EP3114034A1 - Verfahren zur herstellung von polykristallinem silicium - Google Patents
Verfahren zur herstellung von polykristallinem siliciumInfo
- Publication number
- EP3114034A1 EP3114034A1 EP15706827.1A EP15706827A EP3114034A1 EP 3114034 A1 EP3114034 A1 EP 3114034A1 EP 15706827 A EP15706827 A EP 15706827A EP 3114034 A1 EP3114034 A1 EP 3114034A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- polycrystalline silicon
- fragments
- plastic
- ppbw
- less
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000004033 plastic Substances 0.000 claims abstract description 28
- 229920003023 plastic Polymers 0.000 claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004806 packaging method and process Methods 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- -1 polypropylene Polymers 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 239000006223 plastic coating Substances 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052785 arsenic Inorganic materials 0.000 claims description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000005033 polyvinylidene chloride Substances 0.000 claims description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 239000012634 fragment Substances 0.000 abstract description 28
- 239000000463 material Substances 0.000 abstract description 5
- 229920005591 polysilicon Polymers 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000032258 transport Effects 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229920000426 Microplastic Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical group Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007765 extrusion coating Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000010893 paper waste Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B1/00—Packaging fluent solid material, e.g. powders, granular or loose fibrous material, loose masses of small articles, in individual containers or receptacles, e.g. bags, sacks, boxes, cartons, cans, or jars
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B63/00—Auxiliary devices, not otherwise provided for, for operating on articles or materials to be packaged
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D5/00—Rigid or semi-rigid containers of polygonal cross-section, e.g. boxes, cartons or trays, formed by folding or erecting one or more blanks made of paper
- B65D5/42—Details of containers or of foldable or erectable container blanks
- B65D5/56—Linings or internal coatings, e.g. pre-formed trays provided with a blow- or thermoformed layer
- B65D5/563—Laminated linings; Coatings
-
- 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
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B1/00—Packaging fluent solid material, e.g. powders, granular or loose fibrous material, loose masses of small articles, in individual containers or receptacles, e.g. bags, sacks, boxes, cartons, cans, or jars
- B65B1/04—Methods of, or means for, filling the material into the containers or receptacles
Definitions
- the invention relates to a process for the production of polycrystalline silicon.
- Polycrystalline silicon (polysilicon) is predominantly deposited by the Siemens method from halosilanes such as trichlorosilane on thin rods, whereby polycrystalline silicon rods are obtained, which are then crushed into polycrystalline silicon fragments. After breaking up into fragments, it is customary to classify them into specific size classes. After sorting and classifying the fragments are dosed to a specific weight and packed in a plastic bag.
- a corresponding method for sorting, classifying, dosing and packaging of fragments is known from US 2013309524 A1. For applications in the semiconductor and solar industries, the least possible contaminated polysilicon fraction is desired. Therefore, it is desirable that the fragmentation into fragments, the sorting and classifying, the dosing as well as the packaging take place with as little contamination as possible.
- the fragments have to be transported between the individual processing steps from one plant to another, e.g. from the crushing plant to the packaging machine. It is customary, the fragments in so-called. Buffer tank, usually plastic crates to temporarily store. The last processing step is always the packaging in plastic bag, but due to the fact that polysilicon is a sharp-edged, non-free-flowing bulk material, which pierces the plastic bag during filling or in the worst case can even completely destroy, is problematic.
- DE 10 2007 027 1 10 A1 discloses a process for packaging polycrystalline silicon, in which polycrystalline silicon is filled by means of a filling device into a freely hanging, completely formed, bag, the filled bag subsequently being sealed, characterized in that the bag consists of high-purity plastic with a wall thickness of 10 to 1000 ⁇ m, the filling device comprising a freely suspended energy absorber made of a nonmetallic low-contamination material which is introduced into the plastic bag before the polycrystalline silicon is introduced and via which the polycrystalline silicon is deposited. is filled into the plastic bag, and the suspended energy absorber is then removed from the polycrystalline silicon filled plastic bag and the plastic bag is closed.
