EP2495106B1 - Aluminiumband für lithografische Druckplattenträger mit Wasser basierenden Beschichtungen - Google Patents

Aluminiumband für lithografische Druckplattenträger mit Wasser basierenden Beschichtungen Download PDF

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Publication number
EP2495106B1
EP2495106B1 EP20110156689 EP11156689A EP2495106B1 EP 2495106 B1 EP2495106 B1 EP 2495106B1 EP 20110156689 EP20110156689 EP 20110156689 EP 11156689 A EP11156689 A EP 11156689A EP 2495106 B1 EP2495106 B1 EP 2495106B1
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EP
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Prior art keywords
aluminium alloy
aluminum alloy
chlorine
melt
alloy strip
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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.)
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Application number
EP20110156689
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German (de)
English (en)
French (fr)
Other versions
EP2495106A1 (de
Inventor
Bernhard Kernig
Jochen Hasenclever
Gerd Steinhoff
Stefan Knabben
Werner Droste
Katrin Kuhnke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Speira GmbH
Original Assignee
Hydro Aluminium Rolled Products GmbH
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Application filed by Hydro Aluminium Rolled Products GmbH filed Critical Hydro Aluminium Rolled Products GmbH
Priority to EP20110156689 priority Critical patent/EP2495106B1/de
Priority to ES11156689.9T priority patent/ES2544707T3/es
Priority to CN201280009236.0A priority patent/CN103380007B/zh
Priority to PCT/EP2012/053591 priority patent/WO2012117084A1/de
Priority to BR112013020021-9A priority patent/BR112013020021B1/pt
Priority to JP2013555883A priority patent/JP5588075B2/ja
Priority to KR1020137026160A priority patent/KR101541438B1/ko
Publication of EP2495106A1 publication Critical patent/EP2495106A1/de
Priority to US14/013,927 priority patent/US8857332B2/en
Publication of EP2495106B1 publication Critical patent/EP2495106B1/de
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41N—PRINTING PLATES OR FOILS; MATERIALS FOR SURFACES USED IN PRINTING MACHINES FOR PRINTING, INKING, DAMPING, OR THE LIKE; PREPARING SUCH SURFACES FOR USE AND CONSERVING THEM
    • B41N1/00—Printing plates or foils; Materials therefor
    • B41N1/04—Printing plates or foils; Materials therefor metallic
    • B41N1/08—Printing plates or foils; Materials therefor metallic for lithographic printing
    • B41N1/083—Printing plates or foils; Materials therefor metallic for lithographic printing made of aluminium or aluminium alloys or having such surface layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41N—PRINTING PLATES OR FOILS; MATERIALS FOR SURFACES USED IN PRINTING MACHINES FOR PRINTING, INKING, DAMPING, OR THE LIKE; PREPARING SUCH SURFACES FOR USE AND CONSERVING THEM
    • B41N1/00—Printing plates or foils; Materials therefor
    • B41N1/04—Printing plates or foils; Materials therefor metallic
    • B41N1/08—Printing plates or foils; Materials therefor metallic for lithographic printing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D25/00—Special casting characterised by the nature of the product
    • B22D25/06—Special casting characterised by the nature of the product by its physical properties
    • 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
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12993—Surface feature [e.g., rough, mirror]

