CN106660012B - 光催化剂功能性膜及其制备方法 - Google Patents
光催化剂功能性膜及其制备方法 Download PDFInfo
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- CN106660012B CN106660012B CN201580042104.1A CN201580042104A CN106660012B CN 106660012 B CN106660012 B CN 106660012B CN 201580042104 A CN201580042104 A CN 201580042104A CN 106660012 B CN106660012 B CN 106660012B
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Abstract
本发明提供光催化剂功能性膜,上述光催化剂功能性膜为基材层、阻隔层及光催化剂层的层叠结构,上述阻隔层为非结晶性TiO2膜,上述光催化剂层包含非结晶性TiO2膜以及形成于上述非结晶性TiO2膜的表面的可见光活性光催化剂粒子。本发明提供光催化剂功能性膜的制备方法,上述光催化剂功能性膜的制备方法包括如下的步骤:在钛前体中加入醇溶剂及酸,并通过脱水及脱醇反应取得TiO2溶胶的步骤;在基材上涂敷上述TiO2非结晶性溶胶并对上述TiO2非结晶性溶胶进行干燥来形成阻隔层的步骤;以及在上述阻隔层上涂敷如下的组合物并对上述组合物进行干燥来形成光催化剂层的步骤,上述组合物通过在上述TiO2非结晶性溶胶中混合可见光活性光催化剂粒子而成。
Description
技术领域
本发明涉及光催化剂功能性膜及其制备方法。
背景技术
可将使室内空气质量(IAQ,Indoor Air Quality)变得舒适的光催化剂涂敷于室内装饰装修材料的表面来使用。为了涂敷光催化剂,而必须使用使光催化剂附着于基材的粘结剂。但是,在与光催化剂结合的过程中,粘结剂覆盖光催化剂的表面,由此产生使光催化剂的表面露出面积减少的问题。由此,当使用粘结剂时,因粘结剂而降低基于表面反应的光催化剂的性能。
发明内容
本发明要解决的技术问题
本发明的一实例提供如下的光催化剂功能性膜,即,上述光催化剂功能性膜使用不降低光催化剂的效率的粘结剂,并且包含阻隔层。
技术方案
在本发明的一实例提供如下的光催化剂功能性膜,即,上述光催化剂功能性膜为基材层、阻隔层及光催化剂层的层叠结构,上述阻隔层为非结晶性TiO2膜,上述光催化剂层包含非结晶性TiO2膜以及形成于上述非结晶性TiO2膜的表面的可见光活性光催化剂粒子。
上述非结晶性TiO2膜气孔度可以为约5%至约50%。
上述非结晶性TiO2膜的比表面积可以为约5m2/g至约500m2/g。
上述非结晶性TiO2膜可由TiO2非结晶性溶胶形成。
上述可见光活性光催化剂粒子可以为包含孔隙的、浸渍可见光活性赋予金属的多孔性金属氧化物粒子。
上述多孔性金属氧化物粒子可包含选自氧化钛、氧化钨、氧化锌、氧化铌及它们的组合中的至少一种。
含选自钨、铬、钒、钼、铜、铁、钴、锰、镍、铂、金、铈、镉、锌、镁、钙、锶、钡、镭及它们的组合中的至少一种金属的上述可见光活性赋予金属可浸渍于多孔性金属氧化物粒子,或者上述可见光活性赋予金属可以上述金属的氧化物形态浸渍于多孔性金属氧化物粒子。
在上述可见光活性光催化剂粒子中,多孔性金属氧化物与可见光活性赋予金属和可见光活性赋予金属氧化物之和的重量比可以为约99.9:0.1至约99:1。
上述阻隔层的厚度可以为约20nm至约500nm。
上述光催化剂层的厚度可以为约50nm至约500nm。
上述基材可以为室内装饰装修材料。
