CN105189104A - 气凝胶绝缘面板及其制造 - Google Patents
气凝胶绝缘面板及其制造 Download PDFInfo
- Publication number
- CN105189104A CN105189104A CN201480012986.2A CN201480012986A CN105189104A CN 105189104 A CN105189104 A CN 105189104A CN 201480012986 A CN201480012986 A CN 201480012986A CN 105189104 A CN105189104 A CN 105189104A
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- Prior art keywords
- aerogel
- panels
- layer
- aeroge
- thermal conductivity
- Prior art date
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Abstract
本发明提供关于自气凝胶作成的绝缘面板的物件和制造方法,且具体为聚酰亚胺气凝胶。这些绝缘面板具有广泛应用,具体包括航空航天应用。
Description
关于联邦政府赞助研究或开发的声明
本发明由政府支持,由DARPA资助,在W31P4Q-10-C-0209合约下完成。政府拥有本发明的某些权利。
技术领域
本发明关于可用于航空航天应用中的层压面板。该面板包括聚酰亚胺系气凝胶层、至少一层表皮(facesheet)层、以及在该表皮上的反射保护层。
背景技术
本发明针对层压面板,其包括聚酰亚胺系气凝胶层、至少一层表皮层、以及位于该表皮上的反射保护层。该气凝胶层起绝缘和结构上支撑该面板两种作用。
航空航天面板难以设计和生产。航空航天旅行天然地要求面板材料上的环境应力远高于那些材料在典型应用中面对的应力。因此,在设计航空航天面板中使用的材料必须具有足以承受那些压力环境中极端条件的耐久性。航空航天旅行也天然地需要尽可能轻质的面板材料。这些材料在密度和重量上的微小差异可能对面板的功能性以及航空航天装置整体功能性和能量效率产生显着影响。因此,必须选择航空航天面板中的结构性材料和绝缘材料,并将其优化用于航空航天旅行中发现的特殊挑战。
气凝胶复合材料具有的物理性质和化学性质可潜在地优化以承受航空航天面板设计的需求。气凝胶揭示了基于其结构的一类材料;即表面积大(一般为900m2/g或更高)且孔径小于纳米规格的低密度开孔结构。可通过以空气替换湿凝胶中的液体溶剂而基本不改变或崩毁网状结构(如,孔特征)或凝胶体的体积,从而制备气凝胶。使用超临界和亚临界流体萃取技术自该凝胶萃取流体,而不造成孔的崩毁。已知多种不同的无机和有机气凝胶组合物。无机气凝胶通常基于金属玩氧化物,且包括诸如氧化硅、碳化物和氧化铝的材料。有机气凝胶包括碳气凝胶和聚合性气凝胶如聚酰亚胺。
气凝胶主要通过最小化传导(低密度、曲折路径用于热转移通过该纳米结构)、对流(非常小的孔径最小化了对流)和辐射(IR抑制掺杂进可轻易分散于整个气凝胶基质中)而起热绝缘体的功能。依据其配方,气凝胶可在550℃及以上的温度起作用。广泛认为,低至中密度气凝胶材料(典型为约0.01g/cm至约0.3g/cm的范围)是最好的固体热绝缘体,且在37.8℃和大气压力下具有约12mW/m-K及以下的热导率。
也可以在生产过程中以纤维增强气凝胶,以提供显着的结构稳定性和回弹性,尤其是在高挠曲应变应用中。气凝胶薄片(典型为约0.1mm与约25mm之间)的挠曲令大片气凝胶组合物的制造成为可能,该组合物保留气凝胶的大部分有用品质如低密度和低热导率。
