CN107003274A - 用于检测烃类的气体传感器 - Google Patents
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Abstract
气体传感器包括外壳(22),所述外壳中安置有膜电极组件,所述膜电极组件包括传感电极(14)、反电极(16)以及安置于所述传感电极与所述反电极之间的固体聚合物电解质(12)。所述传感电极包含含有贵金属纳米粒子(34)的第一催化剂。所述反电极包含含有贵金属纳米粒子(34)的第二催化剂,其可具有与所述第一催化剂相同的组成或不同的组成。所述传感器外壳还包括与所述传感电极流体连通的开口(24),用于使测试气体接触所述传感电极。所述传感器还包括连接所述传感电极与所述反电极的电路(19)。
Description
背景
在各种工业或实验室环境中已使用用于检测烃类或取代烃类的气体传感器来进行过程控制。由于所述化合物还可能是可燃或可爆的,所以在使用或制造此类化合物的地方还使用气体检测传感器来进行泄漏检测。已使用或提出了各种类型的传感器。实例包括金属氧化物半导体(MOS)传感器、非分散红外检测器(NDIR)传感器、pellistor(粒状电阻器)传感器以及利用由陶瓷(诸如钙钛矿)制成的高温固体电解质的混成电位型传感器。
烃类或取代烃类的新应用对气体检测传感器已经形成并且持续形成新的挑战。一种此类应用是在冷却和加热领域,其中较早的氯化烃(CFC)归因于其对地球臭氧层的不利影响而被排除。最初用氯氟碳化合物R12(二氯二氟乙烷)代替氯化氟碳化合物;然而,关于其臭氧消耗潜能(ODP)的持续担忧以及关于化合物的全球变暖潜能(GWP)的新的担忧使其被氟化烃(如R32)代替。关于ODP和GWP的持续担忧结合蒸气压缩传热系统的性能要求已引起新的制冷剂的发展,诸如氟化不饱和烃(即氟化烯烃),如反-1,333-四氟丙烯(R1234ze)。然而,由于在许多HVAC和制冷系统中制冷剂流动回路至少部分位于内部建筑空间内,由泄漏引起的关于毒性和/或可燃性风险的担忧已对此类化合物的有效气体检测形成扩大的需要。在许多地区,正在制定建筑法规,将强制要求具备此类气体检测的能力。
已使用上述类型的传感器,并且在已采用它们的工业或实验室环境中取得不同程度的成功。然而,许多此类传感器有局限性,所述局限性在需要新的和现有的应用时会影响其有效性。举例来说,MOS和pellistor传感器归因于交叉敏感性而容易发出错误警报。此外,MOS传感器用于检测氟化烃的耐久性是有问题的,因为可能产生HF,从而可能会潜在地损害传感器。NDIR传感器已在低体积应用中使用,但难以制造成达到住宅HVAC市场所要求的适当公差并且较昂贵,并且有可能不适合于如HVAC和制冷系统所期望的广泛实现方式。顾名思义,高温固体电解质系统需要高温(典型地超过500℃),这使它们在成本和寿命限制方面对于许多应用来说不切实际,诸如住宅和商业HVAC和制冷系统。
鉴于对烃类气体传感器的严格要求,仍然需要可能在某些环境中更适合或更好地起作用、提供更好的成本或对整体传感器设计实现有益修改的新的替代方案。
简单描述
根据本公开的一些方面,气体传感器包括外壳,所述外壳中安置有膜电极组件,所述膜电极组件包括传感电极、反电极以及安置于传感电极与反电极之间的固体聚合物电解质。所述传感电极包含含有贵金属纳米粒子的第一催化剂。所述反电极包含含有贵金属纳米粒子的第二催化剂,其可具有与所述第一催化剂相同的组成或不同的组成。所述传感器外壳还包括与所述传感电极流体连通的开口,用于使测试气体接触所述传感电极。传感器还包括连接传感电极与反电极的电路。
根据本公开的一些方面,使用上文所描述的传感器的方法包括相对于反电极或参比电极对传感电极施加正偏压。然后使测试气体与传感电极接触,并且在连接传感电极与反电极的电路中在传感电极处由烃类或取代烃类的氧化产生电化学响应电压或电流。测量此电化学响应电压或电流以确定在测试气体中所测试的烃类或取代烃类的存在和/或浓度。
附图简述
在本说明书结束时在权利要求书中具体指出并清楚地要求本公开的主题。由以下结合附图而进行的详述,本公开的上述和其他特征以及优点是显而易见的,在附图中:
图1展示如本文所描述的气体传感器的简化示意图;
图2展示纳米粒子催化剂与诸如离聚物等离子传导介质一起被负载于催化剂载体上的示例性说明。
图3展示如本文所描述的传感器响应于暴露于丙烯的输出;并且
