Classifications

• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/2403—Layers; Shape, structure or physical properties thereof
  • G11B7/24035—Recording layers
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
  • G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
  • G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
  • G11B7/2433—Metals or elements of Groups 13, 14, 15 or 16 of the Periodic Table, e.g. B, Si, Ge, As, Sb, Bi, Se or Te
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/26—Apparatus or processes specially adapted for the manufacture of record carriers
  • G11B7/268—Post-production operations, e.g. initialising phase-change recording layers, checking for defects
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
  • G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
  • G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
  • G11B2007/24302—Metals or metalloids
  • G11B2007/24304—Metals or metalloids group 2 or 12 elements (e.g. Be, Ca, Mg, Zn, Cd)
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
  • G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
  • G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
  • G11B2007/24302—Metals or metalloids
  • G11B2007/2431—Metals or metalloids group 13 elements (B, Al, Ga, In)
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
  • G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
  • G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
  • G11B2007/24302—Metals or metalloids
  • G11B2007/24314—Metals or metalloids group 15 elements (e.g. Sb, Bi)
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
  • G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
  • G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
  • G11B2007/24302—Metals or metalloids
  • G11B2007/24316—Metals or metalloids group 16 elements (i.e. chalcogenides, Se, Te)
• • G—PHYSICS
  • G11—INFORMATION STORAGE
  • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
  • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
  • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
  • G11B7/2403—Layers; Shape, structure or physical properties thereof
  • G11B7/24035—Recording layers
  • G11B7/24038—Multiple laminated recording layers
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/21—Circular sheet or circular blank

Definitions

• the present invention generally relates to a recordable information carrier (for example a CD-R medium), for example in the form of a compact disc, which is in erasable, of high recording security and legally safe.
• a recordable information carrier for example a CD-R medium
• CD-R medium for example in the form of a compact disc, which is in erasable, of high recording security and legally safe.
• a CD-R medium consists of a polycarbonate flat disk, covered on one of its main faces with a light-sensitive film.
• a light beam emitted for example by a 10 mW laser diode (called writing diode)
• writing diode a 10 mW laser diode
• local transformations of said film are produced. These transformations can induce a measurable change in the physical properties of the film, in particular its optical reflectivity. This modification is used in particular to both incorporate the information on the CD-R and then read it.
• spots are distributed along an elliptical spiral-shaped track that is drawn on the disc using a standard scanning system known from the state of the art.
• the CD-R must present, for its use, the following two essential characteristics:
• a transformation can be generated by various processes: melting, bleaching, evaporation, creating a roughness, ablation, crystallization of an amorphous film or modification of the film chemistry, for example during the synthesis of a compound;
• the morphological stability of the film in relation to ambient conditions such as temperature, visible light, humidity, magnetic field or mechanical alteration (with a tool or during handling), stability which relates to both at the spots and at the surface of the film that is not treated by the laser.
• the light emitted by a diode which is a so-called “reading” diode) or an LED (acronym for a light-emitting device) is scanned on the elliptical track and the light reflected by the film is detected and recorded.
• the beam emitted by the reading diode is continuous and monochromatic. It operates at a wavelength at R between 500 and 750 nm, ie at a photon energy of between 2.4 eV and 1.65 eV.
• the beam intensity of the read diode is much lower than that of the write diode, typically of the order of 1 mW.
• Any local morphological transformation of the film must produce a local change in the reflectivity of the film which is then measured and detected with the readout diode. If this modification is evaluable, the recording of the light reflected by the film allows the reading of the information after decoding of the digital inscription.
• Rv denotes the value of the reflectivity (measured at r ) of the virgin film
• Rs denotes the value of the reflectivity (measured at A r ) of the spots.
• the amplitude of this contrast C is important to evaluate the ability of the CD-R to record the information.
• any material that easily transforms by absorbing a small amount of light energy may be sensitive to small fluctuations in ambient conditions (eg temperature).
• CD-Rs have a highly light-sensitive film that consists of a mixture of organic products (chemicals, polymers).
• the recording of information on such films is easily achieved by locally transforming the film, for example by changing its color (and reflectivity) or by ablating the film following absorption of light and heat generation. resulting.
• the optical contrast C thus obtained is typically of the order of 0.30 and the contemporary CD-Rs burning apparatus are set to read such a contrast.
• Another consequence is that it makes it necessary to re-record the same information at short intervals without ensuring its security.
• the present invention therefore aims to solve these problems and disadvantages, by providing means to ensure a secure and permanent recording of the information on a CD-R.
• the present invention relates to a recordable information medium comprising:
• a light-sensitive film covering one of said main faces and on which information can be recorded.
