WO2012002171A1 - シンチレータ材料、及びシンチレーション検出器 - Google Patents

シンチレータ材料、及びシンチレーション検出器 Download PDF

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Publication number
WO2012002171A1
WO2012002171A1 PCT/JP2011/063886 JP2011063886W WO2012002171A1 WO 2012002171 A1 WO2012002171 A1 WO 2012002171A1 JP 2011063886 W JP2011063886 W JP 2011063886W WO 2012002171 A1 WO2012002171 A1 WO 2012002171A1
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Prior art keywords
fluorescence
scintillator
scintillator material
zinc oxide
single crystal
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Ceased
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PCT/JP2011/063886
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English (en)
French (fr)
Japanese (ja)
Inventor
正孝 加納
若宮　章
航平 山ノ井
清水　俊彦
信彦 猿倉
エーレントラウト ディルク
承生 福田
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Daishinku Corp
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Daishinku Corp
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Priority to CN201180029633XA priority Critical patent/CN102959038A/zh
Priority to EP20110800636 priority patent/EP2589641B1/en
Priority to US13/703,713 priority patent/US8920677B2/en
Publication of WO2012002171A1 publication Critical patent/WO2012002171A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
    • G01T1/2023—Selection of materials
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/62—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing gallium, indium or thallium
    • C09K11/621—Chalcogenides
    • C09K11/623—Chalcogenides with zinc or cadmium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/55—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing beryllium, magnesium, alkali metals or alkaline earth metals
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/003—Scintillation (flow) cells
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
    • G01T1/16—Measuring radiation intensity
    • G01T1/20—Measuring radiation intensity with scintillation detectors
    • G01T1/202—Measuring radiation intensity with scintillation detectors the detector being a crystal
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K4/00—Conversion screens for the conversion of the spatial distribution of X-rays or particle radiation into visible images, e.g. fluoroscopic screens
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K4/00—Conversion screens for the conversion of the spatial distribution of X-rays or particle radiation into visible images, e.g. fluoroscopic screens
    • G21K2004/06—Conversion screens for the conversion of the spatial distribution of X-rays or particle radiation into visible images, e.g. fluoroscopic screens with a phosphor layer

