CN113574043A - 有机溶剂的制造方法 - Google Patents

有机溶剂的制造方法 Download PDF

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CN113574043A
CN113574043A CN202080019703.2A CN202080019703A CN113574043A CN 113574043 A CN113574043 A CN 113574043A CN 202080019703 A CN202080019703 A CN 202080019703A CN 113574043 A CN113574043 A CN 113574043A
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organic solvent
metal
filter cartridge
groups
polyolefin fibers
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大桥智也
吉田丰之郎
佐佐卓
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Nissan Chemical Corp
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    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/16Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B01D39/1607Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
    • B01D39/1623Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
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    • B01DSEPARATION
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    • B01D39/14Other self-supporting filtering material ; Other filtering material
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    • B01D39/1623Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
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    • B01D35/02Filters adapted for location in special places, e.g. pipe-lines, pumps, stop-cocks
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Abstract

提供在半导体装置制造中的光刻工序中,成为晶片上的微小缺陷的原因的、金属杂质被减少了的有机溶剂的制造方法、或减少被精制有机溶剂中金属的方法。一种有机溶剂的制造方法,包含向金属除去用过滤筒进行通液的工序,所述金属除去用过滤筒是在中空状内筒层叠或卷绕有多个种类的过滤用基布的过滤筒,所述金属除去用过滤筒的特征在于,所述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,所述过滤用基布包含无纺布层A和无纺布层B,所述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,所述无纺布层B由化学结合有选自氨基、N‑甲基‑D‑葡糖胺基、亚氨基二乙酸基、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。

