CN1839185A - 用于塑料透镜与装置的氟化高聚物低反射层 - Google Patents
用于塑料透镜与装置的氟化高聚物低反射层 Download PDFInfo
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Abstract
本发明开发了用于塑料基底的单层涂层体系。所述单涂层体系低反射层包括VF2/TFE/HFP、VF2/HFP、VF2/TFE/PMVE。
Description
技术领域
本发明涉及氟化高聚物涂层塑料。更具体地说,本发明涉及具有良好粘合、低反射性、以及拒水性和拒油性的氟化高聚物涂层塑料。
背景技术
已经进行了许多与低反射塑料、特别是用于塑料透镜和光学装置的反射塑料的研究工作。所用的一种方法是在塑料表面上氧化金属的蒸气化分布,然而,该方法使用批处理工艺,并且当基底较大时,生产率变低。另一种方法是施用氟化高聚物溶液的涂层。通过浸渍法形成涂层,并以高生产率应用于较大基底。尽管氟化高聚物具有低反射指数,但是它们与塑料基底的粘合非常差。很长时间以来一直在研究氟化高聚物和基底塑料之间的粘合。本发明的目的是提供使用氟化高聚物溶液以得到低反射指数和良好粘合的技术。
发明简述
本发明提供的单层涂层体系包括由下式表示的氟化共聚物:
VF2/TFE/HFP
其中四氟乙烯(TFE)与六氟丙烯(HFP)的摩尔比为0.1-1.9,并且VF2的含量为47-60摩尔%。优选VF2含量为50-60摩尔%。更优选其中TFE与HFP的摩尔比为0.9-1.9,并且对于聚甲基丙烯酸甲酯(PMMA)基底,VF2的含量优选为47-60摩尔%,对于聚碳酸酯(PC)、聚对苯二甲酸乙二醇酯(PET)、聚砜(PS)和玻璃基底,VF2的含量优选为47-50摩尔%。
还优选其中VF2含量大于50-60摩尔%;更优选其中基底为PMMA、PC、PET、PS或者玻璃。
本发明还提供了单层涂层体系,其包括由下式表示的氟化共聚物:
VF2/HFP,
其中VF2含量为约40-80%。优选地,VF2含量为约40-50摩尔%并且基底为PMMA。还优选VF2含量为约70-80摩尔%并且基底为玻璃。
本发明还提供了单层涂层体系,其包括由下式表示的氟化共聚物:
VF2/TFE/PMVE,
其中VF2含量为约18-60摩尔%并且TFE/PMVE的摩尔比为0.1-1.9。优选VF2含量为约30-35摩尔%,TFE/PMVE的摩尔比为约0.2-0.3并且基底是PMMA。
在本发明的单层涂层体系中,涂层厚度优选为约10-1000纳米,更优选为约30-120纳米,最优选为约70-120纳米。
发明详述
已经发现单层体系赋予在光学透明塑料基底上具有良好粘合的低反射涂层。优选的基底为PMMA、PC、PET和PS以及玻璃。
本发明提供的单层涂层体系包括由下式表示的氟化共聚物:
VF2/TFE/HFP,
其中TFE与HFP的摩尔比为0.1-1.9,并且VF2含量为47-60摩尔%,优选50-60摩尔%。这些组成平衡了低反射所需的高氟化量,光学透明度所需的高HFP含量,以及赋予与基底的良好粘合所需的足够的VF2含量。更优选其中TFE与HFP的摩尔比为0.9-1.9,并且对于PMMA基底,VF2含量优选为47-60摩尔%,对于PC、PET和玻璃基底,VF2含量优选为47-50摩尔%。
单层体系的另一个实施方案包括由下式表示的氟化共聚物:
VF2/HFP,
其中VF2为约40-80摩尔%。该体系基本上由两种单体组成,很少或未引入其他单体。优选地,VF2含量为约40-50摩尔%并且基底为PMMA。还优选VF2含量为约70-80摩尔%并且基底为玻璃。
单层涂层体系的另一个实施方案包括由下式表示的氟化共聚物:
VF2/TFE/PMVE,
其中VF2含量为约18-60摩尔%并且TFE/PMVE的摩尔比为0.1-1.9。优选VF2含量为约30-35摩尔%,TFE/PMVE的摩尔比为约0.2-0.3并且基底为PMMA。
在本发明的单层涂层体系中,涂层厚度需要大于约10纳米,以便观测到明显的反射减少。尽管厚度大于10纳米效果很好,当涂层更厚时,最终产生了实际问题。例如,大于约1000纳米,厚度变化可成为问题,并且如果涂层聚合物昂贵,则不经济。因此,在本发明的单层涂层体系中,涂层厚度优选为约10-1000纳米,更优选为约300-120纳米,最优选为约70-120纳米。
涂层可使用本领域已知的任何方法制备。用于制备涂层的适当的溶剂为那些溶解涂层组分但是对于被涂覆基底为惰性的溶剂。优选的溶剂包括氟化溶剂如Fluorinert(3M Electronic Materials.St.Paul,Minnesota),Vertrel(E.I.DuPont de Nemours,Wilmington,DE)或Novec(3M Electronic Materials,St.Paul,Minnesota),以及酮类溶剂如甲基异丁基酮或者丙酮、乙酸异丁酯,或者其两种或多种的组合。
