CN100525882C - Fluid purification system with low temperature purifier - Google Patents
Fluid purification system with low temperature purifier Download PDFInfo
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- CN100525882C CN100525882C CN 200580036366 CN200580036366A CN100525882C CN 100525882 C CN100525882 C CN 100525882C CN 200580036366 CN200580036366 CN 200580036366 CN 200580036366 A CN200580036366 A CN 200580036366A CN 100525882 C CN100525882 C CN 100525882C
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Abstract
A system and method for processing a matrix fluid to remove one or more impurities (such as moisture from a process gas). The purifier includes a pre-cooler that receives the matrix fluid and cools the matrix fluid to a second, lower temperature. A container is provided to contain a purifier element made up of a high surface area material. The container includes an inlet for receiving the matrix fluid from the pre-cooler and an outlet for outputting the matrix fluid after it is forced to flow through the purifier element. The purifier includes a cooler in thermal contact with an outer surface of the container to cool the outer surface of the container to a purifying temperature, which is selected to be below the ambient temperature and above a phase change point of the matrix fluid and is typically in the range of about 0 to -200 DEG C.
Description
Cross-reference to related applications
The application requires to submit on October 25th, 2004 is entitled as ＂ PICO TRAP ' Cryogenic Purifierfor Removal of Impurities Fluids from a Matrix Fluid, the U.S. Provisional Application the 60/621st of ＂, the priority of the non-temporary patent application of the U.S. that is entitled as ＂ Fluid Purification System withLow Temperature Purifier ＂ that No. 871 and on October 17th, 2005 submit to, these applications all are incorporated by reference into this paper in full.
Background of invention
1. invention field:
The present invention relates to the fluid purification field, comprise the ultra-pure process gas purifying field that for example is used for semi-conductor industry, more particularly relate to fluid purification system, the invention still further relates to relevant method, this method is used the purifier (i.e. Leng Que purifier or low temperature purifier) with cooler, and use remains on the temperature of reduction or the temperature purifying under the cryogenic conditions or filter medium or medium mixture (for example high surface area material) and remove impurity from matrix gas.
2. description of the Prior Art:
People to the demand of impure hardly process gas and other fluid in continuous increase.Many production applications of gas and other application need impurity content (for example moisture) are equal to or less than 10/1000000000ths (10ppb), and these gases often are considered to ultra-pure gas.
Semi-conductor industry provides an ever-increasing object lesson of demand to ultra-pure process gas or fluid (for example needing by removing matrix gas or the fluid that impurity carries out purifying).Along with semiconductor integrated device becomes littler, use the device of semiconductor integrated device to become complicated more, to the continuous increase of the requirement of the physical property of the semi-conducting material of reality and chemical property, so that its character and desirable intrinsic semi-conducting material character are more approaching.Semi-conductive manufacturing comprises the reactant gas that use is made up of various elements.In the semiconductor manufacturing, also use the manufacturing process of metal-organic chemical vapor deposition (MOCVD) manufacturing technology relevant and so in addition with other.In these technologies, the purity of reactant gas has very significant effects to the quality of the semiconductor devices that makes, and the quality of the described semiconductor devices of making comprises its electronic property and feature specifically.Therefore, the demand to ultra-pure process gas is increasing always in the microelectronics industry.Semi-conductor industry only is an example that ultra-pure process gas is had requirements at the higher level, in order to satisfy these requirements, the method for gas superelevation purifying has been carried out science and technology research widely, has obtained progress.
Ultra-pure gas normally makes by the following method: use the purification system with purifier (it uses various filtrations or purification media and/or mechanical filter and other device) that matrix gas or process gas are handled, from matrix gas or process gas, remove impurity, for example remove moisture, make moisture in described matrix gas or the process gas less than 10ppb.At present, it is the medium that is used for purifier about preparation that most research and development is made great efforts, and it can remove impurity effectively when gas (or other fluid) flows through purifier.High surface area material forms base material through being commonly used for the purifier medium, the base material of minimum bead etc. for example, and this base material places purifier canister, forces matrix gas or process gas to cross described base material with specific flow velocity and pressure current.
Obtained to remove the trace impurity of producing in the fluid by development efforts, make the purifier medium of impurity content much smaller than 1,000,000/(1ppm), but in some cases, the characterization of adsorption of purifier medium has limited the Impurity removal level that specific purifier medium can reach.For example, some are used for the purifier medium of semi-conductor industry or material and have been recorded or demonstrated and can remove moisture from the matrix gas (for example HCl gas) in the pressure current downflow of environment temperature and about 30psig, make that moisture is 150-200ppb.Yet such content can't satisfy the demand of semi-conductor industry, and semi-conductor industry still needs its many moistures that are used for the process gas (for example HCl gas) of indoor and chip cleaning application to be equal to or less than 10ppb.
Therefore, people still need to be used for substrate fluid is carried out the improved method and system of purifying, and for example preparation is used for the improved method and system of gas of the higher degree of semi-conductor industry and many other application.Preferably, these method and systems will be designed to be able to satisfy the requirement of ultra-pure gas, simultaneously can also be compatible with many existing gas delivery systems, and can use many existing purifier media and/or high surface area material.
Summary of the invention
The invention provides a kind of system's (with relevant method) that is used for purifying substrate fluid (for example chemical gas), this system can be by improving removal to impurity with purification media or material cooled to being lower than environment temperature.This system generally includes the jar that the purifier element is housed, and described purifier element is for example high surface purified material, previously prepared nickel or stainless steel particulate filter etc.Cooler with described jar thermo-contact is provided, be used for described jar and the purifier element that wherein comprises be cooled to and be lower than environment temperature, normally be cooled to than environment temperature low 20 ℃ or more temperature, but this temperature is higher than substrate fluid in the operation flow velocity of purification system and the transformation temperature under the pressure.In some embodiments, provide forecooler, be used at described substrate fluid with before the purifier element contacts in the upstream of described purifier canister, with its for example be cooled near or reach the temperature of cleansing temp.