因此,对于具有容许航空航天面板的优化设计和制造的强度、热导率和密度性质的结构性和绝缘材料存在需求。具体地,对于具有容许航空航天面板的有效设计和制造的强度、热导率和密度性质的优化气凝胶材料存在需求。对于有效合并该优化气凝胶材料的层压航空航天面板也存在需求。
发明内容
本发明揭示一种层压面板,包含(a)具有两个主面的聚酰亚胺系气凝胶层;(b)位于该气凝胶层至少一个主面上的表皮;以及(c)与该表皮相邻的反射层。该面板可在该气凝胶层的两个主面上均包括表皮。该面板可额外包括边封以密封该面板的边缘。该面板可包含穿透或未穿透该面板的至少一个孔,以便于固定。
该面板包括聚酰亚胺系气凝胶层。本发明中使用的聚酰亚胺系气凝胶可被碳化。碳化可通过在高温及惰性气氛中热解而进行。本发明中使用的碳化形式的气凝胶可具有0与20%之间的氮含量。本发明中使用的气凝胶也可含有氧化硅组分。这些氧化硅组分可以是与聚酰亚胺的物理混合物或共价链接至氧化硅。该气凝胶层也可使用纤维增强。该气凝胶可包含遮光剂,如二氧化钛、碳化硅、碳黑、石墨、磷酸盐、硼酸盐、金属硅酸盐、茂金属、钼酸盐、锡酸盐、氢氧化物、碳酸盐、氧化锌、氧化铝、氧化锑、镁-锌掺混物、镁-锌-锑掺混物、或其组合。
该气凝胶层可包含具有特定物理和化学性质的聚酰亚胺系气凝胶。具体地,本发明的气凝胶层可具有挠曲强度、挠曲模量、密度和热导率的特定组合。该气凝胶材料的挠曲强度为,若未失败,至少150psi、至少200psi、或至少250psi。该气凝胶材料的挠曲模量可为,若未失败,至少5000psi,至少20000psi,或至少40000psi。该气凝胶材料的密度可为低于0.25g/cc、低于0.15g/cc、或低于0.10g/cc。该气凝胶材料在常温常压下的热导率可为低于40mW/m-K、低于30mW/m-K、或低于20mW/m-K。该气凝胶材料在常温及10-5托真空下的热导率为低于10mW/m-K,低于5mW/m-K,或低于3mW/m-K。
该面板包括位于该气凝胶层至少一个主面上的表皮。一个具体实施例中,该面板包括位于该气凝胶层两个主面上的表皮。另一具体实施例中,该表皮包含石墨氰酸酯表皮。
该面板包括与表皮相邻的反射层。该反射层反射至少一个频率的入射能量。一个具体实施例中,该反射层覆盖该表皮的全部。另一具体实施例中,该反射层保护该面板不通过反射可潜在损坏该面板的至少一个频率的入射能量而被损坏。该反射层可包含银聚四氟乙烯涂覆材料。
该面板可包括至少一个令空气流入和流出该面板的通气口。该面板可包括至少一个过滤颗粒物质的过滤器。一个具体实施例中,该面板包括令空气流入和流出该面板的通气口,以及位于该通气口上的将颗粒物质保持在该面板内的颗粒过滤器。另一具体实施例中,该面板包括边封,该边封包括至少一个通气口和至少一个颗粒过滤器。又一具体实施例中,该面板包括边封,该边封包括至少一个通气口和至少一个颗粒过滤器,其中,该边封中的通气口令空气流入和流出该面板边缘,以及,其中,该过滤器捕捉并保留流动空气中的颗粒物质,以防止颗粒物质污染该面板外的空气。
本发明还提供制造层压面板的方法,包含步骤:(a)提供具有两个主面的聚酰亚胺气凝胶层;(b)将表皮粘附至该气凝胶层的至少一个主面;以及(c)将反射层粘附至该表皮。本发明的面板可在边缘处密封。可基于多种原因提供至少一个穿透该面板的孔,包括结构件的适应性。这些孔并非必须穿透该面板的全部厚度,且可令使用固定件或螺杆低将该面板简单地粘附至其它构件成为可能。
一个具体实施例中,本发明包含具有下列的气凝胶绝缘层:(a)密度为0.20g/cc或更低,0.15g/cc或更低,或0.10g/cc或更低;(b)常温常压下的热导率为30mW/m-K或更低,25mW/m-K或更低,20mW/m-K或更低,或15mW/m-K或更低;(c)挠曲强度为150psi或更大,200psi或更大,或250psi或更大;以及(d)挠曲模量为5000psi或更大,20000psi或更大,或40000psi或更大。该气凝胶绝缘层在常温及10-5托真空下的热导率也可为10mW/m-K或更低,5mW/m-K或更低,或3mW/m-K或更低。
