Classifications

• • 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
  • C01B33/02—Silicon
  • C01B33/021—Preparation
  • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01M—CATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
  • A01M1/00—Stationary means for catching or killing insects
  • A01M1/14—Catching by adhesive surfaces
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01M—CATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
  • A01M1/00—Stationary means for catching or killing insects
  • A01M1/02—Stationary means for catching or killing insects with devices or substances, e.g. food, pheronones attracting the insects
• • 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
  • C01B33/02—Silicon
  • C01B33/021—Preparation
  • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
  • C01B33/029—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of monosilane
• • 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
  • C01B33/02—Silicon
  • C01B33/021—Preparation
  • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
  • C01B33/03—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition of silicon halides or halosilanes or reduction thereof with hydrogen as the only reducing agent
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01M—CATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
  • A01M2200/00—Kind of animal
  • A01M2200/01—Insects
  • A01M2200/012—Flying insects

Definitions

• the present invention relates to a method for mass production of granular
• high-purity polycrystalline silicon is used as a basic material for
• the polycrystalline silicon is
• a fluidized bed reactor has recently been developed to prepare granular polycrystalline silicon with a size of 0.5-3 mm. According to this method,
• a fluidized bed of silicon particles is formed by the upward flow of a gas and the size
• the fluidized bed reactor also uses
• silane compound of Si-H-Cl system such as monosilane (SiH 4 ), dichlorosilane
• silicon atom-containing reaction gas which usually further comprises hydrogen
• reaction temperature i.e., temperature of the
• the temperature should be about
• fluidized bed reactor is able to provide a granular polycrystalline silicon product.
• the seed crystals may be prepared or generated in situ in the fluidized bed itself, or supplied into the reactor
• polycrystalline silicon product may be discharged from the lower part of the reactor
• the granular product may be directly used without a
• the reactor wall is weak
• U.S. patent no. 5,165,908 discloses a reactor system where an
• electric resistance heater encloses a reactor tube made of quartz, both of which are
• U.S. patent no. 5,810,934 discloses a fluidized bed reactor for manufacture of
• polycrystalline silicon comprising a reactor vessel, i.e., the reactor tube defining a fluidized bed; a shroud, i.e., a protection tube surrounding the reactor tube; a heater
• quartz be installed in between the reactor tube and the heater to prevent the crack of
• silicon may have a different structure depending on the heating method.
• U.S. patent no. 4,786,477 discloses a method of heating silicon
• cylindrical reactor tube is hold vertically by a metallic reactor shell.
• an object of the present invention is to provide an improved method for preparing polycrystalline silicon by stable, long-term operation of a
• Another object of the present invention is to provide a method for preparing
• Still another object of the present invention is to provide a method for
• a further object of the present invention is to provide a method for preparing
• polycrystalline silicon which may secure a long-term stability while enduring a
• a still further object of the present invention is to provide a method for
• the present invention also aims to provide a method which can be
• a reactor tube is vertically placed within a reactor shell so as to be encompassed by
• silicon deposition does not occur in the outer zone; (b) directly or indirectly
• controlling means directly or indirectly measuring and/or controlling an outer zone
• the reaction gas is a silicon atom-containing gas
• silicon tetrachloride and a mixture thereof.
• reaction gas further comprises at least one gas selected from
• the fluidizing gas is a gas selected from the group
• the inert gas comprises at least one gas selected
• Pressure (Pi) is maintained within the range of 1-15 bar.
• the outer zone pressure (Po) may be controlled in the range of
• zone connecting means which are spatially connected to the the silicon particle bed.
• zone pressure (Pi) is maintained so as to satisfy the condition of 0 bar ⁇ (Po - Pi) ⁇ 1
• pressure-difference controlling means comprised in the inner pressure controlling
• a packed bed of packing materials which are not
• reaction gas inlet means through which the reaction gas is introduced into the
• a reactor tube is encompassed by a reactor shell so that the space inside the
• reactor shell can be divided into an inner zone and an outer zone by the reactor tube.
