CN1730717A - 制备不透气层的设备和方法 - Google Patents
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Abstract
本发明涉及制备不透气层的设备和方法,特别涉及制备不透气合成材料基材涂层的设备和方法。使用所述设备或所述方法,仅用一种溅射设备即可制备可透光的以及不可透光的气体阻挡层。并可进行从一种供气如氩气到第二种供气如氩气、氧气和氮气的简单转换,或进行相反的转换过程。
Description
本发明涉及根据权利要求1和8前序部分制备透明不透气涂层的设备和方法。
通常,合成容器不是完全不漏气的,这对盛放含气饮料(如含碳酸的柠檬水或啤酒)的容器有副作用,其中的碳酸通过扩散逐渐从容器中溢出,因为容器中二氧化碳浓度比容器外高。例如,若PET瓶(PET是指聚对苯二甲酸乙二醇酯)仅用二氧化碳填充,扩散过程将会在瓶内和瓶外混合气体的浓度达到相同时停止。因为不仅仅二氧化碳从瓶中溢出,而且氧气和氮气也会扩散到瓶子中,经过足够长的时间,瓶子将会被充满与环境空气中成分相同的气体混合物。若瓶子填充有过量的CO2气体,扩散过程结束时瓶内的CO2将变得稀薄,并且外部的气压将会压迫瓶子。为了防止碳酸或水蒸气从瓶中溢出以及防止氧气进入瓶中,合成瓶子具有气体阻挡层。
但是,这些气体阻挡层通常因被覆盖的容器膨胀或收缩而产生裂纹。
已知合成瓶体的层系统包括直接涂覆在合成瓶体上的丙烯酸脂层。在该丙烯酸酯层上涂覆不透气材料层,再轮流在该不透气材料层上涂覆丙烯酸脂层(US 6 231 939)。使用不透气材料嵌入其中的两层丙烯酸脂层,所有涂层需要具有一定的弹性。作为不透气金属使用二氧化硅、氧化铝或金属。
但是这些方法的不足在于不透气层相对较厚,若其中含有金属,则不透明或相对无弹性。
本发明解决的问题是使用溅射设备将透明的不透气性涂层涂覆到合成材料基材上,并用相同的溅射设备制备反射阻挡层。
该问题可用本发明权利要求1和8的特征部分得到解决。
因此本发明涉及制备不透气层制品的设备和方法,特别涉及制备不透气性合成基材涂层的设备和方法。利用该设备或该方法仅使用一套溅射装置便可制得不透光和不透气的气体阻挡层。在该方法中发生从一种供气(例如氩气)到另一种供气(例如氩气、氧气和氮气)的简单转换,或发生相反的转变过程。
本发明的优点特别包括通过相同的溅射设备使用铝作为溅射材料可制备透明及不透明的阻挡层。另外,使用氧氮化铝作为阻挡层可反复使用被涂覆的基材。另外,被涂覆的基材可耐加热杀菌。为了确保在PET瓶热灌注过程中以及瓶在压力下的膨胀过程中不产生裂纹,涂层还可以是弹性的。
本发明的具体实现方式如图中所述,并在下文作详细描述。在图中描述如下:
图1 基材上的本发明的涂层
图2 带有外涂层的合成瓶子
图3 为涂覆合成瓶子的溅射装置
图1表示带有涂层的基材1的断面。该基材1是例如PET瓶壁的一部分。在该基材1上沉积有0.2~1.5μm厚的聚合物层2(例如聚丙烯酸层),其上具有1~100nm厚的氧氮化铝层3。在该AlOxNy层3上还有厚为0.2~1.5μm的聚合物层4,该层也可为丙烯酸酯。
图2表示合成瓶5,其包括饮料容器6、瓶颈7和封口8。容器6和瓶颈7由例如PET组成,并且是透明的。为了确保该透明的合成瓶1防止气体扩散,涂层9施加在该容器6的全部或部分。该涂层仅表示在图1中容器6的外部,且该层厚度为层2、3、4厚度的总和。
其目的在于涂层9任选制备成透明或不透明。AlOxNy是透明的,而Al层是不透明的。
图3表示可选地用氧氮化铝或铝作为阻挡层涂覆合成瓶子所用设备示意图。真空涂层室30包括在两个面上的至少一个磁电管阴极31、32。除了阴极,也可将多个阴极一个接一个地设置在每个面上。这些阴极安装有铝靶。在阴极31、32间还可设置有分隔壁35。在真空涂层室30的入口设置有联锁室33,其具有设置在环面上的多个接收室34、11~14。该联锁室33以如箭头15表示的顺时针方向旋转。在联锁室33的入口16处与大气压相通。此处未涂覆的合成瓶17、18、19放置到(未显示)线性传输设备上,随后被输送到环形传输设备中。从而位于传输设备上的瓶子从大气中被移入高真空涂层室30中。其中用标记20~25表示的、绕着它们的纵向轴(用箭头28表示)旋转的瓶子,在其所经过的磁电阴极32或磁电阴极串联组的作用下,再次被输送到(未显示)线性传输设备中。通过磁电阴极的铝靶溅射出金属粒子,其随后与氧和氮反应。得到的氧氮化铝沉积到瓶子的外壁上。所有在真空涂层室30中的瓶子继续绕它们的纵向轴旋转,特别是至少以瓶子经过磁电阴极32前可旋转360°的旋转速度旋转。若瓶子旋转重复多次可得到更均匀的涂层。在右侧涂覆路径的末端26处,将旋转的瓶子翻转约180°,利用磁电阴极31涂覆氧氮化铝。瓶子的新位置用21′~25′表示。
在分隔壁35和磁电阴极31、32间的空间可被认为是真空溅射室。其中至少一个溅射室具有三个进气口,通过这些进气口除了可引入氩气外,还可引入氧气和氮气。