Definitions

  • the invention relates to an aluminum alloy strip for the production of printing plate supports with water-based coatings, wherein the aluminum alloy strip has a maximum thickness of 0.5 mm. Moreover, the invention relates to the use of separated from the aluminum alloy strip sheets for printing plate support and a method for producing an aluminum alloy strip according to the invention.
  • Aluminum alloy strips for lithographic printing plate supports which are produced, for example, from alloys of the type AA1050, AA1100, AA3103, AlMg0.5 and others, not only have high mechanical requirements with regard to continuous use as printing plate supports. After roughening the aluminum alloy strips, which usually have a maximum thickness of 0.5 mm, they are provided with coatings that are photo- and / or thermosensitive and thus allow the transmission of images to be printed or texts. To meet the increasing demands for the lowest possible environmental impact, increasingly water-based coatings are used. Water-based coatings contain water rather than commonly used organic solvents to apply the coating to the sheet. Indeed In the present invention, water-containing coatings are also included under this term.
  • the at least one water-based coating is applied to the aluminum alloy strip or sheet, so that after evaporation of the water a corresponding photo- or thermo-sensitive layer remains on the aluminum strip or the sheet produced therefrom.
  • these water-based coatings it has been shown that increasingly punctiform defects occur in the coating and the corresponding areas could no longer be properly exposed and stripped.
  • Corresponding pressure plate carriers are not suitable for later use and thus broke. This phenomenon has been particularly noted with CTP plate supports which do not undergo a development process using developer chemicals.
  • the present invention has the object to provide an aluminum alloy strip for the production of printing plate supports with a water-based coating, so that punctiform coating defects are prevented.
  • the present invention has for its object to propose an advantageous use of the aluminum alloy strip and a method for producing the aluminum alloy strip.
  • DE-A-19823790 describes an aluminum litho strip with a surface structure of undirected, fibrous recesses.
  • the stated object for an aluminum alloy strip is achieved by preparing the aluminum alloy strip in a manner using water as a lubricant Longitudinal grinding etching figures with cubic etching attack, the longitudinal extent of which is a maximum of 15 microns.
  • etching figures with a maximum longitudinal extent of 15 ⁇ m do not lead to surface defects which influence the printed image of the printing plate supports.
  • Print plate carriers made from the aluminum alloy strip according to the invention with a water-based coating therefore have no defects in the printed image.
  • the presence of etched figures with greater longitudinal extent automatically leads to the occurrence of errors in the printing plates.
  • a further increase in process safety can be ensured by the aluminum alloy strip being etched with a cubic etching attack in a longitudinal section prepared with water as a lubricant Longitudinal extension of a maximum of 10 microns, more preferably at most 5 microns.
  • the number of etching figures with cubic etching attack to 1000 mm 2 is a maximum of 350.
  • the limitation of the number of etching figures per 1000 mm 2 results in the likelihood that several densely adjacent etching figures lead to a printing error is reduced.
  • the aluminum alloy is preferably added to magnesium, manganese and silicon.
  • the aluminum alloy strip can therefore be further improved according to a further embodiment in that the aluminum alloy strip consists of an aluminum alloy with the following alloy constituents in% by weight: mg ⁇ 1 %, Mn ⁇ 0.6%, Fe ⁇ 1 %, 0.05% ⁇ ⁇ Si ⁇ 0.5%, Cu ⁇ 0.04%, Ti ⁇ 0.04%, unavoidable impurities individually a maximum of 0.01, in total a maximum of 0.05% and balance Al.
  • the aluminum alloy strip may preferably consist of an aluminum alloy with the following alloy components: 0.05 % ⁇ mg ⁇ 0.3 % Mn ⁇ 0.3 % 0.4 % ⁇ Fe ⁇ 1 % 0.05 % ⁇ Si ⁇ 0.5 % Cu ⁇ 0.04 % Ti ⁇ 0.04 % unavoidable impurities individually max. 0.01%, in total max. 0.05% and balance Al.
  • Another aspect of the aluminum alloy ribbon may be provided by the aluminum alloy of the aluminum alloy ribbon having the following alloy components in% by weight: 0.1 % ⁇ mg ⁇ 0.6 % Mn ⁇ 0.05 % 0.3 % ⁇ Fe ⁇ 0.4 % 0.05 % ⁇ Si ⁇ 0.25 % Cu ⁇ 0.04 % Ti ⁇ 0.04 % unavoidable impurities individually max. 0.01%, in total max. 0.05% and balance Al.
  • the just-mentioned alternative aluminum alloy strip has an Mg content of 0.1% by weight to 0.3% by weight or 0.3% by weight to 0.6% by weight.
  • the higher Mg contents of 0.3 wt.% To 0.6 wt.% Are intended for aluminum alloy tapes which are intended to provide higher strength and bending resistance during operation.
  • the limitation of the Mg content of 0.1 wt .-% to 0.3 wt .-% leads to a high flexural fatigue, thermal stability and a very good roughening at medium strengths of the aluminum alloy strip at constant parameters during the production of the aluminum alloy strip.
  • plates for printing plate support is advantageous if these are thermal pressure plate carrier, since thermal pressure plate carrier increasingly be prepared using water-based coatings.
  • the steps just described represent the conventional process steps in the production of an aluminum alloy needed for the production of the aluminum alloy strip.
  • the above-described object is achieved in that the aluminum alloy is degassed during casting in a degasser with chlorine gas, wherein the melt is fed to a maximum chlorine content of 7 mg Cl / kg Al.
