CN1024980C - 有机聚合物膜层上的非照像构图方法 - Google Patents
有机聚合物膜层上的非照像构图方法 Download PDFInfo
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- CN1024980C CN1024980C CN90109505A CN90109505A CN1024980C CN 1024980 C CN1024980 C CN 1024980C CN 90109505 A CN90109505 A CN 90109505A CN 90109505 A CN90109505 A CN 90109505A CN 1024980 C CN1024980 C CN 1024980C
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Abstract
在有机聚合物膜层上的非照像构图方法,包括下列步骤:
a)在基片上涂敷无图形的第一层,该层包含分散在预定的洗脱液中的固体有机聚合物;
b)在无图形的第一层上涂敷已构成图形的第二层,第二层中包含能改变固体有机聚合物在预定洗脱液中的分散率的改变剂;
c)使分散率改变剂按已构成的图形扩散进埋在下面的固体有机聚合物层中;和
d)用预定的洗脱液清洗,除去可以分散在洗脱液中的埋在下面的固体有机聚合物的区域。
Description
本申请是美国申请07/425387、申请日为1989年10月20日的待审查专利申请的部分后续申请。
本发明涉及一种有机聚合物膜层上的非照像构图方法,具体的说该方法用于制造单层和多层电子器件,例如厚膜混合电路。
厚膜技术历来重视导体、介质和电阻器制造方法的稳定性和可靠性。这些技术应适合于生产那些生产周期短的,价格经济的产品。在多层结构中的构图能力应该能制出具有电路密度极高的器件。在多层结构中,各导体层由介质层隔开,并由穿过介质层的通孔使它们内连接。
多层结构的制作费用比单层结构制作费用高得多,因为,制作多层结构必须严格检验,使层与层之间对准,并要仔细操作以防止产生砂眼和裂纹。
减少这些涉及多层产品的问题的最明显的途径是减小线条和间隔的尺寸,从而减少给定结构中的层数。这些问题的解决受厚膜丝网印刷分辨率的限制,限定电路层间连接通孔的直径0.25-0.38mm。同样,批量生产时,导体的最细线宽及导线间隔限定在0.125-0.175mm。
人们试图用各种不同的方法获得较细的栅状线条和小的通孔。用极细的网目和改进后的乳胶底板使线条的分辨率在产量有限的情况下能达到4密耳/间距。已开发的光刻胶能使通孔达0.125mm或更小,线/间隔栅状线条宽达0.025-0.038mm、厚膜金属的构图是用光刻胶
和蚀刻法制出细线图形、并镀一层薄膜导体,制成具有高电导率的细线图形。
上述所有方法均有各自的缺点。例如,细目丝网的典型印刷层制成的导体层和介质层均比所要求的薄。光刻胶中有大量有机物,在烧结过程中这些有机物使收缩量增加,并且会出现烧毁,使烧结后的产品报废。用光刻胶制成的导体有不希望的卷边,带卷边的电路的可靠性降低,所有工序都需刻蚀、涂光刻胶、或镀敷,这种工艺方法是漫长的,对工艺敏感而又昂贵的。
本发明提供一种在有机聚合物膜层上的非照像构图方法,它包括下列顺序的步骤:
a)在基片上涂复无图形的第一层,该涂层包含能分散在预定洗脱液中的固体有机聚合物;
b)在无图形的第一层上涂复有图形的第二层、第二层中包含一种能改变固体有机物在预定洗脱液中的分散率的改变剂;
c)分散率改变剂按已构成的图形扩散到埋在下面的第一层中;和
d)用预定的洗脱液清洗、除去可溶于洗脱液的埋在下面的第一层上的面积。
本发明既可以用于制作正像图形,也能用于制作负像图形。
制作负像图形时本方法包括下列顺序步骤:
a)在基片上涂复无图形的第一层,该层包含固体有机聚合物;
b)在无图形的第一层上涂复有图形的第二层,第二层包含一种固体有机聚合物的粘性悬浮液,分散率改变剂和一种任选的溶剂,分散率改变剂<1>是第一层有机聚合物的分散剂,(2)它在常压下的
沸点高于溶剂;
c)干燥有图形的第二层,除去其中的溶剂,并使分散率改变剂按已构成的图形扩散到埋在下面的第一层有机聚合物中;和
d)用洗脱液清洗,除去有图形的第二层和埋在下面的第一层中按照已构成的图形扩散过的区域,第二层和第一层中按已构成的图形扩散过的区域可以分散在所述的洗脱液中。
制作正像图形时,该方法包括下列步骤:
a)在基片上涂复无图形的第一层,该层包含可分散在预定溶剂的固体有机聚合物;
b)在无图形的第一层上涂复有图形的第二层、第二层包含能降低有机聚合物在溶剂中的分散率的分散率改变剂。
c)加热有图形的第二层,使分散率改变剂按已构成的图形扩散到埋在下面的第一层有机聚合物层中,并降低第一层有机聚合的已构图区域在溶剂中的分散率;和
d)用预定的溶剂清洗,除去埋在下面的第一层中无构图区域。
附图中包括两幅图。图1是用本发明方法制作负像图形的示意图。图2是用本发明方法制作正像图形的示意图。
图1表示在有机聚合物膜上用非照像法制作负像图形的方法,它包括下列步骤:
a)在基片1上涂复无图形的第一层固体有机聚合物层3;
b)在无图形的第一层固体有机聚合物层3上涂复有图形的第二层5,第二层包含由固体有机聚合物,增溶剂和溶剂组成的溶液,增溶剂(a)可溶于第一层有机聚合物层3的聚合物中,(b)其常压下的沸点高于溶剂;
c)加热有图形的第二层,除去其中的溶剂,并使增溶剂按已构成的图形扩散到埋在下面的第一层有机聚合物层3a中;
d)在第二种溶剂中清洗,除去有图形的第二层5和埋在下面的第一层固体有机聚合物层中按构成的图形扩散的区域,第二层5的固体有机聚合物和第一层3的按已构成图形的扩散层能溶于第二溶剂。
图2表示在有机聚合物膜层上用非照相法制作正像图形的方法,它包括下列步骤:
a)在基片11上涂复无图形的第一层13,该层包含可溶于预定溶剂的固体有机聚合物;
b)在无图形的第一层13上涂复有图形的第二层15,第二层包含一种能降低有机聚合物在溶剂中的溶解度、本身不溶于所说溶剂的阻溶剂;
c)加热有图形的第二层,使阻溶剂按已构成的图形扩散到埋在下面的第一层有机聚合物层13中,使第一层中按已构成的图形扩散的区域13a的聚合物不溶于上述溶剂;和
d)用预定溶剂清洗,除去埋在下面的第一层13上没构成图形的区域。
假若有图形的第二层15中的阻溶剂已耗尽的区域的聚合物可溶于上述溶剂,那么,该区域的聚合物在用溶剂清洗过程中会被除去。另一方面,假若有图形的第二层15中的阻溶剂已耗尽区域的聚合物不溶于上述的溶剂,那么,在用溶剂清洗之后,该区域的聚合物会留下。
所用术语的定义
所用术语的含义如下:
术语“洗脱液”是指任何一种流体,可以是液体,也可以是气体,它能以溶解或其他方式使埋在下面的无图形层变成可分散状态。
术语“可分散的”是指就给定的材料膜层而言,利用清洗液的物理或化学作用,或用卸去的方法将其排去或除去。
术语“易挥发的溶剂”是指在一个大气压下,在120℃或更低温度时能被蒸发除去的任何一种溶剂。
通过下列几种途径可以除去埋在下面的聚合物层中按已构成的图形扩散的区域:
(1)将按照已构成图形扩散的区域内的聚合物溶解在溶剂中,并清洗掉所生成的溶液;
(2)使按照已构成的图形扩散的区域内的聚合物分解,并清洗掉和/或蒸发掉分解物
(3)用一种洗涤剂使按已构成的图形扩散的区域内的聚合物乳化,并用水溶性清洗液除去分散物;
