-expanded region is at least part ially separated from atleast the expansion wall 109 in the embodiment shown. Inother embodiments the flow of the process gas is separatedfrom either or both the expansion wall 109 and the deflection

Jan. 14,20109

wall 101 depending on the respective geometries of the vari-ous embodiments of the Type-2 nozzle 200. In the Type-2nozzle 200, the volume of the Type-2 over-expanded region218 immediately downstream of the skimmer 112 is reducedas compared to the similar over-expanded region 118 shownin the Type-l nozzle 100. This relatively reduced Type-2over-expanded region 218 the size of the overall flow sepa-ration from the expansion wall 109 and there is a correspond-ing reduction in the size of the recirculat ion zone that formswithin the over-expanded region and allowing a greater por-t ion of the overall flow through the expansion nozzle 102 toremain supersonic and deflected toward the deflection wall101.[0106] As a result of the extended supersonic flow condi-tion created by the extension of the expansion nozzle 102, thereduced pressure of the process gas results in a cooled orsub-temperature region within the Type-2 nozzle 200 wherethe flow is maintained at a reduced temperature due to aero-dynamic velocity and expansion effects and is extended up tothe region of the Type-2 nozzle 200 skimmer 112. In stillanother embodiment of the Type-2 nozzle 200, so a portion isupstream of the expansion nozzle, the skimmer 112 is placedwithin the expansion nozzle 102, upstream of the expansionnozzle exit 107.[0107] The Type-2 nozzle 200 also util izes a rounded, con-tinuous linear, or gentle transition along the expansion wall109 from the expansion nozzle exit 107 into the Type-2 over-expanded region 218. This is compared to the relativelyabrupt transition, piecewise linear transition along the expan-sion wall 109 present depicted in the Type-l nozzle 100described above. Infact, as shown inmore detail inthe NozzleFlow section below the Type-2 over-expanded region 218results in significantly less pressure and temperature recoveryand increased velocity of the process gas flow along theseparation flow path 130. This means that the mean velocityof the process gas flow through the Type-2 over-expandedregion 218 at a greater velocity, with significant portions ofthe flow greater than Mach 1.0 when the beam of gasexhausted from the expansion nozzle exit 107 impinges theskimmer 112. As a result of the extended supersonic flowcondition created by Type-2 over-expanded region 218, thereduced pressure of the process gas results in a cooled orsub-temperature region within the Type-2 nozzle 200 wherethe flow is at a reduced temperature due to velocity effects, isextended up to the region of the Type-2 nozzle 200 skimmer112. Thus, inthe case of a separation nozzle adapted to at leastpartially condense one or more of the constituents of theprocess gas flow, the reduced temperature recovery allowseither partial or full delay in the re-vaporization of the con-densate unti l after the process gas passes downstream of theskimmer throat 103.[0108] In the embodiment of the Type-2 nozzle 200depicted in FIG. 2a, the expansion nozzle exit 107 located atthe angle (uexit) of about 130 degrees. In other embodimentsthe expansion nozzle exit 107 is located at an angle (uexit) ofbetween about 120degrees to about 180degrees. In still otherembodiments the expansion nozzle exit 107 is greater thanabout 180 degrees. In some embodiments wherein the expan-sion nozzle exit 107 is greater than an angle (uexit) of 180degrees the skimmer 112 is shifted upward greater than anangle (uexit) of about 180 degrees.[0109] The embodiment of the supersonic Type-2 nozzle200 depicted is configured with embodiments of featuresidentified previously in the embodiments of the Type-l