• the film is a multilayer film comprising at least two superimposed elementary layers respectively composed of a -A element and a B element, said layers are distributed as follows:
• each layer being substantially the same and the total thickness of the light-sensitive film being at least 35 nm, and preferably at least 40 nm.
• the compound AB for example AlTe
• the synthesis of which can advantageously be caused by the irradiation of a laser beam (referred to as a "laser synthesis writing method"), which is a process used in the context of of the present invention leading to a better contrast of the writing on the sensitive film, and
• Compound AB is covalent.
• the so-called covalent compounds associate with strong interatomic bonds elements belonging respectively to the following columns of the Periodic Table of the Elements:
• the choice of the AB compound is on the one that offers the highest optical contrast vis-à-vis the virgin film at the time of reading the information engraved on the film.
• the choice is made on the AlTe compound, when the upper elemental layer contains Al.
• the film is usually semi-transparent even before any laser irradiation regardless of the choice of the elements present in the film, which reduces the reading contrast. after synthesis of any compound.
• the greater the thickness of the film the greater the intensity of the laser beam used to synthesize the compound in this film, the latter being substantially proportional to the volume of material contained in the film, it is ie to its thickness.
• a compromise must therefore be defined that optimizes the choice of the thickness of the film vis-à-vis the intensity of the writing laser beams commonly used to burn a CD-R, while preserving the optical contrast defined by the choice elements A and B.
• the thickness of a film as manufactured is defined with a precision which is of the order of 2 to 5 nm. This precision affects each elemental layer containing one of the elements and participating in the total thickness of the sensitive film.
• the lower the thickness of an elementary layer the greater the uncertainty of obtaining a ratio of the thicknesses of the elementary layers at A and B in exact proportion corresponding to the stoichiometric composition of the chosen compound.
• the optimum film thickness is 40 nm, this film consisting of two superimposed layers of identical thickness 20 nm, and each containing a single element: Te in the lower layer (directly deposited on the support) and Al in the upper layer.
• the sensitive film of the support according to the invention has a thickness of the order of 35 nm, and that it consists of two superposed layers of identical thicknesses of 18 nm each and each containing a single element (ie Te, ie Al).
• the sensitive layer is composed of two superimposed elementary layers (in Te or Al) of identical thicknesses of up to 25 nm (for a total thickness of the sensitive film of 50nm) or 30nm (for a total thickness of this film of 60nm).
• the elementary layer which is in direct contact with the support is always made of Te and the upper layer which is superimposed on it is always constituted of Al.
• the multilayer film consists of the superposition of two elementary layers each having a thickness of between 18 and 30 nm, and preferably of the order of 20 nm.
• the film is opaque to ambient light.
• it is preferably a multilayer film consisting of two layers, distributed as follows from the polycarbonate flat disk:
• the multilayer film consists of four elementary layers each having a thickness of the order of 10 nm.
• it is a film consisting of four layers distributed as follows from the polycarbonate flat disk:
• the outer layer of the multilayer film is advantageously an aluminum layer, which provides a high reflectivity to the visible light emitted by a standard reading diode.
• a very thin layer of oxide (approximately 2 nm thick) develops on its surface. Being dense, this oxide layer protects the film from moderate mechanical damage and occasional environmental contamination.
• Aluminum-containing compounds may be used on a CD-R disc, for example with the following pairs of elements: Al / Sb, Al / Se, and Al / As.
• Another subject of the present invention is a process for securely and sustainably recording information on a light-sensitive film, characterized in that it comprises:
• the process according to the invention uses for laser synthesis step (b) the process described in patents EP0045551 and EP0048514 of the present applicant.
• This process is unique in that it originates in the instantaneous absorption of optical energy during the interaction of photons with valence electrons in the film irradiated by the laser beam. Although phonons are created during this interaction and heat is generated, the process is not driven by thermodynamic equilibrium considerations. It is indeed an out-of-equilibrium process that is not based on the classical laws of atomic scattering.
• No conventional thermal heat source can simulate the sudden rise in the intensity of any laser source ( ⁇ 10 ⁇ 4 s), such as that produced by the absorption of light emitted by a laser diode (10 ⁇ 6 s).
• the light-sensitive film which is deposited on the polycarbonate substrate consists of a stack of two elementary layers containing atoms A and B respectively.
• the atomic contents of these elementary layers and their respective thicknesses are such that the proportion between the atoms A and B corresponds to the stoichiometric composition of a given compound which would be formed with such A and B atoms, for example the 2/3 proportion for A2B3.
• one or both layers By irradiating the stack of the two layers with a laser beam, one or both layers can be melted very rapidly during the irradiation, thus promoting a very rapid, so-called ballistic migration of the atoms through the interface two layers.
• the atoms originally belonging to one or both layers are mixed before any interatomic reaction (eg to form covalent bonds) can be established.