More particularly, provide low temperature purifier, be used for handling substrate fluid, to remove one or more impurity (for example from process gas, removing moisture).Described purifier comprises the forecooler that is used for receiving the substrate fluid with first temperature, pressure and flow velocity.This forecooler cools off substrate fluid, the substrate fluid that output has second temperature that is lower than described first temperature.In described purifier, comprise the purifier element of making by a large amount of high surface area materials, provide a container to hold described purifier element.Described container comprises and is used for receiving from forecooler the inlet of substrate fluid, and be used for force substrate fluid flow through this purifier element after with the outlet of its output.Described purifier also comprises the cooler that contacts with the outer surface heat of container, this cooler is used for the outer surface of container is cooled to cleansing temp, this temperature is selected, made it be lower than environment temperature, and be higher than described substrate fluid in the pressure of fluid and the transformation temperature under the flow velocity.
Described forecooler can cool off with the independently cooling device of purifier, perhaps can use the same cooler that is used for cooling off purifier canister to cool off.Usually forecooler is cooled off, make substrate fluid second temperature (or output temperature of forecooler) near or approximate cleansing temp.Usually at least about hanging down 20 ℃ than environment temperature, more preferably cleansing temp is about 0 ℃ to-200 ℃ to cleansing temp.Container can be many kinds of forms, in one case, container is a stainless steel tube, be provided with the metal particle filter in the pipe, this filter is by sintering, compacting and/or the nickel of plating and/or stainless steel and/or corrosion resisting alloy (for example HastelloyTM etc.) or be applicable to that other alloy of concrete application makes.In another case, described high surface area material is the combination of modenite, zeolite, aluminium oxide, silica, carbon, molecular sieve or these materials, and described container is the jar that is used for holding these purifier base materials.In another embodiment, described high surface area material is coated with the material that reactive metal or other design are used for removing concrete impurity.
The accompanying drawing summary
Fig. 1 is the schematic diagram of purification system of the present invention or equipment, and it comprises the cooler of the temperature that is used for reducing purifier canister and interior material (for example purifier material and mechanical filter etc.) thereof;
Fig. 2 is according to another kind of purification system of the present invention like the system class with Fig. 1, but difference is, the purification system of Fig. 2 has the forecooler stage (pre-cooler stage), and the same apparatus or the system that are used for cooling off purification phase (purification stage) in this stage are cooled off;
Fig. 3 shown according to purification system of the present invention, shown an embodiment of the temperature required cooler that the cleansing temp or the filtration temperature that are used for the purifier material remain below environment temperature among the figure;
Fig. 4 is that specific purifier medium is with the variation of temperature graph of a relation;
Fig. 5 and Fig. 6 have shown use purifier medium under environment temperature and temperature that is reducing or low cleansing temp, or use cold-trap from the dewatered test result of HCl gas;
Fig. 7 has shown the semiconductor manufacturing decorum that comprises low temperature purifier of the present invention;
Fig. 8 has shown the another kind of semi-conductor manufacturing system similar with semi-conductor manufacturing system shown in Figure 7, the semi-conductor manufacturing system of Fig. 8 does not have additional purifier, comprises forecooler that is positioned at the low temperature purifier upstream and the heater that is positioned at the low temperature purifier downstream.
Detailed Description Of The Invention
Generally, the present invention relates to be designed to be used for removing the medium of impurity or the purifier of medium mixture by comprising, thereby from described substrate fluid, remove the equipment/system and method for one or more impurity by the substrate fluid that makes chemical gas or process gas and so on.Outstanding feature is, described purifier medium or medium mixture are cooled to the cleansing temp that is lower than environment temperature, in some cases, described cleansing temp is far below environment temperature, for example hang down 20-200 ℃ (for example when environment temperature is about 20 ℃ than environment temperature, cleansing temp is 0 ℃ to-200 ℃ or lower, and extremely low cleansing temp provides " low temperature-purifier ").This low temperature or more the purifier of low temperature be specially adapted to from have more lower boiling substrate fluid (for example chemical gas), remove one or more high-boiling-point impurities.Perhaps, if select suitable purified material, can reduce the more lower boiling impurity that has in the more high boiling matrix gas.In purifier, material, purifier medium or the medium mixture of selecting placed container or jar, or remain on by alternate manner in the flow path of fluid.Described purifier is designed to be used for described container or jar and interior material thereof are cooled to selected cleansing temp, in an exemplary embodiment, cooler is provided, this cooler is cooled to the preset temperature that is lower than environment temperature with the outer wall of purifying jar/container, make purifier material, medium, media (media) or device remain on cleansing temp (for example approaching), thereby improve the purification efficacy of purifier with the temperature of described jar.
Fig. 1 has shown an embodiment of purifier, can be referred to as the purifier, low temperature purifier and/or the low temperature-purifier that reduce temperature herein.Aforesaid purifier 100 is designed to be used for reducing the temperature of purifier material or medium 140, described purifier material or medium 140 are used for removing impurity from the substrate fluid of chemical gas and so on, and described substrate fluid will be as the process gas that is used for making semiconductor devices etc.For this reason, show among the figure that purifier 100 has forecooler 110, this forecooler 110 has and is used for receiving first temperature T
1The inlet 112 of input fluid, and be used for that output is cooled to or " precooling " to the second lower temperature T
2The outlet of output fluid.This outlet 114 is communicated with inlet 132 fluids that lead to jar 130 usually, described jar 130 is used for holding (if purifier material of use bead etc. and so on) or carrying (if using mechanical medium) purifier material, medium or media (these sayings can be exchanged use in this article, and can not be construed as limiting describing or inventing).
Forecooler 110 shown in the figure is independent device in the purifier 100, comprises pipeline 118, and this pipeline is being guided the fluid of input by sufficiently long path, and this path is enough to the cooling that provides required, and fluid is cooled to second temperature T
2, this temperature is generally selected in and equals or near the cleansing temp of material 140.Usually preferably the fluid of input or the substrate fluid that enters are carried out precooling, make the fluid of inlet 132 of input jar 130 can not cause heating to the purifier material 140 that touches, this heating can improve the purification efficiency required to the purified material 140 of described cooling.
Inlet 132 by leading to jar or storing apparatus 130 is with the quencher moiety of the fluid input purifier of precooling, with purified material, media and/or medium 140 then.With cooler 120 described material 140 is remained on cleansing temp, with these material 140 purifying substrate fluids, remove impurity, the fluid behind the purifying is in the 3rd temperature T
3Following output, this temperature are generally equal to or near cleansing temp (but implementing the time of the present invention, this temperature can be omited high or lower slightly).Show among the figure that cooler 120 contacts with jar 130 along tank skin 136, in the embodiment shown, described cooler 120 is used for the temperature of tank skin 136 is reduced to predetermined temperature, makes the temperature of the purified material 140 in the container 130 reduce to required cleansing temp then.