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nozzle 100 presented above, including: an inlet gas reservoir106, a expansion diffuser 105, and a deflection diffuser 104, adeflection wall 101, an expansion wall 109, an expansionnozzle exit 107, (at an angle (uexit) of at least about 1200degrees from the nozzle throat 108), a separation skimmer112, with tip 124, a nozzle throat 108, a skimmer throat 103,and the expansion nozzle 102. The tip 124 of the separationskimmer 112 in one embodiment is a substantially sharp tipwith a radius of curvature less than about 0.05". In anotherembodiment the tip 124 of the separation skimmer 112 is asubstantially sharp tip with a radius of curvature less thanabout 0.01". In still another embodiment, the tip 124 of theseparation skimmer 112 has a radius of curvature less thanabout 0.0002".4.3 Twin Skimmer Separation Nozzle[0110] Another embodiment of an aerodynamic separationnozzle is depicted in FIG. 2b. This embodiment depicts a twinskimmer nozzle 260 or a separation nozzle that utilizes acombination of centrifugal force, aerodynamic forces, andexplicit shock effects to enhance separation ofthe gas species.As apparent to one of ordinary skill in the art, the otherembodiments of the separation nozzle presented herein alsoutilize, in part, shock effects from the beam of process gasflow impacting the skimmer 112 to cause separate and con-centrate of the constituents of the gas.[0111] As readily apparent to those of ordinary skill in theart , embodiments of the twin skimmer nozzle 260 are adapt-able to perform in a similar manner to a Type-l nozzle 100 ora Type-2 nozzle 200. The twin skimmer nozzle 260, similar tothe other embodiments of the separation nozzles describedherein, has a twin skimmer inlet reservoir 206 for acceptanceof the process gas to be separated. As known to those of skil lin the art, some embodiments of the present separationnozzle, including the twin skimmer nozzle 260 described inthis section may also include a balance gas mixed with the gasto separated to create a process gas that comprises a mixtureof the constituents of the process gas and the balance gas tomodulate the aerodynamic and transport properties of themixed gas. Similar in operation to the other embodiments ofthe separation nozzle, the incoming process gas is pressurizedand present in the twin skimmer inlet reservoir 206. Thepressure differential urges the gas into the nozzle throat 108.[0112] After entering the nozzle throat 108, the process gasflow along the separation flow path 130 through the expansionnozzle 102. The expansion nozzle 102 causes the process gasto accelerate, with commensurate reduction in pressure andtemperature using the same principles described with respectto the Type-l nozzle 100 and Type-2 nozzle 200 embodimentsdescribed in more detail above. Similarly, the expansionnozzle 102 is adapted by one of ordinary skill in the art toachieve a desired expansion ratio for the process gas to accel-erate to the desired velocity and, in some embodiments, toachieve a desired aerodynamically induced cooling due to theexpansion ofthe process gas within the expansion nozzle 102.[0113] In contrast to the embodiments of the Type-l nozzle100 and the Type-2 nozzle 200, the twin skimmer nozzle 260utilizes a pair of skimmers, namely a deflection skimmer 264and an expansion skimmer 262. The tips ofboth the deflectionskimmer 264 and the expansion skimmer 262 in the embodi-ment depicted protrude slightly through the channel exit 242into the twin-skimmer over-expanded region 268. In otherembodiments, not depicted, the expansion nozzle 102extends to an angle (uexit) of about 180 degrees and the tips of

