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WO2000076915A1 - Purification d'un halogenure inorganique gazeux - Google Patents

Purification d'un halogenure inorganique gazeux Download PDF

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Publication number
WO2000076915A1
WO2000076915A1 PCT/US2000/016051 US0016051W WO0076915A1 WO 2000076915 A1 WO2000076915 A1 WO 2000076915A1 US 0016051 W US0016051 W US 0016051W WO 0076915 A1 WO0076915 A1 WO 0076915A1
Authority
WO
WIPO (PCT)
Prior art keywords
process according
reactive metal
inorganic halide
crude
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2000/016051
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English (en)
Inventor
Dalbir Rajoria
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
UHP Materials Inc
Original Assignee
UHP Materials Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by UHP Materials Inc filed Critical UHP Materials Inc
Priority to AU57328/00A priority Critical patent/AU5732800A/en
Priority to EP00942748A priority patent/EP1409400A4/fr
Publication of WO2000076915A1 publication Critical patent/WO2000076915A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B9/00—General methods of preparing halides
    • C01B9/08—Fluorides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/08—Compounds containing halogen
    • C01B33/107—Halogenated silanes
    • C01B33/10778—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/06—Boron halogen compounds
    • C01B35/061—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B9/00—General methods of preparing halides
    • C01B9/02—Chlorides

