CN107238647A - 气体检测片和具备气体检测片的电化学元件 - Google Patents
气体检测片和具备气体检测片的电化学元件 Download PDFInfo
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- CN107238647A CN107238647A CN201710184229.9A CN201710184229A CN107238647A CN 107238647 A CN107238647 A CN 107238647A CN 201710184229 A CN201710184229 A CN 201710184229A CN 107238647 A CN107238647 A CN 107238647A
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- gas
- detection lug
- gas detection
- coordination polymer
- porous coordination
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Classifications
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- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/406—Cells and probes with solid electrolytes
- G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
- G01N27/4073—Composition or fabrication of the solid electrolyte
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0054—Ammonia
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/14—Arrangements or processes for adjusting or protecting hybrid or EDL capacitors
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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- H01G11/54—Electrolytes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
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- H—ELECTRICITY
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/78—Cases; Housings; Encapsulations; Mountings
- H01G11/82—Fixing or assembling a capacitive element in a housing, e.g. mounting electrodes, current collectors or terminals in containers or encapsulations
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
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- H—ELECTRICITY
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- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
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- H—ELECTRICITY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Combustion & Propulsion (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Materials Engineering (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Examining Or Testing Airtightness (AREA)
Abstract
本发明提供一种能够可见性优异并且灵敏度良好地特定气体泄漏位置的气体检测片。本发明可以提供通过使用以下的气体检测片从而能够可见性优异并且灵敏度良好地特定气体泄漏位置的气体检测片,所述气体检测片其特征在于,通式(1)所表示的多孔配位聚合物被担载于支撑体上,透气度为0.8秒以上且60秒以下。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片以及具备气体检测片的电化学元件。
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。
另外,在专利文献2中提出了使用与气体成分反应变色的气体检测管来检测气氛中的气体的方法。然而,虽然能够检测气体从电化学元件中泄漏到气氛中,但是存在不能特定气体泄漏位置的问题。
现有技术文献
专利文献
专利文献1:日本特开2009-26569号公报
专利文献2:日本特开2005-62026号公报
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能够可见性优异并且灵敏度良好地特定气体泄漏位置的气体检测片。
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片可以达成上述目的,所述气体检测片其特征在于,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),透气度为0.8秒以上且60秒以下,至此完成本发明。
即,根据本发明,可以提供以下的内容。
[1]一种气体检测片,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,