可向上述任何或者全部组成中加入其他成分。除了上述组分外,本发明的组合物可含有通常用于合成聚合物中的添加剂,如着色剂、抗氧化剂、增韧剂、成核剂、紫外线稳定剂、热稳定剂、助剂、交联剂等等。这些成分各自通常以小于1%的比使用。
以下非限制性的例子仅用于说明本发明,而不以任何方式限制本发明。
材料和方法
以下定义用于本文并应用于解释权利要求。
APS-过硫酸铵
HFIB-六氟异丁烯,(CF3)2C=CH2
HFP-六氟丙烯,CF2=CF-CF3
PC-聚碳酸酯
PET-聚对苯二甲酸乙二醇酯
PMMA-聚甲基丙烯酸甲酯
PMVE-全氟甲基乙烯基醚
PVOH-聚乙烯醇
PS-聚砜
TeflonAF-TFE/全氟-2,2-二甲基间二氧杂环戊烯共聚物
TFE-四氟乙烯,CF2=CF2
VAc-醋酸乙烯酯,CH3-C(O)-OCH=CH2
VF-乙烯基氟,CH2=CHF
VF2-1,1-二氟乙烯,CF2=CH2
除非另有说明,使用以下试验方法:
测量透射率的方法
测量光透射的方法使用Shimadzu#_UV-3100分光计在500纳米进行测量。该机器测量部分穿过样品的***波束的持续比较。
粘合试验方法
使用配有间距为1mm的10个刀片的工具将涂层向下切割至塑料基底,先使刀片工具沿一个方向划割,然后再以垂直方向划割,切出100个画有交叉阴影线的正方形。用中等压力将透明胶带施用于交叉阴影线区域,并迅速地拉掉胶带。记录100个正方形中仍然粘合于基底的正方形数目用于评价粘合。
除非另外说明,所有的其它聚合物和单体在市场上可买到。
HFP含量超过30摩尔%的VF2/TFE/HFP三元共聚物和TFE/HFP二元共聚物以US专利5,478,905和5,637,663中所述方法在14,000psi和200-400℃条件下进行聚合可能是最容易制备的。具有较低HFP含量的VF2/TFE/HFP三元共聚物和TFE/HFP二元共聚物以及VF2/TFE/PMVE三元共聚物可通过本领域已知的常用乳液聚合法和本体聚合法制备,参见例如Encyclopedia of Polymer Science andEngineering,1989,Vol.16,第601-603页,和Vol.7,第257-269页,John Wiley & Sons。然后选择表现出良好的光学透明性和溶液易涂覆性的非结晶组合物用于本发明。
实施例
实施例1-9
比较例1-3
PMMA上的单涂层聚(VF2/TFE/HFP)
优选的厚度范围
通过将块状聚合物与溶剂在室温下搅拌数天制备2wt%的聚(VF2/TFE/HFP)在FluorinertFC-75中的溶液。使用2.5cm×5.0cm×3mm厚的PMMA板用于试验。将板以300mm/min的速率降入到聚合物溶液中然后在30秒后将板以2.5-1000mm/min的速率提升出溶液,在5-10分钟风干后,将板在100℃烘箱中以水平方向干燥60分钟,从而进行PMMA板的涂覆。实施例以涂层厚度增加的顺序示出。
表1
PMMA上的单层18.7/43.3/38.0摩尔%的聚(VF2/TFE/HFP)
厚度(纳米) | 透射率(%) | |
比较例#1比较例#2实施例#1实施例#2实施例#3实施例#4实施例#5实施例#6实施例#7实施例#8实施例#9比较例#3 | 未涂层PMMA对照5.020.070.676.390.2106.2133.3209.2394.7572.12000 | 92.192.894.596.797.798.096.693.294.695.294.4不均匀 |
未涂层PMMA表现92.1%的透射率。厚度大于20.0纳米并小于1000纳米的涂层相对于未涂层PMMA得到改进的透射率(>93%)。最大透射率(>96%)由厚度为~30-120纳米的涂层得到。
实施例10-13
比较例4-5
PMMA上的单层聚(VF2/TFE/HFP)
优选的VF2含量
根据实施例1-9制备聚合物膜。透射率和粘合的测量结果如下表2所示,该表2以VF2含量增加的顺序列出了实施例和比较例。
表2
通过标准带牵引试验测量的粘合
PMMA上的单层聚(VF2/TFE/HFP)
摩尔%VF2/TFE/HFP | 粘合(/100) | 透射率(%) | |
比较例#1比较例#4比较例#5实施例#10实施例#11实施例#12实施例#13 | 未涂层PMMA对照0/57/43对照7.8/60.3/31.812.6/51.3/36.118.7/43.3/38.025.2/42.9/31.937.4/28.9/33.7 | --0649699100100 | 92.197.297.597.297.995.196.0 |
相对于未涂层PMMA观察到含有12-50摩尔%VF2的VF2/TFE/HFP聚合物同时表现出良好的粘合(>96/100)和改进的透射率(>97%)。
实施例14
