CN1361001A - 形成塑料片材的方法和装置 - Google Patents
形成塑料片材的方法和装置 Download PDFInfo
- Publication number
- CN1361001A CN1361001A CN01144010A CN01144010A CN1361001A CN 1361001 A CN1361001 A CN 1361001A CN 01144010 A CN01144010 A CN 01144010A CN 01144010 A CN01144010 A CN 01144010A CN 1361001 A CN1361001 A CN 1361001A
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- CN
- China
- Prior art keywords
- die head
- overflow
- sheet material
- resin
- sheet
- Prior art date
- 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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Links
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Abstract
揭示一种以连续方式形成光学品级塑料片材的方法和装置,其中生产的塑料片材能用于各种光学和电子显示器应用。
Description
本发明涉及形成塑料片材的方法和装置。尤其是本发明涉及形成具有低残余应力和高表面质量的塑料片材的方法和装置。根据本发明方法形成的塑料片材特别用于光学和电子显示应用,例如,光学窗户、滤光片、记录介质和液晶显示(LCD)。
光学品级玻璃或石英片作为“基片”用于电子显示应用。在此应用中,“基片”是用于制造电子显示所用的材料片。这种基片可以是透明的,半透明的或不透明的,但一般是透明的。通常,这种片材在用作基片之前其上有涂施的导电涂层。这种基片常常有精确的光学透明度、平整度和最小双折射特性,特别是必须具有对气体和溶剂渗透的高度稳定性。机械性能例如柔软性、抗冲击性、硬度和抗刮伤性也是重要的条件。玻璃或石英片材已被用于显示应用,这是因为这些材料能够满足光学和平整度的要求并且具有良好的热和耐化学性及阻挡性,然而这些材料不具有某些所希望的机械性能,最值得注意的是低的密度、柔软性和抗冲击性。
由于玻璃或石英片在光学或显示器应用中机械性能的限制,因此在这些应用中希望使用塑料片材。尽管塑料片材具有较高的柔软性,而且更耐断裂,还比相同厚度的玻璃或石英片材重量轻,然而很难以合理的成本生产在光学和显示器应用中所需要的具有所需光学特性的塑料片材。此外,许多类型的塑料片材在制造显示器装置过程中当经受加工条件时,尤其是相对于温度时,尺寸将会产生不合格变形。
有几种商业上应用的制造塑料片材的方法,包括铸塑、挤出,和拉伸操作。这些方法中的几种不适于生产高质量的塑料片材。作为贯穿此说明书所使用的术语“高质量”用于说明塑料片材具有以下特性:低表面粗糙度,低波痕,低厚度变化,和极小量聚合物链取向(例如通过不对称物理性能、双折射或热收缩测量)。
例如,注射成型很可能产生大量聚合物链取向,尤其是薄的片材(即1mm或更小厚度),由于熔融塑料流进入模具,这不令人满意地以不可忽视的光弹性系数提高了聚合物双折射。注射压塑是一种改进的成型方法其允许聚合物注射后的挤压以改进表面质量和降低聚合物链取向。然而,即使有这些改进注射压塑生产高质量片材的能力仍受到限制。
压塑和压光可用于生产具有良好表面质量的片材;然而,此方法中固有的挤压流动导致聚合物链取向其造成热循环过程中不合格的收缩。此外这些方法不是可连续操作的因此增加了劳力和生产成本。
拉伸操作(例如,用于生产单轴或双轴取向薄膜)和吹塑薄膜挤出固有地产生大量聚合物链取向因而不适于生产高质量塑料片材。
溶剂铸塑可用于生产高质量薄膜,然而,对由此方法生产的薄膜的最大厚度有实际限制。另外在铸塑中所用的溶剂在形成片材之后必须被除去。