(4)用溶剂和/或塑化作用,使按已构成的图形扩散的区域内的聚合物软化,降低它与基片的粘结力,将软化膜从基片上除去。
(5)使按已构成的图形扩散的区域内的聚合物电离,并用水溶性离子液洗掉基片上已电离的聚合物;
(6)使按已构成图形的区域内的聚合物不溶解,除去该区域以外的聚合物膜。
下面对本发明详细说明。
A、基片
本发明的方法既能用于无机基片上,如Al2O3,SiO2,硅,AlN
及其类似材料的基片,也能用于有机材料基片上、如聚酰亚胺,苯氧基树脂,环氧树脂及其类似材料的基片,或用于复合材料基片,如填充了有机聚合物的基片。
B有机聚合物
许多种固体有机聚合物可用作一层或两层聚合物层的材料,只要它们基本上是非结晶体,和本身具有适当的溶解度特性,或加入增溶剂或阻溶剂后具有合适的溶解度特性。
两层聚合物的基本特性是聚合物在自然状态必须基本上是非晶体的。这里所用的术语“非结晶聚合物”是指结晶度不超过大约50%的聚合物。这种实质上非结晶度主要是为了有图形的第二层(聚合物层)中的溶解度改变剂能容易地扩散到下面的聚合物层中,能在本发明方法中使用的多种类型的非结晶聚合物如下:
Ⅰ、按聚合的方法分:
加聚物
缩聚物
Ⅱ按物理特性分
可水解的聚合物
可交联的聚合物
热塑性聚合物
可电离的聚合物
热固性聚合物
弹性体
Ⅲ按成分分
聚碳酸酯纤维类
聚酰亚胺类
聚酯类
链烯烃共聚物类
聚丙烯酸酯类(包括异丁烯酸酯类)
聚苯乙烯
苯氧基树脂类
酚醛树脂类
纤维素聚合物
聚(乙酸乙烯酯)
聚(乙烯醇缩丁醛)
聚(氯乙烯)
聚(氯乙烯-乙酸乙烯酯)
C、组成和应用
本发明的方法首先用来制造厚度小的膜层,例如用来制造电子元器件。特别是,第二层聚合物的厚度在10至30微米的范围内。而第一层聚合物可以更厚一些,在10至100微米的范围内。图形层的厚度主要受所用方法的限制,而不考虑可操作性。
第二层中必须有足够量的增溶剂,使一定量的增溶剂扩散到埋在下面的第一层中。因此第二层中应含有至少10%重量的增溶剂,可以多达90%重量,增溶剂的含量由各种聚合物的溶解度决定。
因此,在某些情况下,可能需要给埋在下面的第一层中加入增塑剂或其他增溶剂,使从第二层聚合物中扩散下来的增溶剂容易对聚合物起作用。
总之,用本发明的方法制备元件层的单个工艺步骤类似于本领
域普通技术人员所公知的常规厚膜技术,未烧结的生料带技术和聚合物技术的那些工艺步骤。因此,下列各工艺步骤本身可能不是新的,但是本发明采用了所列举的组成和制造材料的最佳方法。
1、工艺浆料的制备和介质底层印刷(underprint)
a)预碾磨;将介电的无机物成分在球磨机中一起研磨使其预分散,例如同大约同等重量的甲醇或异丙醇一起研磨30至90分钟,然后倒出,放置2至16小时,使固体物沉淀下来。然后倒掉浮在上面的醇类,将固体物在氮气气氛下干燥,减少在室温下爆炸的可能性;当固体物干透时放在炉窑中干燥一小时。
b、载体的制备:将溶剂,树脂,抗氧化剂和叔-丁基蒽醌一起加入树脂釜中,加热至溶解。制备浆料之前,溶液中可任意加入润湿剂。若将树脂和溶剂加热到最高温度140℃,然后冷却到70℃,加入亚诺抗氧化添加剂(2,6-二叔丁基对甲酚(Ionol)),叔丁基蒽醌,及任意的湿润剂,因此,树脂和溶剂在各种浆料中有最佳效果。湿润剂也可以在制备浆料工序之后加。
C、浆料制备:将预分散的固体物与载体和其他有机成分充分混合制成浆料。然后研磨到获得令人满意的粉碎尺寸(约12/8μm或更好)。研磨之前可从组分中留出小部分载体和/或溶剂,在研磨之后再加入足够量的载体和/或溶剂,达到所需粘度。最终的组成中溶剂或树脂的含量可以略高于或略低于配方中规定的量。
达到最佳效果的增塑剂量也可以随浆料批号的变化而略有变化。因此,研磨之前也可以从组成成份中扣除少量增塑剂。实际制作过程中,按本厂主批量试验几种组成,然后按最佳组成确定实际的载体和无机固体物的混合物组成。
2、导体底层印刷(Conductor Underprint)
a)载体制备:载体制备与介质底层印刷中的载体制备完全相同。
b)浆料制备:将导体无机物组成分与上述载体和其它有机物组份充分混合。然后将混合物研磨至令人满意的粉碎尺寸(约15/8μm或更好)。研磨之前可以留出一些溶剂,载体和/或增塑剂,使这些组份量最后达到最佳值。研磨和组成工艺与介质制备所用工艺类似。
3、图形套印
制备载体:在高温下将乙基纤维素树脂预溶于由增塑剂和溶剂制成的溶液中制成载体,有助于浆料组成过程中各组分充分混合。载体制备中不是最终组成中的所有溶剂和/或增塑剂都用,因为这些组分中的一些组分可以在研磨后有选择地加入,使在最终组成中它们有最佳量。因此,最终组成中的组分量同本文所给配方不完全相同。因而,所制成的浆料会略有变化。
4浆料制备和印刷
不包含在载体中的图形浆料的无机成分和有机成分与上述的载体充分混合。然后将混合物研磨至令人满意的粉碎尺寸(约15/8μm或更好)。研磨之前可以留出一些溶剂、载体,和/或增塑剂,使这些成分最后达到最佳量。研磨和组成技术与制备介质的那些技术类似。
介质浆料的典型印刷方法是,用200目的丝网,橡皮刮板的涂复速度为每秒一至两英寸印刷两次。图形浆料以较快的速度盖印在介质上,因为丝网仅有小部分是开目的。
用325到400目的丝网印刷导体浆料。网目的选择取决于所要求的导体厚度和分辨率。图形浆料同样用325目到400目的丝网印刷,
使供给底层印刷的增塑剂量达到最佳量。与印刷介质层比较,这里需用较薄的丝网和较少的印刷次数,因为所用的典型的导体膜层较薄。
与其它构图方法
本发明的扩散构图法的优点之一是、能用一层较薄的图形涂层给较厚的底层印刷图形。例如,给底层印刷图形的构图剂如邻苯二甲酸苯甲基丁酯的厚度为底层印刷层厚度的5至10倍。因此,用该方法可以做出非常精确的厚膜图形。例如,用丝网印刷要获得实施例1中的混合物的相同厚度,淀积的厚膜浆料应精确校准到75至175微米(3至7密耳),同时防止浆料流入4密耳小的通孔中。
利用相当薄的薄片印刷而在非常厚的膜层上制作图形的能力已经导致了其它的构图方法,这些方法在生产率方面优于丝网印刷。除丝网印刷外,我们已经证实,用实施例1中的材料通过软片绘图(flexographic)的方法制作图形时,构图浆料是从印刷板转移到下面的介质印刷层上,然后扩散并显影的。用软片绘图(flexograp hic)法的生产潜力大大优于丝网印刷。典型的丝网印刷当速度为每小时26000-32500cm2就是高生产速度了。软版绘图系统或凸片印刷系统,用扩散构图,能达到每分钟39000-130000cm2,并有较好的分辨率。
图形印刷用的其他方法如下:(1)不用制作厚图或曝光板而用绘图仪上的笔直接绘出标准图;(2)用类似市售的计算机打印机的墨汁喷咀印刷头绘图;(3)用固体溶解度改变剂如合适的增塑剂,树脂,酸或碱用激光印刷机对底层印刷调色。
为了充分利用本发明所展示的优点,最好优先采用不同于丝网
印刷的底层印刷(underprimt)如采用模带形式。已构图部分的显影可以成批处理以保持同系统的其他产出协调一致,烘烤也可以在大炉窑中成批处理以适应大量生产。接着,聚合物技术领域中的专业人员将会认识到,每种类型的聚合物应与许多不同类型的增塑剂或不挥发性溶剂相容。因此,适用的聚合物/溶剂/非溶剂混合物有无数种。下面是本发明实际使用的市售的几种聚合物,增塑剂和溶剂/非溶剂系统的几个例子。
D、扩散构图用聚合物/增塑剂混合物
1、乙酸纤维素