另一具体实施例中,该气凝胶绝缘层包含聚酰亚胺气凝胶或其衍生物。该气凝胶绝缘层也可以是纤维增强气凝胶。
再一具体实施例中,本发明包含层压面板,包含:(a)具有至少两个主面的气凝胶层;(b)与该气凝胶层的至少一个主面相邻的表皮;以及(c)与该表皮相邻的反射层。该面板可包括与该气凝胶层第一主面相邻的第一表皮,以及该气凝胶层第二主面相邻的第二表皮。该面板也可通过至少一个边封在边缘处密封。
再一具体实施例中,该面板包括至少一个通气口和至少一个通气口过滤器。该面板也可包括边封,该边封包括至少一个通气口和至少一个通气口过滤器。
附图说明
图1例示性说明作成聚酰亚胺的合成方案。
图2例示性说明多种聚酰亚胺气凝胶形式参数:整块材料、模塑整块材料、机械加工的整块材料、不透明化的整块材料、和纤维增强材料。
图3例示性说明湿聚酰亚胺凝胶的压缩强度和胶凝时间对催化剂密度。
图4揭示非碳化的未经处理(g)及经退火的(a)碳不透明化PI气凝胶整块材料。
图5例示性说明,对于经不透明或和未经不透明化的PI气凝胶,热导率对最终密度的曲线。
图6例示性说明在单轴压缩之前和之后的聚酰亚胺气凝胶整块材料。
图7例示性说明,对于聚酰亚胺气凝胶整块材料,压缩强度对应变数据的曲线。
图8例示性说明,对于聚酰亚胺、氧化硅、和氧化硅杂化气凝胶整块材料,压缩模量对密度的曲线。
图9例示性说明PI增强气凝胶的图。
图10例示性说明纤维增强聚酰亚胺气凝胶整块材料的密度和热导率数据。
图11例示性说明纤维增强聚酰亚胺气凝胶的1层、2层、3层和4层堆叠体的热导率、厚度和密度。
图12例示性说明纤维增强聚酰亚胺气凝胶的多层堆叠体的厚度和密度的图。
图13例示性说明在多种目标密度制备的PI气凝胶碳纤维复合材料的照片。
图14例示性说明在多种目标密度制备的碳纤维增强聚酰亚胺气凝胶的最终厚度、密度和热导率。
图15例示性说明PI气凝胶碳纤维复合材料的a)30x、b)250x、和c)150kxSEM图像。
图16-1包括使用Kevlar线缝制的4层PI气凝胶碳纤维复合材料的照片。
图16-2例示性说明多层碳纤维增强聚酰亚胺气凝胶的压缩强度和挠曲强度。
图17例示性说明,对于多种纤维增强聚酰亚胺气凝胶,压缩应力对应变的曲线。
图18例示性说明,对于多种纤维增强聚酰亚胺气凝胶,挠曲应力对应变的曲线。
图19例示性说明整块材料和碳纤维增强聚酰亚胺气凝胶的真空水平热导率对温度作图。
图20例示性说明配备含有嵌件和边封的碳纤维增强聚酰亚胺气凝胶的夹层复合材料面板的示意图和原型。
图21a至21k例示性说明将盲嵌安装在夹层复合材料组件中的步骤。
图22例示性说明片段式边封设计的示意图。
图23例示性说明4点弯曲测试后的3”x8”面板取样片,表明表皮与PI气凝胶芯之间在边缘处的脱层。
图24例示性说明2”x2”样品在平拉测试过程中的层间失败。
图25例示性说明3”x4”样品在剪切测试过程中的层间失败。
图26例示性说明2”x2”样品在平压缩过程中的应力-应变曲线。
具体实施方式
本发明提供层压面板,包含:(a)具有两个主面的聚酰亚胺系气凝胶层;(b)位于该气凝胶层的至少一个主面上的表皮;以及(c)与该表皮相邻的反射层。该面板可包括位于该气凝胶层两个主面上的表皮。该面板可额外包括边封以密封该面板的边缘。该面板可包含至少一个穿透或未穿透该面板的孔。
