CN111416101A - 柔性电极纤维膜、柔性电极片及其制造方法与应用 - Google Patents
柔性电极纤维膜、柔性电极片及其制造方法与应用 Download PDFInfo
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- CN111416101A CN111416101A CN202010219429.5A CN202010219429A CN111416101A CN 111416101 A CN111416101 A CN 111416101A CN 202010219429 A CN202010219429 A CN 202010219429A CN 111416101 A CN111416101 A CN 111416101A
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- flexible electrode
- fiber
- carbon
- flexible
- electrode sheet
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Abstract
本发明提供了柔性电极纤维膜、柔性电极片及其制造方法与应用,该方法包括:向含有热塑性粘结剂的混合物料中添加易挥发性溶剂,搅拌以形成糊状物;将糊状物在高剪切作用下进行纤维化处理,然后喷射成丝;将喷射所得的丝条牵伸,然后铺展为纤维网;将纤维网碾压成型,得到柔性电极纤维膜。柔性电极纤维膜中的活性物质、导电剂和热塑性粘结剂之间为三维网络体系,代替传统技术中的点接触体系。在增强整个柔性电极纤维膜导电性的同时,赋予柔性电极纤维膜强力的物理强度和较大的弹性模量。
Description
技术领域
本发明属于与储能装置相关技术,具体涉及柔性电极纤维膜、柔性电极片及其制造方法与应用。
背景技术
当前,锂离子二次电池、超级电容器、锂空气电池等已经成为诸多卡片式或可穿戴式智能设备的储能装置,其经常遇到的使用场景是需要放到钱包里或者口袋中随身携带。由于储能装置较为笨重却又十分重要,在组装时并不能很好地进行调整,产品开发者在设计一个新的智能设备时,总是会被储能装置的尺寸、形状和灵活性所限制。因此大多数智能设备的形状都取决于其储能装置的形状。
一般的,储能装置的电极片的制备方法主要是将活性物质、导电剂、粘结剂以及可以溶解该粘结剂的溶剂混合成浆料后涂覆在铝箔或铜箔集流体上,所使用的粘结剂主要为聚偏氟乙烯(PVDF)、丁苯橡胶乳液、聚丙烯腈、聚丙烯酸酯、聚苯乙烯丙烯酸酯等,所使用的溶剂主要为N-甲基吡咯烷酮、乙醇、丙酮、去离子水等。
通过以上方法制备得到用于储能装置的电极片,活性物质、导电剂、粘结剂之间为点接触。当该电极片受到一定的弯曲或扭曲时,电极片中的活性物质、导电剂、粘结剂容易从集流体上脱落,造成储能装置的容量急剧衰减。
发明内容
本发明提出一种新的柔性电极纤维膜、柔性电极片及其制造方法与应用,通过该方法,可以制造物理强度和弹性模量大的柔性电极纤维膜,该柔性电极纤维膜包括活性物质、导电剂、热塑性粘结剂,活性物质、导电剂、热塑性粘结剂之间为三维网络体系。
第一方面,本发明提供了一种柔性电极纤维膜的制造方法,包括:
步骤一:向含有热塑性粘结剂的混合物料中添加易挥发性溶剂,搅拌以形成糊状物;
步骤二:将所述糊状物在高剪切作用下进行纤维化处理,然后喷射成丝;
步骤三:将喷射所得的丝条牵伸,然后铺展为纤维网;
步骤四:将所述纤维网碾压成型,得到柔性电极纤维膜。。