Definitions

  • the present invention relates to a scintillator material that emits fluorescence when irradiated with radiation, and a scintillation detector including a scintillator made of the scintillator material.
  • the scintillation detector irradiates the scintillator with ionizing radiation such as X-rays, ⁇ -rays, and ⁇ -rays, whereby the fluorescence emitted by the scintillator is amplified and detected by a photomultiplier tube.
  • ionizing radiation such as X-rays, ⁇ -rays, and ⁇ -rays
  • a scintillation detector is a PET device (Positron Emission Tomography) that detects ⁇ -rays emitted when positrons disappear.
  • a scintillation detector having high sensitivity and high response speed is employed to detect ⁇ rays having relatively high energy by coincidence counting.
  • next-generation PET devices such as TOF (Time-Of-Flight) type has been attempted.
  • TOF Time-Of-Flight
  • Such a next-generation type PET apparatus requires a high time resolution, and therefore requires a scintillator with a particularly short fluorescence lifetime.
  • Patent Document 1 discloses a scintillator material made of zinc oxide single crystal doped with Al, Ga, In or the like.
  • the scintillator material disclosed in Patent Document 1 emits fluorescence having a fluorescence lifetime of about 600 ps upon incidence of radiation.
  • Patent Document 2 discloses a scintillator material made of a zinc oxide single crystal doped with Sb, Bi, In, or Ge as a donor impurity and Li as an acceptor impurity.
  • the fluorescence emitted by the radiation of the scintillator material disclosed in Patent Document 2 is composed of two components having a fluorescence lifetime of 30 to 60 ps and 250 to 800 ps.
  • the fluorescence lifetime of one component of 30 to 60 ps is extremely shorter than the fluorescence lifetime of 600 ps emitted by the scintillator material disclosed in Patent Document 1.
  • the scintillator material disclosed in Patent Document 2 is suitable as a scintillator material for a next-generation PET apparatus that requires a shorter fluorescence lifetime and higher time resolution than the scintillator material disclosed in Patent Document 1. .
  • the next generation PET apparatus requires high time resolution. Since the time resolution is improved as the fluorescence lifetime of the scintillator is shorter, further reduction in the fluorescence lifetime is desired in the scintillator material. Specifically, it is desired that the scintillator material has a fluorescence lifetime of less than 20 ps of fluorescence emitted from the scintillator material upon incidence of radiation.
  • the present invention has been made in view of such a situation, and an object thereof is to provide a scintillator material having a short fluorescence lifetime and a scintillation detector including a scintillator made of this scintillator material.
  • the scintillator material according to the present invention is a scintillator material that emits fluorescence upon incidence of radiation, and has grown on the + C plane or the ⁇ C plane of a plate-like zinc oxide seed crystal having a C plane as a principal plane.
  • the zinc oxide single crystal is composed of In and Li, and the fluorescence lifetime of the fluorescence is less than 20 ps.
  • the fluorescence lifetime is the time from when the fluorescence emission intensity reaches the maximum value until the emission intensity decays to 1 / exp of the maximum value.
  • DAP emission donor-acceptor pair emission
  • the DAP emission observed by the incidence of radiation has a component with a fluorescence lifetime of less than 20 ps.
  • the fluorescence lifetime of this component is the same as that of a conventional scintillator material made of zinc oxide single crystal. As compared with the fluorescence lifetime of 30 to 60 ps of one component of fluorescence emitted by For this reason, the scintillator material of the present invention has a shorter fluorescence lifetime than a conventional scintillator material that emits fluorescence composed of a plurality of components having a fluorescence lifetime of 30 ps or more.
  • the fluorescence emitted from the scintillator material upon incidence of radiation preferably comprises only one component having a fluorescence lifetime of less than 20 ps. In this case, the fluorescence lifetime of the fluorescence emitted by the scintillator material can be further shortened.
  • the Li concentration in the zinc oxide single crystal is preferably 0.15 to 11 times the In concentration, preferably 0.15 to 6.74 times. It is particularly preferred that A zinc oxide single crystal having a Li concentration of 0.15 to 11 times the In concentration can be manufactured in a high quality state with few crystal defects by a hydrothermal synthesis method or the like.
  • the scintillation detector according to the present invention is characterized by including a scintillator made of the above-described scintillator material according to the present invention.
  • the scintillation detector according to the present invention includes the scintillator made of the scintillator material according to the present invention, it has a high time resolution.
  • a scintillator material having a short fluorescence lifetime and a scintillation detector provided with a scintillator made of this scintillator material can be provided.
  • FIG. 1 is a cross-sectional view showing an internal configuration of a single crystal growth furnace used for manufacturing a scintillator material according to the present embodiment.
  • FIG. 2 is a diagram showing the fluorescence lifetime relative to the Li / In ratio of the scintillator material according to the present embodiment in comparison with the comparative example.
  • FIG. 3A is a diagram showing a change with time of the emission intensity of fluorescence emitted by the scintillator material according to Comparative Example 5 upon incidence of radiation.
  • FIG. 3B is a diagram showing a change with time of the emission intensity of the fluorescence emitted by the scintillator material according to Example 1 upon incidence of radiation.
  • the scintillator material according to the present embodiment is made of a zinc oxide single crystal containing In and Li. Then, the manufacturing method of the zinc oxide single crystal which comprises the scintillator material which concerns on this invention is demonstrated below.
  • the growth furnace 1 is configured such that an electric furnace 3 is disposed around the outer periphery of the furnace body 2.
  • the furnace body 2 is heated by the electric furnace 3.
  • the furnace body 2 has a bottomed cylindrical shape with an open top, and a lid 22 for sealing the inside of the furnace body 2 is attached to the upper end opening 21.
  • a pressure gauge 22 a for measuring the internal pressure of the furnace body 2 is attached to the lid body 22.
  • a cylindrical growth vessel 24 made of platinum is housed inside the furnace body 2.
  • the inner space 4 of the growing container 24 is sealed, and a convection control plate 23 is disposed at an intermediate position in the vertical direction of the inner space 4.
  • the internal space 4 of the growth vessel 24 is partitioned into a lower raw material chamber 41 and an upper growth chamber 42.
  • the raw material chamber 41 zinc oxide single crystal raw materials 5, 5,...
  • the growth chamber 42 a plurality of seed crystals 6, 6,... Supported by the single crystal growth shelf 61 are accommodated.
  • the inner space 4 of the growing container 24 is filled with a growing solution (alkali solution).
  • a mixture of zinc oxide powder having a diameter of 1 to 10 ⁇ m and indium oxide (In 2 O 3 ) powder having a diameter of 1 to 25 ⁇ m is formed on the single crystal raw material 5 by a pressure press machine, and 1000 to 1400 ° C.
  • a sintered body fired in an oxygen atmosphere or an air atmosphere was used.
  • the seed crystal 6 a plate-like zinc oxide single crystal having a C plane as a main surface cut parallel to the (0001) plane which is a hexagonal C plane was used.
  • a solution obtained by adding Li or a Li compound (for example, LiOH) to an aqueous solution of KOH was used.
  • the furnace body 2 is heated by the electric furnace 3.
  • the raw material chamber 41 is set to be higher in temperature than the growing chamber 42, and due to this temperature difference, the growing solution is naturally convected between the raw material chamber 41 and the growing chamber 42 under high temperature and pressure.