通过将块状聚合物与溶剂在室温下搅拌数天制备2wt%的聚(VF2/TFE/HFP=46.9/13.5/39.6摩尔%)在VertrelXF中的溶液。使用2.5cm×5.0cm×3mm厚的PMMA板用于试验。将板以300mm/min的速率降入到聚合物溶液中然后在30秒后将板以50mm/min的速率提升出溶液,在5-10分钟风干后,将板在100℃烘箱中以水平方向干燥60分钟,从而对PMMA板进行涂覆。透射率和粘合的测量结果在以下列出实施例的表中示出。
表3
PMMA上的单层46.9/13.5/39.6摩尔%的聚(VF2/TFE/HFP)
摩尔%VF2/TFE/HFP | 粘合(/100) | 透射率(%) | |
实施例#14B比较例#1 | 46.9/13.5/39.6未涂层PMMA对照 | 100-- | 97.492.1 |
相对于未涂层PMMA观察到含有VF2/TFE/HFP=46.9/13.5/39.6摩尔%的三元共聚物同时表现出良好的粘合(100/100)和改进的透射率(>97%)。
实施例15-17
比较例6-9
聚碳酸酯上的单层聚(VF2/TFE/HFP)
优选的VF2含量
使用实施例14的方法在聚碳酸酯(PC)片材上涂覆具有不同VF2含量的聚(VF2/TFE/HFP)三元共聚物。聚碳酸酯由Kyoto-Jushi SeikoCo.,Ltd.生产,聚碳酸酯片材的尺寸为2.5cm×5.0cm×3mm厚度。
透射率和粘合的测量结果如下表4所示,该表4以VF2含量增加的顺序列出了实施例和比较例。
表4
PC上的单层聚(VF2/TFE/HFP)
摩尔%VF2/TFE/HFP | 粘合(/100) | 透射率(%) | |
比较例#6比较例#7比较例#8比较例#9实施例#15实施例#16实施例#17 | 未涂层PC对照0/57/437.8/60.3/31.812.6/51.3/36.118.7/43.3/38.025.2/42.9/31.937.4/28.9/33.7 | --005370100100 | 87.295.290.594.794.092.093.8 |
相对于HFP/TFE共聚物的粘合(0/100),VF2含量为约18-40摩尔%得到了改进的粘合(>70/100),并且相对于未涂层PC的透射率(87.2%)得到了改进的透射率(>92%)。
实施例18
比较例10-11
PET上的单层聚(VF2/TFE/HFP)
根据实施例1-9制备涂层。尺寸为2.5×5.0cm×0.12mm厚度的PET片材用作基底。透射率和粘合的测量结果在以下列出实施例和比较例的表中示出。
表5
PET上的聚(VF2/TFE/HFP)层
摩尔%VF2/TFE/HFP | 粘合(/100) | 透射率(%) | |
比较例#15比较例#11实施例#18 | 00/57/4318.7/43.3/38.0 | --299 | 85.096.096.0 |
未涂层PET表现85.0%的透射率。相对于未涂层PET观察到同时表现出良好的粘合(>99/100)和改进的透射率(>96%)。
实施例19
比较例12-13
聚砜上的单层聚(VF2/TFE/HFP)
根据实施例1-9制备涂层,使用尺寸为2.5×5.0cm×0.05mm厚度的聚砜片材作为基底。透射率和粘合的测量结果在以下列出实施例和比较例的表中示出。
表6
聚砜上的单层聚(VF2/TFE/HFP)
摩尔%VF2/TFE/HFP | 粘合(/100) | 透射率(%) | |
比较例#12比较例#13实施例#19 | 未涂层PS0/57/4318.7/43.3/38.0 | --97100 | 88.598.295.0 |
未涂层聚砜表现88.5%的透射率。相对于未涂层聚砜(88.5%)观察到同时具有良好的粘合(>97/100)和改进的透射率(>95%)。
实施例20-26
比较例20-23
通过将块状聚合物与溶剂在室温下搅拌数天制备2.5wt%聚(VF2/TFE/HFP)在NovecHFE 7100(3M Electronic Materials,St.Paul,Minnesota)和聚(TFE/HFP)在Fluorinert(3MElectronic Materials,St.Paul,Minnesota)FC-75中的溶液。使用尺寸为2.5cm×5.0cm×3mm厚度的PMMA和PC板,尺寸为2.5cm×5.0cm×120微米厚度的PET薄膜和尺寸为2.5cm×5.0cm×1mm厚度的玻璃板用于试验。将板以300mm/min的速率降入到聚合物溶液中然后在30秒后将板以125mm/min的速率提升出溶液,在5-10分钟风干后,将板在烘箱中干燥10分钟,对于PMMA板,烘箱温度为100℃,对于PC板,温度为120℃,对于玻璃板,温度为300℃。PET薄膜在100℃烘箱中干燥60分钟。透射率、粘合和涂层厚度的测量结果如表7所示。
表7
实施例#20 | 实施例#21 | 实施例#22 | 实施例#23 | 实施例#24 | 实施例#25 | |