• any interatomic reaction eg to form covalent bonds
• this inter-atomic migration can result in either a homogeneous metal alloy or a compound thus synthesized.
• the synthesis of a compound induced by laser irradiation offers specific advantages. Indeed, the so-called composite materials are characterized by strong interatomic bonds (covalent or ionic).
• this type of bond results in an optical absorption threshold at a particular photon energy which is characteristic of the compound.
• This energy defines E G the absorption threshold of the compound. This is the minimum energy required to allow this compound to absorb photons.
• these compounds may be either semitransparent or possibly opaque to the monochromatic light emitted by the readout diode.
• the laser-induced synthesis of a specific compound A n B m can lead to a very high contrast C between the high reflectivity of a metal, that is to say that of the virgin Al aluminum film before laser irradiation, and the reflectivity of laser irradiated spots which consist of the synthesized composite material.
• Achieving the highest contrast C has particular advantages: i) the size of the transformed spots distributed along the elliptical track can be reduced, and ii) the detection of a spot can be faster. In other words, on a standard CD-R disc with a diameter of 12.5 cm, the volume of recorded information can be larger and can be read faster.
• the morphological stability and the integrity of the sensitive film described above must be established both before and after the integration of the information on the disc. This stability can be disturbed in two ways: i) by migration of foreign species (eg water) along the interface between the film and the surface of the polycarbonate support, and
• the laser irradiation synthesis method of a specific compound A n B m can be used to seal the virgin film securely to the ambient and for example to prevent the migration of water at the interface between film and support.
• the synthesis of a compound is an exothermic process. Once the fusion is initiated by the absorption of the laser light, the synthesis of the compound is developed by itself through the entire volume of the sensitive film now consisting of a homogeneous mixture of A and B atoms, this synthesis simultaneously generating heat that diffuses out of the film. By softening the surface of the polycarbonate, this heat helps to very strongly adhere the synthesized compound on the support, to the point that the film thus transformed can not be removed by peeling the support.
• the complete sealing of the virgin film of a support according to the invention comprising an orifice at its center adapted to the mounting of said support in a reader, is achieved by scanning the beam of a writing laser diode along two test leads.
• cords being disposed at a distance of between 1 mm and 2 mm from said borders. Sealing is installed before any disk use ⁇
• thermodynamic type Any atomic diffusion of thermodynamic type is necessarily slow. This is the case of atomic diffusion at low temperature (for example at room temperature) through the interface between the two layers of the sensitive film. During such slow diffusion, covalent bonds have time to form, causing the formation of a very thin layer (barrier) of compound which blocks any further slow migration of atoms. As a result, surfaces not treated by the writing laser remain blank, a situation that can only be drastically changed by laser irradiation and the rapid migration of atoms that results.
• the compound thus synthesized is homogeneous and very stable. It can no longer decompose and return to the original form of the metal stack of the two individual layers. In other words, the writing of information in the form of the coded sequence of tasks is an irreversible process.
• the integrity of the film is ensured both before and after writing the information on the CD-R.
• access to the incorporation of information on any blank CD-R is maintained over very long periods of time.
• the atomic elements A and B of the specific compound A n B m are distributed on the Periodic Table of the Elements, on either side of the 4th Column:
• aluminum tellurides Al 2 Te 3 and AlTe
• the two aluminum tellurides have an optical absorption threshold in the infrared of 1.0 eV: these compounds totally absorb visible light and are black;
• the outer layer of the sensitive film is made of aluminum, metal with high reflectivity in the visible, the information recorded on the film has a very high contrast C:
• Aluminum a standard constituent that is widely used in the CD media industry.
• another subject of the present invention is a method for protecting, indefinitely, the physical integrity of the sensitive film of the recordable information medium according to the invention, said support possibly being circular and comprising an orifice in its center adapted to the mounting of said support in a reader,
• said method being characterized in that it comprises a step of sealing the useful part of the film on its support, by etching two continuous beads of a compound synthesized by laser irradiation and of a width preferably greater than or equal to 1 ⁇ m, this sealing step being performed before any use, the film being thus still virgin, said cords defining the useful part of the film and distributed as follows: a first bead on the outer edge of the useful part of the film, and
• said cords being disposed at a distance of between 1 mm and 2 mm from said borders.
• the support of the sensitive film may have any geometry, for example circular, square or rectangular, this geometry being distributed on a flat or curved surface, the useful part of the film being delimited and protected by one or more cords etched at the periphery of the film. useful part of the film.
• This method of infinite protection of the physical integrity of the sensitive film makes it possible to manufacture and market any CD-R type information medium on which information can be etched in a completely secure and legally secure way, with a longer lifetime (but not limited) at age 25, as shown in the examples below.