在此基础上,所述糊状物的形成在高速混合机中进行,搅拌速度为10000-20000rpm,搅拌时间为30-60min。
在此基础上,通过螺杆挤出机的高剪切作用,将所述糊状物进行纤维化处理,以使所述热塑性粘结剂发生纤维化。在此基础上,采用狭缝式牵伸装置进行喷射成丝的操作;所述狭缝式牵伸装置的喷射成丝模头的孔径直径优选为1μm-100μm,更优选为5μm-50μm。
相应地,所述丝条直径优选为1μm-100μm,更优选为5μm-50μm
丝条直径如过小容易发生喷丝孔堵塞、断丝等问题,但丝条直径也不宜过大,否则容易造成丝条取向性、外观不良,且容易因单位长度的质量过重而造成牵伸过程中的丝条变形、断丝等问题。
在一些实施方式中,所述狭缝式牵伸装置的喷射成丝模头的孔径直径优选为5μm-30μm,例如:5μm、10μm、15μm、20μm、25μm、30μm,等等。
在此基础上,向含有热塑性粘结剂的混合物料中添加易挥发性溶剂,以使形成的糊状物的固含量为30%-80%,优选30%-50%,例如:30%、31%、33%、35%、40%、45%、50%,等等。
一些实施例中,所述易挥发性溶剂包括如下的至少一种:甲醇、乙醇、丙醇等烷基醇类,丙酮、甲乙酮等烷基酮类,四氢吠喃、二甘醇二甲醚等醚类,二乙基甲酞胺、二甲基乙酞胺、N-甲基吡咯烷酮等酞胺类溶剂;其中,优选异丙醇或四氢呋喃。
在此基础上,所述混合物料中包括混合均匀的活性物质、导电剂和热塑性粘结剂。
混合均匀的程度决定了热塑性粘结剂经螺杆挤出机中的强力剪切力而达到的纤维化程度。
一些实施例中,所述活性物质包括如下的至少一种:磷酸铁锂、锰酸锂、钴酸锂、镍酸锂、镍钴锰酸锂、磷酸锰锂、镍钴铝酸锂、钛酸锂、石墨、膨胀石墨、石墨烯、氧化石墨烯、碳纳米管、碳纳米纤维、中间相碳微球、硬碳、活性炭、富勒烯、硅碳材料。
在一个优选实施例中,正电极片的柔性电极纤维膜包括磷酸铁锂或镍钴锰酸锂,负电极片中的柔性电极纤维膜包括石墨烯或碳纳米管。
一些实施例中,所述导电剂包括如下的至少一种:金属粉末、乙炔黑、科琴黑、炉黑、导电炭黑、导电石墨、碳纳米管、碳纤维、石墨烯;更优选为乙炔黑、科琴黑或导电炭黑。
一些实施例中,所述热塑性粘结剂包括如下的至少一种:聚四氟乙烯、聚偏氟乙烯、聚丙烯、聚氯乙烯、聚苯乙烯、聚甲醛,聚碳酸酯,聚酰胺、丙烯酸类塑料、其它聚烯烃及其共聚物、聚砜、聚苯醚、羧甲基纤维素;更优选为聚四氟乙烯或聚氯乙烯。
在此基础上,所述活性物质、导电剂、热塑性粘结剂的质量比为1:0.01-0.2:0.05-0.5,优选为1:0.01-0.1:0.05-0.2,例如:1:0.01:0.05-0.2、1:0.02:0.05-0.2、1:0.03:0.05-0.2、1:0.04:0.05-0.2、1:0.05:0.05-0.2、1:0.06:0.05-0.2、1:0.07:0.05-0.2、1:0.08:0.05-0.2、1:0.09:0.05-0.2、1:0.1:0.05-0.2、1:0.01-0.1:0.05、1:0.01-0.1:0.06、1:0.01-0.1:0.07、1:0.01-0.1:0.08、1:0.01-0.1:0.09、1:0.01-0.1:0.1、1:0.01-0.1:0.11、1:0.01-0.1:0.12、1:0.01-0.1:0.13、1:0.01-0.1:0.14、1:0.01-0.1:0.15、1:0.01-0.1:0.16、1:0.01-0.1:0.17、1:0.01-0.1:0.18、1:0.01-0.1:0.19、1:0.01-0.1:0.2,等等。