• a reactor tube 2 is vertically placed within a reactor shell 1 to be
• particles 3 i.e., a silicon particle bed is formed and silicon deposition occurs in the
• polycrystalline silicon is prepared according to the
• granular polycrystalline silicon may be prepared by
• inner pressure controlling means directly or indirectly measuring and/or
• granular polycrystalline silicon may be prepared by introducing
• reaction gas inlet means introducing an inert gas into the outer zone 5, whereby
• Figures 2 and 3 are cross-sectional views of the high-pressure fluidized bed
• invention is composed of a reactor tube and a reactor shell. An inner space of the
• the reactor shell 1 is separated from an outer space.
• the reactor shell 1 is separated from an outer space.
• the reactor tube 2 encompasses the reactor tube 2 that is substantially vertically placed within the reactor shell 1.
• the reactor tube 2 divides an inner space of the reactor shell 1 into
• the reactor shell 1 is preferably made of a metallic material with reliable
• the reactor shell 1 may be divided into a plurality of components such
• the components may have
• each component may be coated with a protective layer
• a protective tube or wall which may be made of a metallic
• cooling medium such as water, an oil, a gas and air for protecting the equipment or
• the components that need to be cooled may preferably be equipped with a coolant-circulating means at their inner
• the reactor shell 1 may comprise an insulating material.
• the reactor tube 2 may be of any shape only if it can be hold by the reactor
• the reactor tube 2 may be of a structure of a
• ellipsoid and either one end or both ends of the reactor tube 2 may be formed into a
• the reactor tube 2 may comprise a plurality of components
• the reactor tube 2 is preferred to be made of an inorganic material, which is
• nitride silicon carbide, graphite, silicon, glassy carbon or their combination.
• a carbon-containing material such as silicon carbide, graphite,
• glassy carbon may generate carbon impurity and contaminate the polycrystalline
• the reactor tube 2 is made of a carbon-containing material
• the inner wall of the reactor tube 2 is preferred to be coated or lined with materials
• the reactor tube 2 may be any suitable material such as silicon, silica, quartz or silicon nitride. Then, the reactor tube 2 may be
• the reactor tube 2 is of one-layered or
• each layer of which is made of a
• Sealing means 41a, 41b may be used for the reactor shell 1 to safely hold the
• the sealing means are preferred to be stable at a temperature of
• above 200 0 C and may be selected from organic polymer, graphite, silica, ceramic,
• the sealing means 41a, 41b may be installed less
• the partition of the inner space of the reactor shell 1 by the reactor tube 2 may
• a plurality of heating means 8a, 8b may be installed in the inner zone 4 and/ or the
• a heating means may be installed
• a plurality of heating means may be installed in
• a plurality of heating means 8a, 8b may be installed
• a single heating means may be installed in the outer zone 5 only.
• the electric energy is supplied to the heating means 8a, 8b through an electric
• the reactor and an electric source E outside the reactor may comprise a conductive
• metallic component in the form of a cable, a bar, a rod, a shaped body, a socket or a
• the electric energy supplying means 9a-9f may comprise an
• Electrode that is made of a material such as graphite, ceramic (e.g., silicon carbide),
• supplying means can be prepared by extending a part of the heating means 8a, 8b.
• electrical insulation is also important besides the mechanical sealing for preventing
• a gas inlet means should be installed at the fluidized bed reactor
• silicon particles can move by gas flow, within the
• reactor tube 2 i.e., in a lower part of the inner zone 4, for preparation of
• the gas inlet means comprises a fluidizing gas inlet means 14, 14' for introducing a fluidizing gas 10 into the silicon particle bed and a reaction gas inlet
• granular polycrystalline silicon may be prepared according to
• reaction gas 11 into the silicon particle bed using a reaction gas inlet means 15.