片材挤出可连续操作运行,但是由于在模头中及在叠辊机中抛光辊之间的聚合物流动特性这种方法造成不合格聚合物链取向。
因此仍旧需要以连续方式生产相对廉价高质量塑料片材的方法,其中所得的塑料片材能用作光学和电子显示器应用中的基材。
本发明的目的在于一种生产高质量塑料片材的方法,包括以下步骤:a)提供熔融塑料树脂;b)引导熔融树脂至具有进口和出口的溢流模头;c)用所说的溢流模头成型熔融塑料树脂为熔融料片;d)引导所说的熔融料片离开所说的溢流模头;和e)冷却所说的熔融料片形成固体片材。
本发明的目的还在于一种生产高质量塑料片材的装置,包括:a)提供熔融塑料树脂的料源;b)具有长度和宽度的溢流模头,其包括基本上呈蛋形截面顶点,导管开口,和与所说的导管开口连接的计量装置,其中熔融塑料树脂通过导管开口流入模头,从计量装置流出模头,并围绕模头侧面在所说的顶点形成熔融料片;c)从所说的料源输送所说的熔融塑料树脂至所说的溢流模头的装置;和d)用于引导所说的熔融料片离开所说的溢流模头的导向装置。
本发明的目的还在于一种用于形成高质量塑料片材的溢流模头,所说的溢流模头具有内部和外部并包括:a)由模头外部形成的溢流表面并包括一对模唇;b)连接到所说的溢流表面的两个外侧面;c)由所说的两个外部侧面汇合形成并设置在大体上在所说的溢流表面相对位置的顶点,其中该模头具有基本上蛋形的截面;d)从外部至内部的导管开口;和e)设置在模头内部的计量装置,其中该计量装置与所说的导管开口和所说的溢流表面连接。
图1是本发明代表性的装置的前视图。
图2是图1装置的侧视图。
图3A-3C是溢流模头20的特写。图3A是带有附着加热集料管模头的透视图。图3B是模头的顶视图;图3C是模头的侧视图。
图4是溢流模头20的剖面图。
图5-7是本发明溢流模头的另一实施方案。图5说明在模头20的缝口22处具有一系列孔的溢流模头;图6说明具有非锥形模缝的溢流模头;和图7说明具有“衣架式”配置的溢流模头。
作为在此说明书中所用的以下术语具有以下定义,除非该内容清楚地指明其它含义。“玻璃化转变温度”或“Tg”是窄温度范围的中间点,在此温度范围内聚合物从相当硬和脆变为相当软和粘(橡胶态)。“塑料”指聚合物,例如热塑性聚合物,其可形成片材。术语“聚合物”和“树脂”贯穿整个说明书可互换使用。“片材”指具有厚度大约25mm或更小的片材,并且趋于包括“薄膜”(厚度<0.5mm)。“收缩”指不可逆尺寸变化,其出现在片材经受加热-冷却循环中。在说明书中使用以下的缩写:cm=厘米;mm=毫米;nm=毫微米;μ=微米;g=克;mL=毫升;Pa=帕斯卡;kPa=千帕斯卡;Pa-s=帕斯卡-秒;sec=秒钟;min=分钟;hrs=小时;UV=紫外线;IR=红外线。所有的温度都是℃除非另有说明。应将具体范围的两端值理解为包括在该范围内,除非该内容清楚地指明其它含义。
由本发明方法形成的高质量塑料片材可用于许多应用,包括但不限定:用于电子显示器装置例如LCD和场致发光显示器的基材;光学窗户和过滤器;用于光、磁、化学或其它类型记录介质的基材;用于成象,例如摄影或X-射线应用的基材。根据由本发明的方法生产的特殊用途的片材,片材特性例如低收缩性,低双折射和表面质量在相对重要性方面不同。所希望的片材厚度也可以根据实际应用而变化,但是一般为大约25mm或更小,优选10-5000μ,最优选50-1000μ。片材厚度可以通过改变输送熔融聚合物至模头的速度或通过改变收卷装置的速度而调整。在400mm长样品上的厚度变化一般是10%或更小,优选5%或更小,最优选1%或更小。
本发明的代表性装置示于图1-4。作为本领域熟练人员都清楚,由这些图中所示装置的变化在本发明的范围内。
由料源10的熔融聚合物通过料道12被输送到溢流模头20(优选由输送装置14控制),其中物料通过导管开口21至导管22被引入模头20。当熔融聚合物被输送到模头20时其温度通过使用设置在紧邻模头20的加热器15维持。当熔融聚合物充入开口21时其穿过计量装置,模缝23,压出到模唇40和41上,并围绕模头20的侧面24和25流出。在模头20的顶点26,从侧面24和25流出的熔融聚合物汇合形成熔融料片27的开端。
