CN1121866A - 热固性增强的耐腐蚀层压制品 - Google Patents
热固性增强的耐腐蚀层压制品 Download PDFInfo
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- B29K2105/0854—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts of continuous length, e.g. cords, rovings, mats, fabrics, strands or yarns in the form of a non-woven mat
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Abstract
根据本发明,提供了一种热塑性氟聚合物的耐腐蚀面纱,以及具有热塑性氟聚合物面纱的耐腐蚀性的、增强的热固性塑料层压制品。
Description
本发明涉及增强的聚合物层压制品。更具体地说,本发明涉及耐腐蚀的、增强的热固性塑料层压制品,以及引入该层压制品内的面纱(surfacing veil)。
面纱作为主要的防腐层用于热固性树脂的、纤维增强的层压制品中在玻璃纤维增强的塑料工业上是众所周知的。
在美国试验与材料协会(下文称ASTM)C582—87中标题为“用于耐腐蚀设备的接触模压的、增强的热固化塑料层压材料的标准说明”(Standard Specification for Contact—Molded ReinforcedThermosetting Plastic(RTP)Laminates for Corrosion ResistantEquipment)的章节中,接触模压在3.4节中被定义为“…一种制造方法,其中玻璃纤维以短切原丝薄毡或方格布的形式通过手或经过绕丝机应用于模压,或以来自切断机—喷枪的连续玻璃纤维的短切原丝的形式应用于模压。树脂母料可通过各种方法(包括刷、辊或喷枪)施用。通过辊压来加固复合层压材料。”
面纱或薄毡在ASTM C582—87,ASTM D4097—88和ASTMD3299—88中有定义。面纱或薄毡在ASTM C582—87,ASTMC582—87的5.2.1节中定义为“主要用来在增强塑料上产生光滑表面的细纤维薄毡。”,ASTM C582—87的5.2.1.2节指出,可接受的面纱的要求是:
“(a)树脂相容性,
(b)纤维均匀分布,
(c)单丝(不扭成一束),
(d)面纱层的干燥厚度应该是最小10密耳,每10密耳干面纱产生10—15密耳树脂饱和的面纱层,和
(e)最小纤维长度应是0.5英寸。
注9——RTP层压材料的耐化学性由树脂提供。在与固化的树脂结合后,面纱帮助确定富树脂层的厚度,减少微裂隙,并提供非芯给(nonwicking)的耐化学性层。
在选择特定用途的面纱时其它需要考虑的包括以下几个方面:
(a)悬垂性(面纱应与模的形状相适应),
(b)干和温的抗张强度,
(c)粘合剂溶解能力(如果使用的话),
(d)均匀润湿,
(e)面纱应浸湿透,在层压过程中没有截留空气,和
(f)面纱不应该抑制树脂固化。”
面纱是当用树脂饱和(有时称作“浸湿”)时保持很高的树脂/增强比时的增强材料。热固性树脂是非常耐化学品的,而现有技术的面纱在许多情况下易受所含化学药品的侵蚀。如果现有技术的面纱暴露于所含的化学药品中,那么将因树脂的破裂,开始侵蚀增强材料,导致使用寿命缩短和设备故障。
现有技术的面纱通常由玻璃单丝或聚酯纤维制成。最常使用的单丝玻璃纤维在现有技术中已知的是“C”玻璃。用于面纱的最常使用的聚酯纤维是由E.I.Dupont de Nemours & Co.出售的,商标为Dacron。
相关技术的举例是下述美国专利:
美国专利5,077,115公开了包括热塑性母料的热塑性复合材料,它用涂敷陶瓷填料进行充分的填充。在本发明的重要特征中,陶瓷填料已用粘结于填料的橡胶状聚合物涂敷过。在一个优选的实施方案中,热塑性母料包括氟聚合物,优选氯氟聚合物,陶瓷填料是一种熔化无定形硅石,它用橡胶状聚合物材料进行涂敷过。这一发明的热塑性复合材料表现出很多优点,它非常适合用作粘合用膜,尤其是适合于制造多层印制电路接合物的粘合用膜。
美国专利4,943,473公开了一种柔性层压的含有氟聚合物的复合材料,其具有耐火和耐化学性,柔性复合材料由柔性纺织的、无纺的和编织的基材和含有氟聚合物的膜制成。
美国专利4,886,699公开了一种玻璃纤维增强的氟聚合物电路层压制品,该制品包括一层或多层夹在一层或多层“无规”微纤维玻璃增强的氟聚合物当中的氟聚合物浸渍的玻璃布。