在本发明的另一实例中提供如下的光催化剂功能性膜的制备方法,即,上述光催化剂功能性膜的制备方法包括如下的步骤:在钛前体中加入醇溶剂及酸,并通过脱水及脱醇反应取得TiO2非结晶性溶胶的步骤;在基材上涂敷上述TiO2溶胶并对上述TiO2非结晶性溶胶进行干燥来形成阻隔层的步骤;以及在上述阻隔层上涂敷如下的组合物并对上述组合物进行干燥来形成光催化剂层的步骤,上述组合物通过在上述TiO2非结晶性溶胶中混合可见光活性光催化剂粒子而形。
上述醇溶剂可以为选自由异丙醇、乙醇、甲醇、丁醇及它们的组合组成的组中的至少一种。
相对于100重量份的可见光活性光催化剂粒子,上述组合物可包含约20至约100重量份的上述TiO2非结晶性溶胶。
有益效果
上述光催化剂功能性膜可响应于可见光来实现室内的空气净化、除臭及抗菌效果。
可通过使用上述光催化剂功能性膜的制备方法来提供维持高效率的光催化剂性能且解决基材的分解问题的光催化剂功能性膜。
附图说明
图1为以图示化的方式示出作为本发明一实例的光催化剂功能性膜的截面。
具体实施方式
以下,详细说明本发明的实例。但下述实施例仅仅是以例示提出的,本发明并不受其限制,并且本发明由发明要求保护范围的范畴来定义。
光催化剂功能性膜
在本发明的一实例提供如下的光催化剂功能性膜,即,上述光催化剂功能性膜为基材层、阻隔层及光催化剂层的层叠结构,上述阻隔层为非结晶性TiO2膜,上述光催化剂层包含非结晶性TiO2膜以及形成于上述非结晶性TiO2膜的表面的可见光活性光催化剂粒子。
通常,为了将可见光光催化剂涂敷于室内装饰装修材料的表面,而需要用于附着可见光光催化剂的粘结剂物质,例如硅溶胶等。
但是,在使粘结剂物质与可见光光催化剂相结合的过程中,由于粘结剂物质覆盖可见光光催化剂的表面,从而产生使上述光催化剂表面的露出面积减少的问题。在上述情况下,存在对粘结剂物质实现表面反应的上述光催化剂的光催化剂性能降低的问题。
并且,将上述光催化剂直接涂敷于由有机物形成的基材来使用的情况下,可通过上述光催化剂的有机物分解反应来分解基材,在上述情况下,存在可降低基材的稳定性且因基材的分解而产生有害物质的问题。
为此,开发了不降低光催化剂的效率且赋予附着力的粘结剂物质,可将TiO2非结晶性溶胶用作上述粘结剂物质。
将上述TiO2非结晶性溶胶作为粘结剂物质来形成光催化剂层时,上述TiO2非结晶性溶胶可通过抑制可见光活性光催化剂粒子的光活性能力的降低来最大程度地维持粒子状态的光活性性能。
并且,为了防止因光催化剂而引起的基材的分解,通过在基材与光催化剂层之间形成阻隔层来阻隔光催化剂和基材的接触。
上述阻隔层作为非结晶性TiO2膜,可由上述TiO2非结晶性溶胶形成。
图1为以图示化的方式示出作为本发明的一实例的光催化剂功能性膜的截面,参照图1,上述光催化剂功能性膜100可以为基材10、阻隔层20、光催化剂层30的层叠结构。
上述基材10可以为室内装饰装修材料。上述装修材料包括玻璃、壁纸、瓷砖膜等,上述光催化剂层30可因流入室内的光而被光活化,从而产生有机物分解反应,由此可提供空气净化、除臭及抗菌效果。
上述阻隔层20可以为非结晶性TiO2膜。在基材10及光催化剂层30之间包括作为非结晶性TiO2膜的阻隔层20,可通过防止基材和光催化剂层的接触来防止因光催化剂层的光催化剂而引起的基材层的腐蚀现象,并且由于可抑制因基材层的腐蚀而产生的有害物质的产生,因此即使时间流逝也可维持基材的稳定性。
上述光催化剂层30可包含非结晶性TiO2膜以及形成于上述非结晶性TiO2膜的表面的可见光活性光催化剂粒子。为了使上述可见光活性光催化剂粒子附着于上述阻隔层20,而需要粘结剂物质,将TiO2非结晶性溶胶作为粘结剂物质来形成的TiO2膜作为与阻隔层相同的物质,可提高附着力且不降低上述光催化剂粒子的光效率。
上述非结晶性TiO2膜的气孔度可以为约5%至约50%。上述非结晶性TiO2膜作为多孔性膜,可具有上述范围的气孔度,此时,可更加提高上述可见光活性光催化剂粒子的针对可见光的催化活性效率。