  • degasification of the melt during degassing for example using a multi-rotor degasser, is a particularly critical source of contamination of the aluminum alloy with chlorine, as there is a solidified ingot or a solidified casting strip immediately after casting.
  • Chlorine is fed to the degasser to re-purify the molten aluminum alloy to be cast and, for example, reduce the levels of sodium, lithium and calcium.
  • the aluminum alloy melt also passes through a filter which comprises a packed bed filter or a ceramic foam filter.
  • a filter which comprises a packed bed filter or a ceramic foam filter.
  • printing plate supports can be produced from aluminum alloy strips produced according to the invention, which can be provided with water-based coatings without errors, without tilting to punctiform printing defects.
  • the amount of chlorine is reduced to 2 to 4 mg Cl / kg Al in order to further reduce the contamination of the aluminum alloy with chlorine and the ⁇ tzfiguren in Aluminum alloy tape with cubic etching attack to further reduce.
  • the gas purging in the melting or casting furnace is carried out with addition of chlorine, wherein the supplied amount of chlorine is a maximum of 40 mg Cl / kg Al.
  • the amount of chlorine introduced during the gas purging in the melting or casting furnace plays a role for the occurrence of printing errors in the printing plate carriers.
  • the gas flushing in the melting or casting furnace with addition of chlorine, although the content of sodium and calcium in the aluminum melt is further reduced. If the amount of chlorine supplied is limited to a maximum of 40 mg Cl / kg Al, etching figures with a cubic etching attack with a maximum size of 15 ⁇ m can be ensured despite addition of chlorine in the gas flush in the melting or casting furnace.
  • an aluminum alloy ribbon made from a suitably treated aluminum alloy melt can be provided to water-based printing plate supports.
  • no chlorine gas is used in the gas purging in the melting or casting furnace and in the degassing during casting in the degasser.
  • the purification of the melt of sodium, lithium and calcium components is carried out by adding salts, in particular chlorides, preferably potassium chloride magnesium chloride, wherein the aluminum alloy melt may be supplied to a maximum of 60 mg Cl / kg Al.
  • the gas flushing in the melting or casting furnace and the degassing during casting in the degasser in this case, for example, using argon and possible addition of other inert gases, such as nitrogen.
  • potassium chloride magnesium chloride in an amount such that a maximum of 60 mg Cl / kg Al are supplied to the aluminum alloy melt, allows sufficient cleaning without the chlorine residues in aluminum melt to ⁇ tzfiguren with cubic ⁇ tzangriff and a longitudinal extension of more than 15 microns to lead.
  • Aluminum alloy tapes made from this aluminum alloy melt are particularly suitable for use as printing plate supports with water-based coatings because punctiform printing defects are suppressed.
  • Fig. 1 shows a schematic flow diagram of the manufacturing steps of aluminum alloy strips, as required for printing plate support.
  • the aluminum alloy is melted from primary aluminum and melted using molten scrap, ingots, liquid metal from a furnace sump or even recycled metal or other master alloys to form an aluminum alloy melt.
  • the molten aluminum alloy may then be alloyed with additional alloying ingredients, such as magnesium, manganese, or other alloying ingredients to achieve the desired aluminum alloy composition.
  • the aluminum alloy is transferred to the casting or smelting furnace, in which then according to process step 2 a targeted melt treatment, in particular for the purification of the aluminum alloy melt he follows.
  • a melt treatment 2 in the casting or melting furnace gas flushing be performed.
  • the melt is etched off, ie the components floating on the melt are sucked off and the slag is removed.
  • the gases introduced into the aluminum melt by the gas purging additionally escape, so that further purification takes place.
  • the melt treatment 2 in the casting or smelting furnace are usually carried out with addition of chlorine, since chlorine has the property of effectively sodium, lithium and calcium components of the aluminum alloy melt by formation of the corresponding salts, which are impurities in the melt, even the lowest concentrations of the Remove aluminum alloy melt.
  • the sodium, lithium and / or calcium content of the aluminum alloy melt can thus be reduced to a few ppm.
  • the casting of the aluminum alloy melt to a rolling bar 4a or to a casting belt 4b takes place via a degasser, which is usually arranged in the channel system required for casting.
  • the degassing 3 of the aluminum alloy melt in the degasifier which is often designed as Mehrcrotorentgaser and upstream of a filtration stage, has the task to clean the aluminum alloy melt again to remove unwanted alloying constituents, in particular sodium, lithium and / or calcium components. Therefore, chlorine gas is also usually used in degassing step 3.
  • the aluminum alloy strip 6 is produced by rollers 5a, 5b from the casting ingots produced by casting 4a or casting belts 4b.
  • the produced aluminum alloy strips 6 are roughened electrochemically and provided with a water-based coating, so that the aluminum alloy strip 6 cut into sheets as print plate carrier, for example, as a thermal printing plate is usable.
  • Table 1 shows the pattern alloys Nos. 1 to 9 and their composition.
  • Table 1 Pattern no tape Si Fe Cu Mn mg Cr Zn Ti B 1 M1 See. 0.0798% 0.3633% 0.0013% 0.0040% 0.2120% 0.0011% 0.0088% 0.0069% 0,0005% 2 M3 See. 0.0796% 0.3644% 0.0013% 0.0040% 0.2183% 0.0010% 0.0085% 0.0067% 0,0004% 3 M4 See.
