CN117296193A - 包含含氟聚合物的电池绝缘组件零件 - Google Patents
包含含氟聚合物的电池绝缘组件零件 Download PDFInfo
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- CN117296193A CN117296193A CN202280033894.7A CN202280033894A CN117296193A CN 117296193 A CN117296193 A CN 117296193A CN 202280033894 A CN202280033894 A CN 202280033894A CN 117296193 A CN117296193 A CN 117296193A
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- 229920002313 fluoropolymer Polymers 0.000 title claims abstract description 32
- 239000004811 fluoropolymer Substances 0.000 title claims abstract description 32
- 238000009413 insulation Methods 0.000 title claims description 25
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 37
- BLTXWCKMNMYXEA-UHFFFAOYSA-N 1,1,2-trifluoro-2-(trifluoromethoxy)ethene Chemical compound FC(F)=C(F)OC(F)(F)F BLTXWCKMNMYXEA-UHFFFAOYSA-N 0.000 claims abstract description 22
- KHXKESCWFMPTFT-UHFFFAOYSA-N 1,1,1,2,2,3,3-heptafluoro-3-(1,2,2-trifluoroethenoxy)propane Chemical compound FC(F)=C(F)OC(F)(F)C(F)(F)C(F)(F)F KHXKESCWFMPTFT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000155 melt Substances 0.000 claims abstract description 7
- 238000001746 injection moulding Methods 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 19
- BZPCMSSQHRAJCC-UHFFFAOYSA-N 1,2,3,3,4,4,5,5,5-nonafluoro-1-(1,2,3,3,4,4,5,5,5-nonafluoropent-1-enoxy)pent-1-ene Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)=C(F)OC(F)=C(F)C(F)(F)C(F)(F)C(F)(F)F BZPCMSSQHRAJCC-UHFFFAOYSA-N 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 14
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- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 description 38
- 238000012360 testing method Methods 0.000 description 17
