CN107238646A - 气体检测器和具备气体检测器的电化学元件 - Google Patents
气体检测器和具备气体检测器的电化学元件 Download PDFInfo
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- CN107238646A CN107238646A CN201710183677.7A CN201710183677A CN107238646A CN 107238646 A CN107238646 A CN 107238646A CN 201710183677 A CN201710183677 A CN 201710183677A CN 107238646 A CN107238646 A CN 107238646A
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Abstract
本发明提供一种可见性优异并且灵敏度优异的气体检测器以及具备气体检测器的电化学元件。本发明可以提供通过使用以下的气体检测器从而可见性优异并且灵敏度优异的气体检测器以及具备气体检测器的电化学元件,所述气体检测器其特征在于,通式(1)所表示的多孔配位聚合物被担载于支撑体上,每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上且0.3mg/cm2以下。Fex(吡嗪)[Ni1‑yMy(CN)4](1)(0.95≤x<1.05、M=Pd、Pt、0≤y<0.15)。
Description
技术领域
本发明涉及一种气体检测器以及具备气体检测器的电化学元件。
背景技术
伴随着近年来的便携式电子设备的小型化、高功能化,对于电化学元件期待进一步的小型化、轻量化以及高容量化。
电化学元件能够以多种形态制得,代表性地可以列举角型、圆筒型以及袋型等。
其中,袋型电化学元件由于使用以铝复合膜等的薄片形成的袋型箱体,因此,可以制造成轻的各种的形态,有制造工序也简单的优点,另一方面,与圆筒型或角型相比存在由于损伤或内压增加而容易发生膨胀的问题。
电化学元件中,在锂离子二次电池或锂离子电容器中通常将如碳酸乙烯酯的环状碳酸酯与如碳酸二乙酯的链状碳酸酯的混合溶剂作为电解液的溶剂使用,在双电层电容器中将乙腈或碳酸丙烯酯等作为电解液的溶剂使用,在铝电解电容器中将乙二醇等作为电解液的溶剂使用。在电化学元件的箱体的密封性不充分时或箱体中产生了小孔等时,这些溶剂存在部分成为蒸气挥发、从密闭容器中漏出而产生的异臭、或特性的降低等的问题。
一直以来提出了各种从密闭容器中泄露的气体的检测方法。
例如,在专利文献1中提出了在氦或氩等的检测气体气氛的密闭容器内制作密闭型电池,其后,除去了密闭容器内的检测气体之后进行减压,利用气体传感器检测从密闭型电池内泄露的检测气体的方法。
然而,专利文献1的检测方法中,由于需要在制造工序中导入密闭容器,因此,不仅设备大型化,而且需要检测气体供给、减压装置、利用传感器的检测气体的检测等的操作,所以,存在不能简易地进行检测的问题。进一步,存在不能检测出在检测工序的前后有气体泄漏的情况的问题。
而且,金属离子和有机配位体自组装地形成了规则的高分子量的配合物被称为多孔配位聚合物。已知霍夫曼型多孔配位聚合物具有攀登架型的骨架扩展的结构,在其内部具有无数的空间,因此,吸附各种分子等。在非专利文献1~3中记载了具有特定的结构的多孔配位聚合物发生由于热或光、分子吸附等的外部因素而在高自旋和低自旋这2个状态间变化的被称为自旋翻转的现象。存在使用该现象可以检测气体的可能性,但是有对于低浓度的气体的判定明敏度不充分的问题。
现有技术文献
专利文献
专利文献1:日本特开2009-26569号公报
非专利文献
非专利文献1:无机化学,2001年,第40卷,p.3838-3839
非专利文献2:应用化学国际版(Angewandte Chemie International Edition),2008年,第47卷,p.6433-6437