图3中显示了带有截止阀40、41、42的三个气缸37、38、39,其通过进气口43、44、45与溅射空间相连。当关闭氧气和氮气的进气口44、45时,纯铝沉积到瓶子上。若其没被氧化,这些纯铝可象银那样反射。若打开所有阀门40~42,则形成AlOxNy并沉积到瓶子上。除了气缸38、39外,也可仅提供一个盛放空气的气缸。空气由70.084%N2和20.946%O2组成。
在瓶子被传输到真空溅射室中之前,其上涂覆有丙烯酸酯层。用不透气层Al或AlOxNy涂覆后,可再涂覆丙烯酸酯层。其中涂覆丙烯酸酯层的设备没有显示。
利用铝作为溅射材料,使用相同的涂覆设备可制备装饰性金属以及透明的阻挡层,并且不需要转换多次便可实现这一点。该透光的及不透光的层均可通过低廉的DC溅射法来制备。
厚度约4nm的AlOxNy层足以获得所需的阻挡性能。可在完全亚化学剂量条件下且不损失所需的透明性和阻挡性制备该厚度的层。此处的x和y优选满足条件0<x<0.6或0<y<0.5,该条件可通过对溅射参数的相应调整来满足。
除了用简单的DC溅射法外,相同的Al和AlOxNy层也可用更精密的MF/RF溅射技术来获得,但该技术会显著增加涂覆费用。
为了获得这些层,在下列实验室条件下选择溅射参数:在4×10-3mbar压力下的16立方厘米的空气和110立方厘米的氩气气流。电压为500W时,通过绕着其纵向轴旋转,而不是经过所述阴极来涂覆合成瓶子。
仅由空气流在13~19标准立方厘米间变动。空气的组成保持不变。氩气流被调整至80~140标准立方厘米,且涂覆时间在3~7秒之间。溅射层厚度为2~9纳米,并发现至少需要6~7nm厚的层可使BIF值>5。BIF值(BIF=阻挡改进因子)可被理解为带涂层基材的透气性与不带涂层基材的透气性的比值。
如图3所示的设备每小时可涂覆约20,000个瓶子,涂覆时间被降低至约5.55秒。为此,溅射功率可被提高至630W,从而使产品的涂覆时间和阴极功率保持常数,因此如第一次估算,结果可沉积相同厚度的层。因为与实验室条件相比,设备是连续传输设备,可动态进行涂覆,即基材经过阴极32、31的同时绕其纵向轴旋转。除了增加其溅射功率外,也可使用更长的阴极,从而可保持实验室试验的溅射功率,且瓶子以可确保每5.55内秒瓶子从溅射设备移至联锁室的传输速度移动。
溅射阴极31、32和基材21~25及21′~25′间的距离对涂层的生长速度也有影响。若设备中的该距离与实验室设备中的距离不同,功率也必须作相应的调整。距离越大需要的功率越高,在距离较短时可降低功率。
设备中氩气与空气的比率与实验室设备中的相似,但准确的气流取决于设备的电导系数和电容。设备电导系数取决于其内部结构,而设备的内部结构根据与实验室设备的不同需要决定。
以上描述了与涂覆瓶子相关的涂层。
但是,应当理解具有相同结构的层和其它网状材料也可被涂覆。适当的喷丝涂层设备已知,参考EP申请04 012 165.9。除了装有O2或N2的两个气缸38、39或同时装有两种气体的一个气缸外,也可直接与环境气体相通,并且可完全省略气缸38、39。在这种情况下,第二个气体容器是环境空气。
Claims (20)
1.一种制备不透气层的设备,特别是制备不透气合成材料基材涂层的设备,其特征在于:
a)具有至少一个铝靶(31、32)的真空溅射室(30);
b)至少两个气体容器(37、38),其通过至少一个可被关闭的气体进入管线(43~45)与真空溅射室(30)连接。
2.如权利要求1的设备,其特征在于第一个气体容器(37)含有氩气,第二个气体容器(38或39)含有空气。
3.如权利要求1的设备,其特征在于提供三个气体容器(37、38、39),第一个气体容器(37)含有氩气,第二个气体容器(38)含有氧气,第三个气体容器(39)含有氮气。
4.如权利要求1、2或3任一项的设备,其特征在于两个或三个气体进入管线(43~45)全部是开启的。
5.如权利要求1,2或3任一项的设备,其特征在于仅氩气的进入管线(43)是开启的。
6.如权利要求4和5的设备,其特征在于安装有转换设备(40~42),通过该设备可在供应氩气与供应氩气、氧气和氮气间相互转换。
7.如权利要求1的设备,其特征在于合成材料基材是中空体(5)。
8.一种制备不透气层的方法,其特征在于如下步骤:
a)在真空室中安装铝靶;
b)将氩气引入真空室作为溅射气体,氧气和氮气作为反应气体,
c)铝靶被溅射。
9.一种制备不透气层的方法,其特征在于如下步骤:
a)在真空室中安装铝靶;
b)将氩气引入真空室作为溅射气体;
c)铝靶被溅射。
10.根据权利要求8的方法,其特征在于空气被引入真空室作为反应气体。
11.如权利要求8的方法,其特征在于这样设置溅射过程的操作参数,以得到透明的、不透气的AlOxNy涂层,其中0<x<0.6且0<y<0.5。
12.如权利要求9的方法,其特征在于这样设置溅射过程中的操作参数,以得到不透明的Al涂层。
13.如权利要求11的方法,其特征在于AlOxNy层厚度为1~100nm。
14.如权利要求11~13的方法,其特征在于AlOxNy层被嵌入在聚合物层之间。