- 230000004580 weight loss Effects 0.000 description 12
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
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- 125000004122 cyclic group Chemical group 0.000 description 3
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- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
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- -1 perfluoroalkyl vinyl ether Chemical compound 0.000 description 2
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- HFNSTEOEZJBXIF-UHFFFAOYSA-N 2,2,4,5-tetrafluoro-1,3-dioxole Chemical compound FC1=C(F)OC(F)(F)O1 HFNSTEOEZJBXIF-UHFFFAOYSA-N 0.000 description 1
- YSYRISKCBOPJRG-UHFFFAOYSA-N 4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxole Chemical compound FC1=C(F)OC(C(F)(F)F)(C(F)(F)F)O1 YSYRISKCBOPJRG-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
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- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
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- 230000007774 longterm Effects 0.000 description 1
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- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
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- 229910052618 mica group Inorganic materials 0.000 description 1
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- 239000008188 pellet Substances 0.000 description 1
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Abstract
本发明涉及一种用于电化学电池单元的绝缘组件零件,其包含一种或多种含氟聚合物,所述含氟聚合物包含‑按摩尔计87%‑99%的衍生自四氟乙烯(TFE)的重复单元‑按摩尔计1%‑13%的衍生自全氟甲基乙烯基醚(PMVE)的重复单元‑按摩尔计0%‑3%的衍生自全氟丙基乙烯基醚(PPVE)的重复单元并且具有从40至300g/10min的熔体流动速率(MFR)(在372℃下在5kg载荷下测量)。
Description
技术领域
本申请要求于2021年5月12日提交的欧洲专利申请号21173659.0的优先权,出于所有目的将该申请的全部内容通过引用并入本文。