• a fluidizing gas 10 refers to a gas introduced to cause some
• HCl hydrogen chloride
• SiC14 silicon tetrachloride
• reaction gas 11 refers to a source gas containing silicon
• silicon tetrachloride SiCl 4
• SiCl 4 silicon tetrachloride
• reaction gas 11 may further comprise at
• At least one gas selected from hydrogen, nitrogen, argon, helium and hydrogen
• reaction gas 11 contributes to the fluidization of the silicon particles 3 as the
• the fluidizing gas inlet means 14, 14' and the reaction gas inlet means 15 may comprise a tube or nozzle, a chamber, a flange, a fitting, a gasket, etc, respectively.
• the silicon particles 3 are preferred to be made of a tube, a liner or a shaped article
• the lower part of the fluidized bed 4a in the inner zone 4 may be any one of the lower part of the fluidized bed 4a in the inner zone 4.
• the gas distributing means 19 may have any geometry or structure
• the gas distributing means 19 is additionally employed, its component, like the
• particles 3 is preferably made of an inorganic material that can be used for the
• reaction gas 11 is injected into the interior of the fluidized bed, is preferably
• fluidized bed 4a of silicon particles may be supplied in various ways depending on
• the fluidizing gas 10 may be supplied by a fluidizing gas inlet means 14, 14' coupled with the reactor shell 1 so that a gas chamber may be formed in lower
• a fluidizing gas 10 may be supplied by a fluidizing gas inlet
• ⁇ nozzle outlet may be positioned in between the gas distributing means 19 that
• means 14, 14' may be constituted by using both the distribution plate and the
• the packing materials may have a sufficient size or mass, so as not to be
• fluidized by the flow of the fluidizing gas 10 may be shaped like a sphere, an
• composition may be selected from those applicable to the reactor tube 2 as well as
• high-purity silicon with their average size being within the range of 5-50 mm.
• the polycrystalline silicon particles are prepared in the present invention.
• granular polycrystalline silicon may be prepared by discharging
• a particle outlet means 16 is also required to be combined with the reactor
• An outlet pipe, which constitutes the particle outlet means 16, may be
• reaction gas inlet means 15 may be installed independently of the reaction gas inlet means 15 as
• an additional zone may be combined with the
• the additional zone can be provided at some part or a lower part of the fluidizing gas inlet means 14', allowing a space for the silicon particles 3b to
• Silicon particles 3 i.e., silicon particles 3 discharged from the inner zone 4 to
• the outside of the reactor according to the present invention may be delivered to a
• particles 3b may have a particle-size distribution due to nature of the fluidized bed
• discharged from the inner zone 4 to the outside of the reactor may be delivered to a
• particle separation member where the particles can be separated by size. Then the
• larger particles may be delivered to the storage member or the transfer member,
• the silicon particles 3b are preferred to be cooled
• a cooling gas such as hydrogen, nitrogen, argon, helium, or a mixture
• oil or gas may be circulated through the wall of the particle outlet means 16.
• means 16 may be constituted in combination with the inner space of the reactor shell 1 (e.g. 14' in Figure 2) or a lower part of the reactor shell (e.g., Ib in Figures 2 and 3),
• high-temperature silicon product particles 3b may be made of a tube, a
• the wall may be made of a metal-material tube, a liner or a shaped product, the inner
• the silicon product particles 3b may be discharged from
• a particle separation member may be installed in between the
• the off-gas 13 comprises a
• off-gas 13 may be separated from an additional off-gas treating means 34.