非专利文献3:美国化学会志,2009年,第131卷,p.10998-11009
发明内容
发明所要解决的技术问题
本发明是鉴于上述问题点而成的,其目的在于提供一种相比现有技术可见性优异,并且灵敏度优异的气体检测器以及具备气体检测器的电化学元件。
解决技术问题的技术手段
本发明者们进行了专门研究,发现:通过使用如下的气体检测器可以达成上述目的,所述气体检测器其特征在于,通式(1)所表示的多孔配位聚合物被担载于支撑体上,Fex(吡嗪)[Ni1-yMy(CN)4] (1)(0.95≤x<1.05、M=Pd、Pt、0≤y<0.15),每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上且0.3mg/cm2以下,至此完成本发明。
即,根据本发明,可以提供以下的内容。
[1]一种气体检测器,其特征在于,通式(1)所表示的多孔配位聚合物被担载于支撑体上,
每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上且0.3mg/cm2以下,
Fex(吡嗪)[Ni1-yMy(CN)4] (1)
0.95≤x<1.05,M=Pd、Pt,0≤y<0.15。
[2]如[1]所述的气体检测器,其特征在于,在支撑体上形成有每单位面积的多孔配位聚合物的担载量不同的2个以上的区域。
[3]一种电化学元件,其特征在于,所述电化学元件使用了含有挥发性有机化合物的电解液,在表面附近具备[1]或[2]所述的气体检测器。
发明的效果
根据本发明,可以提供一种可见性优异并且灵敏度优异的气体检测器以及具备气体检测器的电化学元件。
附图说明
图1是表示本发明所涉及的多孔配位聚合物的基本的化学结构的示意图。
图2是表示本发明所涉及的气体检测器的示意图。
符号的说明
1…多孔配位聚合物、2…铁离子、3…四氰基镍酸离子、4…吡嗪、5…气体检测器、6a…多孔配位聚合物a、6b…多孔配位聚合物b、7…支撑体。
具体实施方式
基于用于实施本发明的方式(实施方式),一边参照附图一边进行详细地说明。本发明不被以下的实施方式所记载的内容限定。
对于本实施方式的气体检测器,通式(1)所表示的多孔配位聚合物被担载于支撑体上,
Fex(吡嗪)[Ni1-yMy(CN)4] (1)
(0.95≤x<1.05、M=Pd、Pt、0≤y<0.15)
每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上且0.3mg/cm2以下。
如图1所示,本发明的多孔配位聚合物1在铁离子2上自组装地规则地配位四氰基镍酸离子3和吡嗪4而具有攀爬架型的骨架舒展开的结构,可以在内部的空间中吸附各种分子等。另外,一部分镍可以被钯和铂的至少一种置换。
在多孔配位聚合物1中发现有,铁离子具有的电子构型由于热、压力、分子吸附等的外部刺激而在被称为高自旋状态和低自旋状态的2个状态间变化的被称为自旋翻转的现象。自旋变化通常可以说为数十纳秒,特征为具有非常快的应答速度。
高自旋状态是指在配合物中的铁离子的d电子的5个轨道中按照洪特规则(Hund'srule)配置电子成为自旋角动量成为最大的状态,低自旋状态是指配置电子成为自旋角动量成为最小的状态,由于各自电子状态和晶格间距离不同,因此,在2个状态间配合物的颜色和磁性不同。即,通过利用由于分子吸附至多孔配位聚合物上产生的自旋翻转现象,则能够可见性优异并且灵敏度良好地检测气体。
高自旋状态的多孔配位聚合物是橙色,如果用液氮等进行充分地冷却,则变化为低自旋状态的紫红色。另外,如果暴露于乙腈或丙烯腈等特定的有机化合物的气体中,则结晶内部吸附气体,成为低自旋状态。如果在低自旋状态下将紫红色的多孔配位聚合物暴露于诱发高自旋状态的有机化合物的气体中,则在攀爬架型的骨架内部吸入气体,由于自旋翻转现象而成为高自旋状态的橙色。作为这些有机化合物的气体,例如可以列举有机可燃性气体或挥发性有机溶剂的蒸气等。即,低自旋状态的多孔配位聚合物吸附作为锂离子二次电池或锂离子电容器用电解液中所含的溶剂的碳酸二甲酯(以下称为DMC)、碳酸二乙酯(以下称为DEC)以及碳酸乙基甲基酯(以下称为EMC)等、或者所述溶剂分解产生的乙烯和丙烯等、或者作为双电层电容器用电解液中所含的溶剂的碳酸丙烯酯等、进一步作为铝电解电容器用电解液中所含的溶剂的乙二醇等的气体,变化为高自旋状态的橙色。