图4展示如本文所描述的传感器分别响应于暴露于2,333-四氟丙烯(R1234yf)和反-1,333-四氟丙烯(R1234ze)的输出。
详细描述
图1中示意性示出了气体传感器,其中膜电极组件(MEA)具有安置于传感电极14与反电极16之间的固体聚合物电解质(SPE)(即离子传导聚合物)12。将集电器15和17附连至电极,并且连接至电路18,所述电路包括测量和/或控制装置19。在一些实施方案中,可将任选的参比电极23安置于SPE 12中传感电极14与反电极16之间的位置。集电器15、17可由传导性网或毡形成,并且被展示为具有一定的厚度,使得它们还可充当测试气体和参考气体到达电极14、16的表面的气体扩散介质。在其他实施方案中,集电器15、17可为电极14、16的表面上的相对薄的几乎为二维的传导性筛网,并且相邻气体扩散介质不必为传导性的。可由诸如石墨化碳或不锈钢等耐氧化材料形成与传感电极14相关联的集电器/气体扩散介质15。可由诸如碳等传导性材料形成集电器/气体扩散介质17。测量和/或控制装置19可为伏特计(voltmeter)或安培计(ampere meter),但在许多情况下包括恒电位电路、微处理器或具有集成电压和或安培数测量功能的类似电子装置,并且还可在传感器的操作期间在传感电极14与反电极16之间施加偏压。
围绕MEA安置外壳22,其具有开口24以允许测试气体以受开口尺寸调控的气体通量进入传感器。开口被示出为完全打开,不过应了解,可将它们用筛网或气体渗透膜或吸附剂覆盖。另外,出于说明的目的将开口24示出为使测试气体直接通向腔室28,但还可通过从传感器的外表面通向内部腔室的通道将气体引入内部腔室。可将电极组件膜的边缘密封到密封件27,所述密封件由诸如橡胶等密封材料制成,从而将测试气体保持在MEA的传感电极侧,不过还可使用本领域中已知的其他技术(例如将MEA安置于被密封至外壳边缘的框架(未示出)中)。虽然所述密封件阻止测试气体进入反电极侧,但发现即使在存在测试气体进入反电极侧的通道的情况下,传感器仍可适当地发挥功能来确定烃类或取代烃类的存在。因此,还可使反电极16从由开口24或由外壳22中的另一开口产生的通道(未示出)暴露于测试气体。可如图1中所展示将电极14、16粘合至固体聚合物电解质,但也可通过诸如机械夹持力等其他手段使其保持在一起,而不会损害传感器的功能性。
当然,图1中所展示的实施方案在本质上为示意性和示例性的,并且同样可使用其他配置。在例如US 5,650,054、US 5,573,648、US 6,200,443、US 6,948,352、US 2009/0184005A1以及US 2010/0012494A1中公开了示例性气体传感器配置和其变化型式,所述专利的公开内容以全文引用的方式并入本文中。
虽然本公开不受任何理论或已认识到操作机制的约束,但据信烃类(诸如烯烃)的电化学氧化是经由如以下反应式(1a)和/或(1b)中所示的两个一电子过程来进行(用丙烯进行例示),反电子处的伴随反应如反应式(2)中所示:
CH3CH=CH2+2H2O-2e-→CH3CH(OH)CH2OH+2H+ (1a)
CH3CH=CH2+2H2O-2e-→CH3C(O)CH3+2H+ (1a)
1/2O2+2H++2e-→H2O (2)
电极的精确组成和制造它们时使用的材料将取决于针对与其一起使用的传感器和其他系统组件所测试的特定烃类以及与其一起使用的传感器和其他系统组件的设计参数。可使用各种催化性贵金属和其合金(例如铱、铼、钯、铂、铜、铟、铷、银、金)来形成电极。在一些示例性实施方案中,传感电极和/或反电极包含铂或二元或三元铂合金,诸如PtNi、PtFe、PtCo、PtRu、PtRuNi、PtCr、PtCoCr、PtIrCo或PtCuFe,其中Pt含量以原子比率计在20%至100%范围内。在一些钯或铂和钯的混合物或合金中。在一些示例性实施方案中,传感电极和/或反电极包含钯或钯合金,诸如PdAg、PdNi、PdCu、PdRu或PdY。反电极可包含催化剂,所述催化剂包括不同于传感电极催化剂金属的贵金属。可对反电极中的催化剂加以选择来促进氧还原反应。电化学传感器中所用的电极典型地除贵金属催化剂外还包括导电材料,并且常常通过将贵金属催化剂的纳米粒子安置于诸如碳黑等导体的更大的粒子上来提供此导电材料,其通常被称为碳负载型催化剂。然而,对于涉及在传感电极上进行烃类氧化的烃类检测来说,有效氧化诸如烯烃和取代烯烃(例如氟化烯烃)等烃类所需的电极电位超过碳载体材料的热力学氧化(例如相较于标准氢电极为207mV)。