  • the growing solution in which the single crystal raw material 5 is dissolved moves from the raw material chamber 41 to the growing chamber 42. At this time, the growth solution in which the single crystal raw material 5 is dissolved is cooled in the growth chamber 42 and becomes supersaturated. Thereby, the single crystal raw material 5 is deposited and grown on the seed crystal 6. By performing this operation continuously for a predetermined period, a zinc oxide single crystal having a predetermined size can be obtained.
  • the zinc oxide single crystal thus obtained is cut, and a portion grown on the (0001) plane which is the + C plane or the (000-1) plane which is the ⁇ C plane of the seed crystal 6 is taken out.
  • a zinc oxide single crystal was used as a scintillator material.
  • a scintillator made of this scintillator material was provided in a scintillation detector.
  • the scintillator materials according to Comparative Examples 1 to 6 are composed of a zinc oxide single crystal grown on the M-plane of a seed crystal having the M-plane as a main plane. That is, as the seed crystal 6, a plate-like zinc oxide single crystal whose principal surface is the M-plane cut parallel to the (10-10) plane which is a hexagonal M-plane is used. A zinc oxide single crystal was obtained, the obtained zinc oxide single crystal was cut, a portion grown on the M plane was taken out, and this portion of the zinc oxide single crystal was used as a scintillator material according to Comparative Examples 1-6.
  • the zinc oxide single crystals constituting the scintillator materials according to Examples 1 to 6 are all good quality with fewer crystal defects than the zinc oxide single crystals constituting the scintillator materials according to Comparative Examples 1 to 6. there were.
  • the zinc oxide single crystals constituting the scintillator materials according to Examples 1 to 5 were of high quality with very few crystal defects.
  • Li / In (atomic ratio) shown in Table 1 is the ratio of Li concentration (atoms / cm 3 ) to In concentration (atoms / cm 3 ) in the zinc oxide single crystal.
  • the In concentration and the Li concentration in the zinc oxide single crystal were analyzed by secondary ion mass spectrometry using a secondary ion mass spectrometer (ims6F manufactured by CAMECA).
  • the fluorescence lifetime of the fluorescence emitted by the scintillator materials of Examples 1 to 6 and Comparative Examples 1 to 6 upon incidence of radiation was measured using a streak camera (HAMAMATSU C1587).
  • fluorescence consists of a several component, the fluorescence lifetime of each of those components and the ratio of each of these components are shown.
  • FIG. 2 shows the relationship between Li / In (atomic ratio) and fluorescence lifetime.
  • the square-shaped plot relates to the scintillator materials of Examples 1 to 6, and the round-shaped plot relates to the scintillator materials of Comparative Examples 1 to 6.
  • the relationship between the fluorescence lifetime of the component with the shortest fluorescence lifetime and Li / In (atomic ratio) is shown.
  • the scintillator materials of Examples 1 to 6 made of the zinc oxide single crystal grown on the + C plane or the ⁇ C plane of the seed crystal are composed of components having a fluorescence lifetime of less than 20 ps. It was recognized that the component emitting fluorescence and having a fluorescence lifetime of less than 20 ps is shorter than the fluorescence lifetime of any component of the fluorescence emitted by the scintillator materials of Comparative Examples 1 to 6 grown on the M-plane of the seed crystal.
  • the scintillator materials of Examples 1 to 6 having different Li / In (atomic ratio) in the range of 0.15 to 11 in the zinc oxide single crystal do not depend on the Li / In (atomic ratio). , Both were found to emit fluorescence of a component having a short fluorescence lifetime of 10.7 ps to 17.2 ps.
  • the fluorescence emission intensity composed of only one component is represented by the following formula 1.
  • the emission intensity when the maximum value is 1 is I
  • the fluorescence lifetime of component 1 is ⁇ 1
  • the elapsed time after the emission intensity reaches the maximum value is t.
  • the emission intensity when the fluorescence of the component 1 reaches the lifetime is 1 as the maximum value due to the presence of the fluorescence of the component 2. Greater than / exp. That is, since the fluorescence lifetime of the fluorescence composed of component 1 and component 2 is longer than the fluorescence lifetime of component 1, the fluorescence lifetime of the scintillator materials of Comparative Examples 1 to 5 that emit fluorescence composed of component 1 and component 2 is It is recognized that the fluorescence lifetime of 1 is longer than 62.7 ps to 122 ps.
  • the fluorescence emitted by the scintillator material of Example 1 upon incidence of radiation consists only of component 1 having a fluorescence lifetime ⁇ 1 of 17.2 ps.
  • the fluorescence lifetime of the fluorescence composed only of component 1 is the same as the fluorescence lifetime of component 1, the fluorescence lifetime of the scintillator materials of Examples 1 to 6 that emit fluorescence composed only of component 1 is the fluorescence lifetime of component 1. It is recognized that it is less than 20 ps, specifically 10.7 ps to 17.2 ps.
  • the fluorescence emitted from the scintillator materials of Examples 1 to 6 is faster than the fluorescence emitted from the scintillator materials of Comparative Examples 1 to 6. Is fast and has a short fluorescence lifetime.
  • the fluorescence lifetime of the fluorescence emitted by the scintillator materials of Examples 1 to 6 upon incidence of radiation is less than 20 ps, and the scintillator materials of Examples 1 to 6 are fluorescences composed of a plurality of components having a fluorescence lifetime of 30 ps or more.
  • the scintillator materials of Comparative Examples 1 to 6 that emit light it is recognized that the fluorescence lifetime is short. Therefore, by providing the scintillation detector with the scintillator made of the scintillator material according to the first to sixth embodiments, the time resolution of the scintillation detector can be improved.
  • the fluorescence lifetime of the zinc oxide single crystal constituting the scintillator material is the quenching lifetime in which electrons excited from the valence band to the conduction band return to the valence band without light emission. It seems to be related.
  • Fluorescence lifetime ⁇ all of a zinc oxide single crystal is expressed as follows, where ⁇ rad is the lifetime of light emitted when electrons excited to the conductor from the valence band return to the valence band, and ⁇ def is the lifetime of quenching: It is shown by the following formula 3.
  • Equation 4 when the quenching lifetime ⁇ def is extremely shorter than the emission lifetime ⁇ rad , it can be concluded that the fluorescence lifetime ⁇ all of the zinc oxide single crystal is almost equal to the quenching lifetime ⁇ def . That is, it can be said that the fluorescence lifetime ⁇ all of the zinc oxide single crystal is determined by the quenching lifetime ⁇ def .
  • the fluorescence lifetime of the scintillator materials according to Examples 1 to 6 is considered to be as short as 10.7 ps to 17.2 ps.
  • a sintered body made of a mixture of zinc oxide powder and indium oxide powder that is, a raw material containing Zn and In is used as the single crystal raw material 5.
  • the growth solution was prepared by adding Li to an aqueous solution of KOH, but in order to improve the crystallinity of the finally obtained zinc oxide single crystal, the single crystal raw material or the growth solution contains Al. , Fe, Ga, Ce, and Pr may be included. That is, the scintillator material of the present invention may contain at least one of Al, Fe, Ga, Ce, and Pr in the zinc oxide single crystal.
  • the present invention irradiates the scintillator with ionizing radiation such as X-rays, ⁇ -rays, and ⁇ -rays, thereby amplifying the fluorescence emitted by the scintillator with a photomultiplier tube or detecting the scintillation detector It is applicable to the scintillator material of such a scintillation detector.
  • ionizing radiation such as X-rays, ⁇ -rays, and ⁇ -rays