熔融料片27在其边缘由两对引导装置(例如槽支撑31,32,33和34)拾起该装置引导熔融料片从模头20离开。当熔融料片27被从模头20引出时,料片的温度逐渐降到聚合物的玻璃化转变温度以下结果形成冷却的片材40。在任选的实施方案中,设置在紧邻引导装置31,32,33,34的冷却装置36帮助降低料片的温度。
可以以许多方式中的任何一种来提供熔融树脂。例如可从聚合反应器、混合器、排气装置(例如闪蒸塔、落丝脱挥发组份器(falling stranddevolatilizer)或摩擦闭合薄膜蒸发器(wiped film evaporator)),或挤出机提供熔融树脂。挤出机是优选的,因为它也可以作为聚合物输送装置(参见以下的讨论)。最优选使用单螺杆挤出机,尽管也可以使用双螺杆或多螺杆挤出机。如果使用双螺杆或多螺杆挤出机,其可以是任何类型的,例如反转,同向旋转,啮合或非啮合型。
熔融树脂可以含有一种或多种塑料添加剂例如抗氧剂、紫外线吸收剂、紫外线稳定剂、荧光剂或吸收染料、抗静电添加剂、脱模剂、填料和颗粒。对于特殊树脂的特殊用途所用添加剂的类型和量对于塑料领域的熟练人员是已知的因此在此不再详述。
加工树脂的温度取决于树脂组合物并且可在加工过程中变化。该温度必须足够高使树脂流动但不高至降解塑料。操作条件将根据被加工的聚合物类型变化,并且在本领域熟练人员所知的范围内。然而,作为一般的准则,操作温度在100和400℃之间。例如PMMA在挤出机内加工时挤出机机筒温度为150-260℃,熔体温度为150-260℃。其它聚合物例如聚碳酸酯或聚甲基丙烯酰亚胺也可以在相当高的熔体温度(200-330℃)使用。优选在形成片材之前从熔融塑料树脂中除去挥发性材料和不希望的颗粒物质。这可根据本领域熟练人员所知的方法完成。
为了调整流动速率和提供穿过料道12,导管开口21和导管22至模头20输送熔融聚合物所需的压力,需要用于输送熔融聚合物恒定料流的输送装置14。该输送装置可以包括任何类型的机械熔体泵,包括但不限于任何合适的挤出机(如以上所述),齿轮泵,或其结合。在简单的形式中,输送方式可以是重力加料,或静液压压力。优选使用齿轮类型熔体泵因为它可以控制流动速率并使流动速率波动极小化,结果造成片材厚度更均匀。另外使用熔体泵通过降低聚合物的剪切热可以降低熔融树脂的降解。熔体泵的温度可以通过所用塑料树脂来确定,其类似于标准挤出工艺中所用的温度,一般在树脂Tg以上50-200℃之间。可以使用一种以上的输送装置,例如,用于生产宽片材。在本发明中,输送装置应以50-70000kPa,优选300-7000kPa,更优选1000-3500kPa的范围,提供熔融聚合物至溢流模头的入口。
该溢流模头用于从熔融塑料树脂形成片材。该模头包括计量装置和带有聚料侧面的溢流表面,其在截面中顶点处达到顶点。该模头在纵向结构中可以基本上是线性、曲线、椭圆形或圆形。模头高度对宽度的比率一般应在1∶1-10∶1,优选2;1-5;1,更优选2.5∶1-4∶1的范围。长度(圆周)对高度的比率一般应至少1∶2,优选至少2;1,最优选至少3;1。
溢流模头的计量结构部分包括流动分布元件例如孔、缝、“衣架”结构或其结合,其控制横穿模头的熔融树脂的流动分布,从而控制片材厚度断面。这种计量结构的例子在图5-7中说明。可以使用本领域那些熟练人员所知的其它计量结构。优选缝结构。模头的长度取决于要制造的片材宽度,但平均缝隙(缝23的平均宽度)对平均导管直径(导管22的平均直径)的比率一般应至少1;5,优选至少1∶10,最优选至少1;20。对于具有完成厚度为1mm或更小的片材,优选基本上恒定的横穿模头缝宽度。对于较大的厚度,优选锥形模缝,其中该模缝在进料端较薄,在另一边较厚。如果希望宽片材,可在模头两端设置导管开口21和21’(参见图6),并且可以在两端有斜削的模缝23。
溢流表面由模头20的外表面形成并包括一对模唇,40和41,其与进料结构连接并直接将熔融聚合物射向汇合侧面,24和25。该汇合侧面直接将熔融料流射向顶点26,在该处熔融料片从模头离去。尽管溢流表面可以起纹理或是平滑的,但是优选是平滑的。此外,溢流表面优选高度抛光以使片材中的变形和疵点极小化。溢流表面可用涂层处理(例如电镀或其它沉积技术)以改进模头表面光滑度,提供耐腐蚀性,或改进流过模头的流动性能。
模头结构的材料是重要的。优选金属因为它们的热传导性高,耐腐蚀性好,模量高,而且可被抛光。然而,就原理而论可以使用其它材料例如玻璃和陶瓷。优选使用不锈钢或工具钢。