Because the heat transfer efficiency in the material 140 is very low, the temperature of cleansing temp or material 140 is usually above the temperature of tank skin 136, may be in jar 130 varied slightly (for example, the temperature of the material 140 adjacent may than approximate more near the temperature of tank skin 136) away from the temperature of the material 140 (for example material 140 of jar 130 centers) of tank skin 136 with tank skin 136.Therefore in the process of operation purifier 100, jar 130 should be cooled to and be lower than the required temperature of described material 140, this temperature difference is along with the structure of jar 130, the material and the material 140 of tank skin 136 change.In the following discussion,, consider that the temperature of material 140 can be omited height, cleansing temp can be called the temperature of tank skin 136 for the ease of discussing and experimental measurement.(not shown) can provide the heat-exchange apparatus that extends into jar inside in some embodiments, with the heat transfer of improvement with material 140, material 140 more effectively is controlled at required cleansing temp.
The inventor expects that described low temperature purifier 100 is unit of a kind of compactness, can be unit or be incorporated in the bigger equipment independently.Described jar 130 can be encapsulated in the jacket of the cooling device that comprises described cooler 120.The use of can connecting with the purification unit of routine as shown in Figure 7 of described low temperature purifier 100 is perhaps used separately as shown in Figure 8.
In conventional embodiment of the present invention, material, purifier medium or the medium mixture of selecting 140 placed container or the jar 130 that cools off with cooler 120.110,120 used cooling means or devices almost can be well-known arbitrarily can be used to implement method of the present invention or devices.For example, forecooler 110 and cooler 120 (can use identical or different cooling devices or method) can use refrigeration system, thermoelectric (al) cooler (Stirling, Peltier etc.), solid or liquid cooling bath, eddy current cooling, Venturi cooling or other cooling device or method arbitrarily.Key character of the present invention is not used concrete cooling technology, but purifier 100 is designed and operates, fluid or substrate fluid that use remains below environment temperature, preferably significantly be lower than purifier material, media and/or 140 pairs of inputs of medium under the condition of environment temperature carry out purifying, significantly improve described material 140 is removed impurity from the substrate fluid of flow through purifier jar or container 130 effect.
The inventor thinks that the theory of using low-temperature surface to remove impurity from the fluid of semiconductor production gas and so on is novel theory, will bring many useful application in the years afterwards.In the fluid purification device medium of operating by initial surface adsorb traces impurity (for example material or medium 140), the purification efficacy of particular medium is to determine from the surperficial adsorption equilibrium of matrix by the object material.Reduce surface temperature and can improve physical absorption balance and chemisorbed balance simultaneously owing to slow down the speed of desorption usually (for example referring to A.Adamson; ＂ The Physical Chemistry of Surfaces; ＂ the 5th edition, New York:WileyInterscience, 1990).The a large amount of examples that in whole Surface Science documents and industrial technology, shown this phenomenon.In an example of this phenomenon, in the high vacuum cryogenic pump, use cryogenic temperature to improve the ability that molecular sieve is captured the trace gaseous substance and obtained the vacuum of raising.But before the present invention, the theory of using low-temperature surface raising purifier material to remove impurity from fluid is not behaved and is understood or know, and the inventor thinks that this theory can be used for handling a large amount of chemical gas and other fluid.Will make the end user can obtain purity that conventional method is beyond one's reach by the present invention.In addition, by the present invention described herein, can remove the specific impurities that those can't effectively be removed by the physical absorption and the chemisorbed of routine.
In the operating process of low temperature purifier according to the present invention (for example purifier 100),, should consider some conditioned disjunction operating parameters for the result of the purifying that is improved.At first, the operating temperature of purifier 100 or cleansing temp (for example temperature of the wall 136 of the container 130 that comes close to or in contact with of material 140) should remain on and be higher than substrate fluid the specific operation pressure of described matrix or input fluid and any transformation temperature under the flow velocity (be described transformation temperature should as the lower limit of cleansing temp scope).For example, if described substrate fluid is a gas, then operating temperature preferably remains on and is higher than condensation point.If substrate fluid is a liquid, then operating temperature preferably remains on and is higher than freezing point, if described substrate fluid is a solution, then operating temperature preferably remains on the saturation point that is higher than solute.
Secondly, the adsorption equilibrium costant of specific impurities (for example target impurity of removing from described matrix or input fluid) on purifier medium (for example element 140 of jar 130) preferably makes the object removal amount to be issued in the temperature of the transformation temperature that is higher than substrate fluid.The 3rd, should select purifier matrix (for example element 140), making it is being stable to substrate fluid under operating temperature of purifier or under cleansing temp.
When the purifier material of routine is used for element 140, select described purifier material usually, this is because known its can be removed one or more target impurity at ambient temperature from substrate fluid.Then in the process of operation purifier 100, the temperature of purifier (the perhaps temperature at wall 136 places of jar 130) is reduced to chosen temperature, this temperature is higher than described matrix or the pressure of input fluid substrate fluid in described purifier 100 and the condensation point under the flox condition, but enough low again, be enough to improve the absorption of impurity to the purifier surface.In some cases, described operation or cleansing temp can be any temperature that is lower than environment temperature.But more preferably, the operating temperature of selected purifier is far below environment temperature, and for example than low 20-220 ℃ or more of environment temperature, this is because these temperature ratios are easier to obtain, and the absorption that can improve purifier material or medium to a greater degree.
