CN102459683A - 生产具有改善外观的涂覆金属带材的方法 - Google Patents
生产具有改善外观的涂覆金属带材的方法 Download PDFInfo
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- CN102459683A CN102459683A CN2010800286899A CN201080028689A CN102459683A CN 102459683 A CN102459683 A CN 102459683A CN 2010800286899 A CN2010800286899 A CN 2010800286899A CN 201080028689 A CN201080028689 A CN 201080028689A CN 102459683 A CN102459683 A CN 102459683A
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
本发明涉及制造具有金属腐蚀防护涂层的金属带材的方法,该方法包括在于以下的步骤:使金属带材穿过熔融金属的浴液,该浴液包含0.2-8重量%的铝和如下百分比的镁:0.1-8重量%的镁,对应的铝含量大于或等于0.2重量%但小于4重量%,或者镁含量大于5重量%但小于或等于8重量%,对应的铝含量大于或等于4重量%但小于或等于8重量%,并且包含至多0.3重量%的添加元素,余量为锌和不可避免的杂质;然后通过喷嘴对带材的两侧喷射气体来干燥涂覆的金属带材,所述气体具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力;然后使带材穿过密闭区,该密闭区受限于如下:在底部,干燥线和所述干燥喷嘴的上部外表面,在顶部,两个放置在带材两侧的密闭箱的上部部分,正位于所述喷嘴上方,并且具有与干燥线相距至少10cm的高度,在侧面,所述密闭箱的侧面部分,在所述密闭区中的气氛具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力和高于由0.15体积%氧气和99.85体积%氮气构成气氛的氧化能力。本发明还涉及能够通过该方法获得的金属带材和通过变形该带材获得的金属部件。
Description
本发明涉及制造具有改善的外观、更特别地是旨在用于制造陆用机动车辆外壳部件的金属带材的方法,但是不限于此。
旨在用于制造陆用机动车辆部件的钢板通常涂覆有用于腐蚀防护的锌基金属层,该锌基金属层通过在锌基液体浴液中热浸涂覆或者通过在含有锌离子的电解浴液中电沉积来进行沉积。
然后,将旨在用于制造外壳部件的镀锌板进行成形操作以及组装形成白车身,然后将白车身涂覆至少一个涂料层,从而提供更好的腐蚀防护和良好的表面外观。
为此目的,常规地,机动车辆制造商首先向白车身施加电泳涂层,随后是底涂料层、基础涂料层和任选的清漆涂层。为获得令人满意的涂漆表面外观,通常施加90-120μm的总涂料厚度,其构成例如为20-30μm厚的电泳涂层、40-50μm厚的底涂料层和30-40μm厚的基础涂料层。
为将涂料***的厚度减小到小于90μm,某些机动车辆制造商提出了免除电泳步骤或者减少涂料的层数以便提高生产率。然而,在目前,涂料***的这种厚度降低总是损害部件的最终涂漆表面外观,并且在工业生产中并未得到实施。
这是因为充当基础基材的锌基涂层具有称作“波纹”的表面,其目前仅可通过厚的涂料层来弥补,否则代价是车身部件具有不可接受的所谓“桔皮”外观。
表面的波纹度W是相当长波长(0.8-10mm)的轻微、准周期性几何不平度,其不同于与较短波长(<0.8mm)几何不平度对应的粗糙度R。
在本发明中,使用波纹度轮廓的算术平均值Wa(以μm计)表征板材的表面波纹度,并且截止阈值为0.8mm的波纹度测量结果用Wa0.8表示。
因此,本发明的一个目的是提供制造涂有腐蚀防护涂层的金属带材的方法,其波纹度Wa0.8与现有技术的带材的波纹度Wa0.8相比较小,因而使得能够制造所需的总漆厚度小于现有技术部件的涂漆金属部件。
为此目的,本发明的第一主题由制造具有用于腐蚀防护的金属涂层的金属带材的方法形成,该方法包括在于以下的步骤:
-使金属带材穿过熔融金属浴液,该浴液包含0.2-8重量%的铝和如下百分比的镁:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于4重量%而言,或者
-大于5重量%但小于或等于8重量%的镁含量,对于铝含量大于或等于4重量%但小于或等于8重量%而言,
并且包含至多0.3重量%的添加元素,余量为锌和不可避免的杂质;然后
-通过对带材两侧喷射气体的喷嘴来干燥涂覆的金属带材,所述气体具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力;然后
-使带材穿过密闭区,该密闭区:
·在底部,由干燥线和所述干燥喷嘴的上部外表面界定,
·在顶部,由两个放置在带材每侧的密闭箱的上部部分界定,其正位于所述喷嘴上方,并且具有相对于干燥线至少10cm的高度,
·在侧面,由所述密闭箱的侧面部分界定,
在所述密闭区中的气氛具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力,且高于由0.15体积%氧气和99.85体积%氮气构成气氛的氧化能力。
在优选的实施方式的方法中,本发明的工艺可以进一步单独或组合地包括如下特征,
-密闭箱具有相对于干燥线至少15cm的高度,甚至20cm和更特别地优选至少30cm的高度;
-密闭箱供应气体,该气体具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力,且优选具有高于由0.15体积%氧气和99.85体积%氮气构成气氛的氧化能力;
-还使带材穿过位于干燥线之前的密闭区;
-位于干燥线之前的密闭区开始于熔融金属浴液的出口,并终止于在干燥线之下;
-干燥气体由氮气构成;和
-金属带材是钢带材。
本发明的主题还是经热浸涂覆但尚未冷轧平整的冷轧金属带材,其可通过根据本发明的方法获得,其金属涂层具有小于或等于0.70μm的波纹度Wa0.8,优选地具有小于或等于0.65μm的波纹度Wa0.8,并且包含0.2-8重量%的铝和如下百分比的镁:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于2重量%而言,或者
-大于5重量%但小于或等于8重量%的镁含量,对于铝含量大于或等于2重量%但小于或等于8重量%而言,
并且包含至多0.3重量%的添加元素,余量为锌和不可避免的杂质。
在一个优选的实施方案中,根据本发明的金属带材由钢构成。
本发明的主题还是通过使根据本发明的金属带材变形而获得的金属部件,其涂层具有小于或等于0.65μm的波纹度Wa0.8,优选具有小于或等于0.60μm的波纹度Wa0.8。
本发明的另一个主题是通过使根据本发明的金属带材变形,并且在变形之前经受冷轧平整操作而获得的金属部件,其涂层具有小于或等于0.70μm的波纹度Wa0.8,优选具有小于或等于0.60μm,更优选0.55μm的波纹度Wa0.8。
在下面以非限制性实施例的方式给出的描述的过程中,本发明的特征和优点将变得更为清楚明显。
参照图1,根据本发明方法的第一步在于使金属带材B,例如钢带材,连续地通过盛放在熔锅3中的包含熔融金属的涂覆浴液2。在浸入所述浴液2前,带材通常经受在炉1中的退火操作,特别是为了调质表面。
在工业生产线上,带材行进速度通常例如为40m/min-200m/min,优选大于120m/min或者甚至大于150m/min。
待用于根据本发明的方法中的涂覆浴液的组合物是基于锌的,并且初始含有0.2-8重量%铝。该元素一方面能够使得涂层对金属带材的附着性得到改善,另一方面能够防护带材免受腐蚀。
含量小于0.2%时,没有观察到对附着性的影响,而大于8%的含量会造成问题,如随后施加涂料的分层。
浴液还含有镁以便改善镀锌涂层的抗腐蚀性、特别是其抗红锈性。镁以如下百分比存在:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于4重量%而言,或者
-大于5重量%但小于或等于8重量%的镁含量,对于铝含量大于或等于4重量%但小于或等于8重量%而言。
在一个优选的实施方案中,镁以如下百分比存在:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于2重量%而言,或者
-大于5重量%但小于或等于8重量%的镁含量,对于铝含量大于或等于2重量%但小于或等于8重量%而言。