因此,本文所描述的传感器的传感电极可包含非负载型催化剂或负载于不同于碳黑的耐氧化载体上的催化剂。对于非负载型催化剂与负载型催化剂两者,可通过形成包含纳米粒子(纳米粒子意味着粒子具有小于20nm、更具体地说2-10nm的公称直径)和分散于溶剂混合物中的离聚物的油墨,并且通过丝网印刷、喷墨印刷或类似方法向固体聚合物电解质膜的表面上沉积油墨层来将传感电极施加于固体聚合物电解质上。在蒸发溶剂之后,所得电极呈具有包含于离聚物基质中的催化剂纳米粒子的复合结构的层状物的形式,其中离聚物充当其中散布有催化剂纳米粒子的传导性基质材料。用于制造MEA的第二种方法是将电极油墨沉积至衬底(即TeflonTM或KaptonTM薄片)上,以在溶剂蒸发之后形成贴花,随后进行热压以将催化剂层转移至膜上。在用于传感电极的负载型催化剂的情况下,将催化剂负载于耐氧化传导性载体上,所述传导性载体可包含耐氧化载体粒子,所述耐氧化载体粒子典型地大于催化剂纳米粒子。在一些示例性实施方案中,载体粒子可具有20至200nm的公称直径。图2中展示了负载型催化剂,该图展示完全或部分由离聚物36的薄层覆盖的具有传导性载体粒子33与其上所安置的催化剂粒子34的附聚物32的一部分。“耐氧化意味着在传感器的可操作正偏压(即100至400mV)下,载体粒子的材料产生漂移小于由测试气体或诸如R1234ze等制冷剂所产生的信号的1/5的基线信号。稳定的基线可展现小于0.48μA/cm2/yr或0.011μA/cm2/1000h的漂移速率。用于传感电极中的耐氧化载体的材料的实例包括但不限于石墨化碳、碳纳米管(CNT)以及传导性或半传导性金属氧化物,诸如TiO2、WO3、SnO2等。在另一实施方案中,可将含贵金属的催化剂和传导性氧化物共加载至载体上以实现更高的活性,例如Pt-WO3/CNT。这些传导性金属氧化物可为未掺杂的,或者它们可掺杂有金属,诸如Sb、V、Tl、Mn、Co、Fe等。
还可由在存在传导性或非传导性粘合剂(即TeflonTM)的情况下催化剂粒子负载于更大的碳粒子上的常规碳负载型催化剂形成反电极,并且还可由碳筛网、网或毡形成与反电极相关联的集电器。在一个示例性实施方案中,可由公称直径为约20-200nm的传导性碳载体粒子与其上所安置的催化剂粒子(公称直径为约2-10nm)的由粘合剂(例如离聚物,诸如或非传导性粘合剂)的薄层覆盖的附聚物形成反电极。
可由能够跨越传感电极与反电极之间的电解质膜传导质子的任何离聚物形成固体聚合物电解质。示例性离子聚合物包括附接至聚合物使得聚合物具有离子交换能力的离子基团,此类基团包括但不限于磺酸、膦酸以及磺酰亚胺酸。示例性离聚物包括全氟化磺酸(“PFSA”)(诸如离聚物和Solvey Solexis AuqivionTM离聚物)、磺化聚苯乙烯、磺化聚砜、二磺化聚(亚芳醚砜)嵌段共聚物(“BPSH”)。还可向聚合物基质中添加常规添加剂,例如表面活性剂、溶剂(例如聚乙二醇)以及精细粒子(诸如官能化或非官能化二氧化硅、碳基粉末、金属氧化物粒子)。还可使用上文所描述的用于固体聚合物电解质的离聚物作为用于电极的离聚物。
在一些实施方案中,可将电极中的固体聚合物电解质和/或离聚物用诸如离子性液体(即熔点接近或低于室温的盐)等极性液体浸渍。在一些实施方案中,膜电极组件不含水或不用水浸渍,除了存在在反电极处通过上文所描述的反应(2)以电化学方式产生的水。
可如下操作传感器:相对于反电极或参比电极对传感电极施加正偏压,使传感电极暴露于正在测试的气体,测量连接传感电极与反电极的电路中的电压或电流,并且将测得的电压或电流转化成指示正在测试的气体中的组分的存在和/或浓度的读数。传感电极处烃类或取代烃类的氧化将引起电化学响应,所述电化学响应可被检测为电路中的电压或电流。在一些实施方案中,将恒电位电路、微处理器或类似装置19配置成施加正偏压并且测量响应电压或电流。在一些实施方案中,相对于反电极对传感电极施加的正偏压为20mV至800mV。在一些实施方案中,可以在200mV至400mV范围内的恒定正偏压的形式来施加所施加的正偏压。在一些实施方案中,正偏压可在20mV至800mV范围内变化达400mV的量。