合适的增塑剂是柠檬酸三乙酯、柠檬酸乙酰三乙酯、环氧型增塑剂、乙酸甘油酯(单、双、三)、己二酸二甲酯、己二酸十三酯、壬二酸双正-己酯,乙二醇二乙酸酯,二甘醇酯类及衍生物,三甘醇酯类(例如,甲基、乙基、丙基、丁基),二-和三-丙二醇酯类。也有由美国纽约Dover化学公司供应的长链烃类和芳烃类、氯化石蜡类,磷酸三甲苯酯,邻苯二甲酸烷基酯类(二甲基至二丁基),癸二酸二甲酯,和磺酸衍生物类、如邻甲苯磺酰胺和对甲苯磺酰胺。
2 乙酸丁酸纤维素
合适的增塑剂是:柠檬酸酯类(乙基至丁基)乙酰环氧硬脂酸酯类,二乙酸丙三醇酯和三乙酸丙三醇酯、己二酸二甲酯和己二酸二
丁酯,己二酸十三烷基酯,己二酸二己基酯,二甘醇二壬酸酯,二丙二醇辛酸酯类和二丙二醇庚酸酯类,烃类,蔗糖乙酸酯异丁酸酯,间苯二甲酸二辛酯,甘油单月桂酸酯,偏苯三酸三辛酯,偏苯三酸三异癸酯,肉豆蔻酸异丙酯、肉豆蔻酸正-丁酯,油酸丁酯,油酸四氢糠酯,氯化石蜡类及其衍生物,磷酸烷基酯(三乙基至三丁基),磷酸三甲苯酯,磷酸三苯酯,磷酸苯基三异丙酯,磷酸三-二甲苯酯、苯二甲酸酯类(二甲基至二己基)混合醇邻苯二甲酸酯类,如邻苯二甲酸苯甲基丁酯、邻苯二甲酸丁基-乙基己基酯,邻苯二甲酸双环己酯,各种聚酯类,蓖麻酸甲酯,癸二酸二甲酯,许多硬脂酸的衍生物,如硬脂酸烷基酯(丙基至辛基),1,2-丙二醇单硬脂酸酯,和对苯二酸二辛酯。
3 硝酸纤维素
硝酸纤维素与许多稀有的增塑剂相容。一些增塑剂是:松香酸的酸性酯类(松香甲酯),乙酸酯类(乙酸枯苯酯),己二酸衍生物(例如,己二酸苯甲基辛酯,己二酸二异癸酯,己二酸十三烷基酯),壬二酸酯类,如,壬二酸二异辛酯,二苯甲酸二甘醇酯,二苯甲酸三甘醇酯、柠檬酸酯类,如柠檬酸三乙酯,环氧型增塑剂,聚乙烯甲醚,丙三醇单乙酸酯,丙三醇二乙酸酯和丙三醇三乙酸酯,乙二醇二乙酸酯,聚乙二醇200至1000,邻苯二甲酸酯类(二甲基至二丁基),间苯二甲酸酯类(二甲基,二异辛基,二-2-乙基己基),苯六甲酸酯类,如三苯六甲酸三辛酯,三苯六甲酸异辛基异癸基酯,肉豆蔻酸异丙酯),油酸甲酯和油酸丙酯、棕榈酸异丙酯和棕榈酸异辛
酯,氯化石蜡、磷酸衍生物,如磷酸三乙酯,磷酸三丁酯,磷酸三丁氧基乙基酯、磷酸三苯酯,聚酯类,癸二酸二丁酯,癸二酸二辛酯、硬脂酸酯类,如硬脂酸辛酯,硬脂酸丁氧基乙酯、单硬脂酸1,4-丁二醇酯,蔗糖衍生物类如蔗糖八乙酸酯,磺酸衍生物,如苯磺甲酰胺,或对苯二甲酸二辛酯。
4、乙基纤维素
大多数与硝酸纤维素相容的增塑剂也与乙基纤维素相容。因此乙基纤维素与许多增塑剂相容。一些增塑剂是:松香酸的酸性酯(松香甲酯)、乙酸酯类(乙酸枯苯酯),己二酸衍生物类(例如己二酸辛苄酯,己二酸二异癸酯,己二酸十三烷基酯),壬二酸酯类,如壬二酸二异癸酯,二苯甲酸二甘醇酯,二苯甲酸三甘醇酯,柠檬酸酯类、如柠檬酸三乙酯,环氧型增塑剂,聚乙烯甲醚,单乙酸甘油酯,二乙酸甘油酯,三乙酸甘油酯,二乙酸乙二醇酯,聚乙二醇200至1000,邻苯二甲酸酯类(二甲基至二丁基),间苯二甲酸酯类(二甲基,二异辛基,二-2-乙基己基),苯六甲酸酯类,如三苯六甲酸三辛酯,三苯六甲酸异辛基异癸基酯、肉豆蔻酸异丙酯、油酸甲酯和油酸丙酯,棕榈酸异丙酯和棕榈酸异辛酯,氯化石蜡,磷酸衍生物类,如磷酸三乙酯,磷酸三丁酯,磷酸三丁氧基乙基酯,磷酸三苯酯,聚酯类,癸二酸二丁酯,癸二酸二辛酯,硬脂酸酯类如硬脂酸辛酯、硬脂酸丁氧基乙酯、1,4-丁二醇单硬脂酸酯,蔗糖衍生物如蔗糖八乙酸酯,磺酸衍生物类,如苯磺甲酰胺或对苯二甲酸二辛酯
5 聚苯乙烯
典型的增塑剂是松香酸甲酯,氢化松香酸甲酯、己二酸苯甲基辛酯,许多己二酸烷基酯(丁基到癸基和混合酯类),壬二酸酯类如二-2-乙基己基壬二酸酯、一些苯甲酸酯类,如二苯甲酸二甘醇酯,柠檬酸衍生物如柠檬酸三-正丁酯,油酸酯类,如油酸甲酯、氯化石蜡,磷酸烷基酯类和磷酸芳基酯类,如磷酸三丁酯或磷酸三甲苯酯,许多邻苯二甲酸酯类如邻苯二甲酸二甲酯,邻苯二甲酸二丙脂,邻苯二甲酸二丁酯,或邻苯二甲酸二辛酯,邻苯二甲酸苯甲基丁酯,和邻苯二甲酸的烷基芳香基混合酯。还有,蓖麻油酸酯类和癸二酸酯类;某些硬脂酸酯类,如硬脂酸正-丁酯;聚α-甲基苯乙烯;和对苯二甲酸二辛酯
6 聚(乙酸乙烯酯)
增塑剂是磺酸衍生物类,如邻甲苯磺酰胺和对甲苯磺酰胺;蔗糖衍生物类如蔗糖八乙酸酯;一些硬脂酸酯类,如丙三醇三乙酸基硬脂酸酯;癸二酸二苄酯;蓖麻油酸酯类;聚酯类;某些邻苯二甲酸酯类如邻苯二甲酸二丁酯和邻苯二甲酸丁苄酯;大多数磷酸酯类,如磷酸三丁酯类和磷酸三苯酯类;大多数氯化石蜡;一油酸甘油酯;二-正-丁基马来酸酯;某些乙二醇衍生物类例如聚乙二醇二-(2-乙基己酸酯)。还有柠檬酸酯和柠檬酸三乙酯或柠檬酸三-正-丁酯。
7 聚乙烯醇缩丁醛
松香酸甲酯,乙酸枯苯酯,己二酸二丁酯,己二酸二-2-乙基己酯;还有,己二酸十三烷基酯、二己二酸二甘醇酯,聚乙二醇(200)二苯甲酸酯,氢化三联苯、柠檬酸烷基酯类,如棕檬酸三乙酯,柠檬酸三-正-丁酯;环氧化豆油;环氧化树脂酸酯;枯苯基苄基醚;二丙二醇二辛酸酯;三甘醇三壬酸酯;少数烃类增塑剂;间苯二甲酸二异辛酯;甘油-月桂酸酯;苯六甲酸三异壬酯;油酸正-丙酯;甘油-油酸酯;许多氯化石蜡;季戊四醇四异戊酸庚酸酯;许多磷酸酯如磷酸烷基酯(三丁基,三-2-乙基己基,三苯基等),磷酸三氯丙酯,磷酸二苯辛酯、磷酸二苯-二甲苯酯,苯异丙基苯磷酸酯。还有许多邻苯二甲酸酯,如邻苯二甲酸二甲酯,邻苯二甲酸二乙酯,邻苯二甲酸二丙酯,邻苯二甲酸二丁酯、邻苯二甲酸苯甲基丁酯,邻苯二甲酸二辛酯(dioctyl or dicapry1 phthalate);混合的邻苯二甲酸酯类;邻苯二甲酸双十三烷基酯;还有聚酯类;某些蓖麻油酸酯,如蓖麻油酸甲基乙酰酯;硬脂酸酯类,如,甘油三-乙酸基硬脂酸酯。还有邻甲苯-乙基磺酰胺和对甲苯-乙基磺酰胺。
8 聚氯乙烯
松香酸甲酯,乙酸枯苯酯,己二酸二丁酯,己二酸二-2-乙基己基酯;还有己二酸十三烷基酯、二己二酸二甘醇酯,聚乙二醇(200)二苯甲酸酯,氢化三联苯,柠檬酸烷基酯,如柠檬酸三乙酯,柠檬
酸三-正-丁酯;环氧化豆油;环氧化树脂酸酯;枯苯苄基醚;二辛酸二丙二醇酯;三壬酸三甘醇酯;少数烃类增塑剂;间苯二甲酸二异辛酯;甘油-月桂酸酯;苯六甲酸三异壬基酯;油酸正丙酯;甘油一油酸酯;许多氯化石蜡;季戊四醇四异戊酸庚酸酯;许多磷酸酯类,如磷酸烷基酯(三丁基,三-2-乙基己基,三苯基等),磷酸三氯丙酯,磷酸二苯基辛酯,磷酸二苯基二甲苯酯,磷酸苯基异丙基苯基酯。还有许多邻苯二甲酸酯,如邻苯二甲酸二甲酯,邻苯二甲酸二乙酯,邻苯二甲酸二丙酯,邻苯二甲酸二丁酯、邻苯二甲酸丁苄酯,邻苯二甲酸二辛酯;混合的邻苯二甲酸酯类;邻苯二甲酸双十三(烷)酯;还有聚酯类;某些蓖麻油酸酯,如蓖麻油酸甲基乙酰酯;硬脂酸酯类,如甘油三-乙酸基硬脂酸酯;还有许多其它的环氧型增塑剂;还有合适的:聚乙二醇二-2-乙基己酸酯;癸二酸二丁酯;癸二酸二辛酯和癸二酸二壬酯;和对苯二甲酸二辛酯。
9 氯乙烯/乙烯基乙酸酯共聚物
松香酸甲酯,乙酸枯苯酯,己二酸二丁酯,己二酸二-2-乙基己酯;还有己二酸十三烷基酯、二己二酸二甘醇酯,聚乙二醇(200)二苯甲酸酯,氢化三联苯,柠檬酸烷基酯类,如柠檬酸三乙酯,柠檬酸三-正-丁酯;环氧化豆油;环氧化树脂酸酯;枯苯基苄基醚;二丙二醇二辛酸酯;三甘醇三壬酸酯;少数烃类增塑剂;间苯二甲酸二异辛酯;甘油一月桂酸酯;苯六甲酸三异壬酯;油酸正-丙酯;甘油-油酸酯;许多氯化石蜡;季戊四醇四异戊酸庚酸酯;