- rod-shaped round bodies weighing more than 2 kg and one size from 90 to 170 mm, wherein in each case at least one film in a cuboid, the dimensions of the packaged polycrystalline silicon fitted cardboard plugged, the polycrystalline silicon is introduced into the at least one film, wherein the at least one film is then welded and the polycrystalline silicon wraps.
- the polycrystalline silicon which is in the form of a fragment or a rod-shaped round and has a weight greater than 2 kg and a size of 90 to 170 mm, is surrounded by at least one 10 to 200 pm thick film which wraps around the polycrystalline silicon, wherein said at least one film is surrounded by another film having a reinforcing structure. After welding the films, the polycrystalline silicon is introduced into a transport container comprising separating elements or cardboard.
- Transports can be avoided more effectively. Basically, it is therefore intended to transport the fragments in plastic crates and to pack them as a final step in plastic bags or films.
- the object is achieved by a method for the production of polycrystalline silicon comprising providing polycrystalline silicon rods, comminuting the polycrystalline silicon rods into polycrystalline silicon fragments and packaging the polycrystalline silicon fragments by introducing the polycrystalline silicon
- the polycrystalline silicon is preferably deposited on heated silicon thin rods, using as the reaction gas a silicon-containing component and hydrogen (Siemens process).
- the silicon-containing component is a chlorosilane, more preferably trichlorosilane.
- the deposition is done according to the prior art, e.g. Reference is made to WO 2009/047107 A2.
- the comminution is carried out by means of a crusher, e.g. with a jaw crusher.
- a crusher e.g. with a jaw crusher.
- Such a crusher is described for example in EP 338 682 A2.
- the broken silicon if necessary by means of a mechanical sieve in the o.g. Fraction sizes classified. Previously, it is preferably packaged in a cardboard box and transported from the crushing plant to a plant through which it is sorted and classified.
- the fragments are cleaned before final packaging.
- the classified silicon is packed in a cardboard container and transported to the cleaning plant.
- the same cardboard container is used, in which the fragments were packed after crushing.
- a cleaning solution containing HNO 3 and HF is preferably used.
- the polysilicon fragments are washed in a pre-cleaning in at least one stage with an oxidizing cleaning solution, washed in a main cleaning in a further stage with a cleaning solution, the HNO 3 and HF, and in a hydrophilization in yet another step with an oxidizing cleaning liquid.
- the pre-cleaning is preferably carried out by means of HF / HCl / H 2 0 2 .
- the hydrophilization of the silicon surface is preferably carried out by means of HCl / H 2 0 2 .
- the polysilicon fragments are packed in a cardboard container.
- a cardboard container containing a bottom, a wall and an opening, wherein at least the inner surfaces of the bottom and wall, which come into contact with the polycrystalline silicon fragments, are coated with plastic.
- the same cardboard box is used in the packaging after cleaning, in which the fragments were packed after crushing.
- Cardboard is a material produced from pulp, groundwood and waste paper, whose use in the packaging industry is usual for the protection of packaged goods. Essentially, this is paper with a larger thickness. Cardboard is usually multi-ply, so it consists of several layers of paper of different thickness, which are pressed together without the use of adhesive.
- the cardboard container is closed after filling with the polycrystalline silicon fragments.
- a cover which also consists of cardboard (cardboard cover).
- the inner, the polycrystalline silicon fragments facing surfaces of the cover are also coated with plastic.
- the plastic coating preferably has a thickness of 50 m to 500 ⁇ on.
- the plastic used preferably contains less than 100 ppbw of boron, less than 100 ppbw of phosphorus, and less than 10 ppbw of arsenic.
- the plastic is preferably selected from the group consisting of polypropylene (PP), polyethylene (PE), polyurethane (PU), polyvinylidene fluoride (PVDF), polyvinylidene chloride (PVDC) and polysiloxane (silicone).
- PP polypropylene
- PE polyethylene
- PU polyurethane
- PVDF polyvinylidene fluoride
- PVDC polyvinylidene chloride
- siloxane silicone
- the cardboard container can be laminated with plastic, laminated, sprayed or steamed.