该聚酰亚胺气凝胶可优化以具有特定的物理性质和化学性质。具体地,本发明的气凝胶层可优化以具有挠曲强度、挠曲模量、密度和热导率的特定组合。该气凝胶材料的挠曲强度可为,若未失败,至少150psi、至少200psi、或至少250psi。该气凝胶材料的挠曲模量可为,若未失败,至少5000psi,至少20000psi,或至少40000psi。该气凝胶材料的密度可为低于0.25g/cc、低于0.15g/cc、或低于0.10g/cc。该气凝胶材料在常温常压下的热导率可为低于40mW/m-K、低于30mW/m-K、低于20mW/m-K、或15mW/m-K或更低。该气凝胶材料在常温及10-5托真空下的热导率为低于10mW/m-K,低于5mW/m-K,或低于3mW/m-K。
材料的挠曲强度是材料在荷载应力下抵抗灾难性形变的能力。挠曲强度可使用3点横向弯曲挠曲测试技术如ASTMD790测试来测量。通常,挠曲强度定义为材料由于荷载应力而在破裂或灾难性物理事件时刻遭受的压力(psi或Mbar)。该值典型取自材料挠曲强度测试所产生的应力-应变曲线(见图18)。
材料的挠曲模量是材料弯曲的倾向性,或者,更具体地,材料挠曲形变的应力与应变比。该值自挠曲强度测试(如ASTMD790)所产生的应力-应变曲线的斜率测得。
该层压面板也可包括边封。该边封可沿着该面板的整个边缘连续。该边封也可由片段式设计组成(图22)。一个具体实施例中,该片段式设计可包括2"长的U形玻璃纤维密封片段,该片段沿着该面板的边缘分布。该密封片段包括覆盖有0.5μm颗粒过滤器的0.25”通气口。该通气口令空气进入和离开该面板。因为当面板在不同海拔之间穿越时,本发明令该面板内的气压与环境气压正常化,故本发明在航空航天应用中很重要。该颗粒过滤器防止任何颗粒在升空疏散及/或面板排气过程中自该面板内部逃逸。这些片段被结合至外表皮,且该等片段末端之间有2"的缝隙。片段之间的2"缝隙覆盖有2-mil聚酰亚胺胶带(Kaptontape)以完全密封该面板边缘。这一设计具有某些限制加工优势,形成边封的2"长片段可预制,切割为2"长并存储。
本发明还提供生产纤维增强聚酰亚胺气凝胶复合材料的制程。该制程包括:(a)自二酐和二胺单体的混合物在双极性碱性溶剂如N,N-二甲基乙酰胺(DMAc)或N-甲基吡咯烷酮(NMP)中的溶液形成聚(酰胺酸)溶液;(b)在胶凝前,将该聚(酰胺酸)溶液浇铸于纤维絮中;(c)通过化学亚胺化反应使用醋酸酐和吡啶胶凝该聚(酰胺酸)溶液;以及(d)使用超临界或亚临界CO2移除该凝胶中含有的瞬时液相,以给出纤维/聚酰亚胺气凝胶复合材料。该聚酰亚胺气凝胶可自芳香族二酐和二胺单体如芳香族二胺或至少一种芳香族二胺单体与至少一种脂肪族二胺单体的混合物生产。可优化所得聚酰亚胺气凝胶以令其具有低密度、中等孔、窄孔径分布和良好机械强度。
聚酰亚胺湿凝胶的制备是两步过程(图1):(a)自二酐和二胺的混合物在双极性碱性溶剂如N,N-二甲基乙酰胺(DMAc)或N-甲基吡咯烷酮(NMP)中形成聚(酰胺酸)溶液;以及(b)与醋酸酐和吡啶进行环化反应来形成聚酰亚胺。合成聚酰亚胺气凝胶的先前工作已经显示,第一步典型需要载室温混合至少12小时以令聚(酰胺酸)聚合物显着形成,并获得稳定、强健的湿凝胶。胶凝条件取决于若干因素,包括所制备的溶液的密度。高密度溶液将比密度较低的溶液更快胶凝。一旦该***达到凝胶状态,则将该凝胶在65℃烘箱中热处理16小时,此后,以乙醇重复冲洗该湿凝胶。在CO2萃取前,冲洗至少出现3次,并起移除不溶于超临界CO2和亚临界CO2中的残留DMAc溶剂和未反应单体的作用。CO2可随后用于在该领域中已知的用于湿溶剂萃取的技术中,以创造气凝胶结构。进一步制备和优化聚酰亚胺气凝胶的技术可在美国专利申请案US10/625,501和US11/047,200中找到,两篇专利均通过引用而以其整体并入本文。