透气度为0.8秒以上且60秒以下,
Fex(吡嗪)[Ni1-yMy(CN)4] (1)
0.95≤x<1.05,M=Pd、Pt,0≤y<0.15。
[2]如[1]所述的气体检测片,其特征在于,支撑体的一个面整体被保护层覆盖。
[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]所述的气体检测片。
发明的效果
根据本发明,可以提供一种能够可见性优异并且灵敏度良好地特定泄漏气体位置的气体检测片。
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片的示意图。
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…气体检测片、6…多孔配位聚合物、7…支撑体、8…保护层。
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片,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)
透气度为0.8秒以上且60秒以下。
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进行气体检测。
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片的示意图。在图2中,气体检测片5由多孔配位聚合物6、支撑体7和保护层8构成。
本实施方式的气体检测片5中,在多孔配位聚合物6被担载于支撑体7上,并且透气度为0.8秒以上时,在支撑体内部检测气体容易扩散,多孔配位聚合物的色调变化变得明显,进一步,通过利用透过了支撑体的检测气体产生的多孔配位聚合物的色调变化,可以容易地特定气体泄漏位置。另外,在透气度为60秒以下时,即使在检测气体少量的情况下,透过了支撑体的检测气体产生的多孔配位聚合物的色调变化也明显,可以容易地特定气体泄漏的位置。透气度为0.7秒以下时,支撑体的孔隙变大,发现有被担载的多孔配位聚合物的色调变化不明显的倾向。另外,在透气度为65秒以上时,在检测气体少量的情况下,发现有颜色变化不明显的倾向,直至检测气体透过支撑体为止花费时间,进一步,认为是由于支撑体上可以吸附的气体变多。
本实施方式的气体检测片除了来自检测片的表面的气体以外,对于透过了检测片的支撑体的气体也可以灵敏度良好地进行检测。通过使用本实施方式的气体检测片,评价透过了检测片的支撑体的气体产生的多孔配位聚合物的色调变化,由此可以不需要从电化学元件中取出检测片而特定气体泄漏位置。
支撑体7可以使用例如滤纸等的纤维素类厚纸或人造纤维类或聚酯类的纸过滤器。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,从气体检测片的制造时或使用时的操作容易性的观点出发,优选为50~1000μm。
本实施方式的气体检测片优选一个面整体被保护层8覆盖。保护层的材质只要是不对多孔配位聚合物的自旋状态产生影响的就没有特别地限定,例如可以列举聚对苯二甲酸乙二醇酯薄膜、聚偏二氯乙烯薄膜以及聚乙烯薄膜等或硅树脂或聚酰亚胺树脂等。另外,保护层优选可见光的透过率为70%以上,可以透过保护层确认多孔配位聚合物的色调变化。进一步,保护层优选透湿度以及挥发性有机化合物的透过度低,可以抑制由于试验环境中的水蒸气或挥发性有机化合物而导致的多孔配位聚合物的色调变化。保护层也可以用粘结剂或两面胶等与气体检测片粘结。
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、浸涂法等。
(气体检测片的担载量测定)
本实施方式的气体检测片的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),根据对检测片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元素的单位面积的担载量,计算并求得多孔配位聚合物的担载量。使用Rigaku Corporation制造的ZSX100e,以3mmΦ(5mmΦSUS制的掩模架)对测定点直径进行测定,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。
(透气度的测定)
本实施方式的气体检测片的透气度通过在一定的压力下测定300ml空气通过气体检测片的时间来求得。测定部直径为10mmΦ,测定方法按照JIS8117。
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片。
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片,在箱体的密闭性不充分时或者箱体上产生了小孔等时,通过评价气体检测片的色调变化,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片,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。
(气体检测片的制作)
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。将使得到的多孔配位聚合物10mg分散于35ml的乙腈中而成的分散溶液放入SUS制的盆中,在分散溶液中浸渍厚度为0.5mm且透气度为10秒的卷纸,使SUS制的盆振动之后,静置5分钟。其后,缓慢地从分散溶液中取出卷纸,使之干燥,由此完成了气体检测片。
(气体检测片的担载量测定)
对于得到的气体检测片的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。
(气体检测片的透气度测定)
对于得到的气体检测片的透气度,通过上述的方法求得,结果为10秒。
(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片,向其中送入包含DEC的氮气并装满以使之成为6ppm的浓度,63分钟后可以确认气体检测片变化为橙色。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,可以确认通过评价气体检测片的色调变化,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片的色调变化,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以及气体泄露位置检查)