15.如权利要求14的方法,其特征在于聚合物层为厚度0.2~1.5μm的丙烯酸酯层。
16.如权利要求8的方法,其特征在于反应气体包括约65%~90%氮气和约10%~35%的氧气。
17.如权利要求8的方法,其特征在于反应气体含有高于50%的氮气。
18.如权利要求14的方法,其特征在于聚合物层包括厚度为0.2~1.5μm的阳离子聚合材料。
19.一种用于具有不透气壁中空体的气体阻挡涂层,其特征在于气体阻挡涂层包括至少一层AlOxNy,其中0<x<0.6且0<y<0.5。
20.一种用于具有不透气壁中空体的气体阻挡涂层,其特征在于气体阻挡涂层包括至少一层Al。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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EP04018645.4 | 2004-08-06 | ||
EP04018645A EP1624086B1 (de) | 2004-08-06 | 2004-08-06 | Vorrichtung und Verfahren für die Herstellung von gasundurchlässigen Schichten |
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CN1730717A true CN1730717A (zh) | 2006-02-08 |
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CNA2004100615445A Pending CN1730717A (zh) | 2004-08-06 | 2004-12-24 | 制备不透气层的设备和方法 |
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US (1) | US20060027450A1 (zh) |
EP (1) | EP1624086B1 (zh) |
JP (1) | JP2006045658A (zh) |
CN (1) | CN1730717A (zh) |
AT (1) | ATE544878T1 (zh) |
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ITGE20070021A1 (it) * | 2007-02-28 | 2008-09-01 | Nantech S R L | Contenitore per uso alimentare. |
GB0805328D0 (en) * | 2008-03-25 | 2008-04-30 | Aviza Technologies Ltd | Deposition of an amorphous layer |
US9022715B2 (en) | 2012-09-18 | 2015-05-05 | Applied Materials, Inc. | Load lock chamber designs for high-throughput processing system |
Family Cites Families (16)
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JPS5869743A (ja) * | 1981-10-21 | 1983-04-26 | Toyota Motor Corp | 導電性ガラスとその製造法 |
DE3642161A1 (de) * | 1986-12-10 | 1988-06-23 | Philips Patentverwaltung | Verfahren zur herstellung eines magneto-optischen speichers |
US4842941A (en) * | 1987-04-06 | 1989-06-27 | General Electric Company | Method for forming abrasion-resistant polycarbonate articles, and articles of manufacture produced thereby |
EP0394658A1 (de) * | 1989-04-24 | 1990-10-31 | Siemens Aktiengesellschaft | Verfahren zum Herstellen von Dünnfilmwiderstandsschichten |
US5156912A (en) * | 1989-12-20 | 1992-10-20 | The Standard Oil Company | Multi-layer coatings for reinforcements in high temperature composites |