该聚酰亚胺气凝胶可以为多种形式(图2)。当使用醋酸酐和吡啶催化该聚(酰胺酸)溶液时,所得湿凝胶和气凝胶是透明的橘红色。当使用三乙胺催化时,所得湿凝胶和气凝胶是不透明的黄色。聚酰亚胺气凝胶可制备为不需要支撑物的透明的整块材料,可模塑为具体形状或机械加工为最终气凝胶状态。聚酰亚胺气凝胶也可使用联系纤维絮增强以提供硬质板状复合材料。最终,胶凝前的聚(酰胺酸)溶液可与多种遮光剂掺杂,该遮光剂包括碳黑、石墨、碳纳米管、金属氧化物、金属、二氧化钛、碳化硅、磷酸盐、硼酸盐、金属硅酸盐、茂金属、钼酸盐、锡酸盐、氢氧化物、碳酸盐、氧化锌、氧化铝、氧化锑、镁-锌掺混物、镁-锌-锑掺混物、或其组合。
一个具体实施例中,氧化硅组分也存在于本发明的气凝胶中。氧化硅可作为物理混合物或其可与聚酰亚胺共价键结而并入该聚酰亚胺基质中。美国专利申请案US13/299,677揭示了一些这种共价键结的氧化硅-聚酰亚胺杂化气凝胶,该专利通过引用以其整体并入本文。另一具体实施例中,本发明的聚酰亚胺气凝胶被碳化。碳化导致至少部分该聚合性材料被使用多种已知技术如热解转化为碳。一个优选的具体实施例中,聚酰亚胺气凝胶被加热至足以引发热解的高温。典型热解温度范围是500℃与2000℃之间。可增加温度以降低所得碳气凝胶中的氮含量。热解典型在惰性气氛(即,氮、氦、氖、氩、或其组合)中进行。该碳气凝胶中的氮含量可以是自0%至20%。
本发明进一步提供加工包含纤维增强聚酰亚胺气凝胶复合材料和表皮的层压夹层面板复合材料的制程。该面板还可包括额外元件如反射保护层、边封、通气口、过滤器、和用于组件安装的嵌件。该制程包括:(a)提供具有两个面的气凝胶层以及至少一层表皮;(b)清洁并任选打磨该气凝胶和表皮的表面,以备粘结;(c)将膜状粘结剂施加至该表皮;(d)将该表皮与气凝胶层组合,故该表皮粘结至该气凝胶层的面上;以及(e)固化该气凝胶-表皮层压体以完成粘结。
下述实施例提供本发明的多个具体实施例和性质。
实施例1
对于所制备的初始目标密度(即,含固量)为0.085g/cc的***,测量聚酰亚胺湿凝胶的凝胶强度作为催化剂密度的函数。图3中的催化剂含量表示醋酸酐与吡啶的合并摩尔比。发现,对于9.2与4.4之间范围的催化剂密度,在合成后24小时测得的湿凝胶压缩强度为约4600psi。当催化剂密度为2.8时,胶凝时间可观地延长,但所得湿凝胶强度仅接近使用更高催化剂含量所得的一半(1900psi)。
实施例2
为了降低热导率,在聚酰亚胺气凝胶整块材料的制备中使用碳黑(来自Cabot–Monarch1300)作为遮光剂。优选使用粒径小于微米级的遮光剂作为额外的散热材料。先前揭示的用以制备未不透明化PI气凝胶整块材料的聚(酰胺酸)溶胶也用于合成碳不透明化的PI气凝胶整块材料。使用1和5wt%的碳制备0.03、0.06和0.08g/cc的目标密度。在PI形成的早期加入遮光剂并非优选,因为它可妨碍聚合生长并导致若凝胶。优选在醋酸酐催化剂后但在吡啶催化剂前加入1和5wt%(相对于总含固量)的遮光剂,帮助保留该聚合反应的完整性。为了防止碳在胶凝之前可能的沉降,将该溶液超声处理15分钟,且在浇铸凝胶后,立即于65℃加热16小时(过夜)。同样,在CO2萃取之前,用乙醇冲洗该湿凝胶3次。碳不透明化PI气凝胶的图片可见于图4中。
当采用5wt%的碳时,不透明化导致热导率下降接近10个单位。这于图5和表1中证实。
表1.碳不透明化PI气凝胶整块材料的物理表征
例如,1%-8g的TC为43.0mW/m·K。5%-8g具有几乎相同的最终密度,但TC值为34.0mW/m·K。对于那些经退火的样品1%-6a、1%-8a和5%-8a,结果与未经不透明化的PI气凝胶整块材料一致,其中,密度在退火之后增加导致TC的增加。这说明,至少在常规条件下,不透明化具有降低热导率的潜力。预期在辐射热传递的贡献更大的升高温度下,这一观察将会更加剧烈。超过5wt%碳的不透明化倾向于降低气凝胶的强度,尤其是较低密度的气凝胶的强度,并因此未考虑进行进一步的研究。