对于本实施方式的多孔配位聚合物的组成,可以通过使用ICP发光分光分析法、荧光X射线元素分析法、碳硫分析法以及氧氮氢分析法等来进行确认。
本实施方式的多孔配位聚合物的自旋状态可以通过使用超导量子干涉型磁通量计(SQUID)或振动样品型磁力计(VSM)观察磁化强度相对于磁场的应答来确认。
本实施方式的多孔配位聚合物的制造方法是,首先,在适当的溶剂中使二价的铁盐、抗氧化剂与四氰基镍酸盐、四氰基钯酸盐以及四氰基铂酸盐反应,得到中间体。其次,使中间体分散于适当的溶剂中,在该分散液中加入吡嗪,由此沉淀物析出,将沉淀物过滤、干燥,由此可以得到多孔配位聚合物。
作为二价的铁盐,可以使用硫酸亚铁七水合物、硫酸铵铁六水合物等。作为抗氧化剂,可以使用L-抗坏血酸等。作为四氰基镍酸盐,可以使用四氰基镍酸钾水合物等。作为四氰基钯酸盐,可以使用四氰基钯酸钾水合物等。作为四氰基铂酸盐,可以使用四氰基铂酸钾水合物等。
作为溶剂,可以使用甲醇、乙醇、丙醇以及水等,或者这些的混合溶剂等。
图2是本实施方式所涉及的气体检测器的示意图。在图2中,气体检测器5由多孔配位聚合物6a、多孔配位聚合物6b和支撑体7构成,多孔配位聚合物6a和多孔配位聚合物6b各自每单位面积的多孔配位聚合物的担载量不同。
如果每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上,则多孔配位聚合物媳妇有检测气体时的颜色变化变得明显,如果为0.3mg/cm2以下,则即使是检测气体少量时颜色变化也明显,可见性优异。在担载量为0.01mg/cm2以下时,发现有多孔配位聚合物吸附了检测气体时的颜色变化不明显的倾向,认为容易受到支撑体的颜色的影响或大气中的湿度或挥发性有机化合物的影响。另外,担载量为0.4mg/cm2以上时,在检测气体少量的情况下,发现有颜色变化不明显的倾向,认为是由于发生了颜色变化的多孔配位聚合物和没有发生颜色变化的多孔配位聚合物夹杂存在。如上所述,多孔配位聚合物被担载于支撑体上,通过每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上且0.3mg/cm2以下,从而可以作为可见性优异、并且灵敏度优异的气体检测器使用。
本实施方式的气体检测器优选在支撑体上形成有每单位面积的多孔配位聚合物的担载量不同的2个以上的区域。每单位面积的多孔配位聚合物的担载量不同的2个以上的区域也可以形成于支撑体的同一面上或者形成于支撑体的表面和背面。通过形成了每单位面积的多孔配位聚合物的担载量不同的2个以上的区域,在相同条件下检测气体时,最初担载量少的区域的色调发生变化,与没有发生变化的担载量多的区域的颜色比较,由此可见性提高。进一步,也可以是支撑体上没有担载有多孔配位聚合物的区域。
支撑体7没有特别地限定,可以使用例如滤纸等的纤维素类厚纸或纸过滤器。另外,对于支撑体的颜色,在与通过多孔配位聚合物吸附检测气体而变化后的颜色成为互补色的关系的颜色、或者白色、灰色和黑色时,多孔配位聚合物的颜色变化的可见性提高,因此,更优选。进一步,支撑体的膜厚没有特别地限定,从气体检测器的制造时或使用时的操作容易性的观点出发,优选为50~1000μm。
多孔配位聚合物担载于支撑体上的方法没有特别地限定,可以列举过滤法、喷雾涂布法、刷毛涂布法以及浸涂法等。
(气体检测器的担载量测定)
本实施方式的气体检测器的每单位面积的多孔配位聚合物的担载量的求得方法如下所述。
