WO2014037486A1 - Procédé de nettoyage de chambre utilisant du f2 à basse pression - Google Patents

Procédé de nettoyage de chambre utilisant du f2 à basse pression Download PDF

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Publication number
WO2014037486A1
WO2014037486A1 PCT/EP2013/068439 EP2013068439W WO2014037486A1 WO 2014037486 A1 WO2014037486 A1 WO 2014037486A1 EP 2013068439 W EP2013068439 W EP 2013068439W WO 2014037486 A1 WO2014037486 A1 WO 2014037486A1
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WIPO (PCT)
Prior art keywords
chamber
pressure
bar
equal
abs
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PCT/EP2013/068439
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English (en)
Inventor
Oliviero Diana
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Solvay Sa
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Publication of WO2014037486A1 publication Critical patent/WO2014037486A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/245—Fluorine; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B15/00—Operating or servicing cells
    • C25B15/08—Supplying or removing reactants or electrolytes; Regeneration of electrolytes

Definitions

  • the invention concerns a chamber cleaning method using F 2 which is supplied at a low pressure.
  • F 2 (elemental fluorine) is used, i.a., as an etching agent and as a cleaning agent for cleaning of chambers, e.g. CVD or PVD chambers, used in the manufacture of semiconductors, micro-electromechanical devices, solar cells, TFTs (thin film transistors).
  • HF was considered as undesirable component in F 2 intended for etching or chamber cleaning.
  • WO 2012/016997 for example provides a purification process for the manufacture of highly pure F 2 , useful as etching agent and chamber cleaning agent, with a content of equal to or less than 10 ppm of HF.
  • F 2 is often manufactured by the electrolysis of hydrogen fluoride (HF) in the presence of molten/dissolved fluoride salts ; especially adducts of HF and KF having a formula of about KF (1.8 - 2.3)HF are electrolyzed. Often, production of F 2 for chamber cleaning is performed on site, i.e. on the premises of the point of use.
  • HF hydrogen fluoride
  • KF KF having a formula of about KF (1.8 - 2.3)HF
  • Object of the present invention is to provide a technically and
  • the present invention concerns a method for the cleaning of at least one chamber using elemental fluorine wherein the fluorine is produced in at least one electrolytic cell, and wherein the pressure of F 2 in the electrolytic cell is equal to or lower than 1.1 bar (abs), and the pressure of the F 2 delivered to the at least one chamber is equal to or lower than 0.85 bar (abs).
  • the pressure of the F 2 in the electrolytic cell is equal to or greater than 1 bar (abs).
  • Figure 1 shows a scheme for an assembly useful for performing the invention.
  • the pressure of the F 2 in the at least one electrolytic cell is equal to or lower than 1.05 ⁇ 0.02 bar (abs).
  • a pressure range of from 1 to 1.05 ⁇ 0.02 bar (abs) is very suitable.
  • the chambers which can be cleaned are preferably those used in the manufacture of semiconductors, micro-electromechanical devices, solar cells (photovoltaic items), and TFTs (thin film transistors). In such chambers, items are treated according to known processes. For example, layers of Si, Si0 2 , silicon nitride, silicon oxynitride, metals, metal oxides or carbon- fluorine polymers are formed on the surface or a part of the surface of the items, e.g.
  • PECVD plasma enhanced
  • the chamber cleaning method of the present invention can be performed thermally or supported by in-situ plasma and/or by remote plasma.
  • the temperature during a thermal chamber cleaning is preferably equal to or greater than 400°C. In plasma-supported chamber cleaning, the temperature inside the chamber may often be greater than 100°C.
  • the plant for F 2 manufacture may preferably be located on site of the plant having chambers of which are to be purified. If desired, however, the F 2 may be produced remote from the point of use and be transported from the location of its manufacture to its point of use.
  • the pressure in the electrolytic cell both on the F 2 and H 2 side does not oscillate over a too high range ; often, it is preferred to keep the cell pressure within ⁇ 0.01 to ⁇ 0.05 bar of a preset value.
  • the F 2 is especially preferably generated in the electrolytic cell at a pressure of approximately 1.05 ⁇ 0.02 bar (abs) and forwarded, via several steps to the point of use as chamber cleaning agent.