实施例3
使用具有50kN测压元件和0.050”/min十字头速度的Instron(Model5569)测试,进行本发明样品的单轴压缩分析。测定每一密度的PI气凝胶整块材料的应力-应变曲线,并计算杨氏压缩模量E。当PI气凝胶整块材料被单轴压缩时,它们的压缩情况与有机泡沫体相当。在较低应变,使用初始斜率(约2至5%应变之间)计算杨氏模量。据信,在这一压缩阶段,该整块材料具有弹性特性。经过初始斜率后,该样品展现一平台,在该平台处,随着应变增加,应力最低程度地增加。在此压缩应力,该微孔不可逆地崩毁,且只要微孔大小存在窄分布,则该平台区域即应保持相对水平。随着该微孔在连续应变下完全崩毁,相对侧的微孔壁挤压,且将固体推至固体。这反映在应力的迅速增加中,并往往指代为致密化。图6显示压缩之前和之后的PI整块材料。
实施例4
自图7中所示的PI-4、PI-5、PI-6、PI-8、PI-4a、PI-6a和PI-8a的应力-应变曲线测得相应的压缩强度,并列于后附表中。每一密度的整体应力-应变曲线显现该气凝胶的不在压缩荷载过程中破碎、开裂或断裂的能力。与极度积灰且非常易碎的氧化硅气凝胶相比,当考虑到需要机械加工和最小程度颗粒脱落的客户应用时,这是重要的特征。自2%至5%应变范围内的斜率计算该杨氏模量。自此数据可证实,随着密度增加,杨氏模量及微孔崩毁几率增加。这看起来与在约5%应变后,无论任何密度,孔开始崩毁相一致。
压缩模量与密度之间的典型关系遵循幂函数定律。如图8中所见,相对于密度的增长,PI气凝胶的强度以比任何其它氧化硅或氧化硅杂化***更快的速率增加。
实施例5
考虑将增强PI气凝胶作为增加整体机械强度和简化处置并仍保持程序需求中的最终密度的手段。如后文将揭示的,与其母本未经不透明化的非增强PI气凝胶整块材料相比,在聚酰亚胺气凝胶中的增强体不仅增加挠曲强度,而且降低热导率(TC)。选择3种絮材料或基材用于本研究:密度为0.094g/cc且TC测量值为34.4mW/m·K(在常温常压下热板测试)的碳毡(CF)、密度为0.0069g/cc且TC测量值为38.6mW/m·K的(来自Saint-Gobain,本文中缩写为Q)、和密度为0.0396g/cc且TC测量值为27.2mW/m·K的碳组织(来自TechnicalFibreProducts,Inc.;缩写为CT)。
通过初始密度为0.03、0.04、0.06和0.08g/cc的聚酰亚胺溶液制备增强PI气凝胶。依据该初始密度和基材大小,制备预设体积的聚酰亚胺溶液以完全填充该基材。依次将醋酸酐和吡啶加入聚(酰胺酸)溶液中后,依据预设的胶凝时间,将该溶液直接浇铸在聚丙烯模具内含有的基材中。该PI溶液轻易地渗透纤维,而不妨碍预期胶凝化的时间。一旦该溶液成为凝胶,即将该湿凝胶于65℃加热16小时,以令该凝胶强化。在CO2萃取之前,以乙醇冲洗该凝胶3次,以乙醇残留溶剂、催化剂和未反应的单体。未经处理和经退火的增强PI气凝胶的图像可见于图9。
当使用碳毡、或碳组织增强PI气凝胶时,我们发现热导率全部下降(图10)。尽管我们发现使用碳毡时热导率的下降量可观(TC范围自18.5至23.6mW/m·K),但最终密度远高于该项目所希望的目标密度:最终密度为0.1159g/cc的CF-4g。此外,由于基材相对于该PI气凝胶的不均匀收缩,这一样品在萃取和退火后显现显着的收缩量和开裂。但是,一种轻得多的纤维,显现低最终密度和低热导率(19.0to24.6mW/m·K),但也不均匀收缩。这一最终复合材料的品质通常较弱但挠曲强,而挠曲是人造卫星结构性面板所不需要的特征。使用这一基材的气凝胶可能是其它需要挠曲和良好热效能的应用的强有力的备选。最后,碳组织显现低密度、低热导率且在萃取和退火过程中不收缩。一个实例是最终密度为0.0936g/cc且热导率为18.6mW/m·K的CT-4g。碳组织是自长碳系纤维形成的絮,其主要以平面方式在侧向x方向和y方向行进。这赋予碳组织以卓越的刚性。结果,选定碳组织作为用于进一步增强实验的基材。