- the coating can be carried out, for example, with aqueous polymer dispersions or by extrusion.
- plastic granules are used, which are converted into a liquid thermoplastic melt.
- the liquid melt is applied to the carrier web.
- the polycrystalline silicon fragments are each packaged after crushing, after an optional step of sorting and classification and after an optional cleaning step in a previously mentioned plastic-coated cardboard container and transported to the next processing step.
- the polycrystalline silicon fragments are packed after the last processing step in a previously mentioned cardboard container with plastic coating and transported to the customer.
- the cardboard container is particularly preferably used both for transporting the fragments between installations in the manufacturing process and as a final packaging container, which is transported to the customer.
- a net weight of 5 kg to 1200 kg is preferred.
- a net weight of 5 kg to 500 kg is particularly preferred, most preferably a net weight of 10 kg to 40 kg.
- the cardboard boxes can be automatically welded or closed after filling.
- the cardboard containers Preferably, the cardboard containers have a rectangular shape. This makes it easy to automate the further processing.
- the use of commercially available palletizing systems is possible and preferred.
- the cardboard containers are preferably fastened on a pallet, particularly preferably lashed.
- the fragments can be dosed directly into the container.
- Standard packaging machines or robots with gripping arms can be used. There is relatively little fines content when filling the container.
- gloves made of high-purity polyethylene or PU are preferred.
- the material that makes up the gloves should contain less than 100 ppbw of boron, less than 100 ppbw of phosphorus, and less than 10 ppbw of arsenic.
- it has usually been necessary to preform the bags e.g. by means of a forming tube or by pulling the bag over a shoulder. This is omitted in the method according to the invention, since a cardboard container is used. The known from the prior art problem of punctures does not occur.
- the carton container preferably includes controls that are attached to the outer wall of the container to allow gripping and holding the carton container.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Packages (AREA)
- Cartons (AREA)
- Packaging Frangible Articles (AREA)
- Buffer Packaging (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102014203814.6A DE102014203814A1 (de) | 2014-03-03 | 2014-03-03 | Verfahren zur Herstellung von polykristallinem Silicium |
| PCT/EP2015/054156 WO2015132155A1 (de) | 2014-03-03 | 2015-02-27 | Verfahren zur herstellung von polykristallinem silicium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP3114034A1 true EP3114034A1 (de) | 2017-01-11 |
Family
ID=52595345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP15706827.1A Withdrawn EP3114034A1 (de) | 2014-03-03 | 2015-02-27 | Verfahren zur herstellung von polykristallinem silicium |
Country Status (10)
| Country | Link |
|---|---|
| US (1) | US10202282B2 (de) |
| EP (1) | EP3114034A1 (de) |
| JP (1) | JP6321199B2 (de) |
| KR (1) | KR101875300B1 (de) |
| CN (1) | CN106061845B (de) |
| CA (1) | CA2939825C (de) |
| DE (1) | DE102014203814A1 (de) |
| MY (1) | MY181249A (de) |
| TW (1) | TWI557071B (de) |
| WO (1) | WO2015132155A1 (de) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106391258A (zh) * | 2016-11-16 | 2017-02-15 | 亚洲硅业(青海)有限公司 | 多晶硅棒破碎方法及多晶硅棒破碎装置 |