传感器可检测各种烃类,诸如乙烷、丙烷;以及取代烃类,诸如氟化烃(例如二氟甲烷或R32、1,1-二氟乙烷或R152a、1,1,1,2-四氟乙烷或R134a)或氯化烃(例如氯甲烷或R40)。烯烃,包括作为制冷剂提供低ODP和低GWP潜能以及良好性能的氟取代烯烃使用现有技术传感器可能难以检测。在一些实施方案中,使用本文所描述的传感器来检测烯烃,诸如丙烯。在一些实施方案中,使用本文所描述的传感器来检测取代烯烃,诸如氟取代烯烃,例如四氟丙烯的异构体中的任一种(例如R1234ze、R1234yf、R1234zd)。
以下实施例中提供进一步的描述。
实施例
相对于反电极在传感电极处使用300mV的正偏压来操作如图1中所示而配置的不含参比电极的原型传感器,并且暴露于空气,将所述空气定期与不同浓度的丙烯混合。图3中示出了传感器响应。如图3中所示,传感器有效识别丙烯,并且响应随着丙烯浓度的增加而增加。在一项单独的测试中,将空气定期与不同浓度的R234yf或R1234ze混合。图4中示出了传感器响应,该图显示传感器有效识别所述化合物,并且响应随浓度增加而增加。
虽然仅仅结合有限数量的实施方案对本公开进行了详细描述,但应易于理解,本公开不限于这些所公开的实施方案。相反,可对本公开进行修改以并入任何数量的之前未描述但与本公开的精神和范围相符的变化方案、变更方案、替代方案或等效布置。此外,尽管已描述本公开的各种实施方案,但应理解,本公开的各个方面仅可包括所描述的实施方案中的一些。因此,本公开不应被视为受到前述描述限制,而是仅受所附权利要求书的范围限制。
Claims (24)
1.一种用于烃类或取代烃类的传感器,其包括:
外壳;
安置于所述外壳中的膜电极组件,所述膜电极组件包括传感电极,所述传感电极包含含有贵金属纳米粒子的第一催化剂;反电极,所述反电极包含含有贵金属纳米粒子的第二催化剂;以及固体聚合物电解质,所述固体聚合物电解质安置于所述传感电极与所述反电极之间,其中所述第一催化剂的所述纳米粒子为不带载体的或负载于并非碳黑的载体上;
与所述传感电极电接触的第一集电器;
与所述反电极电接触的第二集电器;
所述外壳包括与所述传感电极流体连通的开口,用于使测试气体接触所述传感电极;以及
连接所述传感电极与所述反电极的电路。
2.如权利要求1所述的传感器,其中所述第一和第二催化剂中的任一者或两者包含铂或二元或三元铂合金。
3.如权利要求2所述的传感器,其中所述第一和第二催化剂中的任一者或两者包含PtNi、PtFe、PtCo、PtRu、PtRuNi、PtCr、PtCoCr、PtIrCo或PtCuFe,其中所述Pt含量以原子比率计在20%至100%范围内。
4.如权利要求1所述的传感器,其中所述第一和第二催化剂中的任一者或两者包含钯或钯合金。
5.如权利要求4所述的传感器,其中所述第一和第二催化剂中的任一者或两者包含PdAg、PdNi、PdCu、PdRu或PdY,其中所述Pd含量以原子比率计在30%至100%范围内。
6.如权利要求1至5中任一项所述的传感器,其中所述第一催化剂的所述纳米粒子为不带载体的。
7.如权利要求1至5中任一项所述的传感器,其中将所述第一催化剂的所述纳米粒子负载于载体上,所述载体包括石墨化碳、石墨烯纳米片、碳纳米管或传导性或半传导性金属氧化物。
8.如权利要求1至7中任一项所述的传感器,其中所述第二催化剂的所述纳米粒子为不带载体的或负载于碳黑、石墨化碳、石墨烯纳米片、碳纳米管或传导性或半传导性金属氧化物上。
9.如权利要求1至7中任一项所述的传感器,其中将所述第二催化剂的所述纳米粒子负载于碳黑上。
10.如权利要求1至9中任一项所述的传感器,其中所述传感电极与所述反电极中的任一者或两者进一步包含离聚物。
11.如权利要求1至10中任一项所述的传感器,其中所述第一集电器包含不锈钢。
12.如权利要求1所述的传感器,其中所述第二集电器包含碳。
13.如权利要求1至12中任一项所述的传感器,其中所述第一集电器、所述第二集电器或所述第一集电器与所述第二集电器中的每一者还充当气体扩散介质。
14.如权利要求13所述的传感器,其中将所述第一集电器、所述第二集电器或所述第一集电器与所述第二集电器中的每一者配置成网或毡。
15.如权利要求1至14中任一项所述的传感器,其进一步包括与所述固体聚合物电解质电接触的参比电极。
16.如权利要求1至15中任一项所述的传感器,其中连接所述传感电极与所述反电极的所述电路包括电子控制器,所述电子控制器被配置成用于相对于所述反电极或参比电极对所述传感电极施加正偏压,以及测量连接所述传感电极与所述反电极的所述电路中的电压或电流以检测来自在所述传感电极处烃类或取代烃类的氧化的电化学响应。