在另一个优选的实施方案中,镁以如下百分比存在:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于1.5重量%而言,或者
-大于5重量%但小于或等于8重量%的镁含量,对于铝含量大于或等于1.5重量%但小于或等于8重量%而言。
为获得对抗腐蚀性的明显作用,优选以至少0.1重量%或0.2重量%加入镁。其在浴液中的最大含量限于8重量%,由于所获得的涂层在随后的成形操作期间,特别是在拉拔操作期间,可具有严重开裂的问题。排除了0.1-5重量%的镁和4-8重量%的铝的范围,因为当带材在这个组成范围内经受根据本发明的密闭干燥过程时观察到可见缺陷(能够通过裸眼看到)。
浴液组合物还可以含有至多0.3重量%的任选的添加元素,例如Si、Sb、Pb、Ti、Ca、Mn、Sn、La、Ce、Cr、Ni、Zr或Bi。例如,这些各种元素特别使得能够改善涂层的抗腐蚀性或其脆性或其附着性。知晓它们对涂层特性的影响的本领域技术人员会根据所需的互补目的对它们加以使用。还证实这些元素不妨碍通过根据本发明方法获得的对波纹度的控制。然而,在某些情况下,优选将钛含量限制到小于0.01%,或甚至小于0.005%,由于该元素可以在汽车制造商所用的除脂和磷化的浴液中导致污染问题。
最后,浴液可以含有源自于填充进入熔锅的坯锭或者源自于穿过浴液的带材的不可避免的杂质。因而,这些可以尤其包含铁等。
使浴液维持在液相线+10℃和700℃之间的温度,液相线温度的变化取决于其组成。因而,对于用于本发明的涂层的范围,该温度将为350℃-700℃。可回顾的是,液相线是高于其时合金完全处于熔融状态的温度。
在穿过熔锅3后,然后通过置于带材B的两侧的喷嘴4对两面上均得到涂覆的金属带材B进行干燥操作,所述喷嘴将干燥气体喷射到带材B的表面上。这种本领域技术人员公知的常规操作使得在涂层尚未凝固时涂层厚度得到准确调节。
根据本发明方法的必要特征之一在于,选择氧化能力低于由4体积%氧气和96体积%氮气构成的气氛的氧化能力的干燥气体。特别是,能够使用纯氮气或纯氩气,或者氮气或氩气和氧化气体(例如氧气、CO/CO2混合物或H2/H2O混合物)的混合物。还能够使用不加入惰性气体的CO/CO2混合物或H2/H2O混合物。
在干燥步骤之后,根据本发明的方法的另一个必要特征是穿过密闭区,该密闭区:
-在底部,由干燥线和干燥喷嘴4的上部外表面界定,
-在顶部,由两个放置在带材两侧的密闭箱5的上部部分界定,其正位于喷嘴4上方,并且具有相对于干燥线至少10cm的高度,
-在侧面,由密闭箱5的侧面部分界定,
在密闭区的气氛具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力,且高于由0.15体积%氧气和99.85体积%氮气构成气氛的氧化能力。
为确定带材周围气氛的氧化能力,测量其等效平衡氧气分压。
当存在的唯一氧化气体是混有惰性气体(氮气或氩气)的O2时,则该压力等于能够通过合适的传感器实时测量的O2体积含量。
当存在混有还原气体(例如H2或CO)的其它氧化气体(例如H2O或CO2)时,通过有关气体温度下的质量作用定律计算等效氧气分压。
例如,对于H2/H2O对,反应可写作如下:
在热力学平衡中,气体的分压遵循以下方程:
其中R是理想气体常数,T是绝对开氏气体温度,ΔG是与反应有关的自由能变化,其可以在热力学表中找到,取决于常数R的取值,以卡/摩尔或焦耳/摩尔计。
有关气体混合物在平衡即等效氧气分压pO2的值由上面方程获得。
在本发明的上下文中,在密闭箱5中pO2为0.0015-0.04是必要的。
实际上,本发明人惊喜地发现,通过使用根据本发明的干燥气体并使带材穿过这样的密闭区,获得了具有小于现有技术中所获得涂覆带材的波纹度的涂层。
在本申请的上下文中,术语“干燥线”理解为是指连接喷嘴与带材的最短部分,对应于干燥气体沿着行进的最小路径,在图1中如字母L表示。
可向根据本发明的方法中使用的密闭箱5供应具有低氧化能力的气体或惰性气体,或者可以简单地通过从喷嘴逸出的干燥气体流供应它们。
密闭气氛和干燥气体的氧化能力限于由4体积%氧气和96体积%氮气构成的混合物的氧化能力,由于高于这个程度的氧化时,涂层的波纹度相对于现有技术中涂层的波纹度不会得到改善。