• an off-gas treating means 34 which is
• a cyclone comprises a cyclone, a filter, a packed column, a scrubber or a centrifuge, may be
• Fine silicon particles thus separated from the off-gas treating means 34, may be
• off-gas treating means 34 may be recycled as seed crystals, but their amount can not
• outlet means 16 Supplying a gas into the pathway in a counter-current manner
• the silicon seed crystals may be prepared by
• prepared seed crystals 3a may be introduced into the inner zone 4 of the reactor in a
• silicon particles may be pulverized into seed crystals inside
• This method has an
• the inner zone 4 comprises all spaces required for
• the inner zone 4 plays a fundamental role for silicon deposition in
• the outer zone 5 is an independently formed
• silicon particle bed 3 is not formed and silicon deposition does not occur because the
• the outer zone 5 may be defined as
• granular polycrystalline silicon may be prepared by introducing an inert
• the outer zone 5 provides a space for protecting the reactor tube 2 by
• the outer zone 5 provides a space for installing an insulating material
• the outer zone 5 provides a space for a heater to be installed around the
• the outer zone 5 provides a space for maintaining a substantially
• the outer zone 5 allows a real-time monitoring of the status of the
• sample from the outer zone connecting means 28 may reveal the presence or
• the outer zone 5 provides a space for installing a heater 8b surrounding
• the outer zone 5 provides a space required for efficient assembly or
• the outer zone 5 plays many important
• the outer zone may be partitioned into several
• the divided sections are preferred to be spatially communicated with each
• blaneket a felt, a foamed product, or a packing filler material.
• fluidized bed reactor may be installed in the outer zone 5 only, or installed alone
• means 8a, 8b may be installed in both the inner zone 4 and the outer zone 5, if
• Figure 3 illustrates an example when a plurality
• independent heating means 8a, 8b are installed in the outer zone 5.
• the power supplying system comprising an electric source
• E and an electric energy supplying means 9a-9f may be constituted independently as
• bed 4a may have an advantage of directly heating silicon particles in the fluidized
• the heater 8a is preferably positioned lower than the reaction gas outlet of
• an inert gas connecting means 26a, 26b is installed on the reactor shell, independently of the inner zone 4, to maintain a substantially
• gas 12 may be one or more selected from hydrogen, nitrogen, argon and helium.
• reactor shell and spatially connected to the outer zone 5 has the function of piping
• connection for supplying or discharging an inert gas 12 may be selected from a
• means 28 may be used to measure and/ or control temperature, pressure or gas
• discharge of an inert gas may be independently performed by using a double-pipe
• inert gas connecting means 26a, 26b maintains an independent
• inert gas atmosphere in the outer zone 5 may also be used for measuring
• outer zone pressure i.e., pressure in the outer zone 5 is measured and/ or
• the outer zone connecting means 28 may be installed to measure and/ or
• the outer zone connecting means 28 has the
• piping connection may be selected from a tube, a nozzle, a flange, a
• the outer zone connecting means 28 may be used to supply or discharge an
• inert gas 12 as well as to measure or control temperature, pressure or gas component.
• pressure may be applied to the nature of the fluidization of solid particles.
• measuring and/ or controlling pressure in the inner zone 4 may be installed at such a
• Pressure controlling means i.e., the inner
• pressure controlling means 30 and the outer pressure controlling means 31 may be
• the the inner pressure controlling means 30 may be spatially connected to the
• reaction gas inlet means 14 a reaction gas inlet means 15, a particle outlet means 16, or a gas outlet
• the outer pressure controlling means 31 may be spatially connected to the outer
• zone 5 through an outer zone connecting means 28 or an inert gas connecting means
• outer pressure controlling means 31 comprise the components necessary for directly
• Either of the pressure controlling means, 30 and 31, comprises at least one
• a connecting pipe or fitting for spatial connection selected from the group consisting of: (a) a connecting pipe or fitting for spatial connection; (b) a manually-operated, semi-automatic, or automatic valve; (c) a
• the inner pressure controlling means 30 is interconnected with the outermost pressure controlling means 30
• pressure controlling means 31 in the form of a mechanical assembly or a signal
• either of the pressure controlling means may be partially or
• control system selected from the group consisting of a
• central control system a distributed control system and a local control system.