许多磷酸酯如磷酸烷基酯(三丁基,三-2-乙基己基,三苯基等),磷酸三氯丙酯,磷酸二苯辛酯,磷酸二苯二甲苯酯,苯异丙苯磷酸酯。还有许多邻苯二甲酸酯、如邻苯二甲酸二甲酯,邻苯二甲酸二乙酯,邻苯二甲酸二丙酯,邻苯二甲酸二丁酯,邻苯二甲酸丁基苄基酯,邻苯二甲酸二辛酯;混合的邻苯二甲酸酯类;邻苯二甲酸双十三烷基酯;还有聚酯类;某些蓖麻酸酯类,如蓖麻油酸甲基乙酰酯;硬脂酸酯类如甘油三乙酸硬脂酸酯。还有许多其他环氧类增塑剂;合适的还有:聚乙二醇二-2-乙基己酸酯;癸二酸二丁酯;癸二酸二辛酯和癸二酸二壬酯;和对苯二甲酸二辛酯。
10 聚甲基丙烯酸甲酯
相容的增塑剂是:松香酸甲酯、樟脑,乙酸枯苯酯、己二酸辛酯和己二酸壬酯,二丙基乙二醇二苯甲酸酯,聚乙二醇(200)二苯甲酸酯,季戊四醇四苯甲酸酯,二甘醇酯类和三甘醇酯类,某些氢化类增塑剂,苯六甲酸酯类如三苯六甲酸三异壬酯,肉豆蔻异丙酯,油酸异丙酯、乙二醇-丁基醚油酸酯,氯化石蜡类,磷酸酯,如磷酸三乙酯和磷酸三丁酯,磷酸叔丁基二苯酯,磷酸三甲苯酯,磷酸烷基芳基酯;许多邻苯二甲酸酯类如邻苯二甲酸二丁酯;邻苯二甲酸二丙酯,或邻苯二甲酸十二酯;还有邻苯二甲酸丁基苄酯;邻苯二甲酸二辛酯;邻苯二甲酸二癸酯或邻苯二甲酸二环己酯。还有癸二酸二丁酯或癸二酸二辛酯;其它的癸二酸酯;蔗糖苯甲酸酯;和对苯二甲酸酯,如对苯二甲酸二辛酯。樟脑也是有用的增塑剂。
E、扩散构图用的溶剂/非-溶剂系统
1、乙酸纤维素
溶剂:
二氯甲烷/甲醇,三氯甲烷/甲醇,苯甲醇,苯酚类,乙二醇乙醚类,二噁烷,二乙醇胺,吡啶,苯胺,丙酮,环己酮,甲酸、乙酸,乙酸甲酯、乙酸乙酯/硝基苯、乙二醇-乙基醚乙酸酯、硝基甲烷。
非溶剂:
烃类、脂族醚、弱无机酸。
2、乙酸丁酸纤维素
溶剂:
苯、甲苯(热的),三氯甲烷,四氯化碳,四氯乙烷,甲醇(热的),丙酮,环己酮,二噁烷,脂族酯类,硝基乙烷。
非溶剂:
脂族烃、甲醇(冷的),乙醇,(二)乙醚。
3、硝酸纤维素
溶剂:(N表示氮含量)
12%>N>10.5%:
醇类(较低的),醇/(二)乙醚,丙酮,乙酸戊酯,乙二醇醚类,乙酸(水的)。
N≥12%:
卤代烃类,乙醇/(二)乙醚,丙酮,甲基戊基酮,环己酮,乙
酸甲酯、乙酸乙酯,丁酸乙酯,乳酸乙酯,乙二醇醚乙酸酯类、碳酸亚乙酯,呋喃衍生物,硝基苯。
非溶剂:
12%>N>10.5%:
较高的醇类,较高的羧酸类,较高的酮类,磷酸三甲苯酯。
N≥12%;
脂族烃类,芳香烃类,较低的醇类,较高的醇类(SW),1,2-亚乙基二醇,二乙基醚,稀羧酸,水。
4、乙基纤维素
溶剂:<D.S表示用乙氧基基团取代的程度)
D.S=1.0至1.5:
吡啶,甲酸,乙酸,水(冷的)。
D.S.=2:
二氯甲烷,三氯甲烷,二氯乙烯,氯代醇类,乙醇,四氢呋喃(THF)。
D.S.=2.3:
苯、甲苯、卤代烷基物,醇类,呋喃衍生物、酮、乙酸酯类,二硫化碳,硝基甲烷。
D.S.=3.0:
苯、甲苯、二氯甲烷、醇类、酯类。
非溶剂:
D.S.=1.0至1.5:
乙醇。
D.S.=2.0:
烃类、四氯化碳,三氯乙烯,醇类,(二)乙醚,酮类,酯类,水。
D.S.=2.3:
1,2-亚乙基二醇,丙酮(冷的)。
D.S.=3.0:
烃类,萘烷,二甲苯,四氯化碳,四氢糠醇,二醇类,正-丙醚。
5、聚苯乙烯
溶剂:
环己烷(>35℃),环己烷/丙酮,甲基环己烷/丙酮,萘烷/草酸二乙酯,苯,甲苯,乙基苯,苯乙烯,较低的氯代脂族烃,苯酚/丙酮,四氢呋喃(THF),二甲基四氢呋喃,二噁烷,丁酮:二异丙酮,环己酮,乙二醇缩甲醛、乙酸乙酯,乙酸丁酯,邻苯二甲酸甲酯,邻苯二甲酸乙酯,邻苯二甲酸正-丁酯,1-硝基丙烷,二硫化碳,磷酸三丁酯,三氯化磷。
非溶剂:
饱和烃类,醇类,苯酚,二醇类,2-氯乙醇,全氟代苯,1、2、3、4-四氟代苯(低于10℃),二乙醚,乙二醇醚,丙酮,乙酸,邻苯二甲酸异丁酯,邻苯二甲酸甲基己酯、磷酸三(氯乙)酯,磷酸三甲苯酯。
6、聚乙酸乙烯酯
溶剂:
苯,甲苯,三氯甲烷,四氯化碳/乙醇,二氯乙烯,乙醇(20:80),氯苯,甲醇,乙醇/水,正丁醇/水,烯丙醇,2、4-二甲基-3-戊醇,苯甲醇,四氢糠醇,四氢呋喃(THF),二甲基四氢呋喃,二噁烷,乙二醇醚类,乙二醇醚酯,丙酮,丁酮,乙酸,较低的脂族酯,乙酸乙烯酯,乙缩醛,乙腈,硝基甲烷,二甲基甲酰胺(DMF),二甲基亚砜(DMSO),三氯甲烷,氯苯。
非溶剂:(SW表示溶胀的)
饱和烃类,二甲苯(SW),
(1,3,5-三甲基苯),四氯化碳(SW),乙醇(无水的,SW),无水醇类C>1,1,2-亚乙基二醇,环己醇、甲基环己醇,二乙醚(无水的,无醇的),较高的酯类C>5,二硫化碳,水(SW),稀酸类,稀碱类。
7、聚乙烯醇缩丁醛
溶剂:
缩醛化作用为70%:
醇类、环己酮、乳酸乙酯、乙酸乙二醇酯,
缩醛化作用为77%:
二氯甲烷、醇类、丙酮,丁酮,环己酮,较低的酯类、二氯甲烷,酮类。
缩醛化作用为83%:
二氯甲烷、醇类、酮类、较低的酯类。
非溶剂:
缩醛化作用为70%:
脂族烃,环脂族烃和芳香烃(SW),二氯甲烷,脂族酮类,大多数酯类,水。
缩醛化作用为77%:
脂族烃、环脂族烃和芳香烃(SW),甲基·异丁基酮,较高的酯族。
缩醛化作用为83%:
脂族烃(SW),环脂族烃(SW)和芳香烃(SW),甲醇,较高的脂族。
8、聚氯乙烯
溶剂:
高分子量(high M·W)
四氢呋喃(THF),丙酮/二硫化碳,丁酮,环戊酮,环己酮,二甲基甲酰胺(DMF),硝基苯,二甲基亚砜(DMSO)。
低分子量(Lower M·W)
甲苯,二甲苯,二氯甲烷,氯乙烯、全氯乙烯/丙酮,1,2-二氯代苯,二噁烷、丙酮/二硫化碳,环戊酮,环己酮、二异丙基(甲)酮、异亚丙基丙酮,异佛尔酮,二甲基甲酰胺(DMF),硝基苯,六甲基磷酰胺(HMPA),磷酸三甲苯酯。
氯化,63%Cl:
芳烃类,三氯甲烷,氯苯,四氢呋喃(THF),二噁烷,丙酮,环己酮,乙酸丁酯,硝基苯,二甲基甲酰胺(DMF),二甲基亚砜(DMSO)。
非溶剂:
总分子量的(All.M.W,′S):
脂族烃,矿物油,芳香烃(SW),氯乙烯,醇,甘醇类,苯胺(SW),丙酮(SW),羧酸,乙酸酐(SW),酯类,硝基烷类(SW),二硫化碳,不氧化的酸类、碱类。
氯化,63%Cl:
脂族和环脂族烃类,四氯化碳,乙酸甲酯,硝基甲烷,有机和无机酸类。
9、氯乙烯/乙酸乙烯酯共聚物
溶剂:
三氯甲烷、氯苯、吡啶、二噁烷、环己酮、乙酸乙酯。
非溶剂:
苯,醇类,二乙醚,水。
10、聚甲基丙烯酸甲酯
溶剂:
二甲基甲酰胺,二氯甲烷,三氯甲烷,二氯(化)乙烯、三氯乙烯、氯苯,甲酸甲酯,乙酸乙酯,乙酸异丙酯,乙酸正丁酯、乳酯丁酯,乙酸溶纤剂,1、4-二噁烷,四氢呋喃,苯,丙酮,丁酮,乙腈,硝基甲烷,硝基乙烷,2-硝基丙烷,甲苯,双丙酮醇。
非溶剂:
甲醇、乙醇、丙醇、戊醇;环己醇;1、2-亚乙基二醇;丙三
醇。还有甲酰胺,四氯化碳;二乙醚和二异丙醚;FREON(商标名)牌的三聚氰酰胺甲醛树脂(MF)和三苯基甲
(TF);己烷,环己烷,溶剂油类,松节油,二异丁酮;环己酮;异佛尔酮;蓖麻油和亚麻油;甲基氯仿。
实施例
实施例1:
配制的两种浆料是:一种介质浆料和一种构图浆料,如下所述:
介质浆料
玻璃A 15.78克
玻璃B 0.83克
氧化铝A 7.89克
氧化铝B 3.24克
铝酸钴 0.08克
聚甲基丙烯酸甲酯 5.36克
湿润剂 1.25克
叔-丁基蒽醌 0.50克