  • the F 2 has a pressure below 1 bar (abs), preferably having a pressure in the range from equal to or greater than 0.2 bar (abs) to equal to or lower than 0.85 bar (abs). Often, it is in a pressure of from 0.2 to 0.55 bar (abs). From the electrolytic cell to the point of use in the chamber, the F 2 is not pressurized in the method of the invention. Thus, the pressure of the F 2 is lower after every treatment step due to a pressure drop in each step.
  • the preferred embodiment of the method of the invention comprises A) a step of electro lytically producing raw F 2 from HF in the presence of KF
  • step B) a step of removing particles entrained in the raw F 2 obtained in step A)
  • the F 2 is not pressurized neither in any of these steps, nor between any of them. This means that the driving force passing the F 2 from step A) to the final use in step E) is the pressure of approximately 1 to 1.1 bar (abs) in the electrolytic cell compartment in which the raw F 2 is generated.
  • the method of the invention consists of these steps.
  • the flow of F 2 can be measured, for example, with a flow indicator, for example, a flow indicator operating according the Coriolis type which is very accurate.
  • Step A) usually is performed by electrolysis of HF in the presence of an electrolyte salt of the approximate formula KF*(1.8-2.3)HF.
  • Step B) may be performed by contacting the raw F 2 from step B) with liquid HF, e.g. by passing the raw F 2 through liquid HF, in a static scrubber or in a jet scrubber.
  • the scrubber can be operated in large range of temperatures ; it may be composed of multiple stages ; two or more scrubbers can be arranged in parallel and/or in series ; and each of these scrubbers can be operated at different pressures and/or different temperatures.
  • the temperature of the scrubber or each of the scrubbers, if there are more scrubbers than one, can vary between -200°C and +20°C.
  • the temperature of the scrubber or each of scrubbers is equal to or higher than -150°C, and more preferably, it is equal to or higher than -82°C.
  • the temperature of the scrubber or each of the scrubbers, if there are more scrubbers than one is equal to or lower than -50°C.
  • a preferred temperature range for the scrubber or each of the scrubbers, if more than one scrubbers are in use, is from -150°C to -20°C ; an especially preferred range is from -80°C to -50°C.
  • the amount of HF which is removed from the F 2 will vary. For example, at a higher pressure, at a lower temperature in the scrubber or scrubbers, and if several scrubbers are assembled in series, the amount of HF removed can be almost completely, such that only a few ppm are left in the treated F 2 .
  • the temperature is in the upper region of the range given above, at a lower pressure and only one scrubber to be passed, the amount of removed HF is low, and the F 2 after treatment may comprise almost all of the HF entrained. Nevertheless, the advantage of scrubbers, namely to remove solids, still will be achieved.
  • Step C) may be performed by passing the F 2 withdrawn from step B) through a filter made from suitably resistant material, e.g. made from Monel metal.
  • the pore size may be equal to or smaller than 100 ⁇ , preferably equal to or smaller than 20 ⁇ .
  • a suitable pore size range is 1 to 20 ⁇ .
  • the pore size is equal to or greater than 0.001 ⁇ .
  • a preferred range is from 0.001 to 20 ⁇ .
  • the F 2 withdrawn from step C) may be passed into a storage tank or in a buffer tank before it is delivered to the point of use in chamber cleaning step E).
  • the F 2 is stored in a sufficiently large buffer tank before its delivery to the point of use for the step of chamber cleaning.
  • F 2 containing more than 0.1 % by weight and less than 2.5 % by weight of HF is produced in steps A) to D.
  • the content of HF in the F 2 is preferably equal to or greater than 0.5 % by weight.
  • it is equal to or lower than 2 % by weight ; and the pressure of the F 2 in the line to the chamber or chambers to be cleaned, i.e. at the point of use, preferably is 0.2
  • the estimated minimal and maximal pressure drop in each step is given in the following table 1. It has to be noted that in the following description, a method is further explained wherein the pressure in the electrolytic cell is 1.05 bar (abs) because this is the preferred embodiment.