• controlling means 31 may be independently constituted in terms of pressure, either
• the pressure controlling means may be partially or completely integrated with a
• either of the controlling means, 30 or 31, may further comprise a
• a separation device such as a filter or a scrubber for separating particles, or a container
• the inner pressure controlling means 30 may be installed at or
• part of the inner zone 4c may be stably measured and/ or controlled although it is
• the inner zone connecting means may be
• the inner pressure controlling means 30 may also be installed at or connected
• a plurality of inner pressure controlling means 30 may be installed at
• the value of Pi is influenced by the characteristics of the fluidized
• controlling means 30 directly or indirectly measuring and/ or controlling an outer
• pressure in the outer zone 5 is preferred to be installed so that it may be spatially
• means 31 may be connected or installed includes, for example, an outer zone
• the outer zone 5 is required to be maintained in a
• the outer zone connecting means 28 may
• inert gas inlet means 26a or the inert gas outlet means 26b may be used as the inert gas connecting means 26 and the outer zone connecting means 28. Further,
• the inert gas inlet means 26a and the inert gas outlet means 26b may be installed
• connecting means 26, 28 as an integrated double tube-type structure. Therefore, it is
• the inner pressure controlling means 30 and/ot the
• 0 outer pressure controlling means 31 may be used to maintain the value of
• controlling means 30 that Pi may vary depending on the position selected for
• Pimin pressure value
• the height of the reactor becomes too high to be used. In contrast,
• the pressure difference in the fluidized bed is preferred to be
• the silicon particle bed but connected to an upper part of the inner zone 4c, the
• the inner pressure controlling means 30 may
• means 31 should comprise a pressure-difference
• controlling means that maintains the value of I Po - Pi I within 1 bar.
• the pressure-difference controlling means may be comprised in only one of
• controlling means with consideration that pressure value varies depending on the
• particle outlet means 16 or an inner zone connecting means, etc., which are spatially
• the pressure-difference controlling means may preferably be operated so
• pressure-difference controlling means enables the outer zone pressure (Po) and inner zone pressure (Pi) to satisfy the requirement of 0 bar ⁇ (Pi - Po) ⁇ 1 bar, with
• the inner pressure controlling means 30 being spatially connected to an inner part of
• Pi is measured at a position that is spatially connected to the
• pressure-difference controlling means enables the requirement of 0 bar ⁇ (Po - Pi) ⁇ 1
• controlling means 30, 31 independently, or in the two controlling means 30, 31 in
• the pressure-difference controlling means maintains the value of I Po - Pi
• reaction pressure i.e., Po or Pi.
• fluidizing gas inlet means 14 can hardly be insulated to achieve a gas preheating to
• reaction pressure exceeds about 15 bar, it is difficult to heat the reaction pressure
• the inner pressure controlling means 30 and/ or the outer pressure controlling means 31 may comprise a
• pressure-difference controlling means that can reduce the pressure difference
• the reaction pressure may be set to a high level by using the
• controlling means 30 for ultimate connection to the inner zone 4, both of the inner
• Pi* and Po* may be controlled at predetermined values of pressure, i.e. Pi* and Po*, respectively,
• the inner pressure controlling means 30 may comprise a
• pressure-difference controlling means that maintains Pi at a predetermined value
• the outer pressure controlling means 31 may also comprise a
• pressure-difference controlling means that maintains Po at such a predetermined
• the outer pressure controlling means 31 may comprise a
• the inner pressure controlling means 30 may also comprise a
• pressure-difference controlling means that maintains Pi at such a predetermined
• inner pressure controlling means 30 may comprise a pressure-difference controlling
• controlling means 31 may comprise a pressure-difference controlling means that
• Po* which are predetermined for maintaining the difference between Po and Po
• sealing may not be obtained at sealing means 41a, 41b for reactor tube 2. Further, its
• control parameters i.e., Pi* and Po*, for the pressure-difference controlling means.
