CN109792075A - 固化的、适型的多孔复合材料及相关的装置、方法和用途 - Google Patents
固化的、适型的多孔复合材料及相关的装置、方法和用途 Download PDFInfo
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Abstract
本发明公开了一种固化的、适型的多孔复合材料,其具有互连的孔并含有热膨胀的聚合物微球和颗粒填充材料。本发明公开了一种能量存储装置,其包含具有互连的孔并且包含热膨胀的聚合物微球和颗粒填充材料的固化的、适型的多孔复合材料。本发明公开了一种制备固化的、适型的多孔复合材料的方法,其中在孔的形成中没有溶剂被引入复合材料或从复合材料中被提出。
Description
版权声明
2017 Amtek Research International LLC。本专利文件的公开内容的一部分包含受版权保护的材料。由于其出现在美国专利和商标局的专利文件或记录中,版权所有者不反对任何人对专利文件或专利公开内容进行摹真复制,但在其他方面保留所有版权。37 CFR§1.71(d)。
技术领域
本发明涉及具有互连孔的固化的、适型的多孔复合材料,并且其包括热膨胀的聚合物微球和颗粒填充材料。该固化的、适型的多孔复合材料(1)在不使用加工油和伴随的萃取溶剂的情况下表现出良好的孔隙率,并且(2)表现出足够的电解液润湿性。这种固化的、适型的多孔复合材料可用作隔膜,以改善诸如铅酸电池组的储能装置的可制造性和性能。
背景技术
随着技术的发展,用于铅酸蓄电池组的隔膜已由不同的材料形成。随着时间的推移,木材、纸张、橡胶、PVC、玻璃纤维和二氧化硅填充的聚乙烯都可使用。目前,发现铅酸蓄电池组通常有两种设计模式,即阀控式重组(阀控铅酸(VRLA))电池和富液式电池。两种模式都包括通过多孔电池组隔膜彼此分开的正电极和负电极。多孔隔膜防止电极物理接触并为电解液提供停留空间。这种隔膜由耐硫酸电解液的材料形成,易于在硫酸中润湿,并且具有足够的多孔性以允许电解液存在于隔膜材料的孔中,从而允许离子电流在相邻的正极板和负极板之间以低电阻流动。
最近,已经开发出增强型富液式电池组(EFB)以满足“启停”或“微混合动力”车辆应用中的高循环要求。在这种应用中,在车辆停止时(例如,在交通灯处)关闭发动机,之后重新起动发动机。“启停”车辆设计的优势在于它可以减少二氧化碳排放并提高整体燃油效率。“启停”车辆的主要挑战是电池组必须在停止阶段期间继续提供所有电气功能,同时能够提供足够的电流以在所需时刻重新起动发动机。在这种情况下,与传统的富液式铅酸蓄电池组设计相比,电池组必须在循环和再充电能力方面表现出更高的性能。
在“启停”应用的情况下,阀控铅酸(VRLA)电池组已经在该领域显示了良好的可循环性,但是它们具有相对高的成本和其他问题。因此,仍然需要机械上坚固、耐酸、高孔隙率的隔膜,其可以在“启停”应用中使用的铅酸蓄电池组的整个寿命周期中使用。
对于二氧化硅填充的聚乙烯隔膜,传统的制造方法包括挤出、提取,然后干燥、切割和卷绕步骤。沉淀二氧化硅通常与聚烯烃、加工油和各种次要成分组合以形成隔膜混合物,其在升高的温度下通过片材机头挤出以形成充油片材。将充油片材压延至其所需的厚度和轮廓,并提取大部分工艺油。将片材干燥以形成微孔聚烯烃隔膜,并切成适当宽度以用于特定的电池组设计。在该制造过程中,加工油的提取和提取溶剂的干燥是限制步骤。生产线的产量取决于可以移除加工油的速度以及溶剂干燥的速度,这两者都取决于隔膜产品的厚度。三氯乙烯(TCE)和己烷通常用作加工油的提取溶剂,它们在健康、安全和有效回收方面存在挑战。
因此,还需要一种不使用危险和/或易燃溶剂制造的电池组隔膜。隔膜应具有所需的性能,例如良好的润湿性、良好的孔隙率,并且允许电池组具有高循环性和再充电能力。
发明内容
已经发现,闭路电池可膨胀微球可与颗粒填充材料组合以形成固化的、适型的多孔复合材料,其具有互连的孔并含有热膨胀的聚合物微球和颗粒填充材料。该固化的、适型的多孔复合材料可以形成具有良好润湿性、良好孔隙率的电池组隔膜,并且允许电池组具有高循环性和再充电能力。