In some embodiments, described sorbing material or purifier material 140 can be high surface area materials arbitrarily, as long as when the surface of these materials contacts with fluid, can get final product by the impurity that one or more mechanism is removed in the substrate fluid.The base material that for example described purifier material 140 can be made up of the purified material of routine, the material that for example is used for semi-conductor industry, it comprises base material or the purifier material of describing in detail in modenite and/or the following patent: United States Patent (USP) the 6th, 110, No. 258; The 6th, 733, No. 734; The 6th, 461, No. 411; The 6th, 425, No. 946; The 6th, 783, No. 577; The 6th, 783, No. 576; With the 6th, 790, No. 358, these full patent texts are incorporated by reference into this paper.Described base material 140 can be made up of metal, organic material and/or inorganic material and/or carbon.Except absorption, also can reduce to a certain temperature by making cleansing temp, impurity became and was insoluble to substrate fluid this moment, be removed by filtration method, thereby remove impurity in the substrate fluid (for example except material 140 by the precipitation method as medium 140 with purifier medium 140, also can provide filter, under some specific situations, even can replace material 140) with filter as medium 140.Having provided the further raising (impurity content of gained obtains improvement in promptly by the fluid behind the purifying of outlet 134 output purifiers) that expection obtains under reducing purifier temperature and exemplary temperature range Impurity removal renders a service with reference to Fig. 4-6 will describe in detail hereinafter.
In another embodiment, when matrix gas stores and is dissolved in the ionic liquid, can use invention as herein described.In this case, Xiang Guan gas storage is in being the polyion material of liquid states of matter.Then by reservoir vessel being applied vacuum or heating and from ionic liquid, remove matrix gas.When described reservoir vessel is removed matrix gas, very the ionic liquid of small concentration also can come out from reservoir vessel, and this is because the vapour pressure of ionic liquid is non-vanishing.Obviously, shown in the accompanying drawing of Fig. 1 and back, the present invention can be used to remove the ionic liquid (impurity of promptly removing is ionic liquid) of trace from matrix gas.The feature of ionic liquid is low melting point, HMW, the low-vapor pressure material that comprises cation and anionic group.At United States Patent (USP) the 6th, 579, among No. 343 and the U.S. Patent application US2004/0206241 A1 number such ionic liquid has been described, these documents are incorporated by reference into herein in full.The content of the ionic liquid in the matrix gas is generally trace; for example content is 100-1000ppb; content is higher through regular meeting; but after handling by the low temperature purifier (for example purifier 200 of Fig. 2) of each embodiment of the present invention; the content of the matrix gas intermediate ion liquid behind the purifying is less than 100ppb; in some cases even less than 10ppb, thereby make the ultra-pure matrix gas that does not contain described ionic liquid substantially.
Fig. 2 has shown another embodiment of low temperature purifier 200 of the present invention.Purifier 200 is similar with purifier 100, can be used as the part of identical unit or device but difference is forecooler, cools off with identical cooler or cooling device.Purifier 200 also shows: before the fluid behind the purifying is transported to manufacture process or other application site, can make the temperature of the fluid behind the purifying get back to required production fluid temperature (F.T.) by for example heater.In addition, purifier 200 can be used to show: the purifier material can in-situ regeneration to improve purification result.
As shown in the figure, purifier 200 comprises and is used for simultaneously providing for forecooler stage 220 and purification phase 230 cooler 210 of cooling.The input fluid or the substrate fluid that provide to the forecooler stage 220 are in first temperature T
1(for example environment temperature, the inlet temperature of production process or use location etc.).Use cooler 210 to provide cooling, make the temperature of substrate fluid reduce to second temperature T as the forecooler stage 220
2, this temperature preferably is about the temperature of cleansing temp and/or purification media/device 238.In this embodiment of purifier 200, with the fluid precooling that enters to (but as shown in Figure 7, be not that all situations all must be carried out this precooling operation) purifier operating temperature (or be cooled to the interior temperature of following scope: this temperature range comprises the temperature above and below operating temperature, but will be higher than the transformation temperature of described substrate fluid).For example, cooler 210 can force the flow through pipeline in path (for example Wan Qu path) in forecooler stage 220 of substrate fluid to carry out heat exchange with limiting.The purpose in forecooler stage 220 is before substrate fluid enters purification phase 230 substrate fluid to be cooled off, so that the temperature fluctuation purifier chamber or jar 234 in reduced to minimum in the process of operation purifier 200 or it is controlled.When described purification media 238 was undesirable heat conductor (many purifier materials and base material are not always the case), this was a particular importance.
To have second temperature T then
2The direct fluid of precooling comprise the purification unit of container or jar 234 or stage 203 (promptly be used for holding described purified material or install 238 and guiding fluid matrix for example one or more devices of element 238 of flowing through), this purification unit or stage comprise the purification media of one or more target impurity in the substrate fluid after design is used for capturing precooling or install 238.The temperature of described purifying jar 234 is controlled (promptly being brought down below the required cleansing temp of environment temperature) with cooler 210, optionally control the temperature of jar 234 by carefulness, can and/or install 238 and control the purified material, the medium that comprise, make and from substrate fluid, to remove object impurity effectively by for example absorption and/or condensation distinctiveness ground.After use purified material 238 was removed impurity, the fluid behind the purifying was with the 3rd temperature T
3From purification phase 230 outputs, described the 3rd temperature T
3Can with the temperature T of fluid after the precooling
2Identical or basic identical, perhaps temperature and the Impurity removal effect according to material 238 is slightly high or lower slightly.
As shown in the figure, in purifier 200, provide heater 240.From the fluid behind the purifying of purification phase 230 by or guiding by heater 240, have the 4th temperature T to provide
4The production fluid, this temperature can be complementary with the required input temp in manufacture process or use location.In some cases, described purification media 238 is reproducible material or purifier medium, under these circumstances, may need to comprise the regenerative system or the equipment 250 that are communicated with jar or container 234 in purifier 200.Regenerative system 250 can be various forms, and regenerative system is well-known in fluid and the purification for gas industry.Described regenerative system or install 250 and be used in position or under need not the prerequisite that in jar 234, shifts out, purifier medium 238 regenerated.In other cases, can design purifier 200 and purification phase 230 effectively, be used for other parts of jar 234 and/or pipeline and purifier 200 are purged.Described purifier 200 also can be preferably designed to and can insert and replace described purifier medium/device 238, to help the maintenance of purifier 200.Except valve, pressure control device etc., vacuum source also can together be provided, be used for operation and maintenance purifier 200, this is that those skilled in the art can understand.