准备2个锂离子二次电池,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在锂离子二次电池的正极端子附近在一个地方开一个小孔,使用实施例1的气体检测片分别包住锂离子二次电池,放入采样袋中在密封的状态下放置63分钟。评价气体检测片的色调变化,结果在形成有小孔的锂离子二次电池的正极端子附近变色为橙色,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6ppm的DEC。另一方面,采取没有发现有气体检测片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和气体泄漏位置检查)
准备2个在电解液中含有碳酸丙烯酯的双电层电容器,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在双电层电容器的正极端子附近开一个小孔,使用实施例1的气体检测片分别包住双电层电容器,分别放入采样袋中在密封的状态下放置66分钟。确认形成有小孔的双电层电容器的正极端子附近变色为橙色,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9ppm的碳酸丙烯酯。另一方面,采取没有发现有气体检测片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2~5以及比较例1和2>
除了使用透气度不同的卷纸,并且以气体检测片的单位面积的多孔配位聚合物的担载量成为0.1mg/cm2的方式变更多孔配位聚合物的分散溶液的浓度以外,与实施例1同样地制作气体检测片。将与实施例1同样地求得的气体检测片的透气度以及目视确认DEC气体的检测试验的气体检测片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2~5的气体检测片,与实施例1同样地评价由DEC气体产生的色调变化,结果确认了气体检测片变化为橙色。对于比较例1和比较例2的气体检测片,与实施例1同样地进行了由DEC气体产生的色调变化的评价,结果经过80分钟后的色调变化不明显,不能目视确认。
(锂离子二次电池的泄露气体检测和气体泄漏位置检查)
对于实施例2~5的气体检测片,与实施例1同样地进行锂离子二次电池的泄露气体检测以及气体泄漏位置检查,评价了气体检测片的色调变化,结果在形成有小孔的锂离子二次电池中分别确认了正极端子附近变化为橙色。对于比较例1和比较例2的气体检测片,与实施例1同样地进行锂离子二次电池的泄露气体检测以及气体泄漏位置检查,评价了气体检测片的色调变化,结果经过80分钟后的色调变化不明显,并且不能目视确认。
<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,除了以气体检测片的单位面积的多孔配位聚合物的担载量成为0.1mg/cm2的方式改变多孔配位聚合物的分散溶液的浓度以外,与实施例1同样地制作气体检测片。将与实施例1同样地求得的气体检测片的透气度以及目视确认DEC气体的检测试验的气体检测片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的气体检测片,与实施例1同样地评价由DEC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的气体检测片,与实施例1同样地评价由DEC气体产生的色调变化,结果经过80分钟后的色调变化不明显,不能目视确认。
(锂离子二次电池的泄露气体检测和气体泄漏位置检查)
对于实施例6~15的气体检测片,与实施例1同样地进行锂离子二次电池的泄露气体检测以及气体泄漏位置检查,评价了气体检测片的色调变化,结果在形成有小孔的锂离子二次电池中分别确认了正极端子附近变化为橙色。对于比较例3~5的气体检测片,与实施例1同样地进行锂离子二次电池的泄露气体检测以及气体泄漏位置检查,评价了气体检测片的色调变化,结果经过80分钟后的色调变化不明显,并且不能目视确认。
<实施例16>
(气体检测片的制作)
在70℃下将与实施例1同样地制作的气体检测片加热1小时,将多孔配位聚合物制成高自旋状态的橙色,制作气体检测片。
(双电层电容器的泄露气体检测和气体泄漏位置检查)
准备2个在电解液中含有乙腈的双电层电容器,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在双电层电容器的正极端子附近开一个小孔,使用实施例16的气体检测片分别包住双电层电容器,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片的色调变化,结果正极端子附近变色为紫红色,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片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17>
(气体检测片的制作)
对于与实施例1同样地制得的气体检测片,作为保护膜以覆盖一个面整体的方式用粘结剂粘贴聚偏二氟乙烯透明薄膜,制作气体检测片。
(锂离子二次电池的泄露气体检测和气体泄漏位置检查)
准备锂离子二次电池,在箱体上设想产生了小孔的状态而通过针人工地在锂离子二次电池的正极端子附近开一个小孔,使用实施例17的气体检测片以保护层成为外侧的方式包住锂离子二次电池,放入5L用采样袋中,送入包含乙醇气体的氮气并装满以使之成为10ppm的浓度,在密封的状态下放置63分钟。评价气体检测片的色调变化,结果在使用了没有形成保护膜的气体检测片的情况下,整体变化为橙色,相对于此,实施例17的气体检测片中可以确认仅正极端子附近变化为橙色。
根据以上的结果,实施例的气体检测片可见性优异,并且可以可以特定气体泄漏的位置,另外,通过使用具有实施例的气体检测片的电化学元件,可以容易地灵敏度良好地进行气体检测。
Claims (3)
1.一种气体检测片,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,
所述气体检测片的透气度为0.8秒以上且60秒以下,
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所述的气体检测片,其特征在于,
一个面整体被保护层覆盖。
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所述的气体检测片。
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