本发明涉及用于构造电化学电池单元、特别地用于二次电池的绝缘组件零件,其包含四氟乙烯(TFE)和全氟烷基乙烯基醚(PAVE)的某些选定的共聚物;涉及一种通过注射模制制造此类绝缘组件零件的方法;并且涉及包括此类绝缘组件零件的电化学电池单元。
背景技术
如技术人员已知的,电池含有一个或多个能够将化学能转化为电能的单独的电化学电池单元。一些电池只能使用一次,而另一些电池可以通过将电能转化为化学能来充电,然后当使用电池时,化学能再一次被释放为电能。这些被称为“可充电电池”或“二次电池”。特别地,由于目前对于电动发动机的兴趣,可充电电池在工业中受到越来越多的关注。
每个电化学电池单元典型地包括直接参与能量转换过程的多个“活性”元件:正极、负极、多孔隔膜和典型地为液体但还呈凝胶或固体形式的电解质。商业的电池典型地将一个或多个电化学电池单元封装在容器内。
除了提及的活性部件,电化学电池单元还含有其他组件零件,这些组件零件本身不具有活性,但是对于确保电池单元的适当构造和性能是必需的且非常重要。事实上,每个电池单元必须通过电池单元外壳与其他电池单元电隔离,并且正极端子和负极端子还必须在电池单元外壳外可获得,以允许电池单元的连接。在典型的单元构造(如圆柱形单元或棱柱形电池单元)中,这通过使用电池单元盖来实现,电池单元盖典型地包括安全排气口以避免在内部形成气体的情况下电池单元鼓起(bulging)。密封和绝缘垫片典型地存在于盖或闭合件周围以密封电池单元以防止电解质泄漏和水分进入,与电池单元的活性部件接触的垫片也必须由电绝缘材料制成。此外,绝缘板典型地存在于电极的两侧,以防止不希望的短路,当然绝缘板也必须由电绝缘材料制成。其他绝缘组件零件,如电极固持器(也称为集流体固持器),典型地存在于本领域技术人员已知的许多电化学电池单元构造中。构造可以变化,并且在一些情况下,相同的零件可以执行多于一种功能,并且在其他情况下,更多的单独零件可以用于执行单一功能。所有这些绝缘组件零件具有以下共同之处:都是电绝缘体、相对于存在于电化学电池单元中的化学物质基本上是惰性的以及不直接参与使电池单元工作以积累和/或释放能量的电化学反应。
所有这些组件零件对于电池单元的寿命和安全都是至关重要的,因为即使一个单一零件的故障都可能导致泄露或短路。特别地,由绝缘材料制成的组件零件与电极和/或与存在于电解质材料中的溶剂直接接触,并且在电池寿命期间暴露于连续的温度变化。因此,这些绝缘组件零件必须使用这样的材料来制造:其不仅是电绝缘的,而且能够承受高温、温度变化、以及与溶剂和腐蚀性化学品接触。绝缘组件零件还必须是足够韧性的,以确保即使长时间重复施加压力或机械应力也能密封和分离。
因此,高性能塑料材料对于电化学电池单元中(特别是在二次电池单元中)的大多数绝缘组件零件典型地是优选的,其甚至在恶劣环境下也必须确保长的使用寿命。
在这些绝缘组件零件中,在电化学电池单元构造中特别重要的一个零件是所谓的“垫片”或“密封垫片”。
垫片是典型地放置在电池盖周围以防止电解质泄露和空气中的水分渗入电池的密封件。密封垫片还提供电绝缘作用以防止正极和负极产生接触并且导致短路。为了确保电池的安全和寿命,必须保证密封垫片的密封和绝缘功能(例如对于汽车的使用)连续使用15年或更久。密封垫片材料必须具有恢复力以在不利的条件(如高温和长期应力,这可能导致蠕变变形)下维持密封的有效性,并且必须在电池的整个寿命内维持这些特性。
另一个重要的绝缘组件零件是所谓的“绝缘板”,其是用于防止两个导体之间短路的塑料片。例如,在圆柱形电池单元中典型地有两个绝缘板。第一个板位于极芯(jellyroll)的底部与罐(can)的底部之间。第二个板位于极芯的顶部与密封垫片之间。如技术人员已知的,绝缘板通常包括在具有相同功能的许多不同的电池单元构造中。
电极固持器典型地用于将电极板维持在正确的位置,并且用于防止短路。如上所述,用于电化学电池单元的绝缘组件零件必须被赋予出色的机械和化学特性,并且长期维持这些特性。因此,含氟聚合物并且特别是全氟化聚合物已经用于形成此类绝缘组件零件。
