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WO1996039263A1 - Production sur place d'acide nitrique d'ultra haute purete pour le traitement de semiconducteurs - Google Patents

Production sur place d'acide nitrique d'ultra haute purete pour le traitement de semiconducteurs Download PDF

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Publication number
WO1996039263A1
WO1996039263A1 PCT/US1996/009215 US9609215W WO9639263A1 WO 1996039263 A1 WO1996039263 A1 WO 1996039263A1 US 9609215 W US9609215 W US 9609215W WO 9639263 A1 WO9639263 A1 WO 9639263A1
Authority
WO
WIPO (PCT)
Prior art keywords
nitric acid
semiconductor
site
column
distillation
Prior art date
Application number
PCT/US1996/009215
Other languages
English (en)
Inventor
Joe G. Hoffman
R. Scot Clark
Wallace I. Yuan
Original Assignee
Startec Ventures, 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 Startec Ventures, Inc. filed Critical Startec Ventures, Inc.
Priority to AU60934/96A priority Critical patent/AU6093496A/en
Priority to KR1019970708704A priority patent/KR19990022225A/ko
Priority to JP9501593A priority patent/JPH11507004A/ja
Priority to EP96918226A priority patent/EP0835168A4/fr
Priority to US08/759,213 priority patent/US6214173B1/en
Publication of WO1996039263A1 publication Critical patent/WO1996039263A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/311—Etching the insulating layers by chemical or physical means
    • H01L21/31105—Etching inorganic layers
    • H01L21/31111—Etching inorganic layers by chemical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
    • B01J39/04—Processes using organic exchangers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/01—Hydrogen peroxide
    • C01B15/013—Separation; Purification; Concentration
    • C01B15/0135—Purification by solid ion-exchangers or solid chelating agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/19—Fluorine; Hydrogen fluoride
    • C01B7/191—Hydrogen fluoride
    • C01B7/195—Separation; Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/19—Fluorine; Hydrogen fluoride
    • C01B7/191—Hydrogen fluoride
    • C01B7/195—Separation; Purification
    • C01B7/197—Separation; Purification by adsorption
    • C01B7/198—Separation; Purification by adsorption by solid ion-exchangers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/02—Preparation, purification or separation of ammonia
    • C01C1/024—Purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/16—Halides of ammonium
    • C01C1/162—Ammonium fluoride
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30604—Chemical etching
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the present invention relates generally to semiconductor processing, and particularly to preparation of ultrapure liquid reagents.
  • Contamination is generally an overwhelmingly important concern in integrated circuit manufacturing.
  • cleanup steps of one kind or another such cleanup steps may need to remove organic con ⁇ taminants, metallic contaminants, photoresist (or inorganic residues thereof), byproducts of etching, native oxides, etc.
  • Plasma etching is performed with photoresist in place, and is not directly followed by high-temperature steps. Instead the resist is stripped, and a cleanup is then necessary.
  • the materials which the cleanup must remove may include: photoresist residues (organic polymers); sodium; Alkaline earths (e.g. calcium or magnesium); and heavy metals (e.g. gold). Many of these do not form volatile halides, so plasma etching can't carry them away. Cleanups using wet chemistries are required.
  • Integrated circuit structures use only a few dopant species (boron, arsenic, phosphorus, and sometimes antimony) to form the required p-type and n-type doped regions.
  • dopant species boron, arsenic, phosphorus, and sometimes antimony
  • many other species are electrically active dopants, and are highly undesirable contaminants. Many of these contaminants can have deleterious effects, such as increased junction leakage, at concentrations well below 10 13 cm "3 .
  • some of the less desirable contaminants segregate into silicon, i.e. where silicon is in contact with an aqueous solution the equilibrium concentration of the contaminants will be higher in the silicon than in the solution.
  • some of the less desirable contaminants have very high diffusion coefficients, so that introduction of such dopants into any part of the silicon wafer will tend to allow these contaminants to diffuse throughout, including junction locations where these contaminants will cause leakage.
  • all liquid solutions which will be used on a semiconductor wafer should preferably have extremely low levels of all metal ions.
  • concentration of all metals combined should be less than 300 ppt (parts per trillion), and less than 10 ppt for any one metal, and less would be better.
  • contamination by both anions and cations must also be controlled. (Some anions may have adverse effects, e.g. complexed metal ions may reduce to mobile metal atoms or ions in the silicon lattice.)
  • Front end facilities normally include on-site purification systems for preparation of high- purity water (referred to as "DI" water, i.e. deionized water). However, it is more difficult to obtain process chemicals in the purities needed.