在一些实施方式中,所述活性物质、导电剂、热塑性粘结剂的质量比为1:0.02:0.09。
在一些实施方式中,所述活性物质、导电剂、热塑性粘结剂的质量比为1:0.06:0.19。
第二方面,本发明提供一种通过第一方面所述法方法制造的柔性电极纤维膜。
在此基础上,所述柔性电极纤维膜的厚度为30-150μm,优选为70-120μm,例如:70μm、75μm、80μm、85μm、90μm、95μm、100μm、105μm、110μm、115μm、120μm,等等。
第三方面,本发明提供一种包括第二方面所述柔性电极纤维膜的柔性电极片。
在此基础上,所述柔性电极片包括柔性电极纤维膜以及涂覆有导电胶的柔性集流体。
在此基础上,所述柔性集流体包括如下的至少一种:石墨纸、碳纤维纸、碳纳米管纸、碳布、聚酯纤维、聚酰胺纤维、聚丙烯腈纤维、聚烯烃纤维、聚乙烯醇纤维、聚氨酯纤维、黏胶纤维、铜氨纤维、醋酸纤维、棉、麻、羊毛、丝;其中,优选碳纤维纸或碳纳米管纸。
在此基础上,所述柔性电极片是将所述柔性电极纤维膜与涂覆有导电胶的柔性集流体进行热复合而成;所述热复合的温度优选为25℃-300℃,更优选为100℃-180℃,例如:100℃、110℃、120℃、130℃、140℃、150℃、160℃、170℃、180℃,等等。
第四方面,本发明提供了第二方面所述柔性电极纤维膜或者第三方面所述的柔性电极片在制备储能装置中的应用。
第五方面,本发明提供了一种储能装置,包括正电极片和负电极片,所述正电极片和/或所述负电极片为第三方面所述的柔性电极片。
通过以上技术方案,与现有技术相比,本发明至少可以获得以下的技术效果:
传统的储能装置的电极片的制备方法主要是将活性物质、导电剂、粘结剂以及可以溶解该粘结剂的溶剂混合成浆料后涂覆在铝箔或铜箔集流体上,所使用的粘结剂主要为聚偏氟乙烯(PVDF)、丁苯橡胶乳液、聚丙烯腈、聚丙烯酸酯、聚苯乙烯丙烯酸酯等,所使用的溶剂主要为N-甲基吡咯烷酮、乙醇、丙酮、去离子水等。通过以上方法制备得到用于储能装置的电极片,活性物质、导电剂、粘结剂之间为点接触。当该电极片受到一定的弯曲或扭曲时,电极片中的活性物质、导电剂、粘结剂容易从集流体上脱落,造成储能装置的容量急剧衰减。
本发明利用高剪切作用使热塑性粘结剂发生纤维化,并使柔性电极纤维膜中的活性物质、导电剂、粘结剂之间形成强力的三维网络体系,以三维网络体系代替传统的点接触,在增强整个柔性电极纤维膜导电性、均匀性的同时,赋予柔性电极纤维膜强力的物理强度和较大的弹性模量。在此基础上,本发明还利用热复合机将柔性电极纤维膜与涂覆有导电胶的柔性集流体进行复合以获得柔性电极片,使得柔性电极纤维膜与柔性集流体之间的接触也是三维网络体系,进而使得柔性电极纤维膜不易从柔性集流体上脱落。同时,通过分切机可将柔性电极片切成任意形状,以满足不同形状储能装置的需求。通过这样的方式,柔性电极片可以制成任意形状,也可以进行任意角度的弯曲而不发生不可逆损害。
附图说明
图1为本发明实施例1提供的负极片的弯曲测试;
图2为本发明实施例2提供的正极片的弯曲测试。
具体实施方式
实施例中未注明具体技术或条件的,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。
下面结合具体实施例,对本发明的原理进行描述。需要说明的是,此处描述的具体实施例仅为了阐述和解释本发明的原理,从任何角度都不能被看作是对本发明保护的限制,本发明的保护范围由权利要求来具体限定,而不限于此处所描述的任何具体特征。
实施例1
通过如下流程,制作负电极片:
将石墨烯、乙炔黑、聚四氟乙烯粉末,按照90:2:8的质量比在高速混合机中经依次混合均匀。向以上混合均匀的物料中加入质量比为200%的异丙醇,设置高速混合机搅拌速度为10000rpm,时间为60min,以获得糊状物。将上述糊状物转移至螺杆挤出机,螺杆速度为100rpm,加热温度为60℃;物料经过螺杆挤出机的旋转推进装置到达狭缝式牵伸装置的喷射成丝模头,喷射成丝模头的孔径为10μm,物料从喷丝孔中喷出形成填充了纤维化热塑性粘结剂的丝条,再将丝条通过狭缝式牵伸装置的气流冷却牵伸后,达到传送帘带上铺展为纤维网,将纤维网送入收料辊筒进行轻度热压成型,辊筒的辊面温度设置为150℃,辊速为0.5m/min,牵引比为1:1,控制热压后纤维膜厚度为75μm,最终得到柔性电极纤维膜。利用instron万能材料试验机测试得到,柔性电极纤维膜的张力强度为2.71N/cm,拉伸应变为15.79%。
利用热复合机在180℃下将75μm柔性电极纤维膜与涂覆有导电胶(Achenson DAGEB-012)的柔性碳纳米管纸进行复合;利用分切机将复合好的柔性电极片切成57×84mm的长方形,得到负电极片。
将得到的负电极片进行弯曲测试,如图1所示,可以进行大角度的弯曲而不发生不可逆损害。
实施例2
通过如下流程,制作正电极片:
将磷酸铁锂、乙炔黑、科琴黑、聚四氟乙烯粉末,按照80:4:1:15的质量比在高速混合机中经依次混合均匀。向以上混合均匀的物料中加入质量比为220%的N-甲基吡咯烷酮,设置高速混合机搅拌速度为15000rpm,时间为45min,以获得糊状物。将上述糊状物转移至螺杆挤出机,螺杆速度为50rpm,加热温度为80℃;物料经过螺杆挤出机的旋转推进装置到达狭缝式牵伸装置的喷射成丝模头,喷射成丝模头的孔径为25μm,物料从喷丝孔中喷出形成填充了纤维化热塑性粘结剂的丝条,再将丝条通过狭缝式牵伸装置的气流冷却牵伸后,达到传送帘带上铺展为纤维网,将纤维网送入收料辊筒进行轻度热压成型,辊筒的辊面温度设置为150℃,辊速为0.5m/min,牵引比为1:1,控制热压后纤维膜厚度为100μm,最终得到柔性电极纤维膜。利用instron万能材料试验机测试得到,柔性电极纤维膜的张力强度为4.13N/cm,拉伸应变为8.11%。
利用热复合机在150℃下将100μm柔性电极纤维膜与涂覆有导电胶(Achenson DAGEB-012)的柔性碳纤维纸进行复合;利用分切机可将复合好的柔性电极片切成35×240mm的长方,得到正电极片。
将得到的正电极片进行弯曲测试,如图2所示,可以进行大角度的弯曲而不发生不可逆损害。
本发明利用高剪切作用使热塑性粘结剂发生纤维化,并使柔性电极纤维膜中的活性物质、导电剂、热塑性粘结剂之间形成强力的三维网络体系,以三维网络体系代替传统的点接触,在增强整个柔性电极纤维膜导电性、均匀性的同时,赋予柔性电极纤维膜强力的物理强度和较大的弹性模量。在此基础上,本发明还利用热复合机将柔性电极纤维膜与涂覆有导电胶的柔性集流体进行复合以获得柔性电极片,使得柔性电极纤维膜与柔性集流体之间的接触也是三维网络体系,使得柔性电极纤维膜不易从柔性集流体上脱落。同时,通过分切机可将柔性电极片切成任意形状,以满足不同形状储能装置的需求。通过这样的方式,柔性电极片可以制成任意形状,也可以进行任意角度的弯曲而不发生不可逆损害。另外需要说明的是,在上述具体实施方式中所描述的各个具体技术特征,在不矛盾的情况下,可以通过任何合适的方式进行组合,为了避免不必要的重复,本发明对各种可能的组合方式不再另行说明。
此外,本发明的各种不同的实施方式之间也可以进行任意组合,只要其不违背本发明的思想,其同样应当视为本发明所公开的内容。
Claims (14)