VF2(mol%) | 48 | 50 | 52 | 57 | 50 | 50 |
HFP(mol%) | 45 | 23 | 22 | 34 | 23 | 23 |
TFE(mol%) | 7 | 27 | 26 | 9 | 27 | 27 |
基底 | PMMA | PMMA | PMMA | PMMA | PC | PET |
厚度(nm) | 90 | 90 | 90 | 90 | 90 | 90 |
粘合(/100) | 100 | 100 | 100 | 100 | 100 | 100 |
透射率(%) | 97 | 98 | 97 | 97 | 95 | 97 |
实施例#26 | 比较例#20 | 比较例#21 | 比较例#22 | 比较例#23 | 比较例#24 | |
VF2(mol%) | 50 | - | - | - | - | 0 |
HFP(mol%) | 23 | - | - | - | - | 43 |
TFE(mol%) | 27 | - | - | - | - | 57 |
基底 | 玻璃 | PMMA | PC | PET | 玻璃 | PMMA |
厚度(nm) | 90 | 未涂层 | 未涂层 | 未涂层 | 未涂层 | 90 |
粘合(/100) | 100 | - | - | - | - | 0 |
透射率(%) | 96 | 92 | 87 | 90 | 90 | 97 |
相对于未涂层基底观察到含有40-60摩尔%VF2的VF2/TFE/HFP聚合物同时表现出良好的粘合(>96/100)和改进的透射率(>95%)。
实施例27-28
通过将块状聚合物与溶剂在室温下搅拌数天制备2.5wt%聚(VF2/HFP=43/57摩尔%)在VertrelXF(E.I.DuPont de Nemours,Wilmington,DE)和聚(VF2/HFP=78/22摩尔%)在MIBK中的溶液。使用尺寸为2.5cm×5.0cm×3mm厚度的PMMA板和尺寸为2.5cm×5.0cm×1mm厚度的玻璃板用于试验。根据实施例49-55制备厚度为90nm的聚合物膜,提升速率为200mm/分钟。透射率和粘合的测量结果如表8所示。
表8
实施例#27 | 实施例#28 | |
VF2(摩尔%)HFP(摩尔%)基底粘合(/100)透射率(%) | 4357PMMA10095 | 7822玻璃10095 |
相对于未涂层PMMA和玻璃观察到含有40-80摩尔%VF2的VF2/HFP聚合物同时表现出良好的粘合(>96/100)和改进的透射率(>95%)。
实施例29
通过将块状聚合物与溶剂在室温下搅拌数天制备3wt%聚(VF2/TFE/PMVE=32/15/53摩尔%)在NovecHFE-7200(3MElectronic Materials,St.Paul,Minnesota)中的溶液。使用尺寸为2.5cm×5.0cm×3mm厚度的PMMA板用于试验。根据实施例1-7制备聚合物膜,提升速率为75mm/min。透射率和粘合的测量结果如表9所示。
表9
实施例#28 | |
VF2(摩尔%)TFE(摩尔%)PMVE(摩尔%)基底粘合(/100)透射率(%) | 321553PMMA10098 |
相对于未涂层PMMA观察到同时具有良好的粘合(>96/100)和改进的透射率(>95%)。
Claims (16)
1.用于涂覆基底的单层涂层体系,包括由下式表示的氟化共聚物:
VF2/TFE/HFP,
其中TFE与HFP的摩尔比为0.1-1.9并且VF2含量为47-60%。
2.权利要求1所述的涂层体系,其中VF2含量大于50-60摩尔%。
3.权利要求2所述的涂层体系,其中基底选自PMMA、PC、PET、PS和玻璃。
4.权利要求1所述的涂层体系,其中VF2含量为47-60摩尔%,TFE与HFP的摩尔比为0.1-1.9,并且基底为PMMA。
5.权利要求1所述的涂层体系,其中VF2含量为47-50摩尔%,TFE与HFP的摩尔比为0.9-1.9,并且基底选自PET、PC和玻璃。
6.权利要求1所述的涂层,其中涂层厚度为10纳米-1000纳米。
7.权利要求6所述的涂层,其中涂层厚度为70纳米-120纳米。
8.用于涂覆基底的单层涂层体系,基本上含有由下式表示的氟化共聚物:
VF2/HFP
其中VF2含量为约40-80%。
9.权利要求8所述的涂层体系,其中VF2含量为约40-50%并且基底为PMMA。
10.权利要求8所述的涂层体系,其中VF2含量为约70-80%并且基底为玻璃。
11.权利要求8所述的涂层,其中涂层厚度为10纳米-1000纳米。
12.权利要求11所述的涂层,其中涂层厚度为70纳米-120纳米。
13.用于涂覆基底的单层涂层体系,包括由下式表示的氟化共聚物:
VF2/TFE/PMVE,
其中VF2含量为约18-60摩尔%并且TFE/PMVE的摩尔比为约0.1-1.9。
