US20120126171A1 - Crystal Growth Atmosphere For Oxyorthosilicate Materials Production - Google Patents
Crystal Growth Atmosphere For Oxyorthosilicate Materials Production Download PDFInfo
- Publication number
- US20120126171A1 US20120126171A1 US12/953,582 US95358210A US2012126171A1 US 20120126171 A1 US20120126171 A1 US 20120126171A1 US 95358210 A US95358210 A US 95358210A US 2012126171 A1 US2012126171 A1 US 2012126171A1
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- Prior art keywords
- crystal
- oxygen
- rare
- atmosphere
- melt
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Classifications
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- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
-
- 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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/77062—Silicates
-
- 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
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/77742—Silicates
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
-
- 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
- C30B29/34—Silicates
Definitions
- This application relates to the growth of crystals.
- a seed crystal is brought into contact with the surface of a melt and then withdrawn from the melt.
- a crystal grows on the seed as it is withdrawn.
- the seed and growing crystal are sometimes also rotated about a vertical axis as they are withdrawn.
- Growth instabilities often occur in large crystals grown using this technique.
- the crystal may begin to grow in a spiral shape instead of a desired cylindrical shape.
- Growth instabilities may result in stresses due to variations in thermal expansion coefficients within the crystal, which may cause the crystal to shatter. This shattering is more likely when significant temperature gradients are present in the melt and in the atmosphere above the melt in which the crystal grows.
- Growth instabilities may be caused by sufficiently large temperature gradients, accumulation of impurities in the melt, changes in the charge states of some of the melt constituents leading to creation of different molecular complexes, as well as by excesses of melt constituents accumulating at the interface between the surface of the melt and the growing crystal.
- oxygen vacancies in the crystal lattice may act as charge traps that lower the amount of charge carriers (electrons and holes) generated when the crystal absorbs ionizing radiation.
- the results are a lowering of scintillation efficiency and an undesirable persistent emission of light from the crystal known as afterglow. Reducing concentration of such oxygen vacancies is therefore desirable. This has been partially achieved by annealing the grown crystal in an oxygen-containing atmosphere. This is an extra step in the preparation of such crystals.
- a method of growing rare-earth oxyorthosilicate crystals and the crystals grown with the method includes providing an atmosphere for crystal growth including an inert gas and a gas including oxygen.
- FIG. 1 shows an example apparatus for growing a crystal.
- FIG. 2 is an example flow chart showing a method for growing a crystal.
- FIG. 3 shows an example crystal boule.
- FIG. 4 shows an example of a scintillation counter.
- FIG. 5 is an example flow chart showing another method for growing a crystal.
- Control of the atmosphere above a melt during crystal growth using a method such as the Czochralski method may be crucial for controlling growth stability and controlling properties of the grown crystal.
- careful control of the atmosphere and the melt composition may simultaneously minimize at least three problems in the growth of these crystals.
- a first problem is the inclusion of oxygen vacancies in the grown crystal, which reduce the scintillation efficiency of the crystal and give rise to an undesirable persistent emission of light from the crystal known as afterglow. These oxygen vacancies may arise from a deficiency of oxygen during crystal growth.
- Rare-earth oxyorthosilicate scintillator crystals may be grown from a melt prepared by melting a rare-earth compound, such as an oxide, with a silicon oxide, such as SiO 2 . Temperatures of 2000° C. or higher may be needed to melt these substances. At these temperatures it may be desirable to use a nearly inert atmosphere to prevent introducing impurities into the melt.
- the SiO 2 may decompose into SiO (silicon monoxide) and oxygen.
- SiO silicon monoxide
- oxygen oxygen
- gases that may decompose and liberate elemental oxygen include, as examples, sulfur trioxide (SO 8 ), several different oxides of nitrogen NO 2 , N 2 O, NO, N 2 O 3 , N 2 O 5 and phosphorous pentoxide P 2 O 6 . However, except for nitrous oxide N 2 O, these gasses are more reactive than CO 2 with materials making up the interior of the furnace.
- the amount of oxygen introduced into the atmosphere must be kept low enough to avoid appreciable oxidation of materials used in the growth apparatus, such as the iridium and iridium alloys of the crucible, often used to contain the melt for the growth of these crystals. Oxidation of an iridium crucible may introduce contaminants into the melt and shorten the usable lifetime of the expensive iridium crucible. Thus, the amount of oxygen introduced must be carefully chosen.
- a second problem with these crystals is cracking of the crystal during growth, which may result from excessive temperature gradients in growth chamber. This problem may be addressed by reducing the thermal conductivity of the growth atmosphere. Thermal conductivity contributes to the thermal diffusivity, which determines how rapidly any temperature change diffuses through an atmosphere. Lower thermal conductivity results in greater stability of temperature gradients in the growth chamber, isolating a crystal boule from any fluctuation in temperature in the surrounding environment.