相反地,在上述非结晶性TiO2膜不具有气孔度且通过溅射法等精细地形成的情况下,未有效地实现甲醛等的反应物的吸附,从而难以期待优秀的光催化活性。
上述非结晶性TiO2膜的比表面积可以为约5m2/g至约500m2/g。由于上述非结晶性TiO2膜具有上述范围的比表面积,从而上述可见光活性光催化剂粒子对可见光的催化活性可更优秀。
上述非结晶性TiO2膜可由上述TiO2非结晶性溶胶形成。上述TiO2非结晶性溶胶的附着力优秀,并且有利于确保将上述TiO2非结晶性溶胶用作粘结剂来形成的光催化剂层30的透明性。
如后述的制备方法,上述TiO2非结晶性溶胶以非结晶的状态使用。由于以未结晶化的状态使用上述TiO2非结晶性溶胶,因此TiO2粒子的大小小于结晶化的情况,由此可实现透明化。完成结晶化的TiO2溶胶处于已维持规定结合的状态,从而表面积小且官能团的含量变低,相反地,与上述完成结晶化的TiO2溶胶相比,上述TiO2非结晶性溶胶的表面积变大且官能团含量变高,从而附着力优秀。
并且,上述TiO2非结晶性溶胶可利用通过使用醇类溶剂来进行脱水及脱醇反应的溶胶凝胶法制备,而不是使用水来进行脱水及脱醇反应。在以下叙述具体的制备方法。
上述光催化剂层30包含形成于上述非结晶性TiO2膜的表面的可见光活性光催化剂粒子,上述可见光活性光催化剂粒子可以为包含孔隙的、浸渍可见光活性赋予金属的多孔性金属氧化物粒子。
上述多孔性金属氧化物粒子可包含选自氧化钛、氧化钨、氧化锌、氧化铌及它们的组合中的至少一种,作为可用作光催化剂的金属氧化物,可无限制地使用已公知的物质。上述多孔性金属氧化物粒子主要对紫外线具有光活性。
只要是可向上述金属氧化物赋予对可见光的光活性的金属,上述可见光活性赋予金属可无限制地使用,具体地,例如,上述可见光活性赋予金属可以为过渡金属、贵金属等。
例如,上述可见光活性赋予金属可包含选自钨、铬、钒、钼、铜、铁、钴、锰、镍、铂、金、铈、镉、锌、镁、钙、锶、钡、镭及它们的组合中的至少一种金属。
并且,上述可见光活性赋予金属能够以上述金属的氧化物形态浸渍于多孔性金属氧化物粒子。
可向上述多孔性金属氧化物粒子内的孔隙掺杂上述可见光活性赋予金属粒子,从而上述可见光活性光催化剂粒子形成于上述非结晶性TiO2膜的表面,如此形成的上述光催化剂层30可具有对可见光的光活性。
由于上述可见光活性光催化剂粒子包含对可见光具有光活性的可见光活性赋予金属粒子,因此不仅可对紫外线具有活性,还可对可见光具有活性,并且可在整个可见光区域吸收光。例如,上述粒子可对380nm至780nm波长范围的可见光具有光活性。
上述可见光活性光催化剂粒子可使通过吸收光来获得的能量中生成的电子和空穴生成超氧化物负离子或羟基自由基等,从而可起到空气净化、除臭、抗菌作用。例如,从上述粒子生成的超氧化物负离子或羟基自由基可分解甲醛等对环境有害的物质。另一方面,由于上述粒子对可见光具有高吸收率,可在室内光源下也呈现优秀的效率,因此无须额外的紫外线供给装置。
在上述可见光活性光催化剂粒子中,上述多孔性金属氧化物与可见光活性赋予金属和可见光活性赋予金属氧化物之和的重量比可以为约99.9:0.1至约99:1。
上述阻隔层的厚度可以为约20nm至约500nm。上述阻隔层作为用于防止上述基材和光催化剂层的相接触的层,可通过保持上述范围的厚度来防止因光催化剂而产生的基材层的分解。并且,在上述阻隔层的厚度小于约20nm的情况下,由于未充分地形成非结晶性TiO2膜,从而无法充分地提供与基材的分离,在大于约500nm的情况下,在费用方面不经济。
上述光催化剂层的厚度可以为约50nm至约500nm。上述光催化剂层包含非结晶性TiO2膜及可见光活性光催化剂粒子,上述非结晶性TiO2膜将TiO2非结晶性溶胶作为粘结剂物质来形成,并且由于不降低上述粒子的光催化剂效率且增加与阻隔层的粘结力,从而可提供稳定的光催化剂功能性膜。