美国专利4,886,689公开了一种母体—母体复合共混粘合剂和粘结非相容聚合物的方法,该粘合剂在粘合剂粘合层中用来粘结非相容的聚合物层。
美国专利4,777,351公开了一种包括导电性聚合物组合物的装置。
美国专利4,770,927公开了一种增强的氟聚合物复合物,它包括一种基材,该基材有一种包括全氟聚合物起始层的涂布母体和一种包括氟弹性体,氟塑料,氟弹性体/氟塑料共混物,或它们的结合物的外套层。起始层中的全氟聚合物可以是全氟塑料、全氟弹性体或它们的共混物。
美国专利4,677,017披露了热塑性氟聚合物与热塑性聚合物的共挤方法。共挤复合膜包括至少一种热塑性氟聚合物层和至少一种邻近该热塑性氟聚合物层的热塑性聚合物层。
美国专利4,539,113公开了完全由氟树脂制造的氟树脂过滤器,同时具有很高的耐腐蚀性和高耐热性。
美国专利4,505,971公开了一种具有橡胶化合物粘结层的氟塑料和金属层压制品,及将橡胶化合物粘接到氟塑料和/或粘接到金属上的方法和组合物。
美国专利4,163,505公开了可折叠的流体贮存罐的衬里,它是多面体形的衬里,垂直安置在圆柱形贮存罐的内侧,并安装在罐的内顶。
美国专利3,833,453公开了一种难燃的、纤维填充的、可冷成形的热塑性片材,它是玻璃纤维增强的乙烯/氯三氟乙烯复合物片材,可以通过在模具的外面温和地预热该片材,而单独地在环境温度下在模具中制成成形物体。
根据本发明,提供了一种耐腐蚀的热塑性氟聚合物面纱和具有热塑性氟聚合物的面纱的耐腐蚀的、增强的热固性塑料层压制品。
单独的绘制图是本发明多层层压制品的放大侧视图。
本发明是由氟聚合物制造的面纱,和利用本发明面纱的接触模压的、增强的塑料层压制品。本文所使用的接触模压法包括在ASTM C582—87、ASTM D4097—88中公开的接触模压法,以及在ASTM D3299—88和ASTM D4097—88中所公开的绕丝模压或制造。
本发明的面纱是由热塑性氟聚合物如氯三氟聚合物,四氟乙烯和全氟烷氧树脂,氟化乙烯丙烯的共聚物,聚氟乙烯和聚偏氟乙烯制成的。
本发明最优选的面纱是由乙烯和氯三氟乙烯的共聚物(有时称作ECTFE)如HALAR制得的纱,这在USP3,833,453中有描述,HALAR是乙烯和氯三氟乙烯的共聚物,由Ausimont USA,Inc.of Morristown,New Jersey出售并在HALARFLUOROPOLY-MER RESIN ADV ANT AGE.EXP ANDED LIST-CHEMICALRESIST ANCE OF HALARFLUOROPOLYMER中有说明。本发明最优选的面纱是熔喷法热塑性氟聚合物纤维过滤介质,由Ausi-mont USA,Inc.of Morristown,New Jersey出售并用HALAR出售。
增强材料除了面纱之外还包括短切原丝薄毡,方格布和由玻璃纤维制成的粗纱。如果需要还可使用其它增强纤维,但玻璃纤维是优选的。
本发明的优选层压制品使用热固性树脂。适宜的热固性树脂包括聚酯或乙烯基酯热固性树脂,和其它由酚类、呋喃类、环氧化物及类似物制成的热固性树脂。ASTM C582—87的1.1节指出可使用“热固性聚酯,乙烯基酯,或其它合格的热固性树脂层压材料”。在本发明中可使用的聚酯和乙烯基酯热固性树脂在ASTM C582—87的3.2节和3.3节中定义如下:
“3.2聚酯…由二羟基衍生物和二元有机酸或酸酐进行缩聚制得的树脂,其中至少一种组分促使形成烯属不饱和树脂,该树脂能与苯乙烯基单体化合和反应得到高度交联的热固性共聚物。
3.3乙烯基酯…特征在于活性不饱和键主要处在端部位置的树脂,该树脂能与苯乙烯基单体化合和反应得到高度交联的热固性共聚物。
注2——这些树脂按照与聚酯在制造RTP组分时同样的方式进行处理。”
理想地是,现有技术中周知的催化剂与用来形成本发明的层压制品的热固性树脂一起使用,引发化学反应,从而导致热固性树脂固化。典型的催化剂包括过氧化物类如丁酮过氧化物,氢过氧化枯烯及类似物。现有技术中周知的促进剂优选用来缩短热固性树脂的固化时间。典型的促进剂包括环烷酸钻、过氧化苯甲酰及类似物。
实施例
根据ASTM C582—87,按照以下方式接触模压耐腐蚀性层压制品的片材:
在制造该实施例的耐腐蚀层压制品时,由Ausimont USA,Inc.of Morristown,New Jersey出售的和从HALARR制造的熔喷热塑性氟聚合物过滤介质用作面纱。在制造该实施例的层压制品时使用的面纱具有3盎司/码2的重量,并表现出应用于静止或旋转模具时所需要的良好机械性能。具有1 1/2盎司/码2的重量的面纱不能表现出应用于旋转模具时所需要的机械性能,因而不能使用。