Fig. 3 has shown another object lesson according to the purifier 300 of theory of the present invention.As shown in the figure, low temperature purifier 300 comprises a pipeline 312 (for example stainless steel pipe/pipeline of 316L SS pipe and so on), this pipeline have the gas that is used for receiving input or fluid inlet and handle remove impurity after, the mouth that the fluid behind the purifying or gas are derived.Described fluid or air-flow are directed to the jar 320 (or purification phase of container/pipeline 312) that comprises purified material or medium 324, and in one embodiment, described purified material or medium are Ni filter frits.Described purified material 324 can also be a high surface area material, for example zeolite, modenite, carbon, aluminium oxide, silica, metal and other combinations organic and/or inorganic substrate or these materials.In addition, in some embodiments, described high surface area material can be used for removing the material coating of specific impurities with reactive metal or other design and/or selection.For example, described reactive materials can be selected from alkaline-earth metal (alkali earth metal), alkaline-earth metal (alkaline earth metal) or transition metal, by selecting to remove specific impurity.
Provide solid-state cooler 330 with described material or install 324 temperature and reduce to required cleansing temp from environment temperature.About this point, described solid-state cooler 330 comprises controller 336, this controller is used for the temperature that the sensor 338 of the outer wall of jar 320 or the surface position of probe sensor (or randomly have in described material/medium 324) senses is responded operating cooler 330.In this embodiment, cooler 330 comprises the heat conductor 332 that links to each other with hot lubricating grease 334, but also can use other cooling device and technology to cool off described material 324 certainly.Described purifying jar 320 contacts with cooler 330, heat conductor 332 and the thermoelectric device direct heat that hot lubricating grease 334 provides, the feasible temperature that can carefully control described purifier material or medium 324.Randomly, can provide described forecooler, perhaps can control, thereby when the fluid to input cools off, conduct heat to material 324 from described matrix gas or fluid to the temperature of material 324 in the upstream of purifier canister 320.Make substrate fluid or the input gas purifier material 324 of flowing through, capture one or more target impurity, fluid behind the purifying or gas for example output to the position of use from pipeline 312 outputs of purifier, perhaps store to treat that the back uses.
The basic embodiment of the principle of the invention comprises the purifier medium in the purifier or medium mixture is cooled off to improve the efficient of purifier.The adsorption equilibrium that this cooling to material in the purifier or material has promoted impurity in matrix gas or the fluid develops to surface absorption direction.Can see similar principle in the design of the high vacuum cryogenic pump of using at present, described principle is used for improving the absorption of molecular sieve to material in moisture and the air.The inventor thinks can improve several magnitude with the adsorption equilibrium of adsorbent of molecular sieve by the sub-cooled to purifier material, medium or medium mixture, and " cryogenic pump " of gained can produce the vacuum of about E-10 holder.
Except gross data, the inventor has obtained the empirical data of some temperature to the influence of the efficient of the purified material of operating under adsorption mechanism.Specifically, Fig. 4 has shown one group of empirical data based on the purifier material that adsorbs that the inventor collects.The chart 400 of Fig. 4 has shown temperature and the variation relation curve 410 that uses the moisture removal efficient of conventional purifier material under room temperature and higher temperature.Data points all in the curve 410 are about 18ppm at moisture concentration, gather under the situation of the HCl gas of 1slpm and 612psig.As shown in the figure, be higher than environment temperature (promptly approximate or be higher than 20 ℃), reduce based on the level of efficiency of the purifier material of absorption along with temperature rises to.On the contrary, shown in curve 410, can think that level of efficiency can improve along with temperature reduces.
By identification reducing and improved efficient shown in the chart 410, and further the theory of described cryogenic pump is used for removing impurity in the mobile substrate fluid, thereby has obtained improved result of the present invention with temperature.So, be lower than the temperature of environment temperature by use, preferred used temperature is far below environment temperature or room temperature, and for example temperature is 0 ℃ to-20 ℃ or lower, for example temperature is lower 20-60 ℃ or more than environment temperature, thereby has improved the performance of specific purifier material.Cooling to purified material has been proved to be the technology that can adsorb as the raising surface especially effectively.
In the preferred embodiment of the present invention, for example in forecooler stage or purification phase, the fluid that flows into to be cooled off with thermoelectric (al) cooler, purification media described cooling or cold is trap or high surface metal base.Described cold-trap can be stainless steel, nickel or other metal trap, for example solenoid or particulate filter.Described high surface metal base or trap can be almost shape or design arbitrarily, as long as can be used for conventional gas diffusion system.In addition, described high surface area material can be frit, cylinder, disk, circular cone or other useful purifier inserted-shape for the form of material sintering or compacting.In order to reach required cooling, cooler is provided, be used for the temperature of described high surface area material is brought down below the required cleansing temp of environment temperature.For example, as shown in Figure 3, base material can contact with the thermoelectric device direct heat, thereby can carefully control the temperature of metal base or purification elements (being purified material, medium, media etc.).
Fig. 5 and Fig. 6 demonstrate by chart 500 and 600, and the cleansing temp by carefully and optionally controlling metal base (for example form and use cold-trap) can and/or filter and remove to distinctiveness target impurity from substrate fluid by absorption, condensation.Test result shown in the chart 500 and 600 is (is about to HCl gas as substrate fluid, with moisture as target impurity) by measure that the moisture remove obtains from HCl gas.These results are by the similar low temperature purifier of operation and purifier shown in Figure 3 300, use the high surface nickel material to obtain as the purifier medium.Referring to Fig. 5, chart 500 has shown the HCl purifying that uses room temperature or environment temperature purifier to carry out at first, and the moisture that obtains is 0.1ppm.In this test, in 15 hours, use cold-trap, the result in the chart 500 shows that the efficient of purification media or material depends on the operating temperature of cold-trap.
For the present invention, along with temperature reduces from environment temperature, the efficient of purified material or medium improves, and can see when temperature and reduce to-20 ℃, and when further reducing to approximately-80 ℃ then, efficient obtains to significantly improve.As shown in the figure, use operation at low temperatures cold-trap can so that the moisture concentration among the HCl near 0.01ppn, with respect to use similar purified material, but the content of the 0.1ppm that obtains at the purifier of environment temperature or (in the case for) 20 ℃ of operations, this is a very big progress.
Notice that use can be connected or engage to cold-trap with the purifier of environment temperature in some embodiments, to remove impurity (as shown in Figure 7) effectively, perhaps sometimes the purifier of environment temperature can be substituted (also being shown in Fig. 8) fully.The chart 600 of Fig. 6 has also shown the application that use is removed the moisture among the HCl 20 ℃ of conventional purified material of operating down, shows among the figure that this conventional purifier can reach the maximum moisture removal efficient of 0.1ppm.When cold-trap was used in combination with purifier, series connection for example shown in Figure 7 was used, and was used for the downstream of purifier, and moisture was reduced to and was approximately 0.01-0ppm this moment.