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both the deflection skimmer 264 and the expansion skimmer262 extend into the expansion nozzle 102 past the expansionnozzle exit 107. In still other embodiments, also not depicted,the deflection skimmer 264 and the expansion skimmer 262are parallel to the channel exit 242. In still other embodi-ments, also not depicted, the deflection skimmer 264 and theexpansion skimmer 262 are above the plane defined by thechannel exit 242.[0114] In the embodiment of the twin skimmer nozzle 260depicted in FIG. 2b, the expansion nozzle exit 107 located atthe angle (uexit) of about 130 degrees. In other embodimentsthe expansion nozzle exit 107 is located at an angle (uexit) ofbetween about 120degrees to about 180degrees. In still otherembodiments the expansion nozzle exit 107 is greater thanabout 180 degrees. In some embodiments wherein the expan-sion nozzle exit 107 is greater than an angle (uexit) of 180degrees the deflection skimmer 264 and expansion skimmer262 are shifted upward greater than an angle (uexit) of about180 degrees.[0115] The deflection skimmer 264 and the expansionskimmer 262 produce shock structures in the gas stream nearthe channel exit 242. These shock structures further enhanceseparation effects. The initial stratification of the process gasflow or stream occurs when it accelerates and passes throughthe expansion nozzle 102 athigh speed, in a similar manner tothe other embodiments of the separation nozzle, such as theType-l nozzle 100 and the Type-2 nozzle 200 describedabove. This stratification causes the heavier species tomigrate toward the deflection wall 101, away from the centerchannel 244 of the twin skimmer nozzle 260. Due to thesupersonic velocity of the gas, shock structures or standingpressure waves are formed off of the tips of the deflectionskimmer 264 and the expansion skimmer 262. These shockstructures encourage the flow already along the expansionwall 109 and deflection wall 101 to continue flowing in thatdirection through the channel exit 242, while the center paththrough the shock structures and the channel exit 242 accu-mulates higher mass species due to momentum required topass through the overlapping shock structures. Thus, the twinskimmer nozzle 260 has three separate outputs: a first heavysteam of the most pure separated gas collected at a twinskimmer deflection diffuser 204, a second heavy stream atthecenter diffuser 266 via the center channel 244, and a lightstream collected at an a twin skimmer expansion diffuser 205.4.4 Nozzle Plate[0116] FIG. 3a is a perspective view of an embodiment ofthe Type-2 nozzle 200 geometry configured into a nozzleplate 300. The nozzle plate 300 in this embodiment isdepicted as a circular plate, although other shapes are readilyadaptable using the knowledge of one of ordinary skil l in theart. In one embodiment, the nozzle plate 300 material isselected to be substantially thermal or heat-conductive. Theoverall thickness of the nozzle plate 300 is adapted to be aratio relat ive to the nozzle throat 108 such that the area of thenozzle throat 108 determines the mass flow rate of the gas,based on the density, pressure, and temperature of the gas asknown to those of ordinary skill in the art.[0117] The nozzle plate 300 comprises features typified byan embodiment of the Type-2 nozzle 200, such as an inlet gasreservoir 106, a deflection diffuser 104, an expansion diffuser105, an expansion wall 109, an expansion nozzle exit 107, adeflection wall 101, and a skimmer 112. The nozzle plate 300further comprises mounting bolt holes 314, and locating pin


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holes 315. In this embodiment, the nozzle plate 300 com-prises a trio of mounting bolt holes 314 and a pair oflocatingpin holes 315. The locating pin holes 315 are adapted usingtechniques known to those of ordinary skill inthe art to locatewithin a desired tolerance, each nozzle plate 300 relative toother structures surrounding the nozzle plate 300, includingother adjoining nozzle plates 300 (not shown in FIG. 3a) thatare assembled to increase the overall height of the separationnozzle. Similarly the mounting bolt holes 314 are placed andfabricated with sufficient tolerance to allow bolts or otherfasteners to be run through the mounting bolt holes 314 ofeach nozzle plate 300 and other mounting structures that havebeen located by locating pins placed through the locating pinholes 315. The bolts that run through the mounting bolt holes314 of the embodiment depicted provide compressive forcesto the nozzle plate 300 to assist in forming an effective sealwith other nozzle plates 300 and other supporting structureswhile the locating pins that are inserted within the locating pinholes 315 lateral ly constrain movement of the nozzle plate300. Persons of ordinary skill inthe art may adapt the embodi-ment oflocating pinholes 315 and mounting bolt holes 314 toaccomplish different goals, and in some embodiments evenremove the either or both of the locating pin holes 315 andmounting bolt holes 314.[0118] The nozzle plate 300 is fabricated using techniquesknown to those of ordinary skill in the art, including fabrica-tion processes such as machining, electro-discharge machin-ing, laser ablation machining, forming, forging, extruding,and photo-lithographic etching. Fabrication processes thatresult in close-tolerances and smooth surfaces are desirable,and in the case of smaller separation nozzle embodiments,advantages are gained from the electro-discharge and etchingprocesses has additional util ity. The nozzle plate 300 in oneembodiment uses a relatively highly thermally conductivematerial to enhance temperature control of the nozzle surfaceand, in some embodiments, allow heat transfer to occurbetween the nozzle plate 300 and the process gas containedwithin the separation nozzle.4.4.1 Twin Nozzle Plate[0119] In another embodiment of the present system andmethod, a pair of separation nozzles are integrated into asingle nozzle plate, in a twin nozzle plate 330 configuration,an embodiment of which is depicted in FIG. 3b. The twinnozzle plate 330 comprises a left Type-1 nozzle 340 and rightType-1 nozzle 342 that are both embodiments of the Type-1nozzle 100 with adaptation for use in a twin nozzle plate 330configuration.[0120] The left Type-1 nozzle 340 and the right Type-1nozzle 342 are both embodiments of a general Type-1 nozzle100 configured with a shared heavy diffuser 344. The rightType-1 nozzle 342 is a mirror of the left Type-1 nozzle 340and thus the respective left separation flow path 350 and rightseparation flow path 352 are oriented so the gas flows togetherto a common center where the shared heavy diffuser 344 isplaced. In another embodiment, the left Type-1 nozzle 340and right Type-1 nozzle 342 share a combined inlet reservoir(not shown) such that the respective nozzle inlet gas reser-voirs 106 are combined into a single shared or combined inletreservoir where inlet process gas enters the separation nozzleand flows into the nozzle throat 108.[0121] The embodiments of the left Type-1 nozzle 340 andright Type-1 nozzle 342 depicted in FIG. 3b in one embodi-ment are adapted for the separation of a si licon process gas,