Definitions

  • the present invention relates to the purification of gaseous inorganic halides.
  • Gaseous inorganic halides have widespread commercial applications. Such compounds have been known m the chemical arts for many years. These compounds are widely used as catalysts m polymers, pharmaceuticals, fine chemical synthesis and m the manufacture of electronic and semiconductor devices. Boron t ⁇ fluoride, m particular, is used m the electronics industry for ion implantation and as a p-type dopant for semiconductor devices. Due to the purity requirements m many of the above applications, particularly m the electronics and semiconductor fields, there is an ever increasing need for ultra high purity gaseous inorganic halide compounds.
  • gaseous inorganic halide compounds are highly reactive to air and water and therefore must be handled m air-free, inert atmospheres. The manufacturing and purification of these compounds can be extremely difficult due to this high reactivity.
  • a particular gaseous inorganic halide of commercial interest is boron t ⁇ fluoride. Boron t ⁇ fluoride is a strong Lewis acid that complexes with water, polar organic solvents, and other compounds having at least one unshared pair of electrons. The synthesis of boron trifluo ⁇ de has been disclosed m U.S. Patent Nos . 2,148,514 and 2,196,907. Boron trifluo ⁇ de is a colorless gas which forms dense white fumes m moist air.
  • boron t ⁇ fluoride typically has a purity of 99.7%.
  • the major impurities are air, at 4,000 to 1,700 parts per million (PPM) and silicon halide (as silicon tetrafluo ⁇ de) at 300 to 50 PPM.
  • Other impurities present as artifacts of the manufacturing process include sulfate (10 PPM), hydrogen fluoride (25 PPM) , hydrogen chloride (10 PPM) , sulfur dioxide and boron trifluoride dihydrate are found m trace amounts. While these amounts are typical, the purity profile of any single lot of gaseous inorganic halide, particularly boron trifluoride, may vary.
  • boron trifluoride is purified through either distillation or adsorption on zeolites to remove some contaminants. Using these techniques, atmospheric gases such as nitrogen, oxygen and carbon dioxide can be reduced to concentrations of 10-20 PPM. However, other impurities listed above still remain. Therefore, a purification means is needed to remove most of the remaining impurities from gaseous inorganic halides and m particular boron trifluoride so that the concentration of the total impurities is reduced to less than about 20 PPM, a concentration suitable for use m electronic and semiconductor applications. It should be noted however that the purified gas provided by the present invention may be used m any application where high purity gas is necessary.
  • the present invention provides an improved purification method for gaseous inorganic halides and m particular boron trifluoride.
  • Preferred processes according to the present invention can meet the needs and demands of today's electronic and semiconductor needs.
  • Preferred processes according to the present invention specifically provides a method of reducing the total contaminant concentration to less than 20 PPM.
  • the present invention also provides an apparatus for practicing the purification method.
  • the present invention generally provides an apparatus and a method of purifying gaseous inorganic halide compounds. Specifically, the present invention involves a process whereby the crude, or unpu ⁇ fied gaseous inorganic halide is contacted with a material capable of reacting and/or adsorbing impurities thereby reducing the same.
  • One aspect of this invention provides a process to reduce or eliminate impurities m gaseous inorganic halides to concentrations acceptable for use m high purity applications such as electronic and semiconductor devices.
  • This purification is achieved by contacting the gaseous inorganic halide with a reactive substance.
  • the reactive substance is a metal.
  • the reactive metal is finely divided or otherwise provided m a form having a high surface area such as shot, foil, sheets, granules or powders.
  • the reactive metal may also be plated or deposited onto or into an inert support.
  • the reactive metal is packed in a column such that the crude gas is allowed to pass through and contact the metal .
  • the metal is provided in a powdered or pelletized form and contained in a fluidized bed such that the crude gaseous inorganic halide material is allowed to pass through thereby contacting the metal and thus react and/or adsorb impurities .
  • the reactive metal used is preferably an alkaline metal, alkaline earth metal or an alloy of such metal .
  • the reactive metal selected is lithium or calcium.
  • the reactive metal selected may be an alloy of lithium or calcium combined with Group III or Group IV elements, and preferably one or more of the following elements: silicon, aluminum, germanium, boron and calcium.
  • the gaseous inorganic halide is contacted with a reactive metal at a temperature above room temperature.
  • Room temperature is defined as any ambient temperature between about 20°C to about 28°C.
  • the reactive metal is heated to a temperature below that of its melting point.
  • the contact time, or residence time, of the gas on the reactive metal is preferably between 30 seconds and 30 minutes, depending on other variables such as the reactor size and shape, the reactive metal used, the inorganic halide used and its purity.
  • a method whereby the crude gaseous inorganic halide is purified by contact with, or distillation over, an adsorbent material prior to being contacted with the reactive metal .
  • the adsorbent material can be molecular sieves.
  • 5A molecular sieves are used to contact the crude gaseous inorganic halide prior to contacting the reactive metal.
  • the crude gaseous inorganic halide is distilled.
  • the inorganic halide may be distilled m the absence of any adsorbant or reactive substances.
  • the distillation of the crude inorganic halide is performed prior to, during or after it is contacted with either the molecular sieves or the reactive metal.
  • the distillation step preferably includes cryogemcally condensing the gaseous inorganic halide at a temperature at or below its melting point followed by evacuation or pumping off the uncondensed gases.
  • an apparatus is provided allowing for the gaseous inorganic halide to be purified m an inert, anhydrous environment.
  • BRIEF DESCRIPTION OF THE DRAWING Fig. 1 is a schematic representation of the apparatus used to purify a gaseous inorganic halide according to the present invention. DETAILED DESCRIPTION
  • the present invention provides a method and apparatus for purifying gaseous inorganic halide compounds.
  • the process embodied m the present invention generally provides for the gaseous inorganic halide to be introduced into an inert atmosphere whereby the gaseous inorganic halide is contacted with a reactive substance.
  • the reactive substance may be a metal and optionally an absorbent material both capable of removing impurities.