  • the present application discloses systems and methods for preparation of ultrapure chemicals on-site at a semiconductor manufacturing facility, so that they can be piped directly to the points of use.
  • the disclosed systems are very compact units which can be located in the same building as a front end (or in an adjacent building), so that handling is avoided.
  • the present inventors have developed a method for preparing ultra-high-purity liquid reagents (including aqueous HF, HC1, NH 4 OH, NH 4 F, and HNO 3 ) in an on-site system located at the semiconductor wafer production site.
  • aqueous ammonia this is performed by: drawing ammonia vapor from a liquid ammonia reservoir, and scrubbing the filtered vapor with high-pH purified water (preferably ultrapure deionized water which has been allowed to equilibrate with the ammonia stream).
  • high-pH purified water preferably ultrapure deionized water which has been allowed to equilibrate with the ammonia stream.
  • the drawing of the ammonia vapor from the supply reservoir serves by itself as a single-stage distillation, eliminating nonvolatile and high-boiling impurities, such as alkali and alkaline earth metal oxides, carbonates and hydrides, transition metal halides and hydrides, and high-boiling hydrocarbons and halocarbons.
  • the reactive volatile impurities that could be found in commercial grade ammonia, such as certain transition metal halides.
  • Group III metal hydrides and halides, certain Group IV hydrides and halides, and halogens, previously thought to require distillation for removal, were discovered to be capable of removal by scrubbing to a degree of ultrapurification which is adequate for high-precision operations.
  • Nitric acid is useful for wet etching of silicon, and is also used, for example, in some recipes for chemical-mechanical polishing of interconnect metallization, and in compounds for etching various heavy metals, and for defect etching.
  • the present inventors have now discovered that on-site distillation of nitric acid can be used to obtain ultrapure nitric acid for semiconductor processing.
  • the HNO 3 /H 2 O system has a high-bp azeotrope (68.5%wt HNO 3 , nbp 122°C).
  • the source material for distillation is provided at a concentration higher than that of the high-bp azeotrope, so that dilution does not occur during condensation.
  • a reflux condenser is preferably used, with a continuous purge to prevent impurities from accumulating. This is performed on-site, at a semiconductor manufac ⁇ turing facility, and the ultrapure chemical thus generated is routed directly, (preferably through ultraclean piping, to the point of use in a semiconductor front end.
  • Figure 1 is a simplified diagram of the distillation system used in the described sample embodiment of nitric acid ultrapurification.
  • Figure 2 shows measured data values achieved with the system of Figure 5.
  • Figure 3 is a block diagram of a semiconductor fabrication process which is connected to use the nitric acid produced by the purification unit of Figure 1.
  • Figure 4 shows a phase diagram of the H**,O/HNO 3 system.
  • Figure 5 shows a benchtop apparatus used to derive actual test results.
  • FIG. 1 is a simplified diagram of an on-site distillation system used for nitric acid ultrapurification at a semiconductor manufacturing facility.
  • Supply tank T-3 (optionally fed from tanks T-l and T-2, to permit mixing up to concentrations above 70%) supplies nitric acid feedstock at greater than 70%wt concentration (preferably 72% wt) to the reboiler portion (R-l) of a column C-1.
  • a top condenser CD-I removes heat of condensation from the vapor out from the column, and aftercooler HX-1 further cools the condensate.
  • a small top stream is vented, but this is only about 0.1% of the total vapor-phase flow.
  • Tanks T-4 and T-5 are used alternately to dilute the product to the desired strength, and the diluted product is fed to reservoir T-6, for metering as desired to the point of use.
  • the condensate (product) draw is further cooled by heat exchanger HX-1.
  • the product is then diluted, in tanks T-4 and T-5, down to the concentration (e.g. 70%wt) desired by the end-user.
  • ultrapure water is used to dilute the acid.
  • Typical standards for ultrapure water are a resistivity of at least about 15 megohm-cm at 25 °C (typically 18 megohm-cm at 25°C), less than about 25ppb of electrolytes, a particulate content of less than about 150/cm 3 and a particle size of less than 0.2 micron, a microorganism content of less than about 10/cm , and total organic carbon of less than 1 OOppb.
  • the column will typically contain a conventional column packing to provide for a high degree of contact between liquid and gas.
  • the column has a packed height of approximately 3 feet (0.9 meter) and an internal diameter of approximately 7 inches (18 cm), to achieve a packing volume of 0.84 cubic feet (24 liters), and is operated at a pressure drop of about 0.3 inches of water (0.075 kPa) or less, and less than 10% flood.
  • the packing material is preferably 8x8mm, but could alternatively be 10x10mm.
  • the units described up to this point may be operated in either batchwise, continuous, or semi-continuous manner. Continuous or semi-continuous operation is preferred.