Shell Ionol
0.03克
卡必醇-丁醚乙酸酯
Acetate)
邻苯二甲酸苄基丁酯 0.75克
玻璃A
SiO2(二氧化硅) 56.2%wt
PbO(氧化铅) 18.0
Al2O3(三氧化二铝) 8.6
CaO(氧化钙) 7.4
B2O3(三氧化二硼) 4.5
Na2O(氧化钠) 2.7
K2O(氧化钾) 1.6
MgO(氧化镁) 0.8
ZrO2(氧化锆) 0.2
玻璃A的粒度等级为D50,颗粒大小约为4至4.5微米;将其碾磨并分类,除去粗的和细的部分。D10级的颗粒大小约为1.6微米;D90级的颗粒大小为10至12微米。表面积是1.5至1.8平方米/克。
玻璃B是硼硅酸钡玻璃,用于降低介质组合物的烧结温度,由于玻璃A有大的颗粒尺寸。
其配方如下:
BaO(氧化钡) 37.5%wt
B2O3(三氧化二硼) 38.3
SiO2(二氧化硅) 16.5
MgO(二氧化镁) 4.3
ZrO2(二氧化锆) 3.0
氧化铝A是颗粒尺寸分布很窄的1微米粉,D10,D50,D90的颗粒大小分别为大约0.5微米,1.1微米和2.7微米。按规定规格分类,除去粗的和细的部分。表面面积约为2.7至2.8米2/克。
氧化铝B是平均颗粒尺寸为0.4微米,表面面积约为5米2/克的粉。
构图浆料
氧化铝A 60克
氢化蓖麻油 1.4克
溶剂油 4.0克
着色剂 2.2克
乙基纤维素T-200 4.3克
松油醇 11.9克
邻苯二甲酸苯
甲基丁酯 16.2克
用厚膜材料配制领域的普通技术人员熟知的方法制备上述浆料组合物。印刷方法如下:
材料的处理方法是,按其需要印刷介质层一层,两层或三层,每印完一层后在80℃至90℃的温度下干燥10至15分钟。然后用带有通孔的丝网印刷图形层,所用丝网上的通孔具有不同的尺寸。然后将印好图形的浆料在80℃至100℃的温度下干燥5至10分钟。
将套印层浸在用超声波搅拌的1,1,1-三氯乙烷中直到套印区被除去和套印有图形浆料下面的区域被溶掉为止,这样就制成了介质层中的图形。
在85微米厚的介质膜中通孔尺寸可到0.125-0.175mm那样小,并且有好的边界。其分辨率和单个构图工序所获得的厚度均远远超过丝网印刷。
实施例2
调整介质浆料(DP)组合物中的增塑剂含量
为了能够制作出较厚的图形层,给要制作图形的底层加入增塑剂常常是有益的。在制作图形的浆料组合物中用不同浓度的增塑剂构成浓度梯度来确定增塑剂最佳含量是常用的方法。
按实例1中的方法配制出介质浆料,但不加增塑剂。由增塑剂含量梯度来确定其在组分中的最佳含量。其结果如下:
在所列显影时间的0.1mm通孔的质量
(秒
增塑剂含量 10 15 22 30 45 60
无 闭 闭 闭 闭 闭 闭
1.5% 闭 闭 部分开 部分开 部分开 部分开
2.4% 闭 闭 闭 部分开 部分开 全开
3.25% 闭 开 质量最佳 表面侵蚀
按实例1中的方法印刷和处理浆料,以确定最佳使用范围。发现最佳范围在2.5至3.5%之间,在该组分范围内,40至50微米厚膜具有良好的可加工性。在可使用范围内中较高的增塑剂含量降低了显影时间,增加了出产量。
实施例3
含铜的导体浆料组成如下:
铜粉,3至4微米 75.0克
玻璃粉C 5.0克
Elvacite 2010牌(商标)聚甲基
丙烯酸甲酯 6.1克
叔丁基蒽醌 0.6克
Acetate) 13.2克
玻璃粉C
Bi2O3(三氧化二铋) 82.0%wt
PbO(氧化铅) 11.0%wt
B2O3(三氧化二硼) 3.5
SiO2(二氧化硅) 3.5
用厚膜浆料配制领域的普通专业人员所熟知的技术将上述组分配制成含铜浆料,并准备印刷。
在氧化铝基片上用325目的丝网印刷一层导体组合物,用实例1中的构图浆料在铜印刷层上印刷一层丝网印刷的导体图形的负像,两层印刷层在85至95℃下干燥。然后将干燥过的部件浸在带超声波搅拌的氯乙烷中15至25秒,构成所需的图形。然后将部件干燥。精密的0.1mm线/间隔的图形就制成了。烧结后的部件为10至12微米厚,其电阻率为大约3毫欧姆/方。在3毫欧姆/方的图形中,要达到0.1mm线/间隔的分辨率即使不是不可能的,那也是困难的。此外,就0.1mm线的顶部图形而言,有精密的边界和指状导体顶部的平坦表面,这些都好于丝网印刷部件。当用400目的丝网进行底层印刷而制成稍薄一些的底层涂层时能分辨的线宽为0.075mm。
实例4
这是一种金导体组合物,其电导率和厚度与上述铜导体类似。
金粉 75.0克
铋酸铜 1.5
聚甲基丙烯酸甲酯 3.1
叔-丁基蒽醌 0.3
卡必醇-丁醚乙酸酯
上述组成用厚膜组成领域的普通技术人员公知的方法制成。在氧化铝基片上用325目的丝网印刷单层金组合物涂层,并在85至95℃下干燥。然后套印构图浆料,构成厚膜导体图形负像,然后在85至95℃下再次干燥。
实例5
带铜的正像导体浆料系统的组成如下:
铜正像底层印刷浆料
铜粉,3至4微米 42.5克
玻璃粉C 1.0克
Carboset牌XPD-1234树脂 1.6克
苯并三唑 0.15克
卡必醇-丁醚乙酸酯(Butyl
Carbitol R Acetate) 3.75克
玻璃粉C
Bi2O3(三氧化二铋) 82.0%
PbO(氧化铅) 11.0
B2O3(三氧化二硼) 3.5
SiO2(二氧化硅) 3.5
铜正像构图浆料
铜粉、3至4微米 46.00克
玻璃粉C 1.25
乙基纤维素T-50 0.75克
Santicizer(商标)S-160 2.83
松油醇异构物 2.29
用厚膜浆料组成领域的普通技术人员公知的技术按上述组分制成铜浆料,并准备印刷。
用325目的丝网在氧化铝基片上印刷一层导体组合物涂层;然后在铜印刷层顶上用本实施例中的构图浆料再印一层丝网印刷的负像导体图形。两层印刷层在85至95℃下干燥。干燥过的部件浸在有超声波搅拌1%的碳酸钾水溶液中5至15秒形成所需的图形。精确的0.1mm线/间隙图形便形成了。干燥过的部件厚49微米。此外,0.1mm线有比丝网印刷的部件更精密的边界。
实例6
用软片图像印刷法扩散构图
按下述方法将软片图像印刷板上的清晰可辨的印刷图形转移到介质浆料(DP)的介电组分上。
在用检测图形成像过的软片图像印刷板上涂复一层邻苯二甲酸苯甲基丁酯增塑剂薄膜。然后将图像印刷板盖在涂有干燥过的介质组合物的陶瓷部件的表面上并滚压(见实例1)。然后在95℃的炉内干燥5分钟,使从板上转移到介质上的增塑剂扩散进入介质中。浸入含1,1,1-三氯乙烷的超声波槽中使介质中的图像显影。从板
上转移来的图形在介质中能清楚地看见,从而证明增塑剂淀积的其他技术能制成扩散图像。
也可以采用其他图像生成方法,如用墨汁喷射激光印刷机印刷或用绘图仪上的笔绘制图形。凹版印刷或凸版印刷技术均可以用。
其他材料系统
按选择溶解原理,有许多形成厚膜图形的方法。图形可以是正像也可以是负像,即像实施例1至4所述的那样,套印图形下的区域可以溶掉,也可以不溶。例如套印一层含不溶于水的增塑剂的并且可在水中显影的聚合物来保护底层区,然后用水溶解除去未增塑化的材料。
下表列出了许多证明能用于本发明方法的丙烯酸聚合物/增塑剂/溶剂系列。
表2
其他丙烯酸材料系列
套印 构图溶剂
底层印刷树脂
增溶剂(负的) 阻溶剂(正的)
聚甲基丙烯酸甲酯 二丁基
邻苯二甲酸酯 甲基三氯甲烷
聚甲基丙烯酸酯 邻苯二甲酸苯甲
基丁酯
乙基羟基乙基
纤维素
聚甲基丙烯酸甲酯 乙醇/水/氨
Carboset牌XPD-1234 三乙醇胺 水
邻苯二甲酸二丁酯 K2CO3/水