面纱纤维的平均纤维直径为7.9—8.5μm,其中“μm”是微米。面纱达到了良好的饱和或浸湿状态,同时有很高的树脂/增强比。该面纱允许截留的空气很容易地辊压出来,并能象普通的面纱一样很容易地通过衬里空隙检查。
该面纱有不同的两面。一面是“光滑的”,另一面是“模糊的”。在制备该实施例的层压制品时,模糊面是面向模具的。
在制造该实施例的耐腐蚀层压制品10时所用的热固性树脂是由Dow Chemical Company以商标Derakane 470—36出售的乙烯基酯树脂,并在Fabricating Tips—Derakane vinyl ester resins(引入本文作参考)和Derakane Resins Chemical Resistance and Engi-neering Guide(引入本文作为参考)有叙述。较好地,促进剂和催化剂与乙烯基酯树脂一起使用。按照Dow Chemical Company的介绍,乙烯基酯树脂Derakane 470—36用来制造层压制品10时,环烷酸钻用作促进剂和丁酮过氧化物用作催化剂。促进剂与树脂混合,然后加入催化剂引发放热反应。
用来增强层压制品10的短切原丝薄毡是“E”型玻璃纤维,11/2盎司/英尺2,经过上胶和使用与树脂相容的粘合剂,按照ASTM C582—87,5.2.2节的要求。
用来增强层压制品10的方格布是“E”型玻璃,24 1/2盎司/码2,5×4方形织物和使用与织物相容的粘合剂,按照ASTM C582—87,5.2.3节的要求。
根据ASTM C582—87,尤其是它的第6节来制造层压制品10,如在以下步骤中所列那样。
步骤1:将催化的乙烯基酯树脂的涂料施加在模具表面。模具是面向加工的那一面或者腐蚀性化学药品与层压制品10接触。
步骤2:使用一层面纱12,让模糊面朝向模具表面,然后使用齿形人力压辊将其辊压入模具表面上的催化的树脂中,消除截留的空气并将该层压成均匀厚度。
步骤3:施加第二层催化的乙烯基酯树脂的涂料。
步骤4:使用第一层1 4的1 1/2盎司/英尺2“E”型玻璃纤维短切原丝薄毡,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤5:施加第三层乙烯基酯树脂的涂料。
步骤6:使用第二层16的1 1/2盎司/英尺2“E”型玻璃纤维短切原丝薄毡,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤7:施加第四层乙烯基酯树脂的涂料,并让层压制件放热。
步骤8:施加第五层催化的乙烯基酯树脂的涂料。
步骤9:使用第三层18的1 1/2盎司/英尺2“E”型玻璃纤维短切原丝薄毡,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤10:施加第六层乙烯基酯树脂的涂料。
步骤11:使用第一层20的24 1/2盎司/码2方格布,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤12:施加第七层乙烯基酯树脂的涂料。
步骤13:使用第四层22的24 1/2盎司/英尺2“E”型玻璃纤维短切原丝薄毡,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤14:施加第八层乙烯基酯树脂的涂料。
步骤15:使用第二层24的24 1/2盎司/码2方格布,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤16:施加第九层乙烯基酯树脂的涂料。
步骤17:使用第五层26的24 1/2盎司/英尺2“E”型玻璃纤维短切原丝薄毡,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤18:施加第十层乙烯基酯树脂的涂料。
步骤19:使用第六层28的28 1/2盎司/英尺2“E”型玻璃纤维短切原丝薄毡,然后使用齿形人力压模将其辊压入该树脂中,消除空气截留并将该层压成均匀厚度。
步骤20:施加第十一层乙烯基酯树脂的涂料,并让层压制件放热。
让层压制品10完全固化,然后准备试验。从层压制品10上切下许多样品(标为A—F)进行试验。树脂涂敷的面纱12的固化厚度约为0.030英寸。根据每一表中所示出的ASTM试验操作程度测试样品A—F,结果记录在以下表1—5中。
表1中所示的抗张性能类似使用现有技术的面纱所达到的抗张性能。
表2中所示的挠曲性能高于使用现有技术的面纱所达到的挠曲性能,表明本发明的面纱和层压制品10具有更高的柔性。
表3中所示的面内剪切强度在含有本发明面纱的层12和含有短切原丝薄毡的层14之间进行测试。层12和14之间的平均面内剪切强度大约是3,300磅/英寸2,并且是可接受的。