  • the absolute pressure (but essentially not the pressure drop) may also be higher if the cell is operated at a higher pressure of the F 2 compartment. Pressure drop in intermediate steps from F 2 generation to the point of
  • the F 2 is preferably not passed through an adsorbent tower, e.g., an NaF tower, or through a cooled trap, e.g. a trap cooled to a temperature equal to or lower than -90°C. That is because the aim of this invention is to keep the process as simple as possible, because simple means cheap, reliable and safe.
  • a finishing step like NaF adsorption or very cold trap (temperature equal to or lower than -90°C)
  • the F 2 can be passed to the point of use via a flow indicator, e.g. a flow indicator operating according to the Coriolis type.
  • a flow indicator e.g. a flow indicator operating according to the Coriolis type.
  • step A) F 2 is produced electrolytically. Often, salt compositions of the approximate formula KF (1.8 - 2.3)HF are applied. Such compositions have a melting point, depending on the composition, around 80°C or above. Usually, an electrolyzer contains several electrolytic cells. Each cell often contains a multitude of anodes. Often, the cell vessel containing the molten salt serves as cathode, or several separate electrodes are used as cathodes. Fresh HF is supplied continuously or batch wise to the cell to replenish electrolyzed HF.
  • HF is electrolyzed to form F 2 and H 2 which are collected in separate cell compartments. H 2 may be dumped.
  • the raw F 2 formed contains up to 10 % by weight of HF, and possibly even more ; the raw F 2 further contains entrained particles which are essentially constituted of solidified electrolyte salt.
  • step A the raw F 2 is withdrawn from the respective cell compartment having a pressure of equal to or greater than 1 bar (abs).
  • the pressure of the raw F 2 in the F 2 compartments is approximately 1.05 ⁇ 0.05 bar (abs).
  • step B) Preferred embodiments of step B) :
  • step B) the raw F 2 is subjected to a purification treatment to separate all or a major part of solid impurities from the raw F 2 .
  • the solid- removing treatment comprises at least one step of contacting the raw F 2 with cooled liquid HF in a static scrubber.
  • the liquid HF with which the raw F 2 is contacted has a low temperature and consequently a low vapor pressure.
  • the temperature of the liquid HF during its purifying contact with the fluorine is equal to or higher than the melting point of the HF at the respective pressure in the static scrubber. Preferably, it is equal to or higher than -83°C, more preferably, it is equal to or higher than -82°C. It is preferably equal to or lower than -60°C.
  • the temperature of the liquid HF is preferably in the range between -60°C and -82°C.
  • the HF can be cooled by cooling machines which provide a suitably cooled liquid to heat exchangers to keep the HF at the desired low temperature.
  • the liquid HF in the scrubber is indirectly cooled by means of liquid N 2 which, when passing from the liquid to the gaseous state, provides the desired cooling effect.
  • the F 2 can be contacted with technical grade liquid HF. If desired, purified liquid HF can be applied.
  • the raw F 2 from step A) may preferably be contacted with a purified liquid HF which is essentially free of at least phosphorous compounds, sulfur compounds and arsenic compounds.
  • HF can be purified according to the process of US patent 5,362,469 and then has a content of water of less than 1 ppm.
  • step B) it is sufficient to perform step B) only once to achieve a desired degree of solids removal. But if desired, the contact between F 2 and liquid HF can be repeated once, or even more often.
  • the raw F 2 is supplied to the static scrubber to be contacted with liquid HF under the pressure it has in the electrolytic cell compartment. No pump or compressor is used to raise the pressure of the raw F 2 withdrawn from the electrolytic cell compartment. Due to the marginal pressure loss in the line from the electrolytic cell compartment to the scrubber, the raw F 2 enters the scrubber with a pressure corresponding to the pressure in the electrolytic cell, i.e. 1.05 ⁇ 0.02 bar (abs).
  • the F 2 after the contact with liquid HF contains more than 0.1 % by weight and less than 2.5 % by weight.
  • the liquid HF which is used in the purification step is preferably circulated or reused, optionally after regeneration, e.g. by a step of distillation, to remove any solids washed out from the raw fluorine as described above.
  • the advantage is that any water initially present in the HF reacts with F 2 to form HF and OF 2 ; after some time, the water is consumed, and the fluorine to be purified will not be consumed by water in a side reaction, and the fluorine will not take up any OF 2 anymore because it is no longer formed.