  • the reboiler flask 2 in this sample embodiment is heated by a 600W heating mantle 1. With this heating mantle the boil up rate is 17.4 g/min. Product is drawn between packed column 4 and condenser 5, and cooled by the following stages 7 and 8. This apparatus was operated in batch mode.
  • the feedstock used was 72% wt technical grade nitric acid from Fisher. (The illustrated configuration of Figure 1 can be used to provide an admixture of fuming nitric, to bring the concentration up high enough, but the presently preferred embodiment simply uses a more concentrated feedstock.)
  • the table of Figure 2 shows results from actual tests run with the bench-scale apparatus of Figure 5. This table gives measured concentrations, in parts per billion, of the various impurities listed. Note that most of the impurities were below the detection limit in the condensate.
  • Nitric acid does decompose during distillation, producing a noticeable amount of red brown NO ⁇ vapor (mostly NO 2 ). Since the density of NO ⁇ vapor is heavier than air but lighter than the water-nitric acid vapor, this red brown cloud tended to stay at the bottom of the condenser during the distillation experiment, and fell down into the reboiler flask after the heater was off.
  • the amount of this decomposition depends on the assay and the amount of the boiling acid as well as the time of distillation.
  • the 71.4% acid was found to decompose much more readily than the 69.4 to 70.0% acid of other experiment.
  • Figure 3 is a block diagram of a semiconductor fabrication process which is connected to use the nitric acid produced by the purification unit of Figure 1.
  • incoming wafers are thoroughly cleaned and tested ("Wafer preparation”). Nitric acid may be used at this step to remove metallic surface contaminants.
  • the n- wells and/or p- wells are formed (for a CMOS process), together with the field isolation regions (typically LOCOS or some variant thereof).
  • a VT implant is performed, a sacrificial oxide is grown and stripped, a gate oxide is grown, an insulated gate is formed (e.g. of a suicided polysilicon on the gate oxide) and patterned, and source/drain regions are formed (typically in multiple steps, to provide LDD or graded-drain structures).
  • a first interlevel dielectric (“ILD”) is now formed, and a second polysilicon (or polycide) layer is now deposited and patterned.
  • a second ILD is now formed and patterned, and a first metallization layer (“Metal- 1") is now formed and patterned.
  • a third ILD is now formed and patterned, and a second metallization layer (“Metal-2”) is now formed and patterned.
  • CMP may be used to planarize the upper ILD layers above or beneath the metal layers.
  • a protective overcoat is deposited, and patterned to expose contact pad locations.
  • the disclosed innovative techniques are not strictly limited to manufacture of integrated circuits, but can also be applied to manufacturing discrete semiconductor components, such as optoelectronic and power devices.
  • the disclosed innovative techniques can also be adapted to manufacture of other technologies where integrated circuit manufacturing methods have been adopted, such as in thin-film magnetic heads and active-matrix liquid-crystal displays; but the primary application is in integrated circuit manufacturing, and applications of the disclosed techniques to other areas are secondary.
  • piping for ultrapure chemical routing in semiconductor front ends may include in-line or pressure reservoirs. Thus references to "direct" piping in the claims do not preclude use of such reservoirs, but do preclude exposure to uncontrolled atmospheres.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Power Engineering (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Cleaning Or Drying Semiconductors (AREA)
  • Weting (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Système et procédé de production de semiconducteurs utilisant une distillation sur place afin d'obtenir un acide nitrique ultra pur à partir d'une matière de départ de qualité industrielle. La matière de départ destinée à la distillation (T-3) se présente à une concentration supérieure à celle de l'azéotrope à point d'ébullition élevé, de sorte qu'une dilution ne se produise pas pendant la condensation (C-1). On utilise un condenseur de reflux (CD-1) avec une purge d'au moins 5 % afin d'empêcher l'accumulation d'impuretés. Ceci est effectué sur place, dans une unité de production de semiconducteurs, et l'agent chimique ultra pur ainsi généré est acheminé directement, par une canalisation ultra propre, jusqu'au point d'utilisation dans une extrémité de tête de semiconducteurs (T-5).
PCT/US1996/009215 1995-06-05 1996-06-05 Production sur place d'acide nitrique d'ultra haute purete pour le traitement de semiconducteurs WO1996039263A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
AU60934/96A AU6093496A (en) 1995-06-05 1996-06-05 On-site manufacture of ultra-high-purity nitric acid for sem iconductor processing
KR1019970708704A KR19990022225A (ko) 1995-06-05 1996-06-05 반도체 공정용 초순도 질산의 온-사이트 제조 시스템
JP9501593A JPH11507004A (ja) 1995-06-05 1996-06-05 半導体処理用超高純度硝酸の現場での製造
EP96918226A EP0835168A4 (fr) 1995-06-05 1996-06-05 Production sur place d'acide nitrique d'ultra haute purete pour le traitement de semiconducteurs
US08/759,213 US6214173B1 (en) 1996-06-05 1996-12-05 On-site manufacture of ultra-high-purity nitric acid