此时,可通过使上述光催化剂层的厚度维持上述范围来容易地实现光催化效果,在上述光催化剂层的厚度小于约50nm的情况下,由于未完整地形成光催化剂层,从而无法提供充分的光催化效果,在大于约500nm的情况下,可存在不参与光催化反应的部分,从而不利于费用及效率方面。
光催化剂功能性膜的制备方法
在本发明的另一实例提供如下的光催化剂功能性膜的制备方法,即,上述光催化剂功能性膜的制备方法包括如下的步骤:在钛前体中加入醇溶剂及酸,并通过脱水及脱醇反应取得TiO2非结晶性溶胶的步骤;在基材上涂敷上述TiO2非结晶性溶胶并对上述TiO2非结晶性溶胶进行干燥来形成阻隔层的步骤;以及在上述阻隔层上涂敷如下的组合物并对上述组合物进行干燥来形成光催化剂层的步骤,上述组合物通过在上述TiO2非结晶性溶胶中混合可见光活性光催化剂粒子而成。
上述光催化剂功能性膜的制备方法可包括在钛前体中加入醇溶剂及酸并通过脱水及脱醇反应取得TiO2非结晶性溶胶的步骤。
上述TiO2溶胶可利用溶胶凝胶法来获得,具体地,可在钛前体中加入醇溶液,将酸作为催化剂使用,并通过水解反应进行脱水及脱醇,从而取得TiO2非结晶性溶胶。在上述溶胶凝胶法不使用额外的水,但能够以混合在酸的溶液形态添加,由此进行水解,另一方面,还可以产生因酸而使醇盐前体的羟基被取代为OH基的水解反应。
上述钛前体可使用可利用于溶胶凝胶法的钛醇盐等已公知的化合物,具体地,可使用四异丙醇钛、四乙醇钛、四丁醇钛等。
上述醇溶剂可以为选自由异丙醇、乙醇、甲醇、丁醇及它们的组合组成的组中的至少一种。
上述酸作为用于使钛前体和醇发生脱水及脱醇反应的催化剂,可使用硝酸、盐酸等的强酸。
所获得的上述TiO2非结晶性溶胶可以为使非结晶性的TiO2粒子以胶质状态分散的溶液。
可在基材上涂敷所获得的上述TiO2非结晶性溶胶并对上述TiO2非结晶性溶胶进行干燥来形成阻隔层。
并且,可在上述阻隔层上涂敷如下的组合物并对上述组合物进行干燥来形成光催化剂层,上述组合物通过在上述TiO2非结晶性溶胶中混合可见光活性光催化剂粒子而成。
可通过在所获得的上述TiO2非结晶性溶胶中混合额外准备的可见光活性光催化剂粒子来制备用于形成光催化剂层的组合物。
例如,可通过如下的方法制备上述可见光活性光催化剂粒子,即,首先,在准备多孔性金属氧化物粒子后,通过将上述多孔性金属氧化物粒子浸渍于可见光活性赋予金属的前体溶液,来使可见光活性赋予金属以离子状态向多孔性金属氧化物粒子的内部渗透,然后使可见光活性赋予金属的离子通过还原成可见光活性赋予金属来浸渍于多孔性金属氧化物粒子的内部。
对上述可见光活性光催化剂粒子的详细说明如上所述。
在一实例中,上述可见光活性光催化剂粒子可以为浸渍有Pt金属的WO3的多孔性粒子。
相对于100重量份的可见光活性光催化剂粒子,上述组合物可包含约20至约100重量份的上述TiO2非结晶性溶胶。按上述含量比使用TiO2非结晶性溶胶,从而可取得基于因TiO2非结晶性溶胶的小的TiO2粒子而引起的大表面积的适当的表面结合。相反地,若TiO2非结晶性溶胶的含量过高,则可能覆盖可见光活性光催化剂粒子的表面,从而降低反应性。
可通过使用上述光催化剂功能性膜的制备方法来制备维持高效率的光催化剂性能且解决基材的分解问题的光催化剂功能性膜。
以下,提出本发明的具体实施例。只是,以下记载的实施例只不过是为了具体地例示本发明或说明本发明,本发明并不局限于此。
实施例及比较例
实施例1
将异丙醇作为溶剂来制备10重量百分比的四异丙醇钛溶液。将上述溶液搅拌30分钟后,添加少量的浓硝酸来进行水解。然后通过30分钟的搅拌来进行脱水、脱醇,从而制备了TiO2溶胶。