Description

有机溶剂的制造方法
技术领域
涉及在半导体装置制造中的光刻工序中,成为缺陷的原因的金属杂质被减少了的有机溶剂的制造方法。
背景技术
在半导体装置制造中的光刻工序中使用的有机溶剂要求成为晶片上的微小缺陷(例如1~100nm左右,被称为defect等)的原因的金属杂质的减少。在专利文献1中公开了金属的吸附除去效率高的过滤器。
现有技术文献
专利文献
专利文献1:日本特开2018-167223号公报
发明内容
发明所要解决的课题
提供在半导体装置制造中的光刻工序中,成为晶片上的微小缺陷的原因的金属杂质被减少了的有机溶剂的制造方法和有机溶剂的金属减少方法。
用于解决课题的方法
本发明包含以下方案。
[1]一种有机溶剂的制造方法,其包含向金属除去用过滤筒进行通液的工序,上述金属除去用过滤筒是在中空状内筒叠层或卷绕有多个种类的过滤用基布的过滤筒,该向金属除去用过滤筒的特征在于,
上述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,
上述过滤用基布包含无纺布层A和无纺布层B,
上述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,
上述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。
[2]根据[1]所述的有机溶剂的制造方法,其还包含向微粒除去用过滤筒进行通液的工序。
[3]根据[2]所述的有机溶剂的制造方法,上述微粒除去用过滤筒的材质为选自聚乙烯和尼龙中的至少一种。
[4]根据[1]~[3]中任一项所述的有机溶剂的制造方法,上述有机溶剂为用于形成抗蚀剂下层膜的有机溶剂。
[5]根据[4]所述的有机溶剂的制造方法,上述有机溶剂为选自丙二醇单甲醚、丙二醇单甲醚乙酸酯、丙二醇单乙醚、γ-丁内酯、乳酸乙酯、乳酸丁酯、和环己酮中的至少一种。
[6]一种减少被精制有机溶剂中金属的方法,是将被精制有机溶剂向金属除去用过滤筒进行通液减少金属的方法,
上述过滤筒是在中空状内筒得层或卷绕有多个种类的过滤用基布的过滤筒,
上述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,
上述过滤用基布包含无纺布层A和无纺布层B,
上述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,
上述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。
发明的效果
通过使用本发明记载的过滤筒进行有机溶剂的制造,可以制造金属杂质被大幅减少了的有机溶剂。通过使用该有机溶剂可以使半导体制造工序中的光刻工序中的各种微小缺陷(defect)减少。
具体实施方式
<有机溶剂的制造方法>
本发明的有机溶剂的制造方法包含将在常温下为溶液状的被精制有机溶剂向以下详述的金属除去用过滤筒进行通液的工序。
上述通液工序,例如可以购买市售品的被精制有机溶剂,将其向与使用该有机溶剂的制造设备(制造用容器)直接连结(入口和出口2处)的金属除去用过滤筒进行通液来进行。上述通液工序可以为1次或2次以上。上述通液工序优选为使用了泵的循环过滤。优选向除了本申请的金属除去用过滤筒以外还串联连接了的微粒除去用过滤筒这两者通液有机溶剂使其循环。循环所需要的时间例如为3~144小时。过滤流量例如为1~1000L/小时。
<被精制有机溶剂>
在本申请中使用的被精制有机溶剂推荐为例如下述记载的通常在光刻工序中使用的有机溶剂,但不限定于此。
作为上述被精制有机溶剂,可举出例如,乙二醇单甲醚、乙二醇单乙醚、甲基溶纤剂乙酸酯、乙基溶纤剂乙酸酯、二甘醇单甲醚、二甘醇单乙醚、丙二醇、丙二醇单甲醚、丙二醇单乙醚、丙二醇单甲醚乙酸酯、丙二醇丙醚乙酸酯、甲苯、二甲苯、甲基乙基酮、甲基异丁基酮、环戊酮、环己酮、环庚酮、4-甲基-2-戊醇、2-羟基异丁酸甲酯、2-羟基异丁酸乙酯、乙氧基乙酸乙酯、乙酸2-羟基乙酯、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸乙酯、3-乙氧基丙酸甲酯、丙酮酸甲酯、丙酮酸乙酯、乙酸乙酯、乙酸丁酯、乳酸乙酯、乳酸丁酯、2-庚酮、甲氧基环戊烷、茴香醚、γ-丁内酯、N-甲基吡咯烷酮、N,N-二甲基甲酰胺、和N,N-二甲基乙酰胺。这些溶剂可以单独使用或组合使用2种以上。
在这些溶剂中优选为丙二醇单甲醚、丙二醇单甲醚乙酸酯、丙二醇单乙醚、γ-丁内酯、乳酸乙酯、乳酸丁酯、和环己酮等。特别优选为丙二醇单甲醚、丙二醇单甲醚乙酸酯和丙二醇单乙醚。
<过滤筒>
作为本申请的过滤筒,优选为日本特开2018-167223号公报所记载的过滤筒。
本发明的过滤筒,其特征在于,是将多个种类的过滤用基布层叠或卷绕于中空状内筒的过滤筒,上述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,上述过滤用基布包含无纺布层A和无纺布层B,上述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,上述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基(亚氨基二乙酸基)、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。
本发明是将多个种类的过滤用基布层叠或卷绕于中空状内筒的过滤筒,上述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,上述过滤用基布包含无纺布层A和无纺布层B。而且,上述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,上述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基(亚氨基二乙酸基)、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。由此可以高效率地除去金属。另外,将不同种类的过滤用基布结合而制成1片过滤用基布的情况也包括在多个种类的过滤用基布的含义内。
在本发明中,无纺布层B特别优选由化学结合有亚氨基二乙醇基的聚烯烃纤维构成。因为金属的除去效率高。关于可以吸附的金属,磺酸基主要吸附Na、Cu、K,亚氨基二乙醇基主要吸附Cr、Al、Fe。
构成无纺布A和B的聚烯烃纤维优选为长纤维。因为长纤维无纺布不易产生纤维屑,过滤器性能高。其中优选为单位面积的质量(目付)为10~100g/m2的熔喷长纤维无纺布。
构成上述无纺布A和B的聚烯烃纤维的单纤维平均直径优选为0.2~10μm。如果为上述范围,则可期待过滤器性能高。此外,可以增大表面积(比表面积),接枝聚合反应的基材表面也增加,因此也可以期待提高接枝率。