可膨胀微球优选是可膨胀聚合物微球,例如(AkzoNobel N.V.)、Advancell EM(Sekisui Chemical Co.,Ltd.)、Kureha Microsphere(Kureha Corp.)、(Chase Corp.)、(PolyChem Alloy)。Expancel微球为小的球形热塑性颗粒,其由包封气体的聚合物壳组成。加热时,来自气体的内部压力增加,同时热塑性外壳软化。因此,在气体被捕获于球体内部的情况下,微球体积增加。
颗粒填充材料优选包括无机材料。无机材料优选包括无机氧化物、碳酸盐或氢氧化物,例如氧化铝、二氧化硅、氧化锆、二氧化钛、云母、勃姆石或其混合物。无机材料为固化的、适型的多孔复合材料提供电解液润湿性。无机材料可以是多孔的或无孔的。无机材料可以为各种形式,例如研磨或未研磨形式的颗粒、纤维(例如微玻璃纤维)、薄片或纳米管。无机材料优选不溶于铅酸电池组中常用的电解液硫酸。无机材料可以不溶于碱性电池组中常用的电解液氢氧化钾。无机材料优选为固化的、适型的多孔复合材料的约30wt%至约90wt%。
优选使用压缩和加热来形成固化的、适型的多孔复合材料。颗粒填充材料优选与可膨胀微球混合,然后在限定的体积空间(例如模具)中加热。该过程可以分批或连续进行。同样,固化的、适型的多孔复合材料可以在电池组的电极之间原位形成。
固化的、适型的多孔复合材料的通过水孔隙率测定的孔隙率优选为30%以上,例如约40%或更大、约50%或更大、约60%或更大、约70%或更大、或约80%或更大。例如,孔隙率可为约30%至约90%、约40%至约90%、约50%至约90%、约60%至约90%、约70%至约90%、约75%至约90%、约80%至约90%或约85%至约90%。
可以添加机械增强材料以增加固化的、适型的多孔复合材料的结构强度。机械增强材料可以是主要形成在固化的、适型的多孔复合材料的一个或两个主表面上或者至少部分地嵌入固化的、适型的多孔复合材料的整体结构中的支撑体。支撑体的实例包括泡沫、片材、薄膜、网状物、膜、织造或非织造垫、丝网或它们的组合。
固化的、适型的多孔复合材料优选为可电解质润湿的,并且具有通过水孔隙率测定(例如针对孔隙率(体积)和水分含量的BCIS-03-6测试方法)的约30-90%的孔隙率。如上所述的固化的、适型的多孔复合材料可用于分离能量存储装置(例如电池组、电化学双层电容器、超级电容器或燃料电池)中的电极,其中孔可以填充有电解液。这种隔膜有利于能量存储装置的制造。
通过以下参考附图进行的优选实施方案的详细描述,其他方面和优点将变得很明显。
附图说明
图1描绘了显示来自实施例3的工艺步骤的图片。
图2A描绘了从实施例9获得的样品的SEM断裂水平视图图像。
图2B描绘了与图2A中相同的样品的SEM断裂垂直视图图像。
图3描绘了显示来自实施例10的单电池的图片。
图4描绘了由实施例11制备的样品。
图5A描绘了从实施例12获得的样品的顶表面的SEM图像。
图5B描绘了与图5A中相同的样品的横截面的SEM图像。
具体实施方式
通过将可膨胀微球与颗粒填充材料混合,可以制备具有互连的孔并含有热膨胀微球和颗粒填充材料的固化的、适型的多孔复合材料。微球可以为干粉或水分散体。同样,颗粒填充材料可以为干粉或水分散体。然后可将混合物置于模具(或其他容积限定的空间)中并加热足够的时间以将材料粘合在一起。微球的膨胀为粘合提供必要的压缩。模具的体积(其随着微球膨胀影响压力)和加热的温度及持续时间可用于使至少一部分热膨胀的聚合物微球由于微球中包封的气体的逸出而破裂。膨胀后,缓慢冷却模具。微球保持膨胀状态,粘合在一起。然后将固化的、适型的多孔复合材料从模具中取出。当存在水分散体时,作为形成过程的一部分,可以将水蒸发掉。在加热混合物之前,可以将机械增强材料放置在模具中。如本文所用,“固化的、适型的多孔复合材料”的意思是复合材料为一种与体积限定的空间的形状同形的固体,可膨胀微球和颗粒状填充材料在该体积限定的空间中被加热。