The purifier or the low temperature purifier that reduce temperature can have many purposes.For example, as shown in Figure 7 and Figure 8, low temperature purifier can be used for the semiconductor integrated circuit process industry, in this industry, described low temperature purifier can be used as the part of the use part of process gas induction system or pipeline, be used for purifying electron level process gas, so that the gas of ultra-high purity to be provided, for example impurity content is equal to or less than other gas of ppb level.Low temperature purifier has much other purposes, comprise the purposes of the fluid that wherein needs extreme high purity, and target impurity is difficult to the situation that the purifying (for example operating purifier under environment temperature or higher temperature) by routine is removed.
What below tabulation provided inventor's anticipation can be with the example of the substrate fluid of low temperature purifier purifying of the present invention, and the possible potential impurity that can effectively remove from these substrate fluids.
| Substrate fluid/ | Target impurity | ||
| 1 | Ammonia | Water, CO
2, carbamate, |
|
| 2 | Argon | Water, CO 2, CO, hydrocarbon, CH 4 | |
| 3 | Arsine | Water, CO 2、CO、GeH 4、H 2S、PH 3、SiH 4, ionic liquid (IL) | |
| 4 | Boron chloride | Volatile metal, CO, CO 2 | |
| 5 | Boron chloride | CO 2、SiF 4、SO 2, HF, water, IL | |
| 6 | Carbon monoxide | Water, carbonyl nickel, carbonyl iron, CO 2, hydrocarbon | |
| 7 | Chlorine | Water, volatile metal, CO, hydrocarbon, CO 2 | |
| 8 | Dichlorosilane | SiCI 4, other chlorosilane, fluorocarbon, hydrocarbon | |
| 9 | Disilane | Chlorosilane (TCS, DCS), siloxanes, other high order silanes, hydrocarbon, water, |
|
| 10 | Germane | Moisture, digermane, germanium oxygen alkane, three germanes, chloro germane, IL, hydrocarbon, CO, CO 2 | |
| 11 | Halogenated hydrocarbons 14 (tetrafluoromethane) | Water, other fluorocarbon, CO, CO 2、HF、SF 6, hydrocarbon | |
| 12 | Halogenated hydrocarbons 23 (fluoroform) | Water, other fluorocarbon, CO 2、HF、SF 6, hydrocarbon | |
| 13 | Halogenated hydrocarbons 32 (difluoromethane) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 14 | Halogenated hydrocarbons 41 (fluomethane) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 15 | Halogenated hydrocarbons 116 (perfluoroethane) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 16 | Halogenated hydrocarbons 125 (pentafluoroethane) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 17 | Halogenated hydrocarbons 134a (HFC-134a) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 18 | Halogenated hydrocarbons 152a (Difluoroethane) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 19 | Halogenated hydrocarbons 218 (perfluoro propane) | Water, other fluorocarbon, CO
2、HF、SF
6, |
|
| 20 | Halogenated hydrocarbons 236a (HFC-236fa) water, other fluorocarbon | CO 2、HF、SF 6, hydrocarbon | |
| 21 | Halogenated hydrocarbons C318 (octafluorocyclobutane) water, other fluorocarbon, CO 2、HF、 SF 6 | Hydrocarbon | |
| 22 | Helium | Water, CO 2, hydrocarbon, CO | |
| 23 | Hydrogen | Water, CO 2, hydrocarbon, CO, | |
| 24 | Hydrogen bromide | Water, volatile metal, hydrocarbon, CO, CO 2 | |
| 25 | Hydrogen chloride | Water, Cl 2、COCl 2, HBr, volatile metal, CO, CO 2, hydrocarbon | |
| 26 | Hydrogen fluoride | Water, SO 2、H 2SO 4, hexafluorosilicic acid | |
| 27 | Methyl-monosilane | Water, chlorosilane, other HMW methyl-monosilane, hydrocarbon | |
| 28 | Nitrogen | Water, CO 2, hydrocarbon, CO | |
| 29 | Nitrogen trifluoride | Moisture, HF, N
2O、SF
6、CO
2、CO、 |
|
| 30 | Nitrous oxide | Water, NH 3、NO、NO 2、N yO x、CO 2, hydrocarbon, CO |
| 31 | The octafluoro cyclopentene | Water, HF, hexafluoro cyclobutane, other fluorocarbon, hydrocarbon |
| 32 | Oxygen | Water, hydrocarbon, CO 2 |
| 33 | Phosphine | Water, CO 2, CO, hydrocarbon, arsine, germane, H 2S, silane, IL |
| 34 | Silane | Water, methyl-monosilane, disilane, hydrocarbon, chlorosilane, siloxanes, IL |
| 35 | Silicon tetrachloride | Other chlorosilane, water, siloxanes, chloro TMOS, hydrocarbon |
| 36 | Ocratation | HF, water, CO, CO 2, hydrocarbon, chlorosilane |
| 37 | Sulfur hexafluoride | Water, CF 4, hydrocarbon, SiF 4 |
| 38 | Trichlorosilane | SiCl 4, other chlorosilane |
| 39 | Tungsten hexafluoride (WF 6) | HF、SiF 4, fluorocarbon, SF 6 |
| 40 | F2 | HF、IL |
| 41 | NO | N xO y、N 2O, water, IL |
| 42 | Diborane | Senior borine, water, IL |
| 43 | Hydrocarbon | Other hydro carbons |
| 44 | Organo-metallic compound | The organo-metallic compound of other organo-metallic compound, |
| 45 | Tetrafluoride germanium | CO 2、HF、SO 2 |
| 46 | Hydrogen selenide | H 2S, water, hydrocarbon |
| 47 | Phosphorus trifluoride | PF 2Br、PFBr 2、HCl、P xO yCl z |
Except the matrix gas or fluid specifically listed, process as herein described also can be used to remove the other substrate fluid below one or more one or more impurity: rare gas (for example krypton, neon and xenon); Carbon dioxide; Nitrogen dioxide; Carbonyl sulfide; Chlorine trifluoride; Halogenated compound includes but not limited to CF
4, NF
3, CHClF
2, CClF
2CF
3, CClF
3, CHCl
2F, CH
2F
2And CH
3F; And amine, it includes but not limited to triethylamine, dimethylamine and single ethylamine.Can include but not limited to butadiene, ethane, ethene, butane, butylene, iso-butane, propane, propylene, allylene-allene (" MAP ") with the hydrocarbon that the techniques described herein are handled and with the allylene-allene mixture of alkane and alkene stabilisation.Organo-metallic compound can comprise trimethyl gallium, trimethyl aluminium, trimethyl indium etc.