  • the pattern alloys Nos. 1-9 were made using six methods V0 to V5, which proceeded through the method steps 1, 2 and 3 Fig. 1 are characterized produced.
  • the amount of chlorine in the gas flush in the furnace was reduced to 20 mg Cl / kg Al and the amount of chlorine, which is fed to the aluminum melt in the degasser, adjusted to the value 6.6 mg Cl / kg Al.
  • the method V5 differs from the methods V0 to V4 by the addition of salts in the melting and alloying of the aluminum alloy in step 1 Fig. 1 in the amount of 60 mg Cl / kg Al In the subsequent steps of oven rinse and degassing, no chlorine was added in process V5.
  • Table 2 method tape Chlorine content by salt addition [mg Cl / kg Al] Chlorine quantity furnace flush [mg Cl / kg Al] Chlorine amount in degasser [mg Cl / kg Al] V0 comparison M1, M3 0 34 6.6 V1 comparison M4, M5 0 40 12 V2 invention M10 0 0 0 V3 invention M8, M9 0 20 6.6 V4 invention M16 0 0 0 V5 invention M7 60 0 0 0
  • Table 2 shows the assignment of the aluminum alloy strips M1 to M16 to the production methods V0 to V5. From the bands M1 to M16, samples were cut out longitudinally to the rolling direction and longitudinal slices were prepared for microscopic examination. For this purpose, initially a plurality of strips were cut out of the respective bands M1 to M16, so that they have a cutting edge parallel to the rolling direction. The strips 7 were positioned in a sample holder 8 and embedded with epoxy resin 9 so that the upwardly facing edge corresponded to the cutting edge in the rolling direction.
  • Fig. 2 shows how strips 7 may be provided from an aluminum alloy strip 6 to make longitudinal cuts of the aluminum alloy strip. As can be seen, a plurality of strips 7 are directly separated from an aluminum alloy strip and then placed in a sample holder 8.
  • FIG. 3 shows in a plan view of a sample holder 8 with molded longitudinal strips 7, have from the longitudinal strips 7, the edge surfaces upwards. If the sample holder 8 is applied upside down for polishing on a polishing station 10 with a polishing plate 11, then the cut edges facing downwards can be polished to form longitudinal cuts.
  • the device for polishing the longitudinal strips is in Fig. 4 in a sectional view only schematically shown.
  • the rotating grinding wheel 11 is covered with an abrasive paper with increasing grain size.
  • an SIC paper with a grain size of 120 is used until the samples in the sample holder 8 have a planar surface.
  • the lubricant is water at each grinding step.
  • the grain size of the grinding wheels is then successively increased from 500 to 1000 and later on an abrasive cloth with about 2400, the grinding time about 10 - 20 sec. was and in turn used as a lubricant water.
  • semi-automatic polishers are further polishing steps with a medium-hard cotton cloth with a polycrystalline diamond suspension with 6 micron grit and then on a cotton cloth with a 3 micron polycrystalline diamond suspension for a period of about 8 - 9 min. carried out.
  • the lubricants used in this step were alcohol-based and oil-based agents, for example "lubricious blue” and "lubricious red”.
  • the samples were cleaned under running water with a rinsing agent and then with Ethanol dried under hot air.
  • the final polishing was carried out with a synthetic synthetic fiber cloth in conjunction with an oxide polishing suspension 0.25 ⁇ m and the lubricant water for a time of 2 - 5 minutes.
  • the longitudinal sections thus produced were examined under 500-fold magnification in the unetched state with the microscope and evaluated.
  • the size of the etching figures was rated “large”, provided that etching figures with cubic etching attack were present, which exceeded a longitudinal extent of 30 microns.
  • etching figures with a maximum longitudinal extent of 15 ⁇ m were referred to as "small” etching figures. Since the evaluated areas of the longitudinal cuts fluctuated, the found number of etching figures with cubic etching attack on an area of 1000 mm 2 was extrapolated.
  • Comparative samples Nos. 1, 2, 3 and 4 showed medium to large etching figures with cubic etching attack.
  • the number of medium and large etch characters with cubic etch attack ranged from 1089 to 298.
  • Comparative Pattern Nos. 1, 2, 3, 4 resulted in an unacceptable printing result because dot-shaped printing defects occurred in the coating.
  • samples No. 5-9 according to the invention exhibited cubic etching attack etch patterns which had a longitudinal extension of less than 15 ⁇ m.
  • the number of etching figures in Comparative Sample No. 2 and the No. 7 of the present invention were almost identical, the size of the etching figures was reflected in an unacceptable printing result in the comparative sample No. 2.
  • Fig. 5 a greatly enlarged section of a longitudinal section of the pattern M3.
  • etching figure which has a cubic etching attack and has a longitudinal extent of 42 microns.
  • the cubic etch attack is typical of the presence of chlorine atoms or chlorine clusters which, when combined with water, react to form hydrochloric acid leaving typical etch patterns in the aluminum crystal cladding.
  • Fig. 6 Figure 3 shows a cubic etch attack etch figure which has a medium size and also results in an unacceptable defect on the water-based coatings coated printing plate supports.
  • the longitudinal extension of this etching figure was 22 microns.
  • an inventive embodiment which in Fig. 7 is shown, extremely small ⁇ tzfiguren with cubic etching attack with a size of less than 5 microns. Pattern M7 was rated positive in the coating trials.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Printing Plates And Materials Therefor (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
EP20110156689 2011-03-02 2011-03-02 Aluminiumband für lithografische Druckplattenträger mit Wasser basierenden Beschichtungen Active EP2495106B1 (de)