如果想要非平面片材,可使用本领域熟练人员已知的方法因此而改进模头几何构型。例如,如果想要曲面片材,模头可沿着其纵向轴线成曲线状。
一般,希望维持熔融塑料的粘度(对于10秒-1的剪切速率)在10和100000泊之间,优选在50和10000泊之间,最优选在100和5000泊之间。另外,每单位模头长度的熔体流动速率(流动速率除以长度)一般在1.0×10-3-10g/s/cm,优选在1.0×10-2-10g/s/cm,最优选在2.0×10-2-2.0×10-1g/s/cm的范围。粘度可通过改变温度进行控制。根据模头设计,温度控制或多或少是重要的。穿过模头的温度越均匀,片材的厚度越均匀。由模头长度下不均匀的温度分布造成的厚度变化可通过改变模缝或其它计量结构的设计而极小化。温度控制可以通过例如,一种或多种以下的装置而实现:电加热筒、红外线灯加热器、加热的油(或其它热传导流体)、热管、或微波加热器。加热的油或其它热传导流体是优选的,因为温度可以通过恒温器控制因此温度的均匀性易于实现。为使温度波动极小化模头优选在特别封闭区域内遮蔽。
优选的,但不是必须的是,熔融塑料料流在经过模头之后向下流动,因为向下流动可通过重力实现。流动速率通过重力的作用结合引出装置所施加的张力来确定。通过将塑料料流向下导向越过模头,重力作用在如片材流动的相同方向,由此降低了引出装置中所需的张力并改进了片材质量。经过模头之后的熔融塑料处于称为“料片”的形式。
引出装置从模头以控制的速度输送熔融塑料料片并使料片冷却。该引出装置可以是,例如辊或“槽形支撑”结构,由此仅仅片材的外缘与引出装置接触。“槽形支撑”结构是优选的,因为其使片材表面的光滑度达到最大化。槽形支撑结构作为图1和2的装置的零件图解说明为31,32,33和34。
引出装置控制塑料片材被生产的速度,其在给定的聚合物流动速率确定片材的厚度;因此引出装置速度的控制是十分重要的。引出装置也支撑片材的重量,由此保持恒定的片材宽度和厚度。希望将引出装置放置在尽可能靠近模头的位置致使未支撑的熔融树脂的量极小化。从模头顶点至引出系统的距离(例如在槽形支撑结构顶部的辊隙区域)一般<25cm,优选<10cm,最优选<5cm。
片材引出速度根据所希望的片材类型,和厚度而变化。例如,对于0.4mm厚的片材,片材引出速度一般在10-1000cm/min,优选20-200cm/min,最优选50-100cm/min的范围;而对于1mm厚的片材,片材引出速度一般在5-500cm/min,优选10-100cm/min,最优选25-50cm/min的范围。在类似的方式中,在弯曲之前,在引出系统内进行冷却期间滞留时间将变化。例如对于0.4mm厚的片材,弯曲之前的滞留时间一般≥10sec,优选≥1min,最优选≥2min;而对于0.2mm厚的片材,滞留时间一般≥5sec,优选≥30sec,最优选≥1min。
在由引出系统输送过程中可以通过自然对流,或强力对流冷却塑料片材。自然对流包括片材穿过空气或流体浴过程中的被动冷却。强力对流通过沿着或对着片材泵送或吹入热传导流体完成以增强热传导。对于使片材起波纹和表面缺陷极小化优选利用风机和增压结构产生强力气体对流。优选使用干净流体(没有颗粒)冷却片材防止表面弄脏或暇疵。例如对于用空气或气体冷却的目的可以使用HEPA纤维。对于片材的冷却可以使用任何流体或流体的结合,只要所用的流体对被加工的塑料片材无害即可。有用的冷却流体的例子是:空气、氮气、水、油,和二元醇。可以通过使用适宜的冷却剂(当其离开冷却裕时起涂层的作用并在塑料片材上作为薄膜沉积)将冷却工艺与涂覆工艺结合。
本领域的那些熟练人员可以判明以下各种可选择的装置均可用作引出装置。可选择的装置的例子包括常规的薄膜加工装置例如薄膜收卷机、边缘切割机、片材切割机,和包装装置。另外,可以利用其它下游装置,例如成形装置、涂覆装置、装潢装置,和层压装置。