基于聚四氟乙烯的热塑性材料满足用于形成电池绝缘组件零件的所有要求。现有技术中充分公开了使用TFE和PAVE的共聚物(特别地使用商业上称为PFA的TFE/全氟丙基乙烯基醚(PPVE)共聚物)以形成此类绝缘组件零件。
例如Daikin的WO 13115374描述了一种用于电池的绝缘组件零件的密封材料,其是基于在372℃下具有约4g/10min的MFR的TFE/PPVE共聚物。
用于电化学电池单元的绝缘组件零件可以使用熔融加工技术(如压缩模制和注射模制)由含氟聚合物来制造。注射模制是特别优选的,因为其允许使用多腔模具,从而允许用单个注射过程制备几个绝缘组件零件。
如模制领域的技术人员已知的,用于注射模制的热塑性材料优选地在相对低的温度下是可加工的,因为设备和模具的腐蚀以及能量消耗都较低。此外,用于注射模制的优选的材料在加工温度下具有低粘度,使得具有更多腔的模具可以被无差错地填充,并且还应该在模具中在高速下是可注射的,而不在最终的物品上形成表面缺陷。
另一方面,尽管已知TFE/PPVE共聚物(如在引用的现有技术中使用的那些)的粘度和熔点可以通过增加PPVE的含量来降低,还已知此类具有高PPVE含量的共聚物不适合用于预期的应用,因为低粘度伴随着机械特性的降低和热稳定性的降低。
热稳定性也与含氟聚合物的注射模制非常相关,不仅因为聚合物本身的稳定性,而且因为重量损失典型地涉及多种化合物的损失,这些化合物包括呈气体形式的氢氟酸(HF),这是用于注射模制的昂贵设备的腐蚀的主要成因,因此在加热时损失重量的材料还将导致较高的腐蚀,并且因此缩短模具的寿命。此外,重量损失可能与气体逸出有关,气体逸出可能导致模制制品中缺陷(如气泡)的形成。
因此,还需要从含氟聚合物组合物获得的用于电化学电池单元的绝缘组件零件,该含氟聚合物组合物满足已知的含氟聚合物的机械稳定性、耐化学品性、绝缘能力、密封能力等的所有要求,但是其可以在较低的温度下注射模制并且在模制期间也是更热稳定的。
发明内容
在一个方面,本发明涉及一种用于电化学电池单元的绝缘组件零件,其包含一种或多种含氟聚合物,所述含氟聚合物包含
-按摩尔计87%-99%的衍生自四氟乙烯(TFE)的重复单元
-按摩尔计1%-13%的衍生自全氟甲基乙烯基醚(PMVE)的重复单元
-按摩尔计0%-3%的衍生自全氟丙基乙烯基醚(PPVE)的重复单元
并且具有从40至300g/10min的熔体流动速率(MFR)(在372℃下在5kg载荷下测量)。
在另一方面,本发明涉及一种制造用于电化学电池单元的绝缘组件零件的方法,所述方法包括通过注射模制热塑性聚合物组合物形成所述绝缘组件零件,所述组合物包含一种或多种如上定义的含氟聚合物。
在另一方面,本发明涉及一种包括此类绝缘组件零件(优选为密封垫片、绝缘板或电极固持器)的二次电池。
具体实施方式
出于本说明书的目的,涉及电化学电池单元的术语“绝缘组件零件”指示不参加电化学反应(即电极、电解质和隔膜)并且不导电(即不包括连接器、缆线等)的电化学电池单元的所有固体部件。这些是例如密封垫片、绝缘体、密封件、电极固持器(也称为集流体固持器)、绝缘壳、绝缘屏障物等。电化学电池单元典型地是电池的单元、优选二次电池单元并且更优选锂电池单元。绝缘组件零件优选地是密封垫片、绝缘板和/或电极固持器。
所有按摩尔计百分比或重复单元是指聚合物中存在的重复单元的总量。
如上所述,本发明涉及用于电化学电池单元的绝缘组件零件,典型地电池单元,此种组件零件包含一种或多种选定的TFE/PAVE含氟聚合物。
选择用于本发明的选择的TFE/PAVE含氟聚合物包含按摩尔计1%-13%、优选1%-10%、更优选2%-8%、甚至更优选3%-7%的衍生自全氟甲基乙烯基醚(PMVE)的重复单元。
选择用于本发明的选择的TFE/PAVE含氟聚合物还可以包含按摩尔计0%-3%、优选0%-2.5%、更优选0%-2%、甚至更优选0.1%-1.5%的衍生自全氟丙基乙烯基醚(PPVE)的重复单元。
通常优选的是,衍生自PPVE的重复单元(如果存在)的摩尔量小于衍生自PMVE的重复单元的摩尔量,即衍生自PPVE的重复单元与衍生自PMVE的重复单元之间的摩尔比(PPVE/PMVE)小于1、优选小于0.5、更优选小于0.3、最优选小于0.2。