17.一种使用如权利要求1至16中任一项所述的传感器的方法,其包括相对于所述反电极或参比电极对所述传感电极施加正偏压,引入测试气体而使之与所述传感电极接触以检测烃类或取代烃类,以及测量连接所述传感电极与所述反电极的所述电路中的电压或电流以检测来自在所述传感电极处烃类或取代烃类的氧化的电化学响应。
18.如权利要求16所述的传感器或如权利要求17所述的方法,其中根据由所述传感器产生的电信号来确定烃类或取代烃类的浓度。
19.如权利要求16所述的传感器或如权利要求17或18所述的方法,其中所述正偏压为20mV至800mV。
20.如权利要求19所述的传感器或方法,其中施加恒定正偏压,所述恒定正偏压在200mV至400mV范围内。
21.如权利要求19所述的传感器或方法,其中所述正偏压在达400mV的范围内变化。
22.如权利要求1至16中任一项所述的传感器或权利要求17至21中任一项所述的方法,其中烃类或取代烃类包括烯烃或取代烯烃。
23.如权利要求22所述的传感器或方法,其中所述烯烃或取代烯烃包括氟取代烯烃。
24.如权利要求23所述的传感器或方法,其中所述氟取代烯烃包括四氟丙烯的一种或多种异构体。
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EP (1) | EP3183565A1 (zh) |
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US11143610B2 (en) | 2013-10-15 | 2021-10-12 | Direct-C Limited | Sensing element compositions and sensor system for detecting and monitoring structures for hydrocarbons |
CN108474772B (zh) | 2015-11-03 | 2021-01-22 | 犹他大学研究基金会 | 用于选择性烷烃蒸汽检测的界面纳米纤丝复合物 |
CN110603439B (zh) * | 2017-05-12 | 2023-04-04 | 开利公司 | 用于气体测试的传感器和方法 |
US10996131B2 (en) | 2017-12-01 | 2021-05-04 | Johnson Controls Technology Company | Refrigerant gas sensing system |
US11054383B2 (en) | 2018-01-22 | 2021-07-06 | InSyte Systems, Inc. | Chip-scale sensing device for low density material |
US11835364B2 (en) * | 2020-01-29 | 2023-12-05 | Hadronex, Inc. | Sensor housing with debris sloughing structure |
TWI725738B (zh) * | 2020-02-18 | 2021-04-21 | 新唐科技股份有限公司 | 阻障層及包括該阻障層的氣體感測器 |
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- 2015-08-20 US US15/505,012 patent/US10697924B2/en active Active
- 2015-08-20 EP EP15757388.2A patent/EP3183565A1/en not_active Ceased
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US20180195995A1 (en) | 2018-07-12 |
US10697924B2 (en) | 2020-06-30 |
WO2016029003A1 (en) | 2016-02-25 |
EP3183565A1 (en) | 2017-06-28 |
CN107003274B (zh) | 2021-03-02 |
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