- Group 2 elements include beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr) and barium (Ba).
- Group three elements include scandium and yttrium.
- Group 6 elements include chromium (Cr), molybdenum (Mo), and tungsten (W).
- Group 7 elements include manganese (Mn) and rhenium (Re).
- FIG. 1 shows an embodiment of a crystal-growing apparatus 100 including a melt 145 .
- Melt 145 may be made by melting a first substance that includes at least one first rare-earth element, and a second substance that includes at least one element 150 from group 2, group 3, group 6, or group 7. Alternatively, at least one rare-earth element and at least one element from group 2, group 3, group 6, or group 7, may both be included in one substance.
- the first substance may be an oxide of the first rare-earth element.
- Melt 145 may also include melted stoichiometric SiO 2 (silica).
- Melt 145 may also include a melted third substance that includes a second rare-earth element distinct from the first rare-earth element.
- Melt 145 may be contained in a crucible 135 , which may be made of iridium.
- Crucible 135 is contained in an enclosure 115 .
- Enclosure 115 may be utilized to control an ambient atmosphere 160 above the melt surface in which a rare-earth oxyorthosilicate crystal is growing as a crystal boule 130 .
- Surrounding enclosure 115 is a thermally insulating material 110 .
- Melt 145 is maintained in a molten state by inductive heating of crucible 135 , the heating produced by RF induction coil 140 .
- Crystal boule 130 grows at or near an interface 125 between a portion of the boule that is already grown and a surface of melt 145 .
- Rod 120 is slowly lifted upward as crystal growth proceeds.
- Rod 120 may also be rotated, as indicated by an arrow. Although the arrow indicates rotation of rod 120 in a clockwise direction as seen from above, rod 120 may also be rotated counterclockwise as seen from above.
- Melt 145 may include a melted third substance that includes a second rare-earth element.
- the second rare-earth element may be, but is not limited to, cerium (Ce).
- the second rare-earth element may be incorporated into crystal boule 130 .
- the second rare-earth element may be incorporated into crystal boule 130 as a dopant. It may be incorporated as a substitutional dopant in the lattice of crystal boule 130 .
- a dopant atom of Ce may occupy a lattice position normally occupied by an Lu atom in a crystalline lattice of lutetium oxyorthosilicate.
- Atmosphere 160 comprises at least one inert gas and at least one gaseous substance that includes oxygen. Atmosphere 160 is in contact with a surface of melt 145 . As explained above, it may be desirable to use an inert gas with a lower thermal conductivity.
- the inert gas may comprise at least one of helium (He), argon (Ar), krypton (Kr), xenon (Xe), or nitrogen. If maintaining thermal gradients is less crucial, nitrogen, having a higher thermal conductivity, may be used.
- Thermal conductivity of the inert gas may be less than or equal to 150 mW/m ⁇ ° K (milliwatts per meter ⁇ ° K) at the temperature of the atmosphere during crystal growth.
- the thermal conductivity of nitrogen at 2000° C. has been measured to be between about 70 and about 125 mW/m ⁇ ° K
- the thermal conductivity of argon at 2000° C. has been measured to be between about 80 and about 100 mW/m ⁇ ° K.
- the gaseous substance including oxygen may include carbon dioxide, which may disassociate to carbon monoxide and additional oxygen.
- the gaseous substance including oxygen may include other oxygen-containing compounds that disassociate to oxygen, such as carbon monoxide, oxygen, sulfur trioxide (SO 3 ), phosphorous pentoxide (P 2 O 5 ) or an oxide of nitrogen, all of these in any combination.
- the oxide of nitrogen may include NO 2 , N 2 O, NO, N 2 O 3 , or N 2 O 5 in any combination.
- Atmosphere 160 may comprise from 100 parts per million (ppm) to 100000 ppm (0.01 to 10 percent) of oxygen by volume, inclusive.
- atmosphere 160 may comprise oxygen by volume in a range between and including any two integer values of ppm between 100 and 100000.
- atmosphere 160 may contain less than 300 ppm oxygen by volume.
- atmosphere 160 may contain less than 200 ppm oxygen by volume.
- FIG. 2 shows a first embodiment of a method of growing a rare-earth oxyorthosilicate crystal in a controlled atmosphere.
- a powdered substance comprising at least one first rare-earth element may be mixed with a powdered silicon oxide such as silica (SiO 2 ) 210 .
- a powdered substance that includes at least one element from group 2, 3, 6, or 7 is added to make a powder mixture 210 .
- the powdered substance comprising at least one first rare-earth element may be a rare-earth oxide or a mixture of such oxides, such as Lu 2 O 3 , Gd 2 O 3 , or La 2 O 3 , or a mixture thereof.
- An oxide of an additional element such as Y 2 O 3 , may also be added 210 .