可以使模具图案化(或其他体积限定的空间)以提供各种棱纹图案。另外,固化的、适型的多孔复合材料在从模具中取出后可以进一步成形。固化的、适型的多孔复合材料可以形成片材或其他所需的几何形状。例如,可以形成片材,其具有至少一个图案化主表面,具有厚度为约0.3mm至约0.6mm或约0.4mm至约0.5mm的区域,以及具有厚度为约0.5mm至约5mm或约1mm至约3mm的区域。
可以在电池组或其他能量存储装置的电池中重复相同的过程。可膨胀微球和颗粒填充材料的自由流动混合物可置于电池的电极之间,为电池加盖,然后加热电池。当微球膨胀时,固定的电池体积提供必要的压缩。没有必要从电池中除去固化的、适型的多孔复合材料。在形成固化的、适型的多孔复合材料之后,可以将电解液直接添加到电池中。
固化的、适型的多孔复合材料(在原位形成或在模具中形成)与电极良好接触,并且没有检测到酸中膨胀的Expancel微球的渗出。固化的、适型的多孔复合材料具有良好的酸润湿性、良好的孔隙率,并且允许电池组具有高循环性和再充电能力。
固化的、适型的多孔复合材料可以与许多能量存储装置一起使用,例如碱性电池组或铅酸电池组。固化的、适型的多孔复合材料可以构成隔膜或其一部分。
固化的、适型的多孔复合材料的颗粒填充材料可包括添加剂。固化的、适型的多孔复合材料可包括有益地影响能量存储装置性能的添加剂。优选的添加剂包括析氢抑制剂、电解液可溶的造孔剂、结构增强剂、润湿性增强剂或它们的组合。某些添加剂可以执行多种功能。
现在转向具体的示例性添加剂,在组装电池组并添加电解液之后,将电解液可溶的造孔剂溶解在电解液中(通常为用于铅酸电池组的硫酸和用于碱性电池组的氢氧化钾水溶液)。电解液可溶的造孔剂的溶解导致隔膜孔隙率的增加、隔膜的相互毗邻的孔之间的互连性(即迂曲度)的改变和孔径分布的增大。在电解液可溶的造孔剂溶解后,任选地用新鲜电解液冲洗电池组。对于铅酸电池组,优选地,电解液可溶的造孔剂为氢氧化镁、氧化镁或它们的组合。电解液可溶的造孔剂可包括锌、锂、铝、镁、锡、钾或钠的硫酸盐。电解液可溶的造孔剂还可包括锂、镁、钾或钠的碳酸盐。电解液可溶的造孔剂可与上述为固化的、适型的多孔复合材料提供电解质润湿性的无机材料相结合。
析氢抑制剂可以分布在固化的、适型的多孔复合材料的整个孔结构中。析氢抑制剂的实例包括苯甲醛衍生物,例如香草醛、邻-茴香醛、2-羟基苯甲醛、4-甲氧基苯甲醛、2,4-二甲氧基苯甲醛、2,5-二甲氧基苯甲醛、藜芦醛(3,4-二甲氧基苯甲醛)和2,3,4-三甲氧基苯甲醛。
固化的、适型的多孔复合材料还可包括不是颗粒填充材料的添加剂,例如表面活性分子,例如十二烷基苯磺酸钠或二己基磺基琥珀酸钠。用于非能量存储装置的其他添加剂包括香料。
能够在原位形成固化的、适型的多孔复合材料的这种能力对于制造有益。例如,固化的、适型的多孔复合材料可以在电池组的组装期间制造。这可以使双极堆叠配置形式的铅酸电池组的制造变得容易,具有伴随的能量密度和均匀电流密度方面的益处。固化的、适型的多孔复合材料(在原位形成或在模具中形成)的其他制造益处对于本领域技术人员而言是显而易见的。
除了隔膜之外,固化的、适型的多孔复合材料可以用于制造能量存储装置的其他部件,例如阻火器。此外,固化的、适型的多孔复合材料可用于非能量储存装置相关的用途,例如香料储存。
实施例
对于每个实施例,通过混合表1中列出的干粉形成牢固且稳定的固化的、适型的多孔复合材料。
对于实施例1-9,将充分混合的干粉在严密密封的4盎司塑料罐(参见图1)中在列出的温度下用烘箱加热1小时,该塑料罐为膨胀微球提供所需的压缩,这使得混合粉末粘合形成牢固且坚硬的固化的、适型的多孔复合材料。
对于实施例10,通过将所列出的混合干粉配方粘合在从Deka YB16B干式荷电摩托车电池组(East Penn Manufacturing Co.,Inc.)获得的一个正极和一个负极组成的单电池中形成固化的、适型的多孔复合材料。盖上电池并置于烘箱中,在所列温度下固化2小时。电池显示出高循环和再充电能力。