  • the present invention also provides for the removal of uncondensed gases such as nitrogen, oxygen and others by evacuating or pumping off the gases occupying head space while the inorganic halide is condensed in the liquid or solid phase.
  • BF 3 is a preferred compound.
  • the present invention may be used to purify gaseous inorganic halides having any purity grade, however a preferred embodiment of the invention is directed to further purifying an already purified gaseous inorganic halide containing about 1.0 to about 0.5% impurities.
  • the reactive substances used to purify the gaseous inorganic halides may be any substance capable of sequestering impurities from gaseous inorganic halides. Although this disclosure is not limited by any theory of operation, it is believed that purification is achieved by the action of heating the crude gas, which as a propensity to complex with impurities, and decouple the impurities from the gaseous inorganic halide whereby the free decoupled impurities selectively react with the reactive substance thereby removing them from the gas phase.
  • the reactive substances used m the present invention may be selected from any ceramic, glass, metallic, semi-metallic material capable of sequestering impurities.
  • a reactive metal may be used containing any alkali metal (Group I) including lithium, sodium and potassium, and alkaline earth metals (Group II) including beryllium, magnesium, calcium, strontium and/or barium and alloys. These metals may be either pure or alloys thereof. Such alloys may have Group III and IV metals present; preferred are silicon, aluminum, germanium, boron and/or calcium as the accompanying alloy metal. The preferred metal is lithium or calcium.
  • the reactive metal may be used m any form to practice the present invention, however forms possessing a large surface area are more preferred.
  • a cut ribbon or foil would have a higher surface area than a cube of equal mass, and therefore the cut ribbon or foil would be preferred.
  • the precise surface area is not critical to the practice of the present invention provided sufficient reactive metal surface is available to react with all or most of the impurities introduced and contacted to the reactive metal . Therefore the amount of reactive metal used is not critical.
  • the amount or loading of the reactive metal will vary according to the form and surface area of the metal and the purity of the gaseous inorganic halide. In one preferred embodiment of the present invention, a molar ratio between about 1:25 of lithium to crude boron trifluoride may be used.
  • a molar ratio of about 1:10 lithium to crude boron trifluoride is used. In another more preferred embodiment, the molar ratio is about 1:0.2 lithium to crude boron trifluoride. In another preferred embodiment of the present invention, an equal molar ratio of lithium to crude boron trifluoride is used.
  • the reactive metal (such as lithium) is used as a fine powder.
  • the reactive metal is provided in a foil, pellet, shot, granule, rod, or sheet.
  • the metal may also be plated or deposited onto or into an inert support.
  • cut lithium foil is placed in a purifier vessel into which the crude gaseous inorganic halide is fed for the purposes of contacting the gas with the metal.
  • the reactive metal is packed in a column, fluidized bed, or other flow through apparatus capable of providing an opportunity for the gaseous inorganic halide to contact the reactive metal.
  • the reactive metal may be contacted with the crude gaseous inorganic halide at temperatures sufficient to decouple the impurities from the gas, and thereby cause the reactive metal to react with the impurities of the crude gaseous inorganic halide.
  • the reactive metal is heated to a temperature between about 25 °C to about 300 °C.
  • the temperature range of the heated reactive metal is between about 50 °C and about 250 °C.
  • the reactive metal is heated to a temperature of about 100 °C to about 180 °C whereby 130 °C is the most preferred embodiment where lithium is used as the reactive metal.
  • the contact, or residence time of the gaseous inorganic halide to the reactive metal will depend upon several factors such as the gaseous inorganic halide being purified as well as its purity. The type of metal and the vessel it is contained m will also effect the contact time. Generally the contact time should be between about 30 seconds to about 30 minutes for batchwise purification. In one preferred embodiment using lithium as a reactive metal, about 5 to about 15 minutes is a suitable contact time, and about 8 to about 10 minutes is most preferable. However, if a constant flow of gas is passed through a column of reactive metal m a steady state, these times may vary depending upon the flow rate of the gas and the amount of reactive metal used.
  • Flow rates of the gaseous inorganic halide used m the present invention where reactive material beds or columns are used may vary according to bed or column configuration. In one preferred embodiment of the present invention flow rates between about 1ml per minute to about 1000ml per minute may be used. In another preferred embodiment, the flow rates may be between about 50ml per minute and about 100ml per minute. In another preferred embodiment, the flow rates may be between about 100ml per minute and about 500ml per minute.
  • the gaseous inorganic halide also may be contacted with an adsorbant material .
  • adsorbant materials are ceramics, organic and inorganic compounds including salts, polymeric materials, metals and supported metal composites and molecular sieves.
  • Molecular sieves are porous structures usually composed of inorganic materials such as aluminum silicates, feldspars and other clay-type materials. Molecular sieves may also be derivitized with organic functional groups. The pore sizes of molecular sieves have a typical range between about 5 and about 10 angstroms.
  • molecular sieves are used (U.O.P. Inc., Des Plains, Illinois) .
  • the function of the molecular sieves m the present invention is probably to absorb carbon dioxide and perhaps other impurities.
  • the molecular sieves used m this embodiment of the present invention may be placed m a vessel m line with the apparatus also containing a vessel for the reactive metal .
  • the molecular sieves m one preferred embodiment may be placed m line before the reactive metal .
  • the molecular sieve vessel may be placed after the reactive metal vessel, or alternatively two molecular sieve vessels may be placed before and after the reactive metal vessel line.
  • the inorganic halide may be contacted with the molecular sieves at temperatures between about -190 to about 0°C where a more preferred range is between about -80 and about 0°C.
  • the inorganic halide may be contacted with the molecular sieves for a time between about 1 to 30 minutes. Another preferred contact time range may be between about 5 to about 10 minutes. In either case the crude gaseous inorganic halide is contacted with the molecular sieves along with the reactive metal to produce a purified inorganic halide .