- the group 7 element may be, but is not limited to, manganese or rhenium.
- one or more substances including at least one element from group 2 of the periodic table may be introduced into the mixture at step 210 .
- the addition of group 2 elements may contribute stabilizing growth of the crystal.
- a second powdered substance comprising a second rare-earth element may be mixed with the powder mixture at step 210 .
- the second powdered substance may be a rare-earth oxide or any rare-earth compound including an oxygen moiety.
- a powdered substance including cerium such as a cerium oxide CeO 2 may be introduced into the powder mixture for the purpose of growing an oxyorthosilicate crystal doped with cerium as a scintillator crystal.
- an atmosphere, 160 in FIG. 1 comprising an inert gas and a gas including oxygen, as described above.
- step 220 the powder mixture is melted in crucible 135 to produce melt 145 , atmosphere 160 being in contact with a surface of the melt.
- step 230 a rare-earth oxyorthosilicate crystal is grown from melt 145 in the presence of atmosphere 160 .
- FIG. 5 shows a second embodiment of a method of growing a rare-earth oxyorthosilicate crystal in a controlled atmosphere.
- a powdered substance comprising a first rare-earth element may be mixed with a powdered silicon oxide such as silica (SiO 2 ) 510 .
- a second powdered substance comprising a second rare-earth element may be mixed with the powder mixture at step 510 .
- the second powdered substance may be a rare-earth oxide or any rare-earth compound including an oxygen moiety.
- a powdered substance including cerium such as a cerium oxide CeO 2 , or any other material that can be calcined to cerium oxide, may be introduced into the powder mixture for the purpose of growing an oxyorthosilicate crystal doped with cerium as a scintillator crystal.
- an atmosphere, 160 in FIG. 1 comprising an inert gas and a gas including oxygen, or a compound that disassociates to oxygen, such that the atmosphere includes less than 300 ppm oxygen.
- step 520 the powder mixture is melted in crucible 135 to produce melt 145 , atmosphere 160 being in contact with a surface of the melt.
- step 230 a rare-earth oxyorthosilicate crystal is grown from melt 145 in the presence of atmosphere 160 .
- FIGS. 2 and 5 include the use of powders for the silicon oxide, for a substance comprising at least one first rare-earth element, for a substance comprising at least one element from group 2, 3, 6, or 7, and, optionally, a substance comprising at least one second rare-earth element.
- Another embodiment includes use of different forms of matter for some or all of these example substances, including, but not limited to, liquids, sintered substances, granulated substances, pressed tablets, or solids that are not powdered.
- FIG. 3 shows an example of a crystal boule 300 grown according to a method described above. To evaluate the scintillation properties of crystals made by the methods illustrated in FIG. 2 or 3 , boules were cut into multiple samples (slabs) and each sample was evaluated separately. FIG. 3 shows a boule cut into twelve samples 310 . Sample 1 is taken from the bottom of the boule, that is, the last part of the boule to be grown. Sample 12 is taken from the top of the boule, that is, the first section to be grown.
- Oxyorthosilicate crystals may be grown over the following ranges of conditions: temperature from 1900° C. to 2200° C. inclusive, withdrawal rates from 0.001 mm/hr to 10 mm/hr inclusive, and rotation rates from 0 to 100 rotations per minute (RPM), inclusive. These ranges are exemplary and under the methods described herein any one or more of these conditions may be varied within or outside these ranges as known in the art. Oxyorthosilicate crystals may be grown over ranges of temperature, withdrawal rate, and rotation rate that are restricted to being between any two integer values, and including those integer values, within the above ranges.
- Exemplary cerium-doped lutetium oxyorthosilicate scintillator crystal boules were grown according to an embodiment of the method described above.
- the crystals were grown in an atmosphere including argon and CO 2 .
- the crystals were grown to about 80 mm in diameter and about 240 mm in length.
- Slabs 20 mm in thickness were cut from the crystals and numbered, starting from the bottom section of the crystal boule as shown in FIG. 3 .
- Light output measurements were done under excitation with Cs 137 gamma source (662 keV). The scintillation light was collected using a Hamamatsu R877 photomultiplier.
- Table 1 shows light output, energy resolution, and decay time of a scintillator crystal grown in an atmosphere as described above. Results are presented in Table 1 using arbitrary scales defined by numbers of channels of a Multichannel Analyzer (MCA) unit used in the measurements.
- MCA Multichannel Analyzer
- a bismuth germinate crystal (Bi 4 Ge 2 O 12 ; BGO) was used as a reference. (BGO photopeak was set to the channel 100 position).
- Results shown in Table 1 are characteristic of rare-earth oxyorthosilicate scintillator crystals of the highest optical quality and efficiency. As pointed out above, this has been achieved without any post growth anneal.