任选地,用于本发明的TFE/PAVE共聚物可以包含高达6%的衍生自环状单体的重复单元,该环状单体选自具有式(20A)的全氟(2,2-二甲基-1,3-二氧杂环戊烯)、具有式(21A)的全氟(1,3-二氧杂环戊烯)、以及具有式(26A)的2,2,4-三氟-5-三氟甲氧基-1,3-二氧杂环戊烯:
当存在时,此类环状单体为优选按摩尔计从0.1%至5%、更优选按摩尔计从0.1%至4%、甚至更优选按摩尔计从0.1%至3%。
选择用于本发明的选择的TFE/PAVE含氟聚合物包含以按摩尔计从87%至99%的量的衍生自TFE的重复单元。除了衍生自TFE、PAVE和如上所述的环状单体的重复单元之外的其他重复单元优选不存在,但是,如果存在,优选是完全氟化的并且优选基于含氟聚合物的重复单元的总量按摩尔计低于2%。
可以存在端链、杂质、缺陷和少量其他共聚单体(相对于聚合物的重复单元的总摩尔量,这些共聚单体的量总体上不超过0.5%、优选不超过0.1%),而这些没有显著影响所述TFE/PAVE共聚物的特性。
选择用于本发明的TFE/PAVE含氟聚合物进一步特征在于具有从40至300、优选从50至200、更优选从60至160、甚至更优选从70至130g/10min的熔体流动速率(MFR)(在372℃下在5kg载荷下测量)。
选择用于本发明的TFE/PAVE含氟聚合物优选进一步特征在于根据ASTM D3418确定的包括在从260℃至310℃、优选从270℃至305℃、更优选从275℃至300℃的熔点Tm。
本发明的绝缘组件零件优选由组合物制成,该组合物优选为热塑性聚合物组合物,其中如上所述的选定的TFE/PAVE含氟聚合物构成所述绝缘组件零件的按重量计至少80%、优选至少90%、更优选至少95%、最优选至少99%。
可以被添加至用于制造本发明的组件零件的组合物中的额外的任选的成分是常规的添加剂,如稳定添加剂、脱模剂、增塑剂、润滑剂、热稳定剂、光稳定剂、抗氧化剂、粘合促进剂、填料、颜料和优选以组合物的按重量计小于10%的量存在的其他添加剂。
如果存在,填料可以选自例如矿物填料,如滑石、云母、高岭土、碳酸钙、硅酸钙、碳酸镁、石墨、炭黑。
本申请人已经出人意料地发现,当制造包含如上所述的选定的TFE/PAVE含氟聚合物的绝缘组件零件时,与使用现有技术的TFE/PPVE含氟聚合物相比,可以在更低的温度和更快的注射速度通过注射模制进行制造,这允许使用多腔模具,这是制造此类绝缘组件零件特别有效的方式。本发明的选定的TFE/PAVE聚合物的使用还与模制期间减少的重量损失和因此减少的脱气物质(包括HF)的逸出有关,这导致模具的使用寿命更长,并且模制制品中的缺陷减少。与根据现有技术使用TFE/PPVE聚合物获得的相似的组件零件相比,本发明的绝缘组件零件具有相当的机械特性、耐化学性和随时间推移的稳定性。参考下面的实验部分以获得支持由本发明提供的益处的实验数据。
制造制品的方法
本发明还涉及制造用于电化学电池单元的绝缘组件零件的方法。该方法包括通过注射模制热塑性聚合物组合物形成用于电化学电池单元的绝缘组件零件,所述组合物包含一种或多种如上所述的选定的TFE/PAVE含氟聚合物。
在本发明的方法中,模具优选地是多腔模具、更优选具有至少4个腔的多腔模具,其中每个腔允许模制单独的绝缘组件零件。组合物的低粘度允许在温和的温度和压力条件下有效地快速填充多个腔,从而产生具有光滑的表面并且无缺陷的单独的模制制品。
可替代地,但是不太优选地,本发明的绝缘组件零件可以通过压缩模制或其他不同于注射模制的熔融加工技术来制造。
注射模制的步骤通常使用冲头或螺杆式柱塞以迫使熔融热塑性组合物进入到模具腔内;在所述模具的腔内,组合物固化成与模具的轮廓相符的形状,该模具可以是单腔模具或多腔模具。
如上所述注射模制工艺优选使用包含按重量计至少80%、优选至少90%、更优选至少95%、最优选至少99%的如上所述的选择的TFE/PAVE含氟聚合物中的一种或多种的热塑性组合物进行。