  • adsorbant material including molecular sieves
  • a sufficient amount of 5A molecular sieves is used to adsorb impurities mixed m the crude inorganic halide.
  • about 150g of 5A molecular sieves is used as an adsorbant.
  • molecular sieves adsorb independently of temperature and pressure, as is known m the art. It is important to note that many adsorbant materials such as molecular sieves should be activated. For the purposes of describing the present invention, activated molecular sieves are pretreated to remove water, adsorbed gases, and other chemicals that may interfere with the adsorption activity during the gaseous inorganic halide purification process of the present invention.
  • the apparatus used m the present invention as illustrated m Fig. 1, may be any manifold system whereby the crude gaseous inorganic halide can be delivered m an inert and anhydrous atmosphere to the molecular sieve vessel or the reactive metal vessel and ultimately collected m a receiving vessel .
  • the apparatus should be capable of withstanding reduced pressures as well as several atmospheres of pressure due to the fact that the gaseous inorganic halide may be either transferred, distilled or condensed during various stages of the practice of the present invention.
  • the apparatus may also have a means for drawing alloquots of gas for analysis. Such means may be a sample port comprising a resilient septum affixed m line to the apparatus.
  • the apparatus may be composed of various vessels such as glass flasks, ceramic containers, metal containers or gas cylinders, or other typical non-reactive chemical reaction vessels.
  • the vessels may be connected using non-reactive polymeric tubing, metal pipe or tube, or glass pipe or tube.
  • the apparatus may be sectioned off using any type of valve stopcock or clamp depending on the composition of the tubing or piping.
  • the gaseous inorganic halide is transferred between vessels either by distillation or by pressure difference.
  • the gas may be cryogenically transferred to an empty vessel, as is known m the art, then subjected to a high vacuum to remove uncondensed gases such as nitrogen and oxygen.
  • the distillation may be performed where the gaseous inorganic halide may be condensed at temperatures between about -190 to about -78°C. Afterwards, the condensed gas may be warmed into the gas phase and distilled to another vessel and contacted with either molecular sieves or a reactive material as desired.
  • the gaseous inorganic halide may be warmed to temperatures between about -50 to about -10°C. Once purified, the gas can be cryogenically transferred to a receiving vessel.
  • the apparatus illustrated m Fig. 1 is only one possible configuration. It is preferable to maintain the vessel at some lower temperature to inhibit desorption of contaminants from the molecular sieve and their subsequent transfer to the purifier (P) . Any configuration may be used to transfer and sample the gas as required depending on the number of purification steps used m the present invention. As is known m the art, line and vessel pressures will vary depending upon the configuration of the apparatus, the condensing temperatures, vacuum pump strength and the total volume of the apparatus in the present invention.
  • the gaseous inorganic halide may be BF 3 and the reactive metal may be lithium or an alloy of lithium, and the metal contacting step may be performed at a temperature between about 100 °C and about 180°, followed by a further contacting step with 5A molecular sieves .
  • the vessel was then closed and the vessel was allowed to come to room temperature. It was cooled again to liquid nitrogen temperature and the headspace evacuated to ensure removal of uncondensed gases. The vessel valve was then closed.
  • the vessel should be cooled to a temperature no greater than the melting point temperature of the inorganic halide and maintained at that temperature while being evacuated. The vessel was then brought to dry ice temperature and allowed to rest for several minutes, after which the vessel was allowed to warm to room temperature.
  • the analysis methods used were specific to the impurities of interest. Nitrogen, oxygen, and carbon dioxide were analyzed by gas chromatography. Sulfate and sulfur dioxide impurities were analyzed by ion chromatography and gravimetric methods. Silicon tetrafluoride was analyzed by gas chromatography and photometric evaluation of reduced B-silicomolybdic acid (silicomolybdenum blue) with a detection limit of less than 0.05 mg/L.
  • boron trifluoride 99.8% was used containing the following impurity profile: 2000ppm of air; 1 ppm of sulfur dioxide; lOppm sulfates and 17ppm of SiF 4 .
  • a vessel Cl containing 5A molecular sieves (150g) was connected in series on the vacuum manifold to a stainless steel container, purifier P, containing lithium metal (4.0g) .
  • the purifier P was evacuated and heated to a temperature between 120 and 130°C.
  • the vessel Cl was cooled with a dry ice bath and the bath was removed. At -20°C, boron trifluoride
  • the sample from the receiver cylinder R was analyzed. Analysis by gas chromatography showed nitrogen and oxygen present at a total concentration of 6 PPM, carbon dioxide present at 1 PPM, and silicon tetrafluoride at a concentration of 1 PPM. This demonstrates that the process of the present invention is more effective than conventional methods m removing impurities from an inorganic halide. It is particularly effective m removing silicon tetrafluoride from boron trifluoride.
  • boron trifluoride was m contact with hot lithium (4.0g) m purifier P for about 5 minutes before it was transferred into the vessel Rl containing 5A molecular sieves and cooled to liquid nitrogen temperatures.
  • valves on purifier P were closed.
  • the cold vessel Rl was then pumped on to remove any uncondensed gaseous impurities.
  • the vessel Rl was then allowed to warm up to about 0°C while transferring the boron trifluoride from it into the liquid nitrogen cold receiver R.
  • the valve on the vessel Rl was closed and head space of receiver R was pumped off.
  • a total of about 23 grams of boron trifluoride was collected m receiver R and was analyzed.
  • the combined concentrations of carbon dioxide, sulfur dioxide, nitrogen and silicon tetrafluoride impurities were observed to be less than 7 PPM.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Silicon Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un appareil et un procédé destinés à la purification d'un halogénure inorganique gazeux utilisant un métal réactif (P) et un tamis moléculaire (C1) pour enlever les impuretés.
PCT/US2000/016051 1999-06-11 2000-06-12 Purification d'un halogenure inorganique gazeux Ceased WO2000076915A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU57328/00A AU5732800A (en) 1999-06-11 2000-06-12 Purification of gaseous inorganic halide
EP00942748A EP1409400A4 (fr) 1999-06-11 2000-06-12 Purification d'un halogenure inorganique gazeux