上述的酯类可以是结合的。例如,异丁烯酸甲酯和异丁烯酸乙酯可以化合成正的或负的图像抗蚀剂。在甲基丙烯酸甲酯/甲基丙烯酸乙酯结合的情况下,增塑剂如三甘醇会生成在乙醇图形溶剂中
的负图像抗蚀剂。
没有过量交联的其他树脂系列,如聚酯类,可以用同样的方式形成图形,只需要确定增溶剂或阻溶剂和合适的图形母溶剂。
如果高度交联的聚合物不具有可溶解的封皮,这种聚合物就不是工艺用的类似选用品。
环氧树脂类
具有环氧树脂的正像扩散图系统可以设计成以下形式:形成预聚合物,例如,双酚A的钠盐与表氯醇缩聚成构成图形的丝网印刷的底层印刷涂层中的树脂。预聚物的聚合度约为12单元长。
将交联的胺或多元酐如二亚乙基三胺或亚乙基二胺,或琥珀酸二酐加入套印浆料中。然后将套印浆料印刷到底层印刷层上,再让组合物固化;套印过胺涂复浆料的区域被交联,交联过的区域在适当的溶剂如三氯乙烷中不会溶解,其余部分的材料被洗掉。
聚酰亚胺:一种负像聚酰亚胺构图浆料系统可以用包含如1,2,4,5-苯四酸二酐(PMDA)和氧化苯胺(ODA)的不完全固化系统制成。用不完全固化的聚合物作底层印刷;套印一层含碱的如含三乙醇胺或颗粒性碳酸钾的浆料涂层作为图形印刷。然后在水或弱碱中清洗,除去套印图形下的区域。
其它有希望的材料是与羟乙基异丁烯酸酯反应后的二苯酮四羧酸二酐。合适的材料还有能从市场上买到的联苯二酐/对苯二胺系统。他们在未固化状态可以负像显影。
实施例7
用催化分解进行扩散构图
第一种介质厚膜浆料由作为有机媒介物粘接剂的聚甲基丙烯酸
甲酯和含乙基纤维素为粘接剂的上层厚膜浆料和作为分解催化剂的少量乙酰丙酮铂构成。用80目的丝网将第一种浆料印刷在几个氧化铝基片上,烧结后,形成22μm厚的膜,在第一种浆料上用具有通孔图形范围5至30密耳的经过检验的丝网印刷第二种浆料。将印刷层整体加热到240℃至360℃的各种温度下20分钟,然后冷却,然后每个部件用水雾清洗。能分辨出7密耳大的通孔。我们已观察到,加热在280℃至320℃范围内制成最均匀的通孔,而且无膜层表面侵蚀。浆料的组分如下:
表3
实例7浆料组分
介质浆料 套印浆料
硅酸锌钙玻璃 52.4克 氧化铝 60克
锆酸钙 2.8 烃类溶剂 2.1
兰色颜料 0.3 Carbitol二丁醚 2.1
邻苯二甲酸苯 氢化蓖麻油 1.3
亚甲基丁酯 4.7
湿润剂 1.25 黑色颜料 2.1
蒽醌 1.0 邻苯二甲酸
苯甲基丁酯 19.7
丁基羟基甲苯 0.1 松油醇异构物 9.7
聚甲基丙烯酸甲酯 13.6 乙基纤维素 3.25
卡必醇-丁醚乙酸
酯 25.0 乙酰丙酮铂 2.0
实例8和9
水扩散构图
硅酸锌钙玻璃由纤维素载体和3%的邻苯二甲酸苯甲基丁酯构成。每种浆料膜层印刷到氧化铝基片上,并在95-100℃下干燥。在干燥后的介质浆料层上丝网印刷含7克氧化铝,3.5克Tergitol牌TMN-6,3.15克松油醇异构物和3.5克乙基纤维素的构图浆料。并在95-100℃的温度下加热使套印的浆料干燥,并使Tergitol牌洗涤剂扩散进下面的介质层中。当干燥后的印刷层在自来水下冲洗以后,6密耳的通孔就能清晰的分辨出来。随后的测试表明,下面的聚合物层中使用附加增塑剂使分辨率得到进一步改进。
实例10
下列的实例中制成了两种介质浆料,每种介质浆料在使用同种构图浆料的氧化铝基片上制成一系列构图系统。在三种介质浆料中的组分差别在于,介质浆料B含有邻苯二甲酸苯亚甲基丁酯,介质浆料A含有更多挥发性的苯二酸氢酯增塑剂。
介质浆料A的组分与实例7相同,介质浆料B的组分除用挥发性更强的邻苯二甲酸二丙酯取代邻苯二甲酸苯亚甲基丁酯外其余组分与上述实例7相同。构图浆料组分除不含乙酰丙酮铂外其他组分与实例7相同。
两种介质浆料均用开孔为6至11密耳的丝网印刷,并在80至85
℃下干燥12分钟。然后将构图浆料印刷盖在干燥过的介质层上,并加热到95-100℃10分钟使印刷层干燥,同时使增塑剂扩散进下面的介质层中。然后将整体构件在氯乙烷喷雾中显影10至15秒,然后用水漂洗并用(空)气刀(片)(air knife)使其干燥。对每个组件中制成的通孔测试表明,含有挥发性更强的增塑剂的介质层来的通孔的尺寸与用作图形层印刷的丝网的开孔尺寸比较一致。
表4
增塑剂的挥发性和丝网尺寸对通孔尺寸的影响
构图丝网
尺寸(密耳) 5.5 6.0 6.5 7.0 11.0
通孔尺寸
介质浆料A 5.5 6.5 6.0 7.5 12.0
介质浆料B 6.5 8.0 7.5 9.0 12.5
术语注释
Carbitol-Union Carbide Corporation(联碳化物公司)Danbury.CT生产的二甘醇乙醚的商标名。
Carboset-B.F.Goodrich & Co.Cleveland.OH生产的酸性异丙烯酸甲酯共聚物的商标名。
Elvacite 2010-E.I.du Pont de Nemours and Co.Wilming-ton,DE生产的甲基丙烯酸甲酯树脂的商标名。
Freon MF and TF-E.I.du.Pont de Nemours and Co Wilmin-gton DE生产的三氯氟代甲烷和三氯氟代乙烷的商标名。
Ionol-Shell Chemical Co,Houston.TX生产的受阻碍酚抗氧化剂的商标名。
Santicizer-Monsanto Chemical.Co,St.Louis,MO生产的N-烷基对甲苯磺酰胺增塑剂的商标名。
T-200-Hercules.Inc.Wilmington DE生产的乙基纤维素的商标名。
Tergitol-Union Carbide Corp(联合碳化物公司)New york NY生产的非离子表面活化剂的商标名。
Claims (12)
1、一种在有机聚合物膜上的非照像构图方法,其特征是:
a)在基片上涂复无图形的第一层,该涂层包含能分散在预定洗脱液的固体有机聚合物;
b)在无图形的第一层上涂敷有图形的第二层,第二层涂层中包含能改变固体有机物在预定洗脱液中的分散率的改变剂;
c)使分散率改变剂按已构成的图形扩散到埋在下面的固体有机聚合物膜层中;和
d)用预定的洗脱液清洗,除去埋在下面的第一层中能分散在洗脱液中区域。
2、按权利要求1的方法,其特征是,分散率改变剂是第一层聚合物的分解催化剂。
3、按权利要求1的方法,其特征是,分散率改变剂是第一层聚合物的增塑剂。
4、按权利要求1的方法,其特征是,分散率改变剂是能使第一层聚合物分散的洗涤剂。
5、一种在有机聚合物膜层上制作负像图形的非照像方法,其特征是,
a)在基片上涂敷包含固体有机聚合物的无图形的第一层固体有机聚合物膜层;
b)在无图形的第一层有机固体聚合物膜层上涂敷已构成图形的第二层,第二层包含固体有机聚合物的粘性悬浮液、分散率改变剂任选的溶剂,分散率改变剂(1)是第一层有机聚合物层的聚合物用的分散剂;(2)其常压沸点高于溶剂;
c)干燥已构成图形的第二层,以除去其中的溶剂,并使分散率改变剂按已构成和图形扩散到下面的第一有机聚合物层中;和
d)用洗脱液清洗,除去第二层和埋在下面的第一层中按已构成的图形扩散后的区域,第二层和第一层中按已构成图形扩散后的区域可以分散在所述的洗脱液中。
6、一种在有机聚合物膜上制作正像图形的非照像方法,其特征是,
a)在基片上涂敷无图形的第一层,该层包含可分散在预定溶剂中的固体有机聚合物:
b)在无图形的第一层上涂敷已构成图形的第二层,第二层包含能降低有机聚合物在溶剂中的溶解度的阻溶剂;