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such as silane (SiH4). In this application embodiment, thepressure at the inlet reservoirs 106 is approximately 60 psig.The nozzle throat 108 in this embodiment has a cross-sec-tional area measured at its narrowest point with a planar widthof about 0.0065" along the dimension (A-A') shown in FIG.3b, and a height of about 0.195" (B-B'). The expansion nozzle102 tapers continuously from the nozzle throat 108 throughan angle (uexit) of about 130 degrees at the expansion nozzleexit 107. The expansion nozzle exit 107, in the embodimentdepicted, has a planar width of about 0.0115" along thedimension (B-B') and a height of about 0.195".[0122] In these embodiments the channel height of the leftType-1 nozzle 340 and right Type-1 nozzle 342 is a constantdefined by the thickness ofthe twin nozzle plate 330. The topand bottom surfaces of the left Type-1 nozzle 340 and rightType-1 nozzle 342 are defined by the interior surfaces of a topplate (not shown) and a bottom plate (not shown) that areaffixed tothe upper and lower surfaces of the twin nozzle plate330 via one or more mounting bolt holes 314 or other meansfor affixing and bonding such plates known to those of ordi-nary skil l in the art.[0123] When the process gas enters the expansion nozzle102, there is a short period of turbulent transition upon entrypast the nozzle throat 108. However, this initial turbulencequickly smooths out and the flow begins to accelerate withdifferential velocities developing across the throat dimension110 due to viscous wall effects within the nozzle throat 108and within the expansion nozzle 102 for the first severaldegrees down the flow path through the first angle (o.) of about45 degrees. As the flow through the expansion nozzle 102fully develops toward the nozzle throat or expansion nozzleexit 107, a relat ively high Mach flow is generated and main-tained in the core of the flow so the magnitude of the meanvelocity vector of the flow near the expansion nozzle exit 107is greater than Mach 1.0. As described above, the flow of theprocess gas within the expansion nozzle 102 is substantiallynonseparated without any substantial or significant recircu-lat ion due to the full expansion of the process gas within theexpansion nozzle 102.[0124] As can be readily seen by those of ordinary skill inthe art, a variety of nozzle plate configurations comprisingmultiple separation nozzles of the various separation nozzletypes presented herein are combinable. In one illustrativeexample, a penta-nozzle plate comprises five separate Type-2nozzles 200 thereby enabling a single nozzle assembly com-prising penta-nozzle plates to provide five separate separationnozzles for use. Other configurations of multiple separationnozzles, including separation nozzles of various embodi-ments and configurations adapted to a variety of flow rates arereadily adapted by those of ordinary skill in the art .4.5 Nozzle Module[0125] FIG. 4a is a perspective side-view of an embodimentof a nozzle module 400. The nozzle module 400 is used tomount a nozzle plate assembly 414 and provide fluidic andthermal connections to the separation nozzle. The nozzleplate assembly 414 is comprised of one or more nozzle plates300 that are aligned via the locating pinholes 315 and mount-ing bolt holes 314 such that the desired overall separationnozzle thickness is achieved. The nozzle module is furthercomprised of an upper module end 401, a lower module end402, fastening bolts 404, and the nozzle module locating pins403. The nozzle module locating pins 403 and the locating pinholes 315 in nozzle plates 300 that comprise the nozzle plate