相比之下,设立了密闭气氛的氧化能力的下限,设置为由0.15体积%氧气和99.85体积%氮气构成的混合物的氧化能力,由于如果该密闭气氛的氧化性不足,其使用会促进锌从尚未固化的涂层中气化,然后其蒸气可以污染密闭箱和/或重新沉积在带材上,从而产生不可接受的可见缺陷。
为限制干燥前的氧化,可期望但不是必须的,使密闭箱延伸直至浴液的表面或者直至浴液和干燥线之间的中间位置,优选位于在干燥线之下10cm的距离处,或甚至15cm的距离处。这是由于当金属板材的表面暴露于自由空气中时,***地形成这种层,但是通常在干燥喷射作用下被除去并返回到涂覆浴液中。因此,这种密闭使得能够减少浴液的氧化物的量,该氧化物可能由行进中的带材带入,并且因而可以产生不可接受的缺陷。但是,其再次具有促进锌从浴液或从液体涂层蒸发的缺点,因而优选这些附加的密闭箱中的气氛具有的氧化能力高于含有0.15体积%氧气和99.85体积%氮气的气氛的氧化能力。
虽然可使用所有种类的干燥喷嘴来实施根据本发明的方法,但是将更特别优选使用具有叶片状出口孔(orifice)的喷嘴,其宽度超过待涂覆带材宽度,因为这种类型的喷嘴允许适当地限制在干燥区的底部。特别地,可以有利地使用三角形横截面的喷嘴,如图1概要性地所示的。这些喷嘴通常位于浴液表面上方30或甚至40cm处。
通过考虑这些设置,观察到所讨论的涂层波纹度的令人惊喜和重要的减少,如下述实验那样。
当涂覆板材己完全冷却时,可以对其进行冷轧平整操作,使其能够产生有利于其随后成形操作的织构。这是因为,通过带材成形之前促进对带材所施用的油的良好保持性,冷轧平整操作对带材表面赋予足够的粗糙度,以便在其上合适地进行成形工艺。
通常对旨在制造用于陆用机动车辆的车身部件的金属板材进行这种冷轧平整操作。例如,当根据本发明的金属板材旨在制造家用电器时,不进行这种附加操作。
然后对不管冷轧平整与否的板材进行成形操作,例如通过拉拔、弯曲或压型,优选通过拉拔,以便形成之后可涂漆的部件。对于家用电器的部件,还可任选地使用本身己知的物理和/或化学方式对该涂料层进行焙烧操作。为此目的,可使涂漆部件穿过感应炉或热风炉,或者UV灯下方或电子束装置下方。
为了生产机动车辆部件,将板材浸没在电泳浴液并且相继施加底涂料层、基础涂料层和任选的清漆上涂层。
在将电泳涂层施加到所述部件之前,首先将部件除脂,然后磷化,以确保所述涂层的附着。电泳涂层给部件提供附加的腐蚀防护。通常喷射涂层施加的底涂料层为部件的最终外观做好准备,并且防护其免受石击和UV辐射。基础涂料层为部件提供了其颜色和其最终外观。清漆涂层给部件表面提供良好的机械强度、对侵蚀性化学物质的抵抗性和吸引人的表面外观。
用于防护镀锌部件和保证最佳表面外观的涂料层(或涂料***)具有例如10-20μm厚的电泳涂层、小于30μm厚的底涂料层和40μm厚的基础涂料层。
在涂料***还包括清漆涂层的情形中,各个涂料层的厚度通常为如下:
-电泳涂层:小于10-20μm;
-底涂料层:小于20μm;
-基础涂料层:小于20μm,且有利地小于10μm;和
-清漆涂层:优选小于30μm。
涂料***还可以不包含电泳涂层,并且可以仅包含底涂料层、基础涂料层和任选的清漆涂层。
试验
在由IF-Ti钢制成的冷轧金属板材上进行试验,使所述金属板材穿过含有金属浴液的熔锅,该金属浴液基于锌并包含可变百分比的铝和镁。使浴液维持在高于所述组合物液相线70℃的温度。
在离开浴液时,通过两种常规喷嘴用氮气干燥所获得的涂层,以便获得约7μm的涂层厚度。
钢带材在涂覆浴液出口与在后干燥区之间的路线分为四个区:
-区1从浴液出口直至干燥线下10cm距离处;
-区2从区1的末端直至干燥线;
-区3从区2的末端直至干燥线上方10cm距离处;
-区4从区3的末端直至金属涂层的固化点。
在这些区中的每个都放置有密闭箱,密闭箱中有各种氮基气氛,其含有氧气的体积分数为下表中表示,或者由空气构成的气氛。特定的传感器用于检查在箱中的氧气含量。
从已涂覆的板材取出三个系列的试样。第一个系列未经受进一步的改性,第二个系列在3.5%的等双轴应变(Marciniak)模式下拉拔,而使第三个系列首先经受1.5%延伸率的冷轧平整操作,然后经受拉拔,如第二个系列中那样。
随着试验进行,测量波纹度值Wa0.8。这种测量在于使用不具有滑动体的机械探针测定长度为50mm的板材轮廓,在与轧制方向成45°处测量。其通常形状的近似值通过5阶多项式从所获得的信号确定。然后通过高斯滤波(Gaussian filter)用0.8mm截止阈值从粗糙度Ra中分离出波纹度Wa。在下表中给出了所获得的结果:
考虑试验1,可看到过高的氧化能力,意味着它是不可能获得波纹度适合于生产车身部件的产品。
试验5、7、9和10显示,如果不控制涂层的干燥,则获得根据现有技术的波纹度值,这些远远高于那些根据本发明可达到的波纹度值。
试验4不允许评价所获得的涂层的波纹度,因为点缺陷判定为对于车身部件产品是不可接受的(夹带渣滓,喷射线)。
最后,可以看到,根据本发明的试验2、3、6、8和11-13确实可获得迄今不可获得的波纹水平。
Claims (11)
1.制造具有用于腐蚀防护的金属涂层的金属带材的方法,该方法包括在于以下的步骤:
-使金属带材穿过熔融金属的浴液,该浴液包含0.2-8重量%的铝和如下百分比的镁:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于4重量%而言,或者
-大于5重量%但小于或等于8重量%的镁含量,对于铝含量大于或等于4重量%但小于或等于8重量%而言,
并且包含至多0.3重量%的添加元素,余量为锌和不可避免的杂质;然后
-通过在带材的两侧上喷射气体的喷嘴来干燥涂覆的金属带材,所述气体具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力;然后
-使带材穿过密闭区,该密闭区:
·在底部,由干燥线和所述干燥喷嘴的上部外表面界定,
·在顶部,由两个放置在带材两侧的密闭箱的上部部分界定,其正位于所述喷嘴上方,并且具有相对于干燥线的至少10cm的高度,
·在侧面,由所述密闭箱的侧面部分界定,
在所述密闭区中的气氛具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力且高于由0.15体积%氧气和99.85体积%氮气构成气氛的氧化能力。
2.如权利要求1所述的方法,其中所述密闭箱具有相对于干燥线至少15cm的高度。
3.如权利要求1或2所述的方法,其中所述密闭箱供应气体,该气体具有的氧化能力低于由4体积%氧气和96体积%氮气构成气氛的氧化能力。
4.如权利要求1-3中任一项所述的方法,其中使带材进一步穿过位于干燥线之前的密闭区。
5.如权利要求4所述的方法,其中位于干燥线之前的所述密闭区开始于熔融金属浴液的出口且终止于干燥线之下。
6.如权利要求1-5中任一项所述的方法,其中干燥气体由氮气构成。
7.如权利要求1-6中任一项所述的方法,其中金属带材是钢带材。
8.一种经热浸涂覆但尚未冷轧平整的冷轧金属带材,其能够通过如权利要求1-7中任一项所述的方法获得,其金属涂层具有0.7μm以下的波纹度Wa0.8,该金属涂层包含0.2-8重量%铝和如下百分比的镁:
-0.1-8重量%的镁,对于铝含量大于或等于0.2重量%但小于2重量%而言,或者
-镁含量大于5重量%但小于或等于8重量%,对于铝含量大于或等于2重量%但小于或等于8重量%而言,
并且包含至多0.3重量%的添加元素,余量为锌和不可避免的杂质。
9.如权利要求8所述的金属带材,其特征在于该金属带材由钢构成。
10.一种通过使如权利要求8或9所述的金属带材变形而获得的金属部件,其涂层具有0.65μm以下的波纹度Wa0.8。
11.一种通过使如权利要求8或9所述的金属带材变形且在变形之前还经受冷轧平整操作而获得的金属部件,其涂层具有0.70μm以下的波纹度Wa0.8。
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Cited By (12)
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CN104487605A (zh) * | 2013-05-13 | 2015-04-01 | 安赛乐米塔尔研究与发展有限责任公司 | 铝元件和具有ZnAlMg合金涂层的钢元件的组件 |
CN104487605B (zh) * | 2013-05-13 | 2017-07-18 | 安赛乐米塔尔公司 | 铝元件和具有ZnAlMg合金涂层的钢元件的组件 |