CA2081912A1 (en) * | 1990-05-01 | 1991-11-02 | Chong T. Wan | Vacuum deposited dark coating on a substrate |
DE59205177D1 (de) * | 1991-12-13 | 1996-03-07 | Balzers Hochvakuum | Beschichtetes transparentes Substrat, Verwendung hiervon, Verfahren und Anlage zur Herstellung der Schichten, und Hafnium-Oxinitrid (HfOxNy) mit 1,5 x/y 3 und 2,6 n 2,8 |
US5400317A (en) * | 1993-04-01 | 1995-03-21 | Balzers Aktiengesellschaft | Method of coating a workpiece of a plastic material by a metal layer |
EP0636702B1 (en) * | 1993-07-28 | 1999-05-19 | Asahi Glass Company Ltd. | Methods for producing functional films |
AU694143B2 (en) * | 1993-10-04 | 1998-07-16 | 3M Innovative Properties Company | Cross-linked acrylate coating material useful for forming capacitor dielectrics and oxygen barriers |
US5763033A (en) * | 1996-01-30 | 1998-06-09 | Becton, Dickinson And Company | Blood collection tube assembly |
JP3689524B2 (ja) * | 1996-03-22 | 2005-08-31 | キヤノン株式会社 | 酸化アルミニウム膜及びその形成方法 |
JP3782608B2 (ja) * | 1998-05-22 | 2006-06-07 | キヤノン株式会社 | 薄膜材料および薄膜作成法 |
US6517687B1 (en) * | 1999-03-17 | 2003-02-11 | General Electric Company | Ultraviolet filters with enhanced weatherability and method of making |
JP4024510B2 (ja) * | 2001-10-10 | 2007-12-19 | 株式会社半導体エネルギー研究所 | 記録媒体、および基材 |
DE10252543A1 (de) * | 2002-11-08 | 2004-05-27 | Applied Films Gmbh & Co. Kg | Beschichtung für ein Kunststoffsubstrat |
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2004
- 2004-08-06 EP EP04018645A patent/EP1624086B1/de not_active Expired - Lifetime
- 2004-08-06 AT AT04018645T patent/ATE544878T1/de active
- 2004-10-19 US US10/968,838 patent/US20060027450A1/en not_active Abandoned
- 2004-11-11 JP JP2004327289A patent/JP2006045658A/ja active Pending
- 2004-12-24 CN CNA2004100615445A patent/CN1730717A/zh active Pending
Also Published As
Publication number | Publication date |
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ATE544878T1 (de) | 2012-02-15 |
JP2006045658A (ja) | 2006-02-16 |
EP1624086B1 (de) | 2012-02-08 |
EP1624086A1 (de) | 2006-02-08 |
US20060027450A1 (en) | 2006-02-09 |
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