本文所述的注射模制工艺特别适合用于制造绝缘组件零件,如密封垫片和绝缘板集流体固持器等。本发明的绝缘组件零件的典型的形状可以根据电化学电池单元的几何形状变化。示例性形状例如是具有0.2-1mm的厚度的扁平的零件(矩形或盘状)、盘、板、o型环、棒等。
如果通过引用并入本文的任何专利、专利申请以及公开物的披露内容与本申请的描述相冲突到了可能导致术语不清楚的程度,则本说明应该优先。
现在将参照以下实例更详细地描述本发明,这些实例的目的仅是说明性的并且不旨在限制本发明的范围。
实验部分
试验方法
MFR:(熔体流动速率)根据ASTM 1238在372℃下在5kg的活塞载荷下测量,并且表示为g/10min。
TGA:重量损失测试根据ISO 11358使用TA公司的TGA5500仪器进行。
熔点的测定
熔点Tm是根据ASTM D 3418标准通过DSC作为第二熔融温度测量的。程序如下:以10℃/min的温度斜升将聚合物样品从10℃加热至400℃熔融。然后将样品保持在400℃下持续5分钟,并且然后以10℃/min的斜降将温度从400℃降低至10℃进行重结晶。然后将聚合物在10℃下保持10min并且然后以10℃/min的温度斜升再次加热至400℃。将熔点确定为该第二次斜升期间的熔化温度。
C-set(压缩形变):遵循ASTM 395B测量压缩形变值。样品由具有120mm的外径和2mm的厚度的注射模制圆盘获得,该注射模制盘通过注射模制根据以下所述的程序制备。从这些较大的圆盘中,切割出具有13mm的直径和2mm的厚度的较小的圆盘状样品。使这些较小的圆盘经受压缩测试。在压缩测试中,将样品沿着厚度压缩,样品最初为2mm,将其压缩至1mm。将样品在压缩下在70℃烘箱中保持120小时。这段时间后,将样品从烘箱中取出,去除压缩,并且室温调节30分钟后,测量样品的厚度。C-set值通过以下等式确定:
C-set(%)=[(t0-ti)/t0-ts)]x 100
to=样品的最初厚度(在这种情况下约2mm)
ts=样品的目标压缩厚度(在这种情况下1mm)
ti=室温调节后样品的最终厚度
拉伸特性:在23℃下根据ASTM D3307在模制基板上以1%偏移测量屈服应力(以MPa计)。使呈粒料形式的测试聚合物在360℃下在立式压力机中经受熔融压缩模制,以制造具有约1.2mm的厚度的基板。
介电特性根据ASTM D149的介电强度和根据ASTM D3638的CTI(相比漏电起痕指数)在用于测量拉伸特性的相同的模制基板上获得,
毛细管测试(鲨鱼皮检测):根据ASTM D 3835进行。在毛细管流变仪设备(Rheograph 2003)中使用L/D=10并且D=1和0.54mm进行测试。通过毛细管挤出熔融材料,并且评估挤出物表面的光滑度/粗糙度。测试用于评估在不示出表面粗糙度的情况下材料可以被挤出(在给定的T下)的最大剪切速率。表面粗糙度(鲨鱼皮)的形成对于进行毛细管测试的技术人员来说通过对样品的简单的触觉检查立刻显而易见。
所使用的材料:
聚合物P1(根据本发明)-TFE/PPVE/PMVE共聚物,其包含按摩尔计4.75%的PPMVE、按摩尔计0.39%的PPVE和按摩尔计94.86%的TFE,具有281℃的Tm、和在372℃-5kg下88g/10min的MFR。
聚合物P2(对比)-TFE/PPVE共聚物,其包含按摩尔计1.6%的PPVE和按摩尔计98.4%的TFE,具有308℃的Tm,并且具有在372℃-5kg下13.3g/10min的MFR。
聚合物P1的制备
在配备有在400rpm下工作的搅拌器的22升AISI 316钢立式反应器中,在真空后顺序引入以下成分:
-13.9升的脱矿质水,
-85g的全氟丙基乙烯基醚(PPVE)
-128g的微乳液,其根据US 4864006通过将39.7g的一种具有羧酸铵端基的离子全氟聚醚、23g的一种具有中性端基的全氟聚醚和65.3g水混合来制备。