耐磨性示于表4,并且是可接受的。而抗压缩性能示于表5。
HALAR氟聚合物(由它制造面纱)的耐化学品性示于表6。
表1
塑料抗张性能标准测试方法
ASTM D 638
试验样品加工(X)浇注( ) | 试验速度0.20英寸/分钟 | |||||||||
典型样品III | 试验温度/湿度(69°F/65%) | 测量长度 2.00英寸 | ||||||||
样品 | 宽度(英寸) | 厚度(英寸) | 面积(平方英寸) | 最大负荷(磅) | 抗张强度(磅/英寸2) | 断裂伸长率 | 模量(磅/英寸2) | |||
ABCDE | 1.0071.0051.0061.0121.013 | 0.2300.2320.2340.2350.232 | 0.2320.2330.2350.2380.235 | 32203470337033203300 | 13,90014,90014,30013,90014,000 | 1.1%1.2%1.2%1.1%1.1% | 1.90E+061.72E+061.74E+061.54E+061.52E+06 | |||
平均 = 14,200 | 平均 = 1.68E+06 | |||||||||
标准偏差= 424 | 标准偏差= 1.57E+05 |
表2
未增强的和增强的塑料和电绝缘材料的挠曲性能
ASTM D790
试验方法/程度=I/A | 全长/厚度比 L/D=@16/1 | 全长=4.00英寸 | |||||||
负载刀尖/支承半径=.12/.12 | 十字头移动速度=0.11英寸/分钟 | ||||||||
样品 | 宽度b | 厚度d | 最大负荷(磅) | 挠曲强度(磅/英寸2) | 斜度m | 弯曲模量(磅/英寸2) | |||
ABCDEF | 0.5860.5570.5580.5770.5640.573 | 0.2300.2270.2260.2300.2380.224 | 137.2125.0122.7140.2130.8134.7 | 26,60026,10025,80027,60024,60028,100 | 437043304000429046204120 | 9.81 E+061.06 E+079.94 E+069.78 E+069.72 E+061.02 E+07 | |||
平均= 26,500 | 平均= 1.00 E+07 | ||||||||
标准偏差= 1,270 | 标准偏差= 3.36 E+05 |
表3
增强塑料的面内强度的标准测试方法
ASTM D 3846
试验样品加工(X)浇注( ) | 试验温度/湿度(68°F/65%) | |||||
样品 | 宽度(英寸) | 厚度(英寸) | 面积(平方英寸) | 最大负荷(磅) | 剪切强度(磅/英寸2) | |
ABCDE | 0.4940.4800.4870.4810.482 | 0.2480.2480.2480.2500.250 | 0.1220.1190.1210.1200.120 | 399398371411411 | 32703340307034203420 | |
注:面内剪切试验在耐腐蚀/编织物层压制品粘结界面之间进行 | 平均 3300 | |||||
标准偏差 145 |
表4
塑料耐磨性能
ASTM D1242
注:耐磨性试验在层压制品的耐腐蚀面进行
试验方法/程度=A/固定磨耗 | 磨料:砂粒度/牌号=80/3M | |||||||
样品 | 宽度英寸 | 长度英寸 | 面积平方英寸) | 负荷磅 | 负载(磅/英寸2) | 试验持续期 | 体积损失(立方厘米) | |
ABCDE | 1.9351.9401.9901.9801.920 | 2.9152.9752.9402.9702.940 | 5.645.775.855.885.65 | 1010101010 | 1.771.731.711.701.77 | 1000回转1000回转1000回转1000回转1000回转平均标准偏差 | 6.466.306.216.276.436.330.11 |
表5
取向纤维组合物的抗压性能
ASTM D 3410
试验样品加工(X)浇注( ) | 片材/粘合剂整体 | |||||||
试验温度/湿度(68°F/65%) | 试验速度0.15英寸/分钟 | |||||||
样品 | 宽度(英寸) | 厚度(英寸) | 面积平方英寸 | 最大负荷(磅) | 抗压强度(磅/英寸2) | 弹性模量磅/英寸2 | ||