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assembly 414 are adapted to provide a locating fit the indi-vidual nozzle plates 300 and the lower module end 402. Inother embodiments, the module locating pins 403 continuethrough the nozzle plate assembly 414 and also locate theupper module end 401. In the embodiment depicted in FIG.10, the nozzle module 400 is formed into a substantiallycanister shaped package. In this manner a canister or nozzlemodule 400 forms a separation nozzle assembly that providesthe separation nozzles assembled into a modular element thatis suitable for connection to external fluid handling devices orpre- and post-processing elements such as a pre-conditioningsystem like the nucleate generation conditioning system 2500shown in FIG. 24.[0126] The fastening bolts 404 in the embodiment depictedare adapted to freely run through the mounting bolt holes 314on the nozzle plates 300 that comprise the nozzle plate assem-bly 414 and fastening into threaded holes inthe lower moduleend 402. In other embodiments the fastening bolts 404 arethrough bolts that are tightened via an external threaded nut.Persons of ordinary skill in the art recognize that other meth-ods are available for fixing the upper module end 401 to thenozzle plate assembly 414 and the lower module end 402,including for example, crimping, welding, soldering, braz-ing, taping, gluing, diffusion bonding, cementing, epoxies,adhesives, cam locks, and spring loading.[0127] In one embodiment, the nozzle module 400 is fab-ricated from a relatively thermally conductive material, andthe upper module end 401 and lower module end 402 areadapted to contain and seal the nozzle plate 300 against high-pressure or vacuum leaks. In still other embodiments, theupper module end 401 and the lower module end 402 areadapted to include a thermal management system to controlthe heat transfer from the nozzle module 400. The thermalmanagement system in one embodiment comprises a series ofpassages within or in a thermally conductive wrappingaround the nozzle module 400 to remove or transfer heat fromthe nozzle module 400. In another embodiment, the thermalmanagement system includes a series of radiators or otherpassive, and semi-passive cooling systems. In stil l anotherembodiment, the thermal management system includes resis-tive heaters. In yet another embodiment, combinations of theforegoing and other heat transfer systems known to those ofordinary skill in the art are used to manage heat flow to andfrom the nozzle module 400.[0128] FIG. 4b shows two views of embodiments of theupper module end 401 and lower module end 402 of thenozzle plate assembly 414. The upper nozzle module end 401is fabricated from thermally conductive material, and com-prises three reservoir ports; the inlet reservoir port 407, theheavy reservoir port 408, and the light reservoir port 411.Each of the reservoir ports 407, 408, and 411 are fitted forpipefittings at the top of the upper module end 401, and beloweach fitt ing of each of the reservoir ports, 407, 408, and 411pass through the length of the upper module end 401 and exitthe upper module end 401 at its bottom or lower face thatwhen assembled with the nozzle module 400 abuts the uppersurface of the nozzle plate assembly 414.[0129] The lower module end 402 similarly comprisesthree ports, the lower inlet port 409, the lower light port 412,and the lower heavy port 410 that align with the respectiveinlet gas reservoir 106, the deflection diffuser 104, and expan-sion diffuser 105 present in the nozzle plate 300 that comprisethe nozzle plate assembly 414. In one embodiment, only thelower heavy port 410 is machined for a tube fit ting, while the

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lower inlet port 409 and the lower light port 412 are sealed toatmosphere. In other embodiments, various combinations ofopen and closed ports are available to those of ordinary skillin the art and adapted based on knowledge of the overallseparation equipment configuration and routing of processgas flows.[0130] When the nozzle plate assembly 414, the uppermodule end 401, and lower module end 402 are assembled ina suitable fashion to form the nozzle module 400, it can beseen that the inlet reservoir port 407, heavy reservoir port 408and light reservoir port 411 are in direct fluid contact withinlet gas reservoir 106, deflection diffuser 104 and expansiondiffuser 105 of the nozzle plate 300 that comprise the uppersurface of the nozzle plate assembly 414. Similarly, the cor-responding lower heavy port 410, lower light port 412, andlower inlet port 409 the lower module end 402 are also indirect fluid contact (i.e. f luidicly coupled) with

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