添加所有成分后,将反应器加热至75℃并且进料0.15巴的乙烷和3.7巴的全氟甲基乙烯基醚(PMVE)。然后通过压缩机添加以21的摩尔比的气态TFE/PMVE混合物,直至达到21绝对巴的压力。通过计量泵进料118ml的0.044M过硫酸铵溶液,从而开始聚合。通过进料上述单体混合物使聚合压力保持恒定,并且当达到20%的转化率时,添加额外量的8.6g的乙烷。进料总计8715g的以上混合物后,中断单体混合物进料,停止搅拌并且使压力降低直至达到7.5绝对巴。然后将反应器冷却至室温,排出乳液并且用65%硝酸溶液使其凝结。将聚合物用水洗涤,在烘箱中在220℃下干燥,并且然后使用Coperion双螺杆挤出机48D在约302℃的挤出温度下造粒。标称聚合物组成为按摩尔计4.75%的PMVE、按摩尔计0.39%的PPVE和按摩尔计94.86%的TFE。MFR为88g/10’并且熔点为281℃。
聚合物P1和P2的注射模制:聚合物P1和P2用于通过注射模制制备具有120mm的直径和2mm的厚度的圆盘。模制在具有30mm的机筒直径的注射模制机Negri-Bossi(NB100)上进行。通过注射模制获得的圆盘用于如上所述的C-set测量。
优化聚合物P1和P2两者的模制条件:聚合物P1(根据本发明)在注射模制机中在C1/C2/C3/C4为315℃/320℃/325℃/330℃的气缸温度、喷嘴温度330℃和高达432巴的压力(保压压力)下进行加工,而聚合物P2(对比)在注射模制机中在C1/C2/C3/C4为370℃/375℃/380℃/385℃的气缸温度、喷嘴温度385℃和高达520巴的压力(保压压力)下进行加工。两种模制操作都需要65秒的循环时间。
所获得的两个圆盘都是完全光滑的,并且没有裂纹或缺陷。该模制实例示出聚合物P1可以如何在比聚合物P2更低的温度和压力下注射模制。
屈服应力的测量
屈服应力在如上所述获得的模制基板上测量。所获得的结果示出聚合物P1和P2两者的样品具有相同的屈服应力,为约12.5MPa。
压缩形变(C-set)的测量
C-set在由如上所述的模制圆盘制备的聚合物P1和P2两者的样品上测量。结果示出两种样品具有相同的C-set值,为约73%。压缩后的测试件不存在缺陷或裂纹。
介电特性的测量
介电强度和CTI在用于测量机械特性的相同的模制基板上测量。所获得的结果示出聚合物P1和P2两者的样品者具有相同的介电强度,为约32KV/mm并且CTI高于600V。
毛细管测试
使聚合物P1和P2两者经受毛细管测试。将熔融的聚合物注入仪器的毛细管中,并且通过毛细管在不同的温度下挤出。评估挤出的材料的表面是否光滑(通过)和粗糙(失败)。将聚合物在每个温度下示出光滑表面的最大剪切速率记录为“鲨鱼皮起始剪切速率”。结果示于表1中。
表1
结果清楚地示出根据本发明选择的聚合物P1可以如何在比聚合物P2快得多的速率下注射模制,而没有形成表面缺陷的风险。
重量损失的测量
在TA公司的TGA5500仪器中在0.030g样品上测量重量损失。进行两次重量损失测试。在第一次测试中,以每分钟10℃的温度斜升将聚合物样品从室温加热至380℃(动态加 热测试)。
在第二次测试中,以相同的斜升将聚合物样品加热至其模制温度(P1为330℃并且P2为380℃)并且将该温度维持4小时(等温测试)。
重量损失数据报告在下表2中:
表2
重量损失数据示出聚合物P1的样品动态加热至380℃后如何展现出重量损失的减少。这意味着在模制期间分解产物(包括HF气体)的逸出减少,并且因此设备的使用寿命更长,并且模制制品中的缺陷(例如气泡)的数量减少。注意,在实际应用中,聚合物P1的模制温度比P2的模制温度低得多,这意味着如等温重量损失测试所示,分解产物的逸出更加显著地减少。
用于电化学电池单元的绝缘组件零件的制备
实例:绝缘板的制备
在注射模制机中加工聚合物P1。将熔体注入具有4个腔的多腔模具中,这些腔呈具有8mm的直径和0.5mm的厚度的圆盘形状。所有环都成型良好,光滑并且无裂纹或缺陷。然后将圆盘用作圆柱形Li电池单元的绝缘板。
总的来说,数据显示了使用本发明的选定的聚合物来制造用于电池的绝缘组件零件如何允许通过注射模制来有效地制造这些零件,相对于本领域中用于相同应用的常见PFA聚合物,使用较低的模制温度、较快的注射模制工艺(因为熔融聚合物可以经受较高的剪切速率)并在模制期间记录较低的重量损失(对应于较低水平的腐蚀性脱气)。出人意料地,所得的零件具有与传统使用的PFA聚合物的那些相一致的机械和电特性。