本发明的方法可用于任何适用的塑料树脂,优选用于热塑性树脂。热塑性树脂是当暴露于热时可逆软化而冷却时变硬的聚合物树脂。热塑性树脂可以是线性或基本上不交联的支链聚合物。优选的是用于本发明方法的热塑性树脂实际上不交联并在熔融加工温度(即,具有104数量级泊的粘度)具有热稳定性(滞留时间高达10分钟或更多)。可用于本发明方法的热塑性树脂的例子包括但不限于:丙烯酸、甲基丙烯酸和其酯的均聚物或共聚物,它们包括但不限于与苯乙烯和其衍生物,N-烷基马来酰亚胺、丙烯腈,和醋酸乙烯酯所形成的共聚物;苯氧基醚;聚苯氧树脂、环氧树脂;纤维素树脂;乙烯基树脂例如聚氯乙烯(PVC);氟聚合物例如氟化乙烯-丙烯和聚(偏二氟乙烯);聚碳酸酯;聚苯乙烯;聚烯烃例如聚乙烯、聚丙烯、聚-4-甲基戊烯-1,并包括环烯烃;聚砜;聚醚砜;聚醚酮;聚醚酰亚胺,聚苯硫;聚亚芳基酯树脂;聚酯;N-H和/或N-烷基戊二酰亚胺的均聚物或共聚物;丙烯腈-丁二烯-苯乙烯树脂(“ABS”);苯乙烯-丙烯腈树脂(“SAN”);苯乙烯-马来酸酐树脂(“SMA”);酰亚胺化的SMA;和聚酰胺(“尼龙”)。也可以使用热塑性树脂的混合物。特别有用的热塑性树脂混合物包括,例如:SAN-聚戊二酰亚胺、聚碳酸酯-聚酯、PMMA-聚(偏二氟乙烯)和聚苯乙烯-聚(苯氧)。乙烯的用于本发明的方法和装置的树脂是:聚碳酸酯;线性丙烯酸均聚物和共聚物;环聚烯烃;和线性酰亚胺化的丙烯酸均聚物和共聚物例如在US4727117(Hallden-Abberton等人)和US4246374(Kopchik)中揭示的那些聚合物。
用于本发明的塑料树脂一般来自加成聚合或缩合聚合工艺。加成聚合工艺包括本体聚合和在水中或有机溶剂介质中的溶液聚合或分散聚合,这种工艺是本领域熟知的并且可引入阳离子、阴离子、或游离基引发和链增长反应。缩合聚合工艺包括本体、溶液和分散聚合工艺。由本体聚合以外的聚合工艺形成的塑料树脂可能需要后处理以便离析树脂。
以下的例子用于进一步说明本发明的各个方面,但是在任何方面都不限制本发明的范围。
例1:丙烯酸酯类薄膜的制备
此例说明本发明用于生产光学品级丙烯酸酯类片材的方法。
将具有平均分子量110000的PMMA树脂不足喂料至2英寸(5厘米)直径单螺杆排气两步挤出机,该挤出机具有30∶1的长径比并用定容喂料器以3.1g/s的速率喂料。该挤出机螺筒具有从204℃(在加料端)至274℃(在排料端)的温度分布。树脂用在720-750mmHg运行的排气口排气。螺杆以30rpm旋转。使用齿轮型熔体泵泵送熔融树脂穿过网叠过滤器至12”(30厘米)长溢流模头,其具有1.27厘米直径内部导管和一系列间隔1.27厘米的计量孔22。计量孔的直径从模头加料端3.18mm增大至下游端3.73mm。熔体泵网叠是274℃。熔体泵的抽吸压力是2100kPa,熔体泵的排料压力大约是4100kPa。溢流模头内部用三个筒式电加热器加热,外部用三个红外加热单元加热至274℃。在模头顶点形成的熔融料片用两对槽形支撑输送,并用由两台压力通风系统施加的强制冷却空气冷却。所得的片材具有0.325mm的厚度,14.6nm的表面粗糙度Rq,和<5nm的光学阻滞性。
例2:酰亚胺化丙烯酸酯类片材的制备
此例说明用于生产光学品级丙烯酸酯类片材的本发明方法。
将一种具有重均分子量为97500和玻璃化转变温度为大约180℃的封端的酰亚胺化丙烯酸酯树脂不足加料至2英寸(5厘米)直径单螺杆排气两步挤出机,该挤出机具有30∶1的长径比并用计重喂料器以2.5g/s的速率喂料。该挤出机螺筒具有从246℃(在加料端)至329℃(在排料端)的温度分布。树脂用在720-750mm Hg运行的排气口排气。螺杆以30rpm旋转。使用齿轮型熔体泵泵送熔融树脂穿过网叠过滤器至25.5英寸(65厘米)长溢流模头,其具有1.588厘米直径内部导管和16英寸(40厘米)长缝,其锥形从0.038-0.042英寸(0.965-1.067mm)。熔体泵的温度是329℃。熔体泵的抽吸压力大约是4100kPa。熔体泵的排料压力大约是1650kPa。模头通过模头内部的孔用热油系统加热(油温=343℃),围绕模头的空气用强力气体烘箱(温度=280℃)加热。在模头顶点形成的熔融料片用两对槽形支撑以1.2cm/s的速度输送,并用室内空气的自然对流进行冷却。
从冷却的片材切割200mm×200mm的试样并进行测试。所得的片材具有0.390mm的厚度,偏差±0.015mm。表面波痕Wy和Wq分别是<0.5μ和0.18μ,表面粗糙度Rq是7.6nm,光学阻滞性是<6nm的。在160℃测量的热收缩是0.03%或更小。