聚烯烃纤维优选为选自聚丙烯、丙烯与乙烯的共聚物、聚乙烯、和乙烯与碳原子数4以上的其它α-烯烃的共聚物中的至少一种,特别优选为高密度聚乙烯。这些聚合物为非活性,对化学溶液是稳定的,能够进行接枝聚合。
上述过滤筒优选为下述过滤筒:是包含中空状内筒和过滤用基布的过滤筒,上述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,上述过滤用基布通过卷绕于上述中空状内筒从而形成叠层结构。
本发明的过滤器为并入了上述过滤筒的过滤器。例如,过滤筒在内筒卷绕过滤用基布,收纳于容器。在将过滤筒并入到过滤器的容器时,例如,在容器收纳了过滤筒的状态下并入到过滤器。另外,在筒型过滤器的情况下,通过仅交换过滤筒,可以将过滤器功能再生。连过滤器的容器一起交换那样的、例如胶囊型过滤器那样的情况也包含于本发明。在胶囊型过滤器那样的情况下,相当于过滤筒的部分成为过滤部。
接下来对使各种官能团与聚烯烃纤维化学结合的方法进行说明。作为该方法,具有例如,向聚烯烃纤维照射了电子射线、γ射线等放射线后使其与包含GMA等反应性单体的乳液接触的方法;在使聚烯烃纤维与包含反应性单体的乳液接触后照射电子射线、γ射线等放射线,使反应性单体与聚烯烃纤维接枝聚合的方法等。在照射电子射线的情况下,只要通常达到1~200kGy,优选为5~100kGy,更优选为10~50kGy的照射量即可。照射优选在氮气气氛下进行。作为电子射线照射装置,可以使用市售品,例如,作为区域束型电子射线照射装置,可以使用EC250/15/180L(岩崎电气(株)社制)、EC300/165/800(岩崎电气(株)社制)、EPS300((株)NHVコーポレーション制)等。
作为上述接枝聚合法,具体而言,可举出例如,液相接枝聚合法,将无纺布通过γ射线、电子射线等放射线照射而活化后,浸渍在包含水、表面活性剂和反应性单体的乳液中,使上述无纺布基材完成接枝聚合。接下来,向形成于上述基材的接枝链导入磺酸基、氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基(亚氨基二乙酸基)、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基、乙二胺三乙酸基等功能性官能团、即离子交换基和/或螯合基。在本发明中,不特别限定于液相接枝聚合法,也可以使用使基材与单体的蒸气接触而进行聚合的气相接枝聚合法、在将基材浸渍于单体溶液后从单体溶液取出而在气相中使反应进行的含浸气相接枝聚合法等。作为代表性的功能性官能团的化学式,在(化1)中显示磺酸基(SC基),在(化2)中显示亚氨基二乙醇基(IDE基),在(化3)中显示亚氨基二乙酸基(IDA基),在(化4)中显示N-甲基-D-葡糖胺基(NMDG基)。
Figure BDA0003252246780000061
Figure BDA0003252246780000071
其中,(化1)~(化3)中的R为下述聚乙烯(PE)+GMA(化5)或聚丙烯(PP)+GMA(化6)。(化4)中的R为甲基。
Figure BDA0003252246780000072
(化5)聚乙烯(PE)+GMA
Figure BDA0003252246780000073
(化6)聚丙烯(PP)+GMA
其中,上述(化5)~(化6)中的n、m为1以上的整数。
<微粒除去用过滤器>
本发明的有机溶剂的制造方法优选在将上述被精制有机溶剂向上述过滤筒通液后,进一步向微粒除去用过滤器通液。微粒除去用过滤器可以使用本身公知的物质。作为微粒除去用过滤器的材质,优选为选自聚乙烯和尼龙中的至少一种。
微粒除去用过滤器的孔径通常为30nm以下,优选为例如0.1nm~30nm、例如0.1nm~20nm、或例如1nm~10nm。
<金属减少方法>
本申请的减少金属的方法是用过滤筒对上述记载的被精制有机溶剂进行过滤而减少金属的方法,
上述过滤筒是在中空状内筒层叠或卷绕有多个种类的过滤用基布的过滤筒,
上述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,
上述过滤用基布包含无纺布层A和无纺布层B,
上述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,
上述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基(亚氨基二乙酸基)、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。
通过经过该工序,从而可以减少包含于被精制有机溶剂的、来源于原料或溶剂的金属杂质,使光刻工序中的缺陷少。
各种金属杂质(例如Na、Cu、Cr、Al、Fe等)通过上述金属减少方法,可以减少到例如0.5ppb以下、例如0.4ppb以下。
上述金属杂质含量通过例如实施例所记载的方法而求出。
实施例
以下参照实施例等进一步详细地说明本发明,但本发明不受以下实施例等任何限制。
<实施例1>
将作为被精制有机溶剂的丙二醇单甲醚(PM-P:KHネオケム株式会社制)20L使用日本特开2018-167223所记载的筒式过滤器(10inch)1根(仓敷纤维加工株式会社制)以每分钟3L的流量实施了100分钟过滤。通过ICP-MS(Agilent8800:アジレントテクノロジー株式会社制)测定了过滤后的有机溶剂的金属含量。
<比较例1>
不将实施例1所使用的被精制有机溶剂过滤,通过同样的方法测定了金属含量。
<比较例2>
将实施例1的筒式过滤器改变为筒式过滤器(尼龙过滤器ABD1ANM3EH1(20nm尼龙过滤器):日本ポール株式会社制),除此以外,通过与实施例1同样的方法实施过滤,通过同样的方法测定了金属含量。
<比较例3>
将实施例1的筒式过滤器改变为强酸性离子交换树脂(XSC-1115-H:室町ケミカル株式会社制)20kg而进行了4小时离子交换,除此以外,通过与实施例1同样的方法实施过滤,通过同样的方法测定了金属含量。
<有机溶剂中的金属浓度>
将实施了实施例1的处理方法后的金属浓度的测定结果示于表1中。
[表1]
表1金属浓度测定结果(ppb)
实施例1 0.1
比较例1 0.4
比较例2 0.2
比较例3 1.3
由表1的结果显示出,实施例1对于金属浓度减少是有效果的。
<实施例2>
将作为被精制有机溶剂的丙二醇单甲醚乙酸酯(EL-PGMEA:东洋合成工业株式会社制)20L使用日本特开2018-167223所记载的筒式过滤器(10inch)1根(仓敷纤维加工株式会社制)以每分钟2L的流量实施了50分钟过滤。通过ICP-MS(Agilent8800:アジレントテクノロジー株式会社制)测定了过滤后的溶液的金属含量。
<比较例4>
不将实施例1所使用的溶剂过滤,通过同样的方法测定了金属含量。
[表2]
表2金属浓度测定结果(ppb)
实施例2 0.0
比较例4 3.9
由表2的结果显示出,实施例2对于金属浓度减少是有效果的。
产业可利用性根据本发明,可以提供特别是金属杂质的量被减少了的有机溶剂。