US11370279B2 (en) | 2013-05-13 | 2022-06-28 | Arcelormittal | Assembly of an aluminum component and of a steel component having a ZnAlMg alloy coating |
CN109563605A (zh) * | 2016-07-20 | 2019-04-02 | 塔塔钢铁艾默伊登有限责任公司 | 提供zn-al-mg涂层的方法以及这种涂层 |
CN109563605B (zh) * | 2016-07-20 | 2021-06-11 | 塔塔钢铁艾默伊登有限责任公司 | 提供zn-al-mg涂层的方法以及这种涂层 |
CN110857459A (zh) * | 2018-08-24 | 2020-03-03 | 金商昊 | 含镁热镀锌钢板的制造方法及制造装置 |
CN110857459B (zh) * | 2018-08-24 | 2022-04-12 | 株式会社M.E.C | 含镁热镀锌钢板的制造方法及制造装置 |
CN113195775A (zh) * | 2018-12-11 | 2021-07-30 | 株式会社 M.E.C | 用于制造熔融镀锌钢板的方法 |
CN113195775B (zh) * | 2018-12-11 | 2023-08-25 | 株式会社 M.E.C | 用于制造熔融镀锌钢板的方法 |
CN114375344A (zh) * | 2019-09-10 | 2022-04-19 | 安赛乐米塔尔公司 | 可移动溢流器 |
CN114375344B (zh) * | 2019-09-10 | 2023-09-19 | 安赛乐米塔尔公司 | 可移动溢流器 |
CN115612974A (zh) * | 2022-09-01 | 2023-01-17 | 中冶南方(武汉)热工有限公司 | 冷轧镀锌用带钢预氧化装置及其方法 |
Also Published As
Publication number | Publication date |
---|---|
KR101420486B1 (ko) | 2014-07-16 |
PL2430207T3 (pl) | 2017-07-31 |
KR20120028922A (ko) | 2012-03-23 |
BRPI1010794A2 (pt) | 2016-03-29 |
CA2761772A1 (en) | 2010-11-18 |
EP2430207B1 (fr) | 2017-01-11 |
ZA201108239B (en) | 2012-06-27 |
US20160002763A1 (en) | 2016-01-07 |
WO2010130890A1 (fr) | 2010-11-18 |
RU2501883C2 (ru) | 2013-12-20 |
CA2761772C (en) | 2013-09-03 |
HUE031389T2 (hu) | 2017-07-28 |
EP2430207A1 (fr) | 2012-03-21 |
WO2010130883A1 (fr) | 2010-11-18 |
JP2012526915A (ja) | 2012-11-01 |
MX2011012005A (es) | 2011-12-08 |
UA110094C2 (uk) | 2015-11-25 |
RU2011150823A (ru) | 2013-06-20 |
US20120107636A1 (en) | 2012-05-03 |
US11371128B2 (en) | 2022-06-28 |
MA33272B1 (fr) | 2012-05-02 |
RU2501883C9 (ru) | 2016-03-20 |
JP5669824B2 (ja) | 2015-02-18 |
US20190271066A1 (en) | 2019-09-05 |
CN102459683B (zh) | 2014-04-23 |
US9181614B2 (en) | 2015-11-10 |
US10344368B2 (en) | 2019-07-09 |
ES2620025T3 (es) | 2017-06-27 |
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