对于实施例11-48,将所列出的充分混合的干粉制剂和玻璃纤维垫在具有垫圈的模具之间压制,并在所列温度下在恒定压力下加热15分钟。在移除样品之前使模具缓慢冷却。将模板设计为其中具有凹槽,使得成品样品具有棱纹表面。实施例11-48的总厚度范围为约0.5mm至约3mm。
使用DC脉冲技术评估实施例26的电阻。将样品浸泡在硫酸中,然后置于测试浴中。该实施例显示出足够低的电阻,表明良好的电解质润湿性。
表1
对于本领域技术人员显而易见的是,在不脱离本发明的基本原理的情况下,可以对上述实施方案的细节进行许多改变。
Claims (20)
1.一种固化的、适型的多孔复合材料,其具有互连的孔并包含热膨胀的聚合物微球和颗粒填充材料。
2.根据权利要求1所述的固化的、适型的多孔复合材料,其中所述固化的、适型的多孔复合材料具有约30%或更大的孔隙率。
3.根据权利要求1所述的固化的、适型的多孔复合材料,其中所述固化的、适型的多孔复合材料为可电解液润湿的并且具有通过水孔隙率测定的约30-90%的孔隙率。
4.根据权利要求1所述的固化的、适型的多孔复合材料,其中至少一部分所述热膨胀的聚合物微球在聚合物微球的热膨胀过程中由于被包封气体的逸出而破裂。
5.根据权利要求1所述的固化的、适型的多孔复合材料,其中所述热膨胀的聚合物微球和所述颗粒填充材料包括粘合的干粉或粘合的水分散体。
6.根据权利要求1所述的固化的、适型的多孔复合材料,其中所述颗粒填充材料包括无机材料。
7.根据权利要求6所述的固化的、适型的多孔复合材料,其中所述无机材料包括无机氧化物、碳酸盐、氢氧化物、氧化铝、二氧化硅、氧化锆、二氧化钛、云母、勃姆石或任何前述物质的混合物。
8.根据权利要求6所述的固化的、适型的多孔复合材料,其中所述无机材料占所述固化的、适型的多孔复合材料的约30重量%至约90重量%。
9.根据权利要求6所述的固化的、适型的多孔复合材料,其中所述颗粒填充材料还包含添加剂。
10.根据权利要求9所述的固化的、适型的多孔复合材料,其中所述添加剂包括析氢抑制剂、电解液可溶的造孔剂、结构增强剂、润湿性增强剂、香料或它们的组合。
11.根据权利要求1所述的固化的、适型的多孔复合材料,其还包括机械增强材料。
12.根据权利要求11所述的固化的、适型的多孔复合材料,其中所述机械增强材料包括主要形成在所述固化的、适型的多孔复合材料的主表面上或至少部分地嵌入所述固化的、适型的多孔复合材料的块状结构中的支撑体。
13.根据权利要求12所述的固化的、适型的多孔复合材料,其中所述支撑体包括泡沫、片材、薄膜、网状物、膜、织造或非织造垫、丝网或它们的组合。
14.根据权利要求1所述的固化的、适型的多孔复合材料,其中所述固化的、适型的多孔复合材料包括具有平坦主表面、图案化主表面或其组合的片材。
15.根据权利要求14所述的固化的、适型的多孔复合材料,其中所述片材具有至少一个图案化的主表面,具有厚度为约0.3mm至约0.6mm或约0.4mm至约0.5mm的区域,以及具有厚度为约0.5mm至约5mm或约1mm至约3mm的区域。
16.一种能量储存装置,其包括固化的、适型的多孔复合材料,所述多孔复合材料具有互连的孔并且包含热膨胀的聚合物微球和颗粒填充材料。
17.根据权利要求16所述的能量存储装置,其中所述固化的、适型的多孔复合材料构成隔膜的至少一部分或阻火器的至少一部分。
18.一种制备固化的、适型的多孔复合材料的方法,其中在孔的形成中没有溶剂被引入复合材料或从复合材料中被提出,所述方法包括:
将可膨胀聚合物微球和颗粒填充材料的混合物置于限定的体积空间中;和
在所述限定的体积空间中加热混合物以充分膨胀聚合物微球,从而在限定的体积空间内将热膨胀的聚合物微球与颗粒填充材料结合,并形成具有互连的孔的固化的、适型的多孔复合材料。
19.根据权利要求18所述的方法,其还包括缓慢冷却所述热膨胀的微球。
20.根据权利要求18所述的方法,其还包括在所述限定的体积空间中加热所述混合物之前,将支撑体放置在所述限定的体积空间中。
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