  • the F 2 which leaves the static scrubber has a pressure which is, as a rule of thumb, approximately 40 to 80 mbar lower than upon entering the static scrubber.
  • the HF content depends from several conditions, e.g. from the initial HF concentration, from the temperature of the liquid HF and from the contact time. The conditions of contact between the liquid HF and the F 2 are selected such that the HF content is in the range given above, and notably, in the preferred ranges.
  • step C) Preferred embodiments of step C) :
  • the F 2 withdrawn from step B) is then treated in step C).
  • no pump or compressor is used to raise the pressure of the F 2 withdrawn from step B) and forwarded to step C).
  • the F 2 is passed in step C) through one or more particle filters with small pores to remove any residual solids content.
  • the filter or filters may comprise pores in the range of 0.01 to 20 ⁇ . Pore size denotes the pore diameter. Particle filters with a pore size greater than 20 ⁇ could be applied but may not be effective enough.
  • the particle filters serve to remove any solid particles before the contact with liquid HF, or to remove solids still entrained after the purifying treatment of the present invention ; the particle filters may be constructed from materials resistant to F 2 , especially from steel or Monel metal.
  • the temperature in the filter should advantageously be lower than the melting point of the solids (which is usually somewhat above 80°C).
  • the temperature in the filter is equal to or lower than 50°C.
  • step C) is performed at ambient pressure.
  • the F 2 leaving the filter in step C) has a pressure which is approximately
  • F 2 having passed steps B) and C) is suitably pure to be used as cleaning agent for chambers used for CVD-enhanced deposition of matter on items. It is especially suitable for cleaning of chambers which have been used for deposition and/or etching of layers, like CVD chambers, used in the manufacture of semiconductors, micro-electromechanical devices, solar cells, TFTs (thin film transistors).
  • step D) Preferred embodiments of step D) :
  • step D) The F 2 leaving step C) is subjected to step D).
  • step D) it is delivered, optionally via a buffer tank or a storage tank, to the point of use, i.e. a chamber or a plurality of chambers to be cleaned. No pressurization is performed, thus it is not passed through a pump or a compressor.
  • the F 2 leaving step C) is stored in a storage tank.
  • the storage tank it is preferably stored at the pressure with which it is withdrawn from step C).
  • a control valve may be applied to reduce the F 2 pressure in the buffer tank.
  • the F 2 pressure preferably is in a range from equal to or greater than 0.2 bar (abs) to 0.8 bar (abs).
  • the buffer tank or tanks may require a large internal volume.
  • one or more buffer tanks having an internal volume from 10 to 50 m 3 are preferred.
  • Using two or more buffer tanks, e.g. 4 buffer tanks, having an internal volume of 25 m 3 provides sufficient capacity to provide a reliable F 2 delivery.
  • the F 2 buffer tanks represent usually the major hold-up of F 2 of all the process and of all the plant, and hence are the most hazardous item in the process.
  • the safety of the process is significantly increased vs. the standard pressurized process, because any leak of F 2 to the external atmosphere is intrinsically impossible.
  • the buffer tanks can also be made double walled, with the jacked kept under vacuum or dry Nitrogen blanket. This intrinsic safety applies actually not only to the Buffer tanks, but to all process items, from the electrolytic cells down to the final user CVD chamber.
  • the chamber cleaning method of the invention is performed such that step A) is performed in an electrolyzer, step B) is performed in a static scrubber, step C) is performed using a metallic filter, step D) is performed in a buffer tank or storage tank, and the F 2 leaving step D) is delivered to at least one chamber and used in the chamber in a chamber cleaning step E), wherein the electrolyzer, the static scrubber, the metallic filter, the buffer tank or storage tank and the at least one chamber are operably connected.
  • step E) Preferrred embodiments of step E) :
  • the chamber cleaning step E) is performed by applying a remote plasma, an in-situ plasma or both.
  • the pressure of the F 2 in each of the steps B) to D) and in step E) is lower than the pressure of F 2 in the preceding step.