Priority Applications (8)

Application Number Priority Date Filing Date Title
EP20110156689 EP2495106B1 (de) 2011-03-02 2011-03-02 Aluminiumband für lithografische Druckplattenträger mit Wasser basierenden Beschichtungen
ES11156689.9T ES2544707T3 (es) 2011-03-02 2011-03-02 Banda de aluminio para soporte de planchas de impresión litográficas con recubrimientos basados en agua
BR112013020021-9A BR112013020021B1 (pt) 2011-03-02 2012-03-02 tira de liga de alumínio para a produção de suportes de chapas de impressão e método de produção de tiras de alumínio
PCT/EP2012/053591 WO2012117084A1 (de) 2011-03-02 2012-03-02 Aluminiumband für lithografische druckplattenträger mit wasser basierenden beschichtungen
CN201280009236.0A CN103380007B (zh) 2011-03-02 2012-03-02 用于具有水基涂层的平版印版载体的铝条
JP2013555883A JP5588075B2 (ja) 2011-03-02 2012-03-02 水性コーティングを含むリソグラフ印刷プレート支持体用アルミニウムストリップ
KR1020137026160A KR101541438B1 (ko) 2011-03-02 2012-03-02 수성 피막을 구비한 평판 인쇄판 캐리어용 알루미늄 스트립
US14/013,927 US8857332B2 (en) 2011-03-02 2013-08-29 Aluminium strip for lithographic printing plate carriers comprising water-based coatings