Claims (6)

1.一种有机溶剂的制造方法,包含向金属除去用过滤筒进行通液的工序,所述金属除去用过滤筒是在中空状内筒层叠或卷绕有多个种类的过滤用基布的过滤筒,所述金属除去用过滤筒的特征在于,
所述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,
所述过滤用基布包含无纺布层A和无纺布层B,
所述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,
所述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。
2.根据权利要求1所述的有机溶剂的制造方法,其进一步包含向微粒除去用过滤筒进行通液的工序。
3.根据权利要求2所述的有机溶剂的制造方法,所述微粒除去用过滤筒的材质为选自聚乙烯和尼龙中的至少一种。
4.根据权利要求1~3中任一项所述的有机溶剂的制造方法,所述有机溶剂为用于形成抗蚀剂下层膜的有机溶剂。
5.根据权利要求4所述的有机溶剂的制造方法,所述有机溶剂为选自丙二醇单甲醚、丙二醇单甲醚乙酸酯、丙二醇单乙醚、γ-丁内酯、乳酸乙酯、乳酸丁酯和环己酮中的至少一种。
6.一种减少被精制有机溶剂中金属的方法,是将被精制有机溶剂向金属除去用过滤筒进行通液而减少金属的方法,
所述过滤筒是在中空状内筒层叠或卷绕有多个种类的过滤用基布的过滤筒,
所述过滤用基布为在聚烯烃纤维上化学结合有金属吸附基团的无纺布,
所述过滤用基布包含无纺布层A和无纺布层B,
所述无纺布层A由化学结合有磺酸基作为金属吸附基团的聚烯烃纤维构成,
所述无纺布层B由化学结合有选自氨基、N-甲基-D-葡糖胺基、亚氨基二乙酸基、亚氨基二乙醇基、偕胺肟基、磷酸基、羧酸基和乙二胺三乙酸基中的至少一种作为金属吸附基团的聚烯烃纤维构成。
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