c)加热有图形的第二层,使阻溶剂按已构成的图形扩散到埋在下面的第一层有机聚合物层中,使第一层中按已构成的图形扩散后的区域内的聚合物不溶解于溶剂中;和
d)用预定的溶剂清洗、除去埋在下面的第一层的未构成图形的区域。
7、一种在有机聚合物膜上构图的非照像方法,其特征是,
a)在其片上涂敷无图形的第一层,该层包含能溶于预定溶剂的固体有机聚合物;
b)在无图形的第一层上涂敷已构成图形的第二层,第二层包含能改变固体有机聚合物在预定溶剂中的溶解度的改变剂;
c)溶解度改变剂按已构成图形扩散进埋在下面的固体有机聚合物层中;和
d)用预定溶剂清洗,除去埋在下面的第一层中能溶于溶剂的区域。
8、在有机聚合物膜中制作负像图形的非照像方法,其特征是,
a)在基片上涂敷无图形的第一层包含固体聚合物的固体有机聚合物层;
b)在无图形的第一层固体有机聚合物层上涂敷有图形的第二层,第二层包含固体有机聚合物的粘性溶液,溶解度改变剂和溶剂,溶解度改变剂(1)是能溶解第一有机聚合物层的聚合物,(2)其常压沸点高于溶剂;
c)干燥有图形的第二层,除去其中的溶剂,并使溶解度改变剂按已构成的图形扩散进埋在下面的第一层有机聚合物膜层中;和
d)用第二种溶剂清洗,除去有图形的第二层和埋在下面的第一层中按已构成的图形扩散过的区域、第二层和第一层中按已构成的图形扩散过的区域能溶解于第二溶剂中。
9、在有机聚合物膜层中制作正像图形的非照像方法、其特征是,
a)在基片上涂敷无图形第一层,该层包含能溶于预定溶剂中的固体有机聚合物;
b)在无图形的第一层上涂敷已构成图形的第二层,第二层包含能降低有机聚合物在溶剂中的溶解度的阻溶剂;
c)加热已构成图形的第二层,使阻溶剂按已构成图形扩散进埋在下面的第一层有机聚合物层中,并使第一层中按已构成图形扩散后的区域不溶于溶剂中;和
d)用预定溶液清洗,除去埋在下面的第一层中未构成图形的区域。
10、在厚膜层中制作图形的非照相方法,其特征是,
a)在基片上涂敷无图形的厚膜层,该层包含分散在有机媒质中的极细的导电固体颗粒,有机媒质包含溶解于挥发性溶剂中的第一固体聚合物;
b)蒸发除去厚膜层中的溶剂;
c)在无溶剂的无图形的厚膜层上涂敷已构成图形的第二层,第二层包含无结晶聚合物的粘性悬浮液,第一聚合物用的增塑剂和第二种溶剂,增塑剂溶于第一层聚合物中并具有比第二溶剂的沸点高的沸点;
d)加热已构成图形的第二层,同时用蒸发方法除去其中的第二种溶剂,并使增塑剂从第二层中按已构成的图形扩散进埋在下面的第一层的区域;
e)用能溶解增塑后的第一聚合物又能溶解第二层聚合物的溶剂清洗涂层,以同时除去已构成图形的第二层和埋在下面的第一层中按已构成图形扩散的区域。
11、按权利要求10的方法,其特征是,第一层的聚合物与有图形的聚合物有相同的组分。
12、按权利要求10的方法,其特征是,第一层聚合物是聚甲基丙烯酸酯,增塑剂是邻苯二甲酸烷基酯,有图形的涂层中的挥发性溶剂是松油醇。
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Application Number | Priority Date | Filing Date | Title |
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US42538789A | 1989-10-20 | 1989-10-20 | |
US425,387 | 1989-10-20 | ||
US573,075 | 1990-08-29 | ||
US07/573,075 US5032216A (en) | 1989-10-20 | 1990-08-29 | Non-photographic method for patterning organic polymer films |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1053769A CN1053769A (zh) | 1991-08-14 |
CN1024980C true CN1024980C (zh) | 1994-06-08 |
Family
ID=27026664
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN90109505A Expired - Fee Related CN1024980C (zh) | 1989-10-20 | 1990-10-20 | 有机聚合物膜层上的非照像构图方法 |
Country Status (10)
Country | Link |
---|---|
US (1) | US5032216A (zh) |
EP (1) | EP0497896B1 (zh) |
JP (1) | JP2592548B2 (zh) |
KR (1) | KR960010009B1 (zh) |
CN (1) | CN1024980C (zh) |
CA (1) | CA2069306A1 (zh) |
DE (1) | DE69030261T2 (zh) |
MX (1) | MX167928B (zh) |
MY (1) | MY106618A (zh) |
WO (1) | WO1991006118A1 (zh) |
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US5292556A (en) * | 1992-12-22 | 1994-03-08 | E. I. Du Pont De Nemours And Company | Method for preparing negative-working wash-off relief images |
DE69328418T2 (de) * | 1993-02-26 | 2001-01-04 | Du Pont | Verfahren zur Herstellung eines Plasma-Anzeigegeräts |
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US6472148B1 (en) | 1994-09-26 | 2002-10-29 | President And Fellows Of Harvard College | Molecular recognition at surfaces derivatized with self-assembled monolayers |
US5620850A (en) * | 1994-09-26 | 1997-04-15 | President And Fellows Of Harvard College | Molecular recognition at surfaces derivatized with self-assembled monolayers |
EP0742585A1 (en) * | 1995-05-08 | 1996-11-13 | E.I. Du Pont De Nemours And Company | Method and compositions for diffusion patterning tape on substrate |