在聚对苯二甲酸乙二醇酯(PET)膜上以100nm的厚度涂敷上述非结晶性TiO2溶胶,并在常温条件下进行干燥来形成阻隔层。
额外准备了浸渍有Pt的WO3光催化剂粒子。
通过混合50重量份的上述非结晶性TiO2溶胶及100重量份的浸渍有Pt的WO3光催化剂来制备组合物,利用刮棒(Bar)涂布机以100nm的厚度将上述组合物涂敷于上述阻隔层,并在常温条件下进行干燥来形成光催化剂层,由此制备光催化剂功能性膜。
比较例1
除了在基材上形成阻隔层之外,以与上述实施例1相同的方法制备光催化剂功能性膜。
比较例2
将蒸馏水作为溶剂制备10重量百分比的四异丙醇钛溶液后,对上述溶液进行搅拌,从而形成均匀的沉淀物。然后添加充分量的作为酸催化剂的硝酸,并通过缩聚反应取得透明的溶胶。在80℃温度下将上述溶胶搅拌8小时以上来制备不透明的结晶性TiO2溶胶。
在聚对苯二甲酸乙二醇酯膜上以100nm的厚度涂敷上述结晶性TiO2溶胶,并在常温条件下进行干燥来形成阻隔层。
额外准备了浸渍有Pt的WO3光催化剂粒子。
通过混合50重量份的上述结晶性TiO2溶胶及100重量份的浸渍有Pt的WO3光催化剂来制备可见光活性光催化剂涂敷组合物。
利用刮棒(Bar)涂布机以100nm的厚度将上述可见光活性光催化剂涂敷组合物涂敷于上述阻隔层,并在常温条件下进行干燥来形成可见光活性催化剂层。
实验例
对实施例1及比较例1~比较例2的光催化剂层进行了针对甲醛去除性能的评价。将在实施例1及比较例1~比较例2中制备的光催化剂层设置于20L的小型腔室(ADTEC公司产品)后,以167cc/分钟的流量持续释放具有0.08ppm的甲醛浓度的净化空气,从而使换气次数成为0.5次/小时。作为光源使用10W的白色荧光灯,并且将照度设定为1000lux。通过检测进入腔室前的浓度和进入腔室后的浓度来计算出甲醛去除率后,将其结果记载于下述表1。分析浓度的方法如下,即,利用2,4-二硝基苯肼(DNPH,2,4-dinitrophenylhydrazine)采样管来浓缩针对10L的量,并利用高性能高效液相色谱法(HPLC,安捷伦科技公司(Agilent)产品)进行分析。
并且,用肉眼判断在实施例1及比较例1~比较例2制备的聚对苯二甲酸乙二醇酯膜是否受损,并记载于下述表1。
表1
从表1可知,即使在实施例1中形成光催化剂层后,上述可见光活性光催化剂粒子也呈现与粒子状态类似的光效率,但是在比较例1、2中,在形成光催化剂层后,光效率显著低于处于粒子状态的情况。
具体地,在上述比较例1的情况下,确认到由于因与基材层的接触而产生副反应,而无法去除腔室内的甲醛。
另一方面,确认如下:借助非结晶性TiO2溶胶在基材层与光催化剂层之间额外地包含阻隔层的实施例1、比较例2的聚对苯二甲酸乙二醇酯膜未受损,但未包括阻隔层的比较例1的聚对苯二甲酸乙二醇酯膜受损。
由此可知,实施例1提供将非结晶性TiO2溶胶用作粘结剂物质来形成的光催化剂层,并且上述光催化剂层的光效率优秀且可通过阻隔层抑制与基材层的副反应。
附图标记的说明:
100:光催化剂功能性膜
10:基材 20:阻隔层 30:光催化剂层
Claims (12)
1.一种光催化剂功能性膜,其特征在于,
上述光催化剂功能性膜为基材层、阻隔层及光催化剂层的层叠结构,
上述阻隔层为非结晶性TiO2膜,
上述光催化剂层包含非结晶性TiO2膜以及形成于上述非结晶性TiO2膜的表面的可见光活性光催化剂粒子;
其中,
i)上述光催化剂层是包含可见光活性光催化剂粒子的非结晶性TiO2膜;
ii)上述可见光活性光催化剂粒子是载有可见光活性赋予金属的多孔性金属氧化物粒子;
iii)上述阻隔层的厚度为20nm至500nm。
2.根据权利要求1所述的光催化剂功能性膜,其特征在于,上述非结晶性TiO2膜的气孔度为5%至50%。
3.根据权利要求1所述的光催化剂功能性膜,其特征在于,上述非结晶性TiO2膜的比表面积为5m2/g至500m2/g。