Fig. 7 has shown the semiconductor fabrication lines with low temperature purifier 750 or the system 700 of the design according to the present invention.Low temperature purifier 750 shown in the figure is arranged in the upstream that production line 700 has the semiconductor reactor 760 of chamber 766 (for example wafer manufacturing chamber), from the gas of purifier 750, perhaps after removing impurity, export the gas of purifying to this chamber to these chamber 766 adding purifying.Purifier 750 can be arbitrary form discussed in this article, example purifier 100,200 or 300 as Figure 1-3.As shown in the figure, provide other purifier 740 in the upstream of purifier 750, Matheson Tri-Gas for example, Inc. provides
MTX
TMThe impurity that the conventional purifier that purifier etc., this purifier 740 are normally operated at ambient temperature, impurity and the low temperature purifier 750 that it is used for removing are removed is identical.Certainly, purifier 740,750 can be used for removing different impurity from substrate fluid mobile system 700 or gas.
The substrate fluid of handling one by one with purifier 740,750 provides with gas cabinet (gas cabinet) or source of the gas 710.Substrate fluid flows through pipe 720, flows to valve distributor box (VMB) 730, herein with selected flow velocity and the pressure purifier 740,750 that it is provided to or leads.Usually substrate fluid is to equal or to export from valve distributor box 730 near the temperature of environment temperature.Low temperature purifier 750 comprises selects to be used for removing purification media, media or the material (as the discussion of carrying out in conjunction with Fig. 1-3) of one or more target impurity in the substrate fluid.Purifier 750 is operated being lower than under the temperature of environment temperature, the efficient of purified material, medium or the media of selecting this temperature to increase to comprise, this temperature is selected (i.e. this temperature be higher than substrate fluid under described pressure and the flow velocity transformation temperature) according to flow velocity and pressure and substrate fluid and target impurity.
Fig. 8 has shown another semiconductor fabrication lines or the system 800 of the design according to the present invention.As shown in the figure, system 800 comprises gas cabinet or source of the gas 810, and this gas cabinet or source of the gas 810 are used for providing to valve distributor box (VMB) 830 by pipe 820 substrate fluid or the gas of input.VMB830 is operated flow velocity and the pressure of controlling the substrate fluid in input semiconductor reactor 860 and the chamber 866 thereof.Described system 800 is with the difference of system 700, provide low temperature purifier 854 according to the present invention as independently unit or independently purifier, be used for removing impurity being lower than to operate under the condition of environment temperature, and output is used for the gas of the purifying of reactor 860 (or other application site).
Described system 800 also is to use the forecooler 852 that is positioned at described subcolling condenser 854 upstreams to control the temperature of substrate fluids with the difference of system 700.As illustrated in figs. 1 and 2, provide forecooler 852 to be cooled to equal or near the operating temperature of low temperature purifier 854 or the temperature of cleansing temp from the matrix of VMB830 input or input fluid from environment temperature (or higher temperature).Fluid after the precooling can a little more than or a little less than implementing the operating temperature of the present invention phase point temperature of substrate fluid (but be not less than), provide hot-swap feature with forecooler 852, this hot-swap feature may be difficult to be finished by purifying media, medium or material in the purifier 854.Provide heater 856 in the downstream of low temperature purifier 854, be used for the adjustment of the gas/fluid of the described purifying production fluids/gases acceptable temperature to the chamber 866 of importing described reactor 860, this temperature can be the temperature of environment temperature or the other process gas that can be used for reactor 860 (or other application site).
Technical staff in the refrigeration/refrigerating industry is appreciated that the cooling of low temperature of the present invention or deep cooling purifier can finish by various technology, for example can use commercially available cooler.Selected cooling technology or cooler can be depending on the substrate fluid that will flow and are cooled to target temperature or the required thermic load of temperature range.Described cooler can be simple refrigerator, or following form: Stirling cooler, Peltier cooler, eddy current cooler, Venturi cooler, sub-cooled bath and/or other form known in the art or exploitation are used for the form of this application-specific/function.Usually preferably described cooler should be simple, the separate unit that the energy that only needs electric energy or other to obtain easily drives with low energy consumption.But also it is often preferred or need the small size cooler.In some embodiments, the ability that can change cryogenic temperature makes and can set cleansing temp to different target impurity, different substrate fluid (and flow velocity and pressure) and/or different purified material, medium or media (and not isomorphism type of the purification elements of these coolings).Described cooler for example preferably can use thermoelectric occasionally other backfeed loop described purifier canister or container and interior material thereof to be remained on the cleansing temp of setting.
More than describe and only be considered to illustrate principle of the present invention.In addition, owing to those skilled in the art can improve and change at an easy rate in a large number, so the present invention is not limited to above-mentioned definite structure and process.Therefore, within the scope of the invention that all suitable improvement and content of equal value all are included in appended claims and are limited.For example, thereby content of the discussions is devoted to emphatically to improve the possibility that physical absorption is raised the efficiency by the cooling purification media, but theory described cooling or low temperature purifier also can be used for other Impurity removal mechanism, and it includes but not limited to the combination of chemisorbed, reversible reaction, precipitation, condensation, filtration and/or these mechanism.
Claims (18)
1. fluid purification system that is used for from substrate fluid, removing one or more impurity, this system comprises:
Forecooler, it receives substrate fluid at first temperature, pressure and flow velocity, and is being lower than second temperature output substrate fluid of first temperature;
The purification elements that comprises a large amount of high surface area materials;
The container that contains steel pipe, steel pipe contains described purification elements, described purification elements comprises the metal particle filter, described filter comprises sintering, nickel compacting and/or plating, stainless steel, or corrosion resisting alloy and/or selection are used for removing specific a kind of alloy in the impurity, described container has the inlet that is used for receiving substrate fluid, and guiding described substrate fluid to be used for after flowing through purification elements from the outlet of described container output substrate fluid at described container, wherein, impurity content from the inflow substrate fluid of forecooler is higher than 100ppb, and the impurity content of output substrate fluid is lower than 100ppb;
Cooler, this cooler contacts with the part of the container that comprises described purification elements, and it is cooled to cleansing temp, and described cleansing temp is lower than environment temperature and is higher than the transformation temperature of this substrate fluid under substrate fluid place pressure and the flow velocity.