• a layer of Antimony (Sb) is deposited on a glass plate, then covered with a layer of Aluminum (Al), itself covered with a layer of Sb and finally with a new layer of Al .
• All these layers each have the same thickness (20 nm) and form a light-sensitive film.
• the stack of these layers forming the film is irradiated by a CW continuous laser beam Argon working at a wavelength of 500 nm, power 20 mW, for 10 seconds on a surface of 0.5 mm in diameter.
• a layer of Sb is deposited on a glass plate, then covered with a layer of Al, the two layers each having a thickness of 20 nm, the assembly forming a light-sensitive film.
• the reflectivity of the film is strong in the visible and corresponds to that of the outer layer in Al.
• This layer is then covered with a layer of tellurium, also with a thickness of 40 nm.
• Irradiation of all two layers forming the light-sensitive film causes the synthesis of the CdTe compound which absorbs light below 620 nm.
• the optical contrast C between the non-irradiated zones of the film and those which have been irradiated is 0.33, demonstrating the importance of the choice of elements chosen to form the sensitive layer. Preserved for 25 years, the layer maintains an unchanged contrast at 0.33.
• EXAMPLE 4 A layer of tellurium (Te) is deposited on a polycarbonate substrate, then this layer of Te is itself covered with a layer of Al.
• the two layers have the same thickness of 20 nm and their stack forms a film sensitive to light.
• the laser irradiation of the film thus formed is carried out for 10 ⁇ 6 s, with a laser diode emitting in the near infrared (690 nm) with a power of 10 m.
• the irradiated zone After irradiation, the irradiated zone is totally black, with an optical contrast C equal to 0.80.
• a layer of tellurium (Te) with a thickness of 20 nm is deposited on a polycarbonate substrate, then this layer of Te is covered successively with a layer of Al with a thickness of 15 nm, then with a Te layer of 20 nm. nm thick and finally with a layer of Al thickness 15 nm forming the upper layer of one stack.
• Te tellurium
• the stack of these layers forms the light-sensitive film, which is then irradiated by the same laser beam as that used in Example 4.
• the irradiated area is then gray, with an optical contrast C equal to 0.54. less than the contrast obtained in Example 4 in which the Al and Te layers have the same thickness.
• Example 4 A film formed of two layers as in Example 4 is maintained at room temperature (24 ° C) for 8 years. Its contrast C is then reevaluated and is measured at 0.80.
• EXAMPLE 7 A film formed of two layers as in Example 4 is maintained at room temperature (24 ° C) for 8 years. Its contrast C is then reevaluated and is measured at 0.80.
• a film identical to that produced for Example 4 is brought to 50 ° C. for 48 hours and its contrast C is then reevaluated at 0.80, without any change since its irradiation.
• the interface between film and polycarbonate substrate may not be impervious to water migration over time.
• aging of the film is usually observed which is characterized by a detachment of the film which modifies and attenuates the writing contrast.
• an isolated area of the film is delimited by the ring, which area is completely separated from the rest of the film that is outside the ring.
• the ring is discontinuous and the zone of the film located inside the ring remains in contact with the part of the film located mainly out of the ring.
• the zone of the film which is contained in the discontinuous ring has the same appearance as the zone of the film located outside the ring, these two zones having a very weak contrast with respect to the ring itself .
• a series of spots of transformed material (compound CdTe) is then produced at regular intervals of 0.1 mm by moving the film perpendicular to the axis of the laser beam. , the irradiation being performed by a laser diode working for a very short period of time (10 ⁇ 6 s). Each spot is limited to a 0.1 mm diameter circular area by focusing the beam - ⁇ laser. This high-contrast writing (0.33) was then periodically monitored over a 25-year period to evaluate the durability of its contrast.

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• Chemical & Material Sciences (AREA)
• Inorganic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Manufacturing & Machinery (AREA)
• Optical Record Carriers And Manufacture Thereof (AREA)
• Thermal Transfer Or Thermal Recording In General (AREA)
• Optical Recording Or Reproduction (AREA)
• Manufacturing Optical Record Carriers (AREA)

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• 2010
  • 2010-09-29 FR FR1003848A patent/FR2965392B1/fr not_active Expired - Fee Related
• 2011
  • 2011-09-28 EP EP11771211.7A patent/EP2622602B1/fr not_active Not-in-force
  • 2011-09-28 US US13/876,261 patent/US8932696B2/en not_active Expired - Fee Related
  • 2011-09-28 CN CN201180047523.6A patent/CN103229239B/zh not_active Expired - Fee Related
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  • 2011-09-28 WO PCT/FR2011/000529 patent/WO2012042129A1/fr not_active Ceased

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