US20040137734A1 (en) * | 1995-11-15 | 2004-07-15 | Princeton University | Compositions and processes for nanoimprinting |
US7758794B2 (en) * | 2001-10-29 | 2010-07-20 | Princeton University | Method of making an article comprising nanoscale patterns with reduced edge roughness |
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US5888287A (en) * | 1997-04-10 | 1999-03-30 | Markem Corporation | Washable fabrics ink |
US7122615B1 (en) * | 1998-09-10 | 2006-10-17 | Rutgers, The State University Of New Jersey | Polyanhydrides with therapeutically useful degradation products |
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US9615463B2 (en) * | 2006-09-22 | 2017-04-04 | Oscar Khaselev | Method for producing a high-aspect ratio conductive pattern on a substrate |
US8741317B2 (en) | 2010-08-19 | 2014-06-03 | Rutgers, The State University Of New Jersey | Slow-degrading polymers comprising salicylic acid for undelayed and sustained drug delivery |
US9144579B2 (en) | 2012-08-17 | 2015-09-29 | Rutgers, The State University Of New Jersey | Polyesters and methods of use thereof |
US20140120057A1 (en) | 2012-10-25 | 2014-05-01 | Rutgers, The State University Of New Jersey | Polymers and methods thereof for wound healing |
US9387250B2 (en) | 2013-03-15 | 2016-07-12 | Rutgers, The State University Of New Jersey | Therapeutic compositions for bone repair |
US9862672B2 (en) | 2013-05-29 | 2018-01-09 | Rutgers, The State University Of New Jersey | Antioxidant-based poly(anhydride-esters) |
WO2015191742A1 (en) | 2014-06-13 | 2015-12-17 | Rutgers, The State University Of New Jersey | Process and intermediates for preparing poly(anhydride-esters) |
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CN113533598B (zh) * | 2021-07-30 | 2023-03-24 | 海南葫芦娃药业集团股份有限公司 | 一种小儿肺热咳喘颗粒中黄芩含量的高效液相色谱分析方法 |
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-
1990
- 1990-08-29 US US07/573,075 patent/US5032216A/en not_active Expired - Lifetime
- 1990-10-11 JP JP2515844A patent/JP2592548B2/ja not_active Expired - Fee Related
- 1990-10-11 DE DE69030261T patent/DE69030261T2/de not_active Expired - Fee Related
- 1990-10-11 EP EP90917075A patent/EP0497896B1/en not_active Expired - Lifetime
- 1990-10-11 CA CA002069306A patent/CA2069306A1/en not_active Abandoned
- 1990-10-11 WO PCT/US1990/005664 patent/WO1991006118A1/en active IP Right Grant
- 1990-10-11 KR KR1019920700903A patent/KR960010009B1/ko not_active IP Right Cessation
- 1990-10-19 MX MX022928A patent/MX167928B/es unknown
- 1990-10-19 MY MYPI90001831A patent/MY106618A/en unknown
- 1990-10-20 CN CN90109505A patent/CN1024980C/zh not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
EP0497896A1 (en) | 1992-08-12 |
MY106618A (en) | 1995-06-30 |
DE69030261T2 (de) | 1997-08-07 |
CA2069306A1 (en) | 1991-04-21 |
EP0497896B1 (en) | 1997-03-19 |
WO1991006118A1 (en) | 1991-05-02 |
US5032216A (en) | 1991-07-16 |
KR960010009B1 (ko) | 1996-07-25 |
KR920702547A (ko) | 1992-09-04 |
JPH05502140A (ja) | 1993-04-15 |
MX167928B (es) | 1993-04-22 |
JP2592548B2 (ja) | 1997-03-19 |
DE69030261D1 (de) | 1997-04-24 |
CN1053769A (zh) | 1991-08-14 |
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