  • the F 2 pressure in step A) is equal to or lower than 1.1 bar (abs), preferably equal to or lower than 1.05 ⁇ 0.02 bar (abs), and preferably, the F 2 is delivered to the chamber in step (II) at a pressure from equal to or greater than 0.2 bar (abs) to equal to or lower than 0.55 bar (abs).
  • the F 2 provided by the invention often contains HF from 0.1 to 2.5 % by weight, and it is very well suited as chamber cleaning agent.
  • An F 2 containing 1 to 2 % by weight of HF can be manufactured technically easy (only a short contact time in the static scrubber is necessary, for example), no NaF tower is used, no cold trap to remove further HF, and nevertheless the F 2 containing HF is very suitable as chamber cleaning agent.
  • steps A) to E) are performed on site.
  • the electrolyzer apparatus, scrubber, filter, storage tank and chamber or chambers are connected through lines in this embodiment.
  • the method of chamber cleaning has many advantages over the prior art.
  • the method does not make use of steps needed to provide F 2 which is free of HF, and compressors or other means to raise the F 2 pressure are not applied ; contrary to the common belief that highly pure F 2 , notably F 2 essentially free of HF, is needed for chamber cleaning, it was found that F 2 containing HF with a content of up to 2.5 % by weight of HF is very suitable for that purpose. Consequently, it is not necessary to subject F 2 to thorough and careful purifying operations to remove even minute amounts of HF.
  • An added advantage is the finding that the purifying steps according to the process of the invention can be performed such that no pump or compressor is needed to subject purified F 2 to pressurization.
  • F 2 is produced electrolytically in an electrolyzer comprising multiple indicated in figure 1 under the reference sign 1.
  • H 2 formed is passed to scrubber 2 where F 2 and HF are removed, e.g. by a caustic aqueous solution. Gases passing scrubber 2 are released to the atmosphere in line 3.
  • Raw F 2 is passed through line 4 (where the pressure of F 2 is approximately 1.05 bar (abs) to a scrubber 5 operated -80°C wherein solids and some HF are removed.
  • F 2 leaves scrubber 5 at a pressure of approximately 0.95 bar (abs) through line 6. It is passed to filter 7 which is operated at 20°C to remove any solids still entrained.
  • F 2 is passed at a pressure of 0.8 bar (abs) to a buffer tank 9.
  • buffer tank assembly For example, 4 tanks, each with a capacity of 25 m 3 , can be foreseen as buffer tank assembly.
  • the pressure in the buffer tank 9 corresponds approximately to the pressure in line 8.
  • F 2 is withdrawn through line 10 to be supplied to chamber 11.
  • the pressure of F 2 withdrawn from buffer tank 9 can be reduced by valves to a pressure in a range of from 0.55 to 0.2 bar (abs).
  • Example 1 Manufacture of F 2 , its purification and its delivery for chamber cleaning
  • Step A) manufacture of F 2
  • An electrolyte salt with a composition of about KF 2HF is filled into an electrolysis cell, heated to about 80 - 120°C and molten therein. A voltage between 8 to 10 V is applied, and current is passed through the composition of electrolyte salt dissolved in the hydrogen fluoride.
  • HF is introduced into the electrolytic cell in an amount corresponding to consumed HF.
  • Raw F 2 under a pressure of about 1.05 bar (abs) and H 2 form in the respective electrode compartments.
  • H 2 is passed through a water scrubber to removed entrained HF and is then released to the atmosphere.
  • Step B) Removal of HF and solids
  • the raw F 2 in the anode compartment of the electrolytic cells contains HF and entrained solids (mainly electrolyte salt) It is withdrawn from the electrolytic cells at a pressure of about 1.05 bar (abs) and contacted in a static scrubber with liquid HF which has a temperature of about -80°C. Most of the solids and the major part of HF entrained in the F 2 are removed in the static scrubber.
  • the F 2 leaving the static scrubber has an HF content of about 1 % by weight, and its pressure is about 0.95 bar (abs).
  • Step C) Additional solids removal in a filter
  • the F 2 leaving step B) is passed through a Monel metal frit with pores having a diameter of approximately 1 ⁇ to further reduce the solids content.
  • the F 2 leaving the metal frit has a pressure of approximately 0.8 bar (abs) and a very low content of entrained solids.