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  • Inorganic Chemistry (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)
  • Nuclear Medicine (AREA)
PCT/JP2011/063886 2010-07-01 2011-06-17 シンチレータ材料、及びシンチレーション検出器 Ceased WO2012002171A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201180029633XA CN102959038A (zh) 2010-07-01 2011-06-17 闪烁体材料及闪烁检测器
EP20110800636 EP2589641B1 (en) 2010-07-01 2011-06-17 Scintillator material and scintillation detector
US13/703,713 US8920677B2 (en) 2010-07-01 2011-06-17 Scintillator material and scintillation detector

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JP2010-151330 2010-07-01
JP2010151330A JP5609327B2 (ja) 2010-07-01 2010-07-01 シンチレータ材料、及びシンチレーション検出器

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US (1) US8920677B2 (enExample)
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WO (1) WO2012002171A1 (enExample)

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JP6032590B2 (ja) * 2012-04-04 2016-11-30 株式会社福田結晶技術研究所 酸化亜鉛単結晶の製造方法
JP5594380B2 (ja) * 2013-01-25 2014-09-24 株式会社大真空 シンチレータ、放射線検出器、放射線検査装置、α線検出器、及びシンチレータの製造方法
CN107209275B (zh) * 2014-07-23 2019-08-20 皇家飞利浦有限公司 用于表征闪烁体材料的表征装置
JP6623412B2 (ja) * 2015-04-23 2019-12-25 株式会社福田結晶技術研究所 酸化亜鉛結晶の製造方法、酸化亜鉛結晶、シンチレータ材料及びシンチレータ検出器
JP6676372B2 (ja) * 2015-12-28 2020-04-08 株式会社Ｓ−Ｎａｎｏｔｅｃｈ Ｃｏ−Ｃｒｅａｔｉｏｎ シンチレータ及び電子検出器
US10490397B1 (en) * 2018-07-18 2019-11-26 Thermo Finnigan Llc Methods and systems for detection of ion spatial distribution

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CN102959038A (zh) 2013-03-06
US8920677B2 (en) 2014-12-30
EP2589641A1 (en) 2013-05-08
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