Claims (15)
1.一种用于电化学电池单元的绝缘组件零件,其包含一种或多种含氟聚合物,所述含氟聚合物包含
-按摩尔计87%-99%的衍生自四氟乙烯(TFE)的重复单元
-按摩尔计1%-13%的衍生自全氟甲基乙烯基醚(PMVE)的重复单元
-按摩尔计0%-3%的衍生自全氟丙基乙烯基醚(PPVE)的重复单元
并且具有从40至300g/10min的熔体流动速率(MFR)(在372℃下在5kg载荷下测量)。
2.根据权利要求1所述的绝缘组件零件,其中,所述一种或多种含氟聚合物包含:
-按摩尔计1%-10%、优选2%-8%、更优选3%-7%的衍生自PMVE的重复单元
-按摩尔计0%-3%、优选0%-2.5%、更优选0%-2%、甚至更优选0.1%-1.5%的衍生自PPVE的重复单元。
3.根据任一前述权利要求所述的绝缘组件零件,其中,所述一种或多种含氟聚合物具有小于1、优选小于0.5、更优选小于0.3、最优选小于0.2的衍生自PPVE的重复单元和衍生自PMVE的重复单元之间的摩尔比(PPVE/PMVE)。
4.根据任一前述权利要求所述的绝缘组件零件,其中,所述一种或多种含氟聚合物具有从260℃至310℃、优选从270℃至305℃、更优选从275℃至300℃的熔融温度Tm。
5.根据任一前述权利要求所述的绝缘组件零件,其中,所述一种或多种含氟聚合物具有从50至200、优选从60至160、更优选从70至130g/10min的MFR(在372℃下在5kg载荷下测量)。
6.根据任一前述权利要求所述的绝缘组件零件,其中,所述一种或多种含氟聚合物构成所述绝缘组件零件的按重量计至少80%、优选至少90%、更优选至少95%、最优选至少99%。
7.根据任一前述权利要求所述的绝缘组件零件,其中,所述电化学电池单元是电池单元、优选二次电池单元、更优选锂电池单元。
8.根据任一前述权利要求所述的绝缘组件零件,其为注射模制的绝缘组件零件。
9.根据任一前述权利要求所述的绝缘组件零件,其是密封垫片、绝缘板或电极固持器。
10.一种制造根据任一前述权利要求所述的用于电化学电池单元的绝缘组件零件的方法,所述方法包括通过注射模制热塑性聚合物组合物形成所述绝缘组件零件,所述组合物包含一种或多种包含以下各项的含氟聚合物:
-按摩尔计87%-99%的衍生自四氟乙烯(TFE)的重复单元
-按摩尔计1%-13%的衍生自全氟甲基乙烯基醚(PMVE)的重复单元
-按摩尔计0%-3%的衍生自全氟丙基乙烯基醚(PPVE)的重复单元
并且具有从40至300g/10min的熔体流动速率(MFR)(在372℃下在5kg载荷下测量)。
11.根据权利要求10所述的制造用于电化学电池单元的绝缘组件零件的方法,其中,所述模具是包括至少4个腔的多腔模具,每个腔允许模制单独的绝缘组件零件。
12.根据权利要求10或11所述的制造用于电化学电池单元的绝缘组件零件的方法,其中,所述热塑性组合物包含按重量计至少80%、优选至少90%、更优选至少95%、最优选至少99%的所述一种或多种含氟聚合物。
13.一种二次电池,其包括至少一个根据权利要求1-9所述的绝缘组件零件。
14.根据权利要求13所述的二次电池,其中,所述至少一个绝缘组件零件是密封垫片、绝缘板和/或电极固持器。
15.包含一种或多种含氟聚合物的热塑性聚合物组合物用于制造电化学电池单元的绝缘组件零件、优选用于制造二次电池的密封垫片、绝缘板和/或电极固持器的用途,所述含氟聚合物包含:
-按摩尔计87%-99%的衍生自四氟乙烯(TFE)的重复单元
-按摩尔计1%-13%的衍生自全氟甲基乙烯基醚(PMVE)的重复单元
-按摩尔计0%-3%的衍生自全氟丙基乙烯基醚(PPVE)的重复单元
并且具有从40至300g/10min的熔体流动速率(MFR)(在372℃下在5kg载荷下测量)。
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