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US13892499P 1999-06-11 1999-06-11
US60/138,924 1999-06-11

Publications (1)

Publication Number Publication Date
WO2000076915A1 true WO2000076915A1 (fr) 2000-12-21

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PCT/US2000/016051 Ceased WO2000076915A1 (fr) 1999-06-11 2000-06-12 Purification d'un halogenure inorganique gazeux

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Country Link
EP (1) EP1409400A4 (fr)
AU (1) AU5732800A (fr)
TW (1) TWI257875B (fr)
WO (1) WO2000076915A1 (fr)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003006374A1 (fr) * 2001-07-12 2003-01-23 Showa Denko K. K. Production et utilisation de tetrafluorosilane
WO2005030642A1 (fr) * 2003-09-25 2005-04-07 Showa Denko K.K. Procede de production de tetrafluorosilane
CN101993088A (zh) * 2010-10-15 2011-03-30 天津市泰源工业气体有限公司 精馏与吸附组合提纯方式制备高纯三氟化硼方法的工艺技术
CN103950949A (zh) * 2014-05-20 2014-07-30 方治文 高纯三溴化硼-11的制备方法
CN103950948A (zh) * 2014-05-20 2014-07-30 方治文 高纯三氟化硼-11的制备方法
CN108821254A (zh) * 2018-09-11 2018-11-16 安徽东至广信农化有限公司 一种三氯化磷合成工艺中去除无机及有机杂质的方法
CN114525485A (zh) * 2022-01-21 2022-05-24 亚芯半导体材料(江苏)有限公司 大尺寸高熵高纯度难熔金属合金溅射靶材及其制备工艺