- FIG. 4 shows a scintillation counter 400 using as a detector a rare-earth oxyorthosilicate crystal 450 grown according to the method described above.
- Radiation 460 such as gamma photons, are absorbed by oxyorthosilicate crystal 450 , resulting in emission of scintillation light 440 from oxyorthosilicate crystal 450 .
- Scintillation light 440 is detected by light detector 430 , such as a photomultiplier tube, avalanche photodiode, or any other light sensor.
- An electrical signal produced by light detector 430 is conveyed by electrical connection 410 to analyzing electronics 420 .
- Information such as energy spectra and timing of radiation 460 may be extracted using analyzing electronics 420 .
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Measurement Of Radiation (AREA)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US12/953,582 US20120126171A1 (en) | 2010-11-24 | 2010-11-24 | Crystal Growth Atmosphere For Oxyorthosilicate Materials Production |
CN2011103780054A CN102477580A (zh) | 2010-11-24 | 2011-11-24 | 用于氧正硅酸盐材料制造的晶体生长气氛 |
US14/623,760 US10227709B2 (en) | 2010-11-24 | 2015-02-17 | Crystal growth atmosphere for oxyorthosilicate materials production |
US16/251,118 US10774440B2 (en) | 2010-11-24 | 2019-01-18 | Crystal growth atmosphere for oxyorthosilicate materials production |
Applications Claiming Priority (1)
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US12/953,582 US20120126171A1 (en) | 2010-11-24 | 2010-11-24 | Crystal Growth Atmosphere For Oxyorthosilicate Materials Production |
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US14/623,760 Division US10227709B2 (en) | 2010-11-24 | 2015-02-17 | Crystal growth atmosphere for oxyorthosilicate materials production |
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US12/953,582 Abandoned US20120126171A1 (en) | 2010-11-24 | 2010-11-24 | Crystal Growth Atmosphere For Oxyorthosilicate Materials Production |
US14/623,760 Active 2031-04-15 US10227709B2 (en) | 2010-11-24 | 2015-02-17 | Crystal growth atmosphere for oxyorthosilicate materials production |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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US20130337631A1 (en) * | 2012-06-15 | 2013-12-19 | Taiwan Semiconductor Manufacturing Company, Ltd. | Semiconductor Structure and Method |
US9328288B2 (en) | 2013-11-15 | 2016-05-03 | Siemens Medical Solutions Usa, Inc. | Rare-earth oxyorthosilicates with improved growth stability and scintillation characteristics |
US10890670B2 (en) | 2004-08-09 | 2021-01-12 | Saint-Gobain Cristaux Et Detecteurs | Dense high-speed scintillator material of low afterglow |
US10901099B2 (en) | 2015-02-26 | 2021-01-26 | Saint-Gobain Cristaux & Detecteurs | Scintillation crystal including a co-doped rare earth silicate, a radiation detection apparatus including the scintillation crystal, and a process of forming the same |
US10907096B2 (en) | 2010-11-16 | 2021-02-02 | Saint-Gobain Cristaux & Detecteurs | Scintillation compound including a rare earth element and a process of forming the same |
US11242485B2 (en) | 2019-08-21 | 2022-02-08 | Meishan Boya Advanced Materials Co., Ltd. | Methods and devices for growing scintillation crystals with short decay time |
US11319645B2 (en) | 2019-08-21 | 2022-05-03 | Meishan Boya Advanced Materials Co., Ltd. | Methods and devices for growing oxide crystals in oxygen atmosphere |
US11655557B2 (en) | 2020-06-05 | 2023-05-23 | Meishan Boya Advanced Materials Co., Ltd. | Methods and devices for growing crystals with high uniformity without annealing |
US11827826B2 (en) | 2019-08-21 | 2023-11-28 | Meishan Boya Advanced Materials Co., Ltd. | Methods and devices for growing scintillation crystals |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US10774440B2 (en) * | 2010-11-24 | 2020-09-15 | Siemens Medical Solutions Usa, Inc. | Crystal growth atmosphere for oxyorthosilicate materials production |
CN106011998B (zh) * | 2016-07-22 | 2018-11-09 | 苏州晶特晶体科技有限公司 | 一种提高掺铈闪烁晶体性能的装置及生产方法 |
CN111455465A (zh) * | 2019-01-18 | 2020-07-28 | 美国西门子医疗系统股份有限公司 | 用于生产氧正硅酸盐材料的晶体生长气氛 |
CN110093661A (zh) * | 2019-04-30 | 2019-08-06 | 清远先导材料有限公司 | 晶体的生长方法 |
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2010
- 2010-11-24 US US12/953,582 patent/US20120126171A1/en not_active Abandoned
-
2011
- 2011-11-24 CN CN2011103780054A patent/CN102477580A/zh active Pending
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2015
- 2015-02-17 US US14/623,760 patent/US10227709B2/en active Active
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