ABCDEF | 0.4950.4830.4840.4900.4850.488 | 0.1220.1210.1150.1140.1080.101 | 0.0600.0580.0560.0560.0520.049 | 1999.81994.21794.11939.11659.51677.5 | 33,33034,38032,04034,63031,91034,230 | 3.24E+063.49E+063.66E+063.58E+063.63E+063.92E+06 | ||
平均 | 33,420 | 3.59E+06 | ||||||
标准偏差 | 1,202 | 2.23E+05 |
表6
耐化学性的最高工作温度
化学药品 | 百分含量 | 可允许的最高温度F° | |
高级乙烯基酯热固性树脂 | HALAR | ||
甲醇 | 100 | 100 | 300 |
丁醇 | 100 | 120 | 300 |
氢氧化铵 | 10-20 | 150 | 300 |
苯胺 | 100 | 70 | 73 |
砷酸 | 全部 | 100 | 300 |
苯 | 100 | 100 | 150 |
硼酸 | 100 | 210 | 300 |
乙酸丁酯 | 100 | 80 | 150 |
四氯化碳 | 100 | 180 | 300 |
湿氯气 | 100 | 250 | 250 |
氯水 | 饱和 | 210 | 250 |
铬酸 | 10 | 150 | 212 |
铬酸 | 30 | N/R | 212 |
表6(续)
耐化学性的最高工作温度
化学药品 | 百分含量 | 可允许的最高温度F° | |
高级乙烯基酯热固性树脂 | |||
HALAR | |||
环己烷 | 100 | 150 | 212 |
洗涤剂 | 100 | 180 | 300 |
氯乙烷 | 100 | 80 | 300 |
二氯乙烷 | 100 | 80 | 73 |
乙二醇 | 全部 | 210 | 300 |
甲酸 | 98 | 100 | 250 |
氟利昂113溶剂 | 100 | 121 | |
无铅汽油 | 150 | 300 | |
盐酸 | 37 | 180 | 300 |
盐酸 | 10 | 150 | 300 |
盐酸 | 20 | 100 | 250 |
氢氧化钠 | 15 | 150 | 300 |
表6(续)
耐化学性的最高工作温度
化学药品 | 百分含量 | 可允许的最高温度F° | |
高级乙烯基酯热固性树脂 | HALAR | ||
氢氧化钠 | 25 | 180 | 250 |
次氯酸钠 | 5 | 180 | 250 |
硫酸 | 25 | 210 | 250 |
硫酸 | 75 | 120 | 250 |
硫酸 | 93 | N/R | 150 |
甲苯 | 100 | 120 | 120 |
二甲苯 | 100 | 120 | 120 |
虽然在上面已经详细地叙述了本发明的优选实施方案,还应明白,决不是由它们限制了本发明,本发明的范围由以下权利要求限定。
Claims (10)
1.一种增强的耐腐蚀性层压制品,包括热塑性氟聚合物的面纱。
2.权利要求1的层压制品,其中该热塑性氟聚合物是乙烯和氯三氟乙烯的共聚物。
3.权利要求2的层压制品,其中该热塑性氟聚合物是熔喷的。
4.权利要求2的层压制品,其中该层压制品是接触模压的。
5.根据权利要求1的层压制品,包括:
a.热固性树脂的起始层,其中有热塑性氟聚合物纤维薄毡,和
b.含有增强玻璃纤维的热固性树脂的第二层。
6.权利要求5的层压制品,其中该热塑性氟聚合物是乙烯和氯三氟乙烯的共聚物。
7.权利要求6的层压制品,其中该热塑性氟聚合物是熔喷的。
8.根据权利要求1—7中任一项的层压制品,其中该层压制品是接触模压的。
9.权利要求1—7中任一项的层压制品,其中该层压制品是由热固性树脂制成。
10.权利要求9的层压制品,其中该热固性树脂是乙烯基酯树脂。
Priority Applications (5)
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US08/043,200 US5534337A (en) | 1993-04-05 | 1993-04-05 | Thermoset reinforced corrosion resistant laminates |
CA 2120544 CA2120544A1 (en) | 1993-04-05 | 1994-04-05 | Thermoset reinforced corrosion resistant laminates |
EP19940105240 EP0622178A1 (en) | 1993-04-05 | 1994-04-05 | Thermoset reinforced corrosion resistant laminates |