使用荧光X射线分析法的薄膜基本参数法(Fundamental Parameter method),根据对检测器的担载有多孔配位聚合物的区域的10个地方进行测定而得到的平均的Fe元素的每单位面积的担载量,计算并求得多孔配位聚合物的担载量。装置使用RigakuCorporation制造的ZSX100e,以测定点直径为3mmΦ(5mmΦSUS制的掩模架)进行测定,将支撑体的空白测定值作为基准除以差分强度,算出Fe元素的每单位面积的担载量。根据利用多孔配位聚合物的组成分析求得的多片配位聚合物的量相对于Fe元素的量的比率,求得多孔配位聚合物的担载量。
本实施方式的电化学元件其特征在于,使用含有挥发性有机化合物的电解液,在表面附近具备所述气体检测器。
通过在使用含有挥发性有机化合物的电解液的电化学元件的表面附近具备本实施方式的气体检测器,在箱体的密闭性不充分时或者箱体上产生了小孔等时,通过评价气体检测器的色调变化,从而可以容易地且灵敏度良好地检测来自电化学元件的泄露气体。
通过使用本实施方式的气体检测器,从而即使在检查工序以外的过程或运输中以及保存中等也可以检测来自电化学元件的泄露气体。
实施例
以下,基于更详细的实施例来说明本发明,但是本发明不限定于这些实施例。
<实施例1>
(多孔配位聚合物的制造)
在三角烧瓶中在蒸馏水和乙醇的混合溶剂240mL中加入硫酸铵铁(II)六水合物0.24g、L-抗坏血酸0.1g和四氰基镍(II)酸钾一水合物0.15g,并进行搅拌,回收沉淀的中间体颗粒。在乙醇中使得到的中间体颗粒0.1g分散,用30分钟投入吡嗪0.10g。将析出的沉淀物过滤,在大气中在120℃下使之干燥3小时,由此得到了橙色的多孔配位聚合物。
(气体检测器的制作)
将实施例1的多孔配位聚合物在25℃下在乙腈中浸渍10小时之后,使用滤纸5种C进行抽吸过滤,并使之干燥,由此在滤纸5种C上得到了紫红色的多孔配位聚合物。对于得到的紫红色的多孔配位聚合物,使用超导量子干涉型磁通量计(SQUID)确认自旋状态,结果为低自旋状态。制作使得到的多孔配位聚合物5mg分散于20ml的乙腈中而成的分散溶液,放入喷雾瓶中,在滤纸5种C上进行3次喷雾涂布,使之在25℃下真空干燥,由此完成了气体检测器。
(气体检测器的担载量测定)
对于得到的气体检测器的每单位面积的多孔配位聚合物的担载量,通过上述的荧光X射线分析法求得,结果为0.1mg/cm2。
(碳酸二乙酯气体的检测)
在5L用采样袋(Tedlar bag)中装入小型风扇和气体检测器,向其中送入包含DEC的氮气并装满以使之成为5ppm的浓度,72分钟后可以确认气体检测器变化为橙色。另一方面,在仅送入氮气的情况下,没有发现有色调变化。由此,通过评价气体检测器的色调变化,可以检测DEC。
(其它气体的检测)
使用乙烯、丙烯、甲苯、二甲苯、丙酮、乙酸乙酯、四氢呋喃、甲醇、乙醇、正丙醇、异丙醇、乙二醇、氨、二甲基胺、三甲基胺、三乙基胺、乙酸、甲醛、乙醛、二乙基醚、DMC、EMC以及碳酸丙烯酯来代替DEC,同样地评价了气体检测器的色调变化,结果可以确认变化为橙色。
(锂离子二次电池的泄露气体检测)
准备2个在锂离子二次电池的箱体表面粘贴制得的气体检测器的样品。对于其中之一,在箱体上设想产生了小孔的状态而通过针人工地开一个小孔,分别放入采样袋中在密封的状态下放置72分钟。评价形成有小孔的锂离子二次电池的气体检测器的色调变化,结果变色为橙色,用气密注射器采取采样袋中的气体10μL,使用色相色谱仪进行成分分析,结果检测出约5ppm的DEC。另一方面,采取没有发现有气体检测器的色调变化的放入了锂离子二次电池的采样袋中的气体,进行成分分析,结果没有检测出来自电解液的气体成分。
(双电层电容器的泄露气体检测)
准备2个在电解液中含有碳酸丙烯酯的双电层电容器的箱体表面粘贴制得的气体检测器的样品。对于其中之一,在箱体上设想产生了小孔的状态而通过针人工地开一个小孔,分别放入采样袋中在密封的状态下放置78分钟。评价形成有小孔的双电层电容器的气体检测器的色调变化,结果变色为橙色,用气密注射器采取采样袋中的气体10μL,使用色相色谱仪进行成分分析,结果检测出约8ppm的碳酸丙烯酯。另一方面,采取没有发现有气体检测器的色调变化的放入了双电层电容器的采样袋中的气体,进行成分分析,结果没有检测出来自电解液的气体成分。
<实施例2~4以及比较例1>