14.权利要求13所述的涂层体系,其中VF2含量为约30-35摩尔%,TFE/PMVE的摩尔比为约0.2-0.3并且基底为PMMA。
15.权利要求13所述的涂层,其中涂层厚度为10纳米-1000纳米。
16.权利要求15所述的涂层,其中涂层厚度为70纳米-120纳米。
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JP5557373B2 (ja) * | 2006-11-21 | 2014-07-23 | アボット ラボラトリーズ | 薬剤溶出性コーティングにおけるテトラフルオロエチレン、ヘキサフルオロプロピレン、及びフッ化ビニリデンのターポリマーの使用 |
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GB871582A (en) * | 1957-08-21 | 1961-06-28 | Du Pont | Improvements in or relating to elastomer-coated fabrics |
US3023187A (en) * | 1958-04-02 | 1962-02-27 | Minnesota Mining & Mfg | Process of copolymerizing hexafluoropropene with vinylidene fluoride in the presenceof silica and the product thereof |
US3235537A (en) * | 1961-06-23 | 1966-02-15 | Du Pont | Fluorine containing terpolymer of a perfluorovinyl ether, vinylidene fluoride and a monomer of the structure cfx=cfy |
FR1350581A (fr) * | 1962-03-22 | 1964-01-24 | Du Pont | Feuilles et autres articles comportant un revêtement d'un copolymère de fluorure de vinylidène et d'hexafluoropropylène |
US3194796A (en) * | 1962-03-22 | 1965-07-13 | Du Pont | Elastomeric fluorocarbon terpolymers of vinylidene fluoride, hexafluoropropylene and a halogen free polar monomer |
CA964786A (en) * | 1971-07-05 | 1975-03-18 | Teijin Limited | Liquid coating composition containing vinyl fluoride-hexafluoropropylene resin |
US4123603A (en) * | 1977-05-31 | 1978-10-31 | E. I. Du Pont De Nemours And Company | Fluoroelastomer composition |
DE2861181D1 (en) * | 1977-12-27 | 1981-12-24 | Hoechst Ag | Fluorised thermoplastic polymer |
DE2906787A1 (de) * | 1979-02-22 | 1980-09-04 | Hoechst Ag | Ueberzugsmittel auf basis eines copolymeren aus tetrafluorethylen und einem perfluor(alkylvinyl)-ether |
US4335238A (en) * | 1980-10-06 | 1982-06-15 | E. I. Du Pont De Nemours And Company | Fluoropolymer hexafluoropropene, tetrafluorethene and 1,1-difluoroethene |
DE3366454D1 (en) * | 1982-07-20 | 1986-10-30 | Hoechst Ag | Primer for coatings containing fluorocarbon polymers with an amount of poly(arylene sulfide) resin, aromatic polyether sulfone resin or aromatic polyether ketone resin, and use thereof |