2. fluid purification system as claimed in claim 1, it is characterized in that, described system can be used to remove the ionic liquid of trace from substrate fluid, described substrate fluid comprises the ionic liquid of first content, comprise the ionic liquid of second content from the substrate fluid of described outlet of container output, described second content is less than first content.
3. fluid purification system as claimed in claim 2 is characterized in that, second content of described ionic liquid is approximately less than 100ppb.
4. fluid purification system as claimed in claim 1 or 2 is characterized in that, described cleansing temp is at least than low 20 ℃ of environment temperature.
5. fluid purification system as claimed in claim 1 is characterized in that, described cleansing temp is less than about-20 ℃.
6. fluid purification system as claimed in claim 1 is characterized in that, at the described substrate fluid of described container entrance reception certain pressure and flow velocity, described cleansing temp is higher than the transformation temperature of substrate fluid under this pressure and flow velocity at described container entrance place.
7. fluid purification system as claimed in claim 1 is characterized in that described cooler provides cooling to forecooler.
8. fluid purification system as claimed in claim 1 is characterized in that, this system also comprises the heater that is communicated with described container outlet fluid, and described heater will be heated at least about equaling environment temperature from the substrate fluid of described container output.
9. fluid purification system as claimed in claim 1, it is characterized in that described high surface area material is to comprise following metal: nickel, stainless steel, corrosion resisting alloy and/or selection sintering, compacting and/or plating are used for removing specific a kind of alloy in the impurity.
10. fluid purification system as claimed in claim 1 is characterized in that, described high surface area material comprises and is selected from following at least a material: modenite, zeolite, aluminium oxide, silica and carbon.
11. fluid purification system as claimed in claim 1 is characterized in that, is coated with on the described high surface area material to select to be used for removing specific a kind of reactive materials in the impurity.
12. fluid purification system as claimed in claim 11 is characterized in that, described reactive materials is alkaline-earth metal, alkaline-earth metal or transition metal.
13. fluid purification system as claimed in claim 1 or 2, it is characterized in that described substrate fluid comprises and is selected from following gas: amine, ammonia, argon gas, arsine, boron chloride, boron trifluoride, carbon dioxide, carbon monoxide, carbonyl sulfide, chlorine, chlorine trifluoride, dichlorosilane, disilane, germane, halogenated hydrocarbons, halogenated compound, helium, hydrogen, hydrogen bromide, hydrogen chloride, hydrogen fluoride, methyl-monosilane, nitrogen, nitrogen dioxide, Nitrogen trifluoride, nitrous oxide, the octafluoro cyclopentene, oxygen, phosphine, rare gas, silane, silicon tetrachloride, ocratation, sulfur hexafluoride, trichlorosilane, WF
6, F
2, NO, diborane, hydrocarbon, organo-metallic compound, tetrafluoride germanium, hydrogen selenide or phosphorus trifluoride.
14. the system as claimed in claim 1 is characterized in that, described cleansing temp is about 0 ℃ to-200 ℃.
15. a method that is used for the substrate fluid in specific pressure and flow velocity current downflow is carried out purifying, this method comprises:
In the flow path of described substrate fluid, provide purification media;
Described purification media is cooled to cleansing temp, and described cleansing temp is about 0 ℃ to-200 ℃ and be higher than the transformation temperature of described substrate fluid under described pressure and flow velocity;
At first guide described substrate fluid by the forecooler stage, in the stage substrate fluid is cooled in the said temperature scope at forecooler;
Guide described substrate fluid to flow through described purification media then.
16. method as claimed in claim 15, it is characterized in that, described purification media comprises high surface area material, and described high surface area material comprises and is selected from following at least a material: modenite, zeolite, aluminium oxide, silica, carbon, sintering, metal or metal alloy compacting and/or plating.
17. method as claimed in claim 16, it is characterized in that, described substrate fluid is cooled to approximate described cleansing temp in the forecooler stage, the cooling step of described purification media comprises that the outer surface that the jar of described purification media will be housed by cooler is cooled to the jar temperature that approximates or be lower than described cleansing temp, and described cooler contacts with the outer surface heat of described jar.
18. method as claimed in claim 15 is characterized in that, before guiding first, the amount of the ionic liquid that described substrate fluid comprises is greater than about 10ppb, and after guiding for the second time, the amount of described substrate fluid intermediate ion liquid reduces to less than about 10ppb.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US62187104P | 2004-10-25 | 2004-10-25 | |
| US60/621,871 | 2004-10-25 | ||
| US11/252,200 | 2005-10-17 |
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| CN110325260A (en) * | 2016-11-08 | 2019-10-11 | 曼瑟森三汽油公司 | The method for removing moisture from hydrazine |
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| US8691167B2 (en) * | 2012-07-19 | 2014-04-08 | Tronox Llc | Process for controlling carbonyl sulfide produced during chlorination of ores |
| CN103922414B (en) * | 2014-04-30 | 2016-04-13 | 邯郸净化设备研究所 | A kind of method of continuous rectification purifying tungsten hexafluoride and device |
| CN104555927B (en) * | 2014-12-31 | 2016-07-20 | 中国船舶重工集团公司第七一八研究所 | A kind of purification process of chlorine trifluoride |
| EP3272375A1 (en) * | 2016-07-22 | 2018-01-24 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Apparatus and method for generating dialysate for dialysis |
| CN112546659B (en) * | 2020-12-08 | 2022-02-15 | 云南临沧鑫圆锗业股份有限公司 | Purification device and method for germanium tetrafluoride |
| CN114950066B (en) * | 2022-07-26 | 2022-11-01 | 济南德洋低温科技有限公司 | Low-temperature dynamic adsorption purification device |
| CN117160179B (en) * | 2023-10-26 | 2024-02-13 | 福建德尔科技股份有限公司 | Raw material purification equipment for preparing electronic grade chlorine trifluoride |
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