• inner zone and the outer zone, respectively, may be predetermined based on the
• sealing means 41a, 41b may be deduced based on the component
• the influx of impurity elements from outer zone 5 into inner zone 4 may be
• impurity elements from inner zone 4 into outer zone 5 may be decreased or
• components between the two zones through the sealing means may be minimized or prevented by appropriate selection of the control parameters for the pressure
• the pressure-difference controlling means may maintain the value of ⁇ P
• the outer pressure controlling means 31 in a manual, semi-automatic or automatic
• pressure-difference controlling means may comprise an equalizing line, which
• ⁇ 5 spatially interconnects a connecting pipe comprised in the inner pressure controlling
• a connecting pipe which is comprised in the the inner pressure controlling
• means 30 and constitutes the equalizing line 23, may be installed at a position
• gas inlet means 15 a particle outlet means 16; a gas outlet means 17; or a seed
• outer pressure controlling means 31 and constitutes an equalizing line 23, may be
• outer zone 5 installed at a position selected for spatial connection with outer zone 5, including but
• the equalizing line 23 which interconnects spatially the inner pressure
• controlling means 30 and outer pressure controlling means 31, may be referred to as
• the impurity may undesirably be interchanged between two zones 4, 5.
• the impurity may undesirably be interchanged between two zones 4, 5.
• a pressure equalizing means which can decrease or prevent the possible interexchange of gas and impurity components between two zones 4, 5,
• the pressure equalizing means may be further added to the equalizing line 23.
• the pressure equalizing means may be further added to the equalizing line 23.
• a 3-way valve a filter for separating particles, a damping container, a packed bed, a
• the pressure-difference controlling means may comprise a manual
• valve for controlling pressure or flow rate, or may further comprise a(n)
• a pressure gauge may be installed in combination with a pressure gauge or a pressure indicator that
• the pressure gauge or the pressure indicator is available commercially in the
• processing means such as a signal converter or a signal processor, etc., and/ or with a
• Figure 1 schematically shows the characteristics of the method for preparing
• Figure 2 is a cross-sectional view of a high-pressure fluidized bed reactor for
• Figure 3 is a cross-sectional view of a high-pressure fluidized bed reactor for
• Reactor shell 2 Reactor tube
• Reaction gas inlet means 16 Particle outlet means 17: Gas outlet means 18: Silicon seed crystals inlet means
• zone pressure (Pi) and the outer zone pressure (Po) are independently controlled at
• an inner pressure controlling means 30 may be any suitable inner pressure controlling means 30.
• a first pressure control valve 30b with a gas outlet means 17 through an off-gas treating means 34 for removing fine silicon particles
• an inert gas connecting means 26a may be constituted by interconnecting an inert gas connecting means 26a, a fourth
• pressure control valve 31b' may be integrated with each other by a circuit, and thus
• the outer zone pressure may be controlled at a
• Po* may be preset at a lower value so that the condition of Pi* ⁇ Po* may be satisfied.
• controlling means 31 may further comprise their own pressure-difference controlling
• zone pressure (Pi) and the outer zone pressure (Po) are independently controlled at
• an inner pressure controlling means 30 may be any suitable inner pressure controlling means 30.
• pressure of the upper part of the inner zone 4 may be controlled at a predetermined
• an inert gas connecting means 26b may be constituted by interconnecting an inert gas connecting means 26b, an on/ off valve 3Ic 7 a third pressure gauge 31a and a third pressure control valve 31b.
• third pressure control valve 31b may be integrated with each other by a circuit
• Example I 7 the supply of an inert gas 12 may be controlled by the
• the outer zone pressure may be controlled at a

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• 2006
  • 2006-02-14 KR KR1020060013973A patent/KR100661284B1/ko not_active Expired - Fee Related
• 2007
  • 2007-02-14 ES ES07708931T patent/ES2429568T3/es active Active
  • 2007-02-14 EP EP07708931.6A patent/EP1986956B1/en not_active Not-in-force
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