4.根据权利要求1所述的光催化剂功能性膜,其特征在于,上述非结晶性TiO2膜是在室温下TiO2非结晶性溶胶的干燥材料。
5.根据权利要求1所述的光催化剂功能性膜,其特征在于,上述多孔性金属氧化物粒子包含选自氧化钛、氧化钨、氧化锌、氧化铌及它们的组合中的至少一种。
6.根据权利要求1所述的光催化剂功能性膜,其特征在于,包含选自钨、铬、钒、钼、铜、铁、钴、锰、镍、铂、金、铈、镉、锌、镁、钙、锶、钡、镭及它们的组合中的至少一种金属的上述可见光活性赋予金属浸渍于多孔性金属氧化物粒子,或者上述可见光活性赋予金属以上述金属的氧化物形态浸渍于多孔性金属氧化物粒子。
7.根据权利要求1所述的光催化剂功能性膜,其特征在于,在上述可见光活性光催化剂粒子中,多孔性金属氧化物与可见光活性赋予金属和可见光活性赋予金属氧化物之和的重量比为99.9:0.1至99:1。
8.根据权利要求1所述的光催化剂功能性膜,其特征在于,上述光催化剂层的厚度为50nm至500nm。
9.根据权利要求1所述的光催化剂功能性膜,其特征在于,上述基材为室内装饰装修材料。
10.一种光催化剂功能性膜的制备方法,其特征在于,包括如下的步骤:
在钛前体中加入醇溶剂及酸,并通过脱水及脱醇反应取得TiO2非结晶性溶胶的步骤;
在基材上涂敷上述TiO2非结晶性溶胶并对上述TiO2非结晶性溶胶进行干燥来形成阻隔层的步骤;以及
在上述阻隔层上涂敷如下的组合物并对上述组合物进行干燥来形成光催化剂层的步骤,上述组合物通过在上述TiO2非结晶性溶胶中混合可见光活性光催化剂粒子而成;
其中,
i)在形成阻隔层的步骤和形成光催化剂层的步骤中的干燥是在室温下进行;
ii)所述可见光活性光催化剂粒子是载有可见光活性赋予金属的多孔性金属氧化物粒子;
iii)所述阻隔层的厚度为20nm至500nm。
11.根据权利要求10所述的光催化剂功能性膜的制备方法,其特征在于,上述醇溶剂为选自由异丙醇、乙醇、甲醇、丁醇及它们的组合组成的组中的至少一种。
12.根据权利要求10所述的光催化剂功能性膜的制备方法,其特征在于,相对于100重量份的可见光活性光催化剂粒子,上述组合物包含20至100重量份的上述TiO2非结晶性溶胶。
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- 2015-07-31 CN CN201580042104.1A patent/CN106660012B/zh not_active Expired - Fee Related
- 2015-07-31 EP EP15829364.7A patent/EP3178551A4/en not_active Withdrawn
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JP2017523913A (ja) | 2017-08-24 |
US20170216818A1 (en) | 2017-08-03 |
KR20160017829A (ko) | 2016-02-17 |
KR101891369B1 (ko) | 2018-08-27 |
JP6352527B2 (ja) | 2018-07-04 |
WO2016021888A1 (ko) | 2016-02-11 |
US10220372B2 (en) | 2019-03-05 |
CN106660012A (zh) | 2017-05-10 |
EP3178551A4 (en) | 2017-08-16 |
EP3178551A1 (en) | 2017-06-14 |
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