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PCT/US1995/007649 WO1996039358A1 (fr) 1995-06-05 1995-06-05 Purification de gaz ammoniac jusqu'au niveau requis pour son utilisation dans la fabrication de composants electroniques
KEPCT/US95/07649 1995-06-06

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US67401696A Continuation-In-Part 1996-06-05 1996-07-01

Publications (1)

Publication Number Publication Date
WO1996039263A1 true WO1996039263A1 (fr) 1996-12-12

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Family Applications (2)

Application Number Title Priority Date Filing Date
PCT/US1995/007649 WO1996039358A1 (fr) 1994-01-07 1995-06-05 Purification de gaz ammoniac jusqu'au niveau requis pour son utilisation dans la fabrication de composants electroniques
PCT/US1996/009215 WO1996039263A1 (fr) 1995-06-05 1996-06-05 Production sur place d'acide nitrique d'ultra haute purete pour le traitement de semiconducteurs

Family Applications Before (1)

Application Number Title Priority Date Filing Date
PCT/US1995/007649 WO1996039358A1 (fr) 1994-01-07 1995-06-05 Purification de gaz ammoniac jusqu'au niveau requis pour son utilisation dans la fabrication de composants electroniques

Country Status (5)

Country Link
EP (2) EP0830316A1 (fr)
JP (2) JPH11506411A (fr)
KR (2) KR19990022281A (fr)
AU (2) AU2862495A (fr)
WO (2) WO1996039358A1 (fr)

Cited By (9)

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EP0970744A2 (fr) 1998-07-07 2000-01-12 Air Products And Chemicals, Inc. Générateur chimique avec conditions de mélange controlées et avec régulation à réaction et ajustement de la concentration
US7091043B2 (en) 1999-12-10 2006-08-15 Showa Denko K.K. Method for measuring water concentration in ammonia
US7871249B2 (en) 1998-04-16 2011-01-18 Air Liquide Electronics U.S. Lp Systems and methods for managing fluids using a liquid ring pump
US7980753B2 (en) 1998-04-16 2011-07-19 Air Liquide Electronics U.S. Lp Systems and methods for managing fluids in a processing environment using a liquid ring pump and reclamation system
CN105056563A (zh) * 2015-08-11 2015-11-18 浙江尚能电子材料有限公司 一种硝酸精馏系统及其精馏方法
EP3118157A1 (fr) * 2015-07-14 2017-01-18 Instytut Lotnictwa Procédé à étape unique pour la production de peroxyde d'essai élevée (hlp) à des fins de propulsion de peroxyde d'hydrogène et système de production de celui-ci
US10316469B2 (en) 2014-12-16 2019-06-11 Ecolab Usa Inc. On-line control and reaction process for pH adjustment
CN110589784A (zh) * 2019-10-08 2019-12-20 中国计量科学研究院 一种实验室级超纯硝酸的精细串联纯化系统与纯化方法
US10739795B2 (en) 2016-06-17 2020-08-11 Air Liquide Electronics U.S. Lp Deterministic feedback blender

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US6576138B2 (en) * 2000-12-14 2003-06-10 Praxair Technology, Inc. Method for purifying semiconductor gases
KR101470311B1 (ko) * 2013-07-24 2014-12-08 코아텍주식회사 공업용 암모니아 정제장치
KR102505203B1 (ko) 2022-08-01 2023-03-02 제이엔에프주식회사 질산정제폐열 재활용 효율이 우수하고, 금속이온 용출이 적은 탄탈륨 소재 리보일러를 이용한 초고순도 질산정제시스템