  • the frits are plugged from time to time by filtered solids. They can be cleaned by a treatment with liquids to dissolve the solids.
  • Step D) Delivery to the buffer tank
  • the F 2 leaving the Monel filter frit in step C) still has a content of about 1 % by weight of HF, but a very low solids content. It is passed into a buffer tank having an internal volume of 25 m 3 ; four such buffer tanks are assembled. In the buffer tank, the F 2 is stored under a pressure of approximately
  • a control valve can be foreseen between the Monel filter of step C) and the buffer tank ; by means of the control valve, the pressure of the F 2 in the buffer tank can be reduced to a still lower level (e.g., it can be stored at a pressure ranging from 0.2 to 0.55 bar).
  • Step E) As soon as F 2 is needed as chamber cleaning agent, it is provided from the buffer tank through a delivery line. It is passed through a control valve which further reduces the pressure, e.g. to 0.5 bar (abs) if the F 2 pressure in the buffer tank is greater than 0.5 bar (abs).
  • the F 2 which finally is delivered to a chamber (used for the manufacture of photovoltaic cells) as cleaning agent has an HF content of 1 % by weight and a pressure of approximately 0.5 bar (abs).
  • F 2 containing HF is introduced as the cleaning agent, an in- situ plasma is ignited and the cleaning agent, having a pressure of about

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Metallurgy (AREA)
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Abstract

Du fluor élémentaire est souvent fabriqué par voie électrochimique à partir d'une solution de KF dans du fluorure d'hydrogène et il contient des quantités variables d'HF en tant qu'impureté. La présente invention porte sur un procédé pour le nettoyage de chambre utilisant du F2 qui est apporté au point d'utilisation en tant qu'agent de nettoyage de chambre à une basse pression, de préférence dans une plage allant d'une valeur supérieure ou égale à 0,2 à une valeur inférieure ou égale à 0,85 bar (abs). L'omission de certaines étapes de nettoyage et de mise sous pression permet un processus plus simple, économique, fiable et sans danger pour apporter du F2 et l'utiliser comme agent de nettoyage de chambre.
PCT/EP2013/068439 2012-09-10 2013-09-06 Procédé de nettoyage de chambre utilisant du f2 à basse pression WO2014037486A1 (fr)

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EP12183650 2012-09-10
EP12183650.6 2012-09-10

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03293726A (ja) * 1990-02-07 1991-12-25 Central Glass Co Ltd 混合ガス組成物
US5362469A (en) 1991-10-31 1994-11-08 Solvay Fluor Und Derivate Gmbh Preparation of ultrapure hydrogen fluoride
US5585085A (en) 1991-10-31 1996-12-17 Solvay Fluor Und Derivate Gmbh Removal of water and/or hydrocarbons from hydrogen fluoride
US6602433B1 (en) * 1999-03-04 2003-08-05 Surface Technology Systems Plc Gas delivery system
US20090001524A1 (en) * 2001-11-26 2009-01-01 Siegele Stephen H Generation and distribution of a fluorine gas
WO2011117234A2 (fr) * 2010-03-26 2011-09-29 Solvay Sa Procédé d'approvisionnement en fluor
WO2012016997A1 (fr) 2010-08-05 2012-02-09 Solvay Sa Procédé de purification du fluor

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03293726A (ja) * 1990-02-07 1991-12-25 Central Glass Co Ltd 混合ガス組成物
US5362469A (en) 1991-10-31 1994-11-08 Solvay Fluor Und Derivate Gmbh Preparation of ultrapure hydrogen fluoride
US5585085A (en) 1991-10-31 1996-12-17 Solvay Fluor Und Derivate Gmbh Removal of water and/or hydrocarbons from hydrogen fluoride
US6602433B1 (en) * 1999-03-04 2003-08-05 Surface Technology Systems Plc Gas delivery system
US20090001524A1 (en) * 2001-11-26 2009-01-01 Siegele Stephen H Generation and distribution of a fluorine gas
WO2011117234A2 (fr) * 2010-03-26 2011-09-29 Solvay Sa Procédé d'approvisionnement en fluor
WO2012016997A1 (fr) 2010-08-05 2012-02-09 Solvay Sa Procédé de purification du fluor

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