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3625651A (en) * 1968-03-09 1971-12-07 Kali Chemie Ag Method for removing sulfur dioxide from boron trifluoride
US4263467A (en) * 1979-11-29 1981-04-21 Gulf Research & Development Company Recovery of boron trifluoride from a hydrocarbon liquid
US4755370A (en) * 1982-03-18 1988-07-05 General Electric Company Purification of silicon halides
US4943423A (en) * 1988-11-29 1990-07-24 Allied-Signal Inc. Process for recovering boron trifluoride from an impure gaseous boron trifluoride residue
US4965055A (en) * 1990-03-27 1990-10-23 The United States Of America As Represented By The Secretary Of The Navy Preparation of ultra-pure metal halides

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3037337A (en) * 1955-09-06 1962-06-05 Thiokol Chemical Corp Purification of boron trichloride
US3043665A (en) * 1955-09-06 1962-07-10 Thiokol Chemical Corp Purification of boron trichloride
US3207581A (en) * 1961-11-14 1965-09-21 American Potash & Chem Corp Process for purifying boron trichloride
US3625661A (en) * 1969-08-11 1971-12-07 Atomic Energy Commission Separation of titanium fluoride and niobium fluoride from gaseous uranium hexafluoride containing same
US4564509A (en) * 1983-06-30 1986-01-14 Northeast Semiconductor Inc. Method and apparatus for improved gettering for reactant gases
JPH01261208A (ja) * 1988-04-11 1989-10-18 Mitsui Toatsu Chem Inc 三弗化窒素ガスの精製方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3625651A (en) * 1968-03-09 1971-12-07 Kali Chemie Ag Method for removing sulfur dioxide from boron trifluoride
US4263467A (en) * 1979-11-29 1981-04-21 Gulf Research & Development Company Recovery of boron trifluoride from a hydrocarbon liquid
US4755370A (en) * 1982-03-18 1988-07-05 General Electric Company Purification of silicon halides
US4943423A (en) * 1988-11-29 1990-07-24 Allied-Signal Inc. Process for recovering boron trifluoride from an impure gaseous boron trifluoride residue
US4965055A (en) * 1990-03-27 1990-10-23 The United States Of America As Represented By The Secretary Of The Navy Preparation of ultra-pure metal halides

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP1409400A4 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003006374A1 (fr) * 2001-07-12 2003-01-23 Showa Denko K. K. Production et utilisation de tetrafluorosilane
US7074377B2 (en) 2001-07-12 2006-07-11 Showa Denko K.K. Production of tetrafluorosilane
WO2005030642A1 (fr) * 2003-09-25 2005-04-07 Showa Denko K.K. Procede de production de tetrafluorosilane
CN101993088A (zh) * 2010-10-15 2011-03-30 天津市泰源工业气体有限公司 精馏与吸附组合提纯方式制备高纯三氟化硼方法的工艺技术
CN103950949A (zh) * 2014-05-20 2014-07-30 方治文 高纯三溴化硼-11的制备方法
CN103950948A (zh) * 2014-05-20 2014-07-30 方治文 高纯三氟化硼-11的制备方法
CN108821254A (zh) * 2018-09-11 2018-11-16 安徽东至广信农化有限公司 一种三氯化磷合成工艺中去除无机及有机杂质的方法
CN114525485A (zh) * 2022-01-21 2022-05-24 亚芯半导体材料(江苏)有限公司 大尺寸高熵高纯度难熔金属合金溅射靶材及其制备工艺

Also Published As

Publication number Publication date
EP1409400A4 (fr) 2004-09-15
AU5732800A (en) 2001-01-02
TWI257875B (en) 2006-07-11
EP1409400A1 (fr) 2004-04-21

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