例3:聚碳酸酯片材的制备
此例说明用于生产光学品级聚碳酸酯片材的本发明方法。
将挤出级聚碳酸酯树脂(GE Lexan 101)不足加料至不足加料至2英寸(5厘米)直径单螺杆排气两步挤出机,该挤出机具有30∶1的长径比并用计重喂料器以4.4g/s的速率喂料。该挤出机螺筒具有从232℃(在加料端)至315℃(在排料端)的温度分布。树脂用在720-750mm Hg运行的排气口排气。螺杆以30rpm旋转。使用齿轮型熔体泵泵送熔融树脂穿过网叠过滤器至37.5英寸(95厘米)长溢流模头,其具有1.905厘米直径内部导管和28英寸(71厘米)长缝,其锥形从0.038-0.045英寸(0.965-1.143mm)。熔体泵温度为315℃,熔体泵的抽吸压力约为3400KPa。熔体泵的排料压力大约是1300kPa。模头通过模头内部的孔用热油系统加热(油温=315℃),围绕模头的空气用强力气体烘箱(温度=260℃)加热。在模头顶点形成的熔融料片用两对槽形支撑以1.2cm/s的速度输送,并用室内空气的自然对流进行冷却。
从冷却的片材切割400mm×400mm的试样并进行测试。所得的片材具有0.43mm的厚度,在横向和机器方向的偏差±0.02mm。Wy是<1μ,Wq是<0.15μ,表面粗糙度Rq是<10nm,平均光学阻滞性是20nm,偏差是10nm。在130℃测量的热收缩是0.02%。
例4:聚碳酸酯薄膜的制备
此例说明用于生产光学品级聚碳酸酯薄膜的本发明方法。
将挤出级聚碳酸酯树脂(GE Lexan 101)不足加料至不足加料至2英寸(5厘米)直径单螺杆排气两步挤出机,该挤出机具有30∶1的长径比并用计重喂料器以2.5g/s的速率喂料。该挤出机螺筒具有从232℃(在加料端)至315℃(在排料端)的温度分布。树脂用在720-750mm Hg运行的排气口排气。螺杆以30rpm旋转。使用齿轮型熔体泵泵送熔融树脂穿过网叠过滤器至37.5英寸(95厘米)长溢流模头,其具有1.905厘米直径内部导管和28英寸(71厘米)长缝,其锥形从0.038-0.045英寸(0.965-1.143mm)。熔体泵温度为315℃,熔体泵的抽吸压力约为3400KPa。熔体泵的排料压力大约是1300kPa。模头通过模头内部的孔用热油系统加热(油温=315℃),围绕模头的空气用强力气体烘箱(温度=250℃)加热。在模头顶点形成的熔融料片用两对槽形支撑以3.1cm/s的速度输送,并用室内空气的自然对流进行冷却。
从冷却的片材切割400mm×400mm的试样并进行测试。所得的片材具有54μ的厚度,在横向和机器方向的偏差±4μ。光学阻滞性<10nm。
测试方法
以下的测试方法用于测试在以上例子中制成的片材。本领域中都明白这些测试方法实际上只是例举,其结果与方法无关。
光学阻滞性
在632.8nm波长的光的阻滞性按以下方式确定。偏振激光束(根据实验室系统在-45°偏振)穿过塑料片材,然后穿过在实验室系统中与设定为0°的光轴线取向的光弹性调制器(PEM)(型号PEM-90,HindsInstruments,Inc;Hillsboro,Oregon)。PEM电压设定为1/4光波阻滞性(158.2nm)。此光然后穿过第二线性偏振器(偏振轴线+45°)并用硅二极管探测器(型号PDA-50,Thorlabs Inc.;Newton,New Jersey)探测亮度。调制PEM和探测器,并对来自探测器的信号经锁定放大器(型号5210,EG&G Princeton Applied Research;Princeton,New Jersey)进行处理。将塑料片材垂直激光束转动以找到最大信号。通过对比最大信号与所测量的对于标准1/4光波板的信号来确定阻滞性。
可通过等分材料的光阻滞性与其厚度的积来得到材料的双折射。例如如果光阻滞性对于0.4毫米厚的塑料片材是4nm,则该材料的双折射是0.00001。对于由本发明方法制成的光学品级塑料片材,材料的双折射如果≤0.0002,优选≤0.00005,最优选≤0.00001则被认为是低的。
片材波痕