CN94109476A CN1121866A (zh) | 1993-04-05 | 1994-08-15 | 热固性增强的耐腐蚀层压制品 |
US08/670,631 US5688600A (en) | 1993-04-05 | 1996-06-26 | Thermoset reinforced corrosion resistant laminates |
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US08/043,200 US5534337A (en) | 1993-04-05 | 1993-04-05 | Thermoset reinforced corrosion resistant laminates |
CN94109476A CN1121866A (zh) | 1993-04-05 | 1994-08-15 | 热固性增强的耐腐蚀层压制品 |
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EP (1) | EP0622178A1 (zh) |
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JPH01139629A (ja) * | 1987-11-26 | 1989-06-01 | Sumitomo Bakelite Co Ltd | 低誘電率熱硬化性樹脂積層板の製造方法 |
US4923737A (en) * | 1988-10-20 | 1990-05-08 | Northrop Corporation | Surface modified plastic and composite articles and method |
WO1991007278A1 (en) * | 1989-11-17 | 1991-05-30 | W.L. Gore & Associates, Inc. | Thin seam sealing tape |
US5077115A (en) * | 1990-05-08 | 1991-12-31 | Rogers Corporation | Thermoplastic composite material |
EP0492036A3 (en) * | 1990-12-20 | 1993-07-14 | E.I. Du Pont De Nemours And Company | Glass fiber-reinforced fluoropolymer compositions |
US5264276A (en) * | 1992-04-06 | 1993-11-23 | W. L. Gore & Associates, Inc. | Chemically protective laminate |
-
1993
- 1993-04-05 US US08/043,200 patent/US5534337A/en not_active Expired - Fee Related
-
1994
- 1994-04-05 EP EP19940105240 patent/EP0622178A1/en not_active Withdrawn
- 1994-04-05 CA CA 2120544 patent/CA2120544A1/en not_active Abandoned
- 1994-08-15 CN CN94109476A patent/CN1121866A/zh active Pending
-
1996
- 1996-06-26 US US08/670,631 patent/US5688600A/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112440488A (zh) * | 2019-08-27 | 2021-03-05 | 科展材料科技股份有限公司 | 复合材料的制造方法 |
Also Published As
Publication number | Publication date |
---|---|
CA2120544A1 (en) | 1994-10-06 |
EP0622178A1 (en) | 1994-11-02 |
US5688600A (en) | 1997-11-18 |
US5534337A (en) | 1996-07-09 |
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