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US5362469A (en) * 1991-10-31 1994-11-08 Solvay Fluor Und Derivate Gmbh Preparation of ultrapure hydrogen fluoride
US5496778A (en) * 1994-01-07 1996-03-05 Startec Ventures, Inc. Point-of-use ammonia purification for electronic component manufacture
US5500098A (en) * 1993-08-05 1996-03-19 Eco-Tec Limited Process for regeneration of volatile acids

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US3383173A (en) * 1965-12-30 1968-05-14 Chevron Res Ammonia purification
DD268230A1 (de) * 1987-12-28 1989-05-24 Dresden Komplette Chemieanlag Verfahren zur reinigung von ammoniakdampf
SU1650579A1 (ru) * 1988-07-18 1991-05-23 Ленинградский институт текстильной и легкой промышленности им.С.М.Кирова Способ очистки газообразного аммиака от масла и механических примесей
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US4144092A (en) * 1975-03-10 1979-03-13 Ruthner Industrieanlagen-Aktiengesellschaft Process for regenerating a nitric acid-hydrofluoric acid pickling solution
US4828660A (en) * 1986-10-06 1989-05-09 Athens Corporation Method and apparatus for the continuous on-site chemical reprocessing of ultrapure liquids
US5164049A (en) * 1986-10-06 1992-11-17 Athens Corporation Method for making ultrapure sulfuric acid
US4756899A (en) * 1987-02-12 1988-07-12 Allied-Signal Inc. Manufacture of high purity low arsenic anhydrous hydrogen fluoride
US4929435A (en) * 1987-02-12 1990-05-29 Allied-Signal Inc. Manufacture of high purity low arsenic anhydrous hydrogen fluoride
US4952386A (en) * 1988-05-20 1990-08-28 Athens Corporation Method and apparatus for purifying hydrogen fluoride
US4980032A (en) * 1988-08-12 1990-12-25 Alameda Instruments, Inc. Distillation method and apparatus for reprocessing sulfuric acid
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US7871249B2 (en) 1998-04-16 2011-01-18 Air Liquide Electronics U.S. Lp Systems and methods for managing fluids using a liquid ring pump
US7980753B2 (en) 1998-04-16 2011-07-19 Air Liquide Electronics U.S. Lp Systems and methods for managing fluids in a processing environment using a liquid ring pump and reclamation system
US8702297B2 (en) 1998-04-16 2014-04-22 Air Liquide Electronics U.S. Lp Systems and methods for managing fluids in a processing environment using a liquid ring pump and reclamation system
EP0970744A2 (fr) 1998-07-07 2000-01-12 Air Products And Chemicals, Inc. Générateur chimique avec conditions de mélange controlées et avec régulation à réaction et ajustement de la concentration
US6224252B1 (en) 1998-07-07 2001-05-01 Air Products And Chemicals, Inc. Chemical generator with controlled mixing and concentration feedback and adjustment
US7091043B2 (en) 1999-12-10 2006-08-15 Showa Denko K.K. Method for measuring water concentration in ammonia
US8317388B2 (en) 1999-12-20 2012-11-27 Air Liquide Electronics U.S. Lp Systems for managing fluids in a processing environment using a liquid ring pump and reclamation system
US10316469B2 (en) 2014-12-16 2019-06-11 Ecolab Usa Inc. On-line control and reaction process for pH adjustment
EP3118157A1 (fr) * 2015-07-14 2017-01-18 Instytut Lotnictwa Procédé à étape unique pour la production de peroxyde d'essai élevée (hlp) à des fins de propulsion de peroxyde d'hydrogène et système de production de celui-ci
CN105056563A (zh) * 2015-08-11 2015-11-18 浙江尚能电子材料有限公司 一种硝酸精馏系统及其精馏方法
US10739795B2 (en) 2016-06-17 2020-08-11 Air Liquide Electronics U.S. Lp Deterministic feedback blender
CN110589784A (zh) * 2019-10-08 2019-12-20 中国计量科学研究院 一种实验室级超纯硝酸的精细串联纯化系统与纯化方法

Also Published As

Publication number Publication date
JPH11507004A (ja) 1999-06-22
EP0835168A1 (fr) 1998-04-15
KR19990022281A (ko) 1999-03-25
EP0830316A1 (fr) 1998-03-25
EP0835168A4 (fr) 1998-08-26
AU6093496A (en) 1996-12-24
KR19990022225A (ko) 1999-03-25
JPH11506411A (ja) 1999-06-08
AU2862495A (en) 1996-12-24
WO1996039358A1 (fr) 1996-12-12

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