DE3227045A1 (de) * | 1982-07-20 | 1984-01-26 | Hoechst Ag, 6230 Frankfurt | Grundierungsmittel mit einem gehalt an aromatischem polyetherketon-harz fuer ueberzuege aus fluorkohlenstoffpolymeren |
IT1207493B (it) * | 1985-02-22 | 1989-05-25 | Montefuols S P A E Franco Piac | Procedimento per la protezione ed il consolidamento di materiali lapidei |
JPH02115253A (ja) * | 1988-10-25 | 1990-04-27 | Daikin Ind Ltd | 電子部品用防湿コーティング材 |
IT1264125B1 (it) * | 1993-03-30 | 1996-09-16 | Ausimont Spa | Fluoroelastomeri dotati di elevata resistenza ai solventi polari ed alle basi |
USH1483H (en) * | 1993-05-24 | 1995-09-05 | Larson; James R. | Liquid developer compositions |
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JPH10274716A (ja) * | 1997-03-31 | 1998-10-13 | Toray Ind Inc | 高開口数プラスチック光ファイバ |
US6169139B1 (en) * | 1998-04-27 | 2001-01-02 | Dupont Dow Elastomers Llc | Fluoroelastomer latex |
JP4758004B2 (ja) * | 1999-03-16 | 2011-08-24 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | プラスチックレンズ用およびデバイス用低反射フルオロポリマー層 |
DE19924439A1 (de) * | 1999-05-28 | 2000-11-30 | Bayer Ag | Schnell vernetzendes Fluorpolymer |
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JP2003004904A (ja) * | 2001-06-25 | 2003-01-08 | Dainippon Printing Co Ltd | 高屈折率化した防眩層を有する反射防止フィルム及び低反射表示装置 |
US7098270B2 (en) * | 2002-09-10 | 2006-08-29 | Freudenberg-Nok General Partnership | Fluoroelastomer composition |
US7056578B2 (en) * | 2002-11-13 | 2006-06-06 | Eastman Kodak Company | Layer comprising nonfibrillatable and autoadhesive plastic particles, and method of preparation |
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- 2003-10-07 AU AU2003277336A patent/AU2003277336A1/en not_active Abandoned
- 2003-10-07 DE DE60326779T patent/DE60326779D1/de not_active Expired - Fee Related
- 2003-10-07 JP JP2005510496A patent/JP5027415B2/ja not_active Expired - Lifetime
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EP1687383B1 (en) | 2009-03-18 |
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JP2007521352A (ja) | 2007-08-02 |
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