1.一种柔性电极纤维膜的制造方法,其特征在于,包括:
步骤一:向含有热塑性粘结剂的混合物料中添加易挥发性溶剂,搅拌以形成糊状物;
步骤二:将所述糊状物在高剪切作用下进行纤维化处理,然后喷射成丝;
步骤三:将喷射所得的丝条牵伸,然后铺展为纤维网;
步骤四:将所述纤维网碾压成型,得到柔性电极纤维膜。
2.根据权利要求1所述的制造方法,其特征在于,所述步骤二中,通过螺杆挤出机的高剪切作用,将所述糊状物进行纤维化处理,以使所述热塑性粘结剂发生纤维化。
3.根据权利要求1所述的制造方法,其特征在于,所述步骤二中,采用狭缝式牵伸装置进行喷射成丝的操作;所述狭缝式牵伸装置的喷射成丝模头的孔径直径优选为1μm-100μm,更优选为5μm-50μm。
4.根据权利要求1-3任意一项所述的制造方法,其特在于,所述步骤一中,向含有热塑性粘结剂的混合物料中添加易挥发性溶剂,以使形成的糊状物的固含量为30%-80%;
优选地,所述易挥发性溶剂包括如下的至少一种:甲醇、乙醇、丙醇等烷基醇类,丙酮、甲乙酮等烷基酮类,四氢吠喃、二甘醇二甲醚等醚类,二乙基甲酞胺、二甲基乙酞胺、N-甲基吡咯烷酮等酞胺类溶剂;其中,优选异丙醇或四氢呋喃。
5.根据权利要求1-3任意一项所述的制造方法,其特征在于,所述步骤一中,所述混合物料中包括混合均匀的活性物质、导电剂和热塑性粘结剂;优选地,
所述活性物质包括如下的至少一种:磷酸铁锂、锰酸锂、钴酸锂、镍酸锂、镍钴锰酸锂、磷酸锰锂、镍钴铝酸锂、钛酸锂、石墨、膨胀石墨、石墨烯、氧化石墨烯、碳纳米管、碳纳米纤维、中间相碳微球、硬碳、活性炭、富勒烯、硅碳材料;
所述导电剂包括如下的至少一种:金属粉末、乙炔黑、科琴黑、炉黑、导电炭黑、导电石墨、碳纳米管、碳纤维、石墨烯;更优选为乙炔黑、科琴黑或导电炭黑;
所述热塑性粘结剂包括如下的至少一种:聚四氟乙烯、聚偏氟乙烯、聚丙烯、聚氯乙烯、聚苯乙烯、聚甲醛,聚碳酸酯,聚酰胺、丙烯酸类塑料、其它聚烯烃及其共聚物、聚砜、聚苯醚、羧甲基纤维素;更优选为聚四氟乙烯或聚氯乙烯。
6.根据权利要求5所述的制造方法,其特征在于,所述活性物质、导电剂、热塑性粘结剂的质量比为1:0.01-0.2:0.05-0.5,优选为1:0.01-0.1:0.05-0.2。
7.权利要求1-6任意一项所述制造方法获得的柔性电极纤维膜。
8.根据权利要求7所述的柔性电极纤维膜,其特征在于,所述柔性电极纤维膜的厚度为30-150μm,优选为70-120μm。
9.包含权利要求7或8所述柔性电极纤维膜的柔性电极片。
10.根据权利要求9所述的柔性电极片,其特征在于,包括:所述柔性电极纤维膜以及涂覆有导电胶的柔性集流体。
11.根据权要求10所述的柔性电极片,其特征在于:所述柔性集流体包括如下的至少一种:石墨纸、碳纤维纸、碳纳米管纸、碳布、聚酯纤维、聚酰胺纤维、聚丙烯腈纤维、聚烯烃纤维、聚乙烯醇纤维、聚氨酯纤维、黏胶纤维、铜氨纤维、醋酸纤维、棉、麻、羊毛、丝;其中,优选碳纤维纸或碳纳米管纸。
12.根据权利要求9或10所述的柔性电极片,其特征在于,是将所述柔性电极纤维膜与涂覆有导电胶的柔性集流体进行热复合而成;所述热复合的温度优选为25℃-300℃,更优选为100℃-180℃。
13.权利要求7或8所述柔性电极纤维膜或权利要求10-13任意一项所述柔性电极片在制备储能装置中的应用。
14.一种储能装置,其特征在于,包括正电极片和负电极片,所述正电极片和/或所述负电极片为权利要求9-12任意一项所述的柔性电极片。
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