使用触头靠模(Surfanalyzer System 5000,FederalProducts;Providence,Rhode Island)按照类似SEMI Standard D15-1296的程序测量片材波痕(Wy和Wq)。测量靠模用Gaussian长波长断开装置(8mm)进行数字滤波。Wy在20mm样品长度内最大和最小值之间的差,Wq是从8mm计算的平均长,和80mm测定长度的平均值的滤波靠模的均方根差。对于由本发明方法生产的光学品级片材,Wy应该≤1.0μ,优选≤0.2μ,更优选≤0.05μ。
片材粗糙度
使用触头靠模(Dektak 3-30,Veeco/Sloan,Santa Barbara,CA)按照类似SEMI Standard D7-94的程序测量片材粗糙度(Rq)。测量靠模用Gaussian长波长断开装置(0.8mm)和短波长断开装置(0.0025mm)进行数字滤波。测定长度是0.4mm。粗糙度参数(Rq)是平均线滤波外形的平均均方根偏差。记录三个不同测量值的平均值。对于由本发明方法生产的光学品级片材,Rq应该≤50nm,优选≤10mm,更优选≤5nm。
收缩率
在热处理之前和之后通过直接测量样品长度而测定收缩率。进行多次测量以确定干燥塑料件的长度。测量值的精确度是0.005%。将样品加热至其Tg以下的设定温度保持4小时。当冷却到室温时,通过多次测量再次测定该长度。记录在加热循环之前和之后长度的百分变化作为收缩率。对于由本发明方法生产的光学品级片材,收缩率应≤0.05%,优选≤0.02%,最优选≤0.005%。
Claims (6)
1.一种生产高质量塑料片材的装置,包括:
a)提供熔融塑料树脂的料源;
b)具有长度和宽度的溢流模头,其包括:
基本上呈蛋形以顶点终结的截面,
导管开口,和
与所说的导管开口连接的计量装置,
其中熔融塑料树脂通过导管开口流入模头,从计量装置流出模头,并围绕模头侧面在所说的顶点形成熔融料片;
c)从所说的料源输送所说的熔融塑料树脂至所说的溢流模头的装置;和
d)用于引导所说的熔融料片离开所说的溢流模头的导向装置。
2.权利要求1的装置,进一步包括从所说的料源输送所说的熔融塑料树脂至所说的溢流模头的输送装置。
3.权利要求2的装置,其中输送装置包括齿轮型熔体泵。
4.权利要求1的装置,进一步包括过滤器以除去杂质颗粒,所说的过滤器设置在所说的料源和所说的溢流模头之间。
5.权利要求1的装置,进一步包括靠近所说的导向装置的冷却装置。
6.一种用于形成高质量塑料片材的溢流模头,所说的溢流模头具有内部和外部并包括:
a)由模头外部形成的溢流表面并包括一对模唇;
b)连接到所说的溢流表面的两个外侧面;
c)由所说的两个外部侧面汇合形成并设置在大体上在所说的溢流表面相对位置的顶点,其中该模头具有基本上蛋形的截面;
d)从外部至内部的导管开口;和
e)设置在模头内部的计量装置,其中该计量装置与所说的导管开口和所说的溢流表面连接。
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CNB2003101026320A Expired - Fee Related CN100480027C (zh) | 1997-11-07 | 1998-11-06 | 形成塑料片材的方法和装置 |
CNB981264492A Expired - Fee Related CN1147390C (zh) | 1997-11-07 | 1998-11-06 | 形成塑料片材的方法和装置 |
Country Status (8)
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US (3) | US6183829B1 (zh) |
EP (1) | EP0914926B1 (zh) |
JP (2) | JP4519211B2 (zh) |
KR (1) | KR100562051B1 (zh) |
CN (3) | CN100480027C (zh) |
CA (1) | CA2252947C (zh) |
DE (1) | DE69807816T2 (zh) |
TW (1) | TW442384B (zh) |
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- 1998-11-02 EP EP98308962A patent/EP0914926B1/en not_active Expired - Lifetime