| WO2021037366A1 (de) * | 2019-08-29 | 2021-03-04 | Wacker Chemie Ag | Verfahren zur herstellung von siliciumbruchstücken |
| DE112022002334T5 (de) | 2021-04-28 | 2024-02-08 | Tokuyama Corporation | Schablonen-Vorrichtung und Verfahren zur Herstellung eines Gehäusekörpers für polykristallines Silizium |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01242762A (ja) | 1988-03-23 | 1989-09-27 | O C C:Kk | 強靭な構造用金属材料の製造法 |
| JPH0335024U (de) * | 1990-02-26 | 1991-04-05 | ||
| JP3035024U (ja) | 1994-10-10 | 1997-03-11 | モレックス インコーポレーテッド | 電気コネクタの位置決め保証装置 |
| JP2002128070A (ja) * | 2000-10-30 | 2002-05-09 | Nippon Kopatsuku Kk | 内側被覆部材付き折畳通い箱 |
| DE10204176A1 (de) * | 2002-02-01 | 2003-08-14 | Wacker Chemie Gmbh | Vorrichtung und Verfahren zur kontaminationsarmen automatischen Verpackung von Polysiliciumbruch |
| DE102004003364A1 (de) * | 2004-01-22 | 2005-08-11 | Wacker-Chemie Gmbh | Vorrichtung zum Transport hochdisperser Pulver und Verfahren zu ihrer Befüllung und Entleerung |
| DE102007027110A1 (de) | 2007-06-13 | 2008-12-18 | Wacker Chemie Ag | Verfahren und Vorrichtung zum Verpacken von polykristallinem Siliciumbruch |
| DE102007047210A1 (de) | 2007-10-02 | 2009-04-09 | Wacker Chemie Ag | Polykristallines Silicium und Verfahren zu seiner Herstellung |
| IT1393915B1 (it) * | 2009-05-11 | 2012-05-17 | Fiorentino Cartonificio | Imballo a cisterna in cartone ondulato |
| DE102009045538A1 (de) * | 2009-10-09 | 2011-04-14 | Wacker Chemie Ag | Atmungsaktiver Handschuh zur Verwendung beim Verpacken und Sortieren von hochreinem Silicium |
| CN201901350U (zh) * | 2010-11-25 | 2011-07-20 | 浙江昱辉阳光能源有限公司 | 一种新型硅片包装盒 |
| DE102012200992A1 (de) | 2012-01-24 | 2013-07-25 | Wacker Chemie Ag | Dotierstoffarmes polykristallines Siliciumstück |
| DE102012206251A1 (de) * | 2012-04-17 | 2013-10-17 | Wacker Chemie Ag | Verpackung von polykristallinem Silicium |
| DE102012208473A1 (de) | 2012-05-21 | 2013-11-21 | Wacker Chemie Ag | Polykristallines Silicium |
-
2014
- 2014-03-03 DE DE102014203814.6A patent/DE102014203814A1/de not_active Withdrawn
-
2015
- 2015-02-27 US US15/123,160 patent/US10202282B2/en active Active
- 2015-02-27 EP EP15706827.1A patent/EP3114034A1/de not_active Withdrawn
- 2015-02-27 WO PCT/EP2015/054156 patent/WO2015132155A1/de not_active Ceased
- 2015-02-27 CN CN201580011528.1A patent/CN106061845B/zh not_active Expired - Fee Related
- 2015-02-27 CA CA2939825A patent/CA2939825C/en not_active Expired - Fee Related
- 2015-02-27 KR KR1020167027203A patent/KR101875300B1/ko not_active Expired - Fee Related
- 2015-02-27 MY MYPI2016001533A patent/MY181249A/en unknown
- 2015-02-27 JP JP2016555456A patent/JP6321199B2/ja not_active Expired - Fee Related
- 2015-03-03 TW TW104106597A patent/TWI557071B/zh not_active IP Right Cessation
Non-Patent Citations (2)
| Title |
|---|
| None * |
| See also references of WO2015132155A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201545978A (zh) | 2015-12-16 |
| MY181249A (en) | 2020-12-21 |
| KR20160128402A (ko) | 2016-11-07 |
| JP2017512159A (ja) | 2017-05-18 |
| US20170057830A1 (en) | 2017-03-02 |
| KR101875300B1 (ko) | 2018-07-05 |
| WO2015132155A1 (de) | 2015-09-11 |
| CA2939825C (en) | 2018-03-13 |
| CN106061845B (zh) | 2017-12-08 |
| US10202282B2 (en) | 2019-02-12 |
| JP6321199B2 (ja) | 2018-05-09 |
| CN106061845A (zh) | 2016-10-26 |
| DE102014203814A1 (de) | 2015-09-03 |
| TWI557071B (zh) | 2016-11-11 |
| CA2939825A1 (en) | 2015-09-11 |
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