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Application Number Priority Date Filing Date Title
EP20110156689 EP2495106B1 (de) 2011-03-02 2011-03-02 Aluminiumband für lithografische Druckplattenträger mit Wasser basierenden Beschichtungen

Publications (2)

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EP2495106A1 EP2495106A1 (de) 2012-09-05
EP2495106B1 true EP2495106B1 (de) 2015-05-13

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US (1) US8857332B2 (zh)
EP (1) EP2495106B1 (zh)
JP (1) JP5588075B2 (zh)
KR (1) KR101541438B1 (zh)
CN (1) CN103380007B (zh)
BR (1) BR112013020021B1 (zh)
ES (1) ES2544707T3 (zh)
WO (1) WO2012117084A1 (zh)

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Publication number Priority date Publication date Assignee Title
US10851263B2 (en) 2015-04-06 2020-12-01 Novelis Inc. Water-based coating compositions and related products and processes
JP6427267B2 (ja) * 2015-05-28 2018-11-21 株式会社Uacj 磁気ディスク用アルミニウム合金基板及びその製造方法、ならびに、当該磁気ディスク用アルミニウム合金基板を用いた磁気ディスク
BR112018070957B1 (pt) * 2016-04-20 2022-08-30 Hydro Aluminium Rolled Products Gmbh Método para produção de uma faixa de alumínio para suportes de placa de impressão litográfica de uma liga de alumínio

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EP1293579A2 (en) 2001-09-12 2003-03-19 Fuji Photo Film Co., Ltd. Support for lithographic printing plate and presensitized plate
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WO2007045676A1 (de) 2005-10-19 2007-04-26 Hydro Aluminium Deutschland Gmbh Aluminiumband für lithographische druckplattenträger
WO2007115167A2 (en) 2006-03-31 2007-10-11 Alcoa Inc. Manufacturing process to produce litho sheet

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PETER WAITE: "A Technical Perspective on Molten Aluminium Processing", LIGHT METALS, 2002, pages 51 - 58, XP055483586
PIERRE LE BRUN: "Melt Treatment-Evolution and Perspectives", LIGHT METALS, 2008, pages 59 - 64, XP055483574
RAJA R. ROY, TORSTEIN A. UTIGARD, CLAUDE DUPUIS: "INCLUSION REMOVAL KINETICS DURING CHLORINE FLUXING OF MOLTEN ALUMINUM", LIGHT METALS, 2001, pages 991 - 997, XP055483565

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US20140000469A1 (en) 2014-01-02
CN103380007B (zh) 2016-05-18
EP2495106A1 (de) 2012-09-05
BR112013020021B1 (pt) 2021-05-18
US8857332B2 (en) 2014-10-14
WO2012117084A1 (de) 2012-09-07
CN103380007A (zh) 2013-10-30
KR101541438B1 (ko) 2015-08-03
BR112013020021A2 (pt) 2017-06-13
JP2014514178A (ja) 2014-06-19

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