- 1998-11-03 TW TW087118267A patent/TW442384B/zh not_active IP Right Cessation
- 1998-11-05 CA CA002252947A patent/CA2252947C/en not_active Expired - Fee Related
- 1998-11-06 KR KR1019980047613A patent/KR100562051B1/ko not_active IP Right Cessation
- 1998-11-06 CN CNB2003101026320A patent/CN100480027C/zh not_active Expired - Fee Related
- 1998-11-06 CN CNB981264492A patent/CN1147390C/zh not_active Expired - Fee Related
- 1998-11-09 JP JP31815698A patent/JP4519211B2/ja not_active Expired - Fee Related
-
2000
- 2000-11-27 US US09/723,303 patent/US6472031B1/en not_active Expired - Fee Related
- 2000-11-27 US US09/723,140 patent/US6451403B1/en not_active Expired - Fee Related
-
2001
- 2001-12-26 CN CNB011440104A patent/CN1196574C/zh not_active Expired - Fee Related
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2010
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101163645B (zh) * | 2005-04-26 | 2011-02-16 | 康宁股份有限公司 | 用于玻璃制造系统的具有连接的延长部分的成形设备 |
Also Published As
Publication number | Publication date |
---|---|
JPH11227026A (ja) | 1999-08-24 |
CN1500623A (zh) | 2004-06-02 |
US6451403B1 (en) | 2002-09-17 |
DE69807816D1 (de) | 2002-10-17 |
TW442384B (en) | 2001-06-23 |
EP0914926A3 (en) | 2000-05-03 |
CN1225307A (zh) | 1999-08-11 |
JP4519211B2 (ja) | 2010-08-04 |
CA2252947A1 (en) | 1999-05-07 |
CA2252947C (en) | 2001-10-30 |
DE69807816T2 (de) | 2003-05-28 |
EP0914926B1 (en) | 2002-09-11 |
KR19990045095A (ko) | 1999-06-25 |
CN1196574C (zh) | 2005-04-13 |
JP2010162899A (ja) | 2010-07-29 |
KR100562051B1 (ko) | 2006-07-03 |
EP0914926A2 (en) | 1999-05-12 |
CN1147390C (zh) | 2004-04-28 |
US6472031B1 (en) | 2002-10-29 |
US6183829B1 (en) | 2001-02-06 |
CN100480027C (zh) | 2009-04-22 |
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