除了变更喷雾涂布次数以外,与实施例1同样地制作气体检测器。将与实施例1同样地求得的多孔配位聚合物的担载量以及目视确认气体检测器的色调变化的时间示于表1中。
<比较例2>
除了变更多孔配位聚合物的乙腈分散溶液的浓度以及喷雾涂布次数以外,与实施例1同样地制作气体检测器。将与实施例1同样地求得的多孔配位聚合物的担载量以及目视确认碳酸二乙酯气体在检测试验中的气体检测器的色调变化的时间示于表1中。
[表1]
(碳酸二乙酯气体的检测)
对于实施例2~4的气体检测器,与实施例1同样地评价由碳酸二乙酯气体产生的色调变化,结果确认了气体检测部变化为橙色。对于比较例1和比较例2的气体检测器,与实施例1同样地评价由碳酸二乙酯气体产生的色调变化,结果经过100分钟后的色调变化不明显,不能目视确认。
<实施例5>
(气体检测器的制作)
激昂与实施例1同样地制作的多孔配位聚合物的乙腈分散溶液放入喷雾瓶中,在滤纸5种C上的一半区域进行3次喷雾涂布,在25℃下使之真空干燥之后,在未涂布区域进行9次喷雾涂布,在25℃再次使之真空干燥,由此完成了气体检测器。与实施例1同样地求得的每单位面积的多孔配位聚合物的担载量在喷雾涂布了3次的区域中为0.1mg/cm2,在喷雾涂布9次的区域中为0.3mg/cm2。
(碳酸二乙酯气体的检测)
与实施例1同样地,在5L用采样袋中装入小型风扇和实施例5中制作的气体检测器,向其中送入包含DEC的氮气并装满以使之成为5ppm的浓度,结果72分钟后通过与喷雾涂布了9次的区域比较可以容易地确认喷雾涂布了3次的区域变化为橙色。
<实施例6~15、比较例3~5>
除了以成为表2记载的组成的方式称量硫酸铵铁(II)六水合物、四氰基镍(II)酸钾一水合物、四氰基钯酸钾水合物以及四氰基铂酸钾水合物以外,与实施例1同样地制作多孔配位聚合物和气体检测器。将与实施例1同样地求得的多孔配位聚合物的担载量以及目视确认气体检测器的色调变化的时间示于表2中。
[表2]
(碳酸二乙酯气体的检测)
对于实施例6~15的气体检测器,与实施例1同样地评价由碳酸二乙酯气体产生的色调变化,结果确认了气体检测部变化为橙色。对于比较例3~5的气体检测器,与实施例1同样地评价由碳酸二乙酯气体产生的色调变化,结果经过100分钟后的色调变化不明显,不能目视确认。
<实施例16>
(气体检测器的制作)
在70℃下降与实施例1同样地制作的气体检测器加热1小时,将多孔配位聚合物制成高自旋状态的橙色,制作气体检测器。
(双电层电容器的泄露气体检测)
准备2个在电解液中含有乙腈的双电层电容器的箱体表面粘贴制得的实施例16的气体检测器的样品。对于其中之一,在箱体上设想产生了小孔的状态而通过针人工地开一个小孔,分别放入采样袋中在密封的状态下放置3分钟。评价形成有小孔的双电层电容器的气体检测器的色调变化,结果变色为紫红色,用气密注射器采取采样袋中的气体10μL,使用色相色谱仪进行成分分析,结果检测出约20ppm的乙腈。另一方面,采取没有发现有气体检测器的色调变化的放入了双电层电容器的采样袋中的气体,进行成分分析,结果没有检测出来自电解液的气体成分。
根据以上的结果,实施例的气体检测器可见性优异,并且灵敏度优异,另外,通过使用具有实施例的气体检测器的电化学元件,可以容易地灵敏度良好地进行气体检测。
Claims (3)
1.一种气体检测器,其特征在于,
通式(1)所表示的多孔配位聚合物被担载于支撑体上,
每单位面积的多孔配位聚合物的担载量为0.02mg/cm2以上且0.3mg/cm2以下,
Fex(吡嗪)[Ni1-yMy(CN)4] (1)
0.95≤x<1.05,M=Pd、Pt,0≤y<0.15。
2.如权利要求1所述的气体检测器,其特征在于,
在支撑体上形成有每单位面积的多孔配位聚合物的担载量不同的2个以上的区域。
3.一种电化学元件,其特征在于,
所述电化学元件使用了含有挥发性有机化合物的电解液,
在表面附近具备权利要求1或2所述的气体检测器。
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