实施例6
我们将6”x6”碳纤维絮叠放为1层、2层、3层和4层的厚度,以增加该气凝胶/纤维复合材料的厚度。将目标密度为0.045g/cc的聚(酰胺酸)溶液浇铸于多层铺层上并令其胶凝。随后对该样品进行老化,冲洗,并超临界干燥以获得图11中所示的样品。在任何热力学或机械测试之前,将该复合材料于200℃加热20分钟以完成酰亚胺化并驱离任何残留的溶剂。在这些步骤的每一步后,没有证据显示层内或层间脱层,表明该复合材料全部为连续PI气凝胶网状结构。
对于每一制备的(上揭)多层铺层,在常温常压下测量每一复合材料的密度和热导率。全部层的最终密度全部处于彼此的误差(0.12g/cc)内。重量和厚度随着层数线性增加。单层复合材料显现的最终厚度约为5mm。为了实现3/4”ITS面板芯,将需要3层或4层的铺层,其厚度分别为0.63”和0.81”。热导率亦不受层数增加的影响。单层铺层的热导率为21.8mW/m-K,但层数增加至2层、3层和4层时,TC并未显着改变,分别为20.7、19.3和20.1mW/m-K。这些趋势和数据显示于图12中。
实施例7
根据先前揭示的相同方法,但使用更高的目标密度,即在聚(酰胺酸)溶胶预料中使用更高的含固量,制备一系列PI气凝胶碳纤维6”x6”复合材料(图13)。我们以努力增加复合材料的整体强度为目的而增加密度。根据目标密度研究,整块材料性PI气凝胶样品的压缩强度以指数方式增加。尽管使用相同碳纤维增强,但制备0.04、0.05、0.06和0.07g/cc的目标密度。
图14总结了这些复合材料的物理特征。将目标密度为0.04g/cc的样品制备为厚度为5.06mm且最终密度为0.120g/cc的对照物。通过增加该目标密度,我们看到了最终厚度的轻微增加以及最终密度的预期增加。该目标密度每增加一个单位,则观察到热导率增加约0.5mW/m-K。
实施例8
为了理解该复合材料中以及该气凝胶与凝胶间界面处的气凝胶网状结构的连续性,通过扫描电子显微镜(SEM)探究PI气凝胶碳纤维复合材料。据信,多种组分间强力连接的复合材料将显现较大的机械强度。缝隙或微裂形式中的不连续性导致机械完整性减弱。根据图15中所见的PI气凝胶/碳纤维复合材料的30x放大SEM图像,证实该PI气凝胶材料在整个纤维中均连续。但是,以250x放大仔细检查,在碳纤维增强体与该PI气凝胶之间存在明显的连续性缺失。这一行为反映在这一材料中所观察到的极差的横向压缩和拉伸强度中。因为絮中的碳纤维主要位于x,y平面且非常坚硬并因此具有高挠曲强度,所以当PI凝胶进行收缩时,该气凝胶收缩远离该纤维,留下微米水平的缝隙。很明显,在平压缩测试过程中,该样品,尤其是具有低复合材料密度的样品,将显现低压缩强度。150kx的图像例示性说明AspenaerogelsPI气凝胶的典型纤维网状结构。
为了增加z向的拉伸强度,我们使用Kevlar线(46号)以十字图案缝合(手工)多层铺层,如图16中所见。将缝合的复合材料强度明显更大。当测试其挠曲强度时,观察到强度增加13%。图16证实,通过缝合缓解了层-层剪切应力,并因此维持更高的挠曲荷载。
实施例9
使用具有50kN测压元件且十字头速度为0.050”/min的Instron(Model5569)检查上揭TD=0.04g/cc的增强样品,进行单轴压缩分析。测定每一增强PI气凝胶的应力-应变曲线,并计算杨氏压缩模量。
自图7中所示的CF-4g、CF-4a、Q-4g、Q-4a、CT-4g、CT-4a的应力-应变曲线测得相应的压缩强度。与极度积灰且非常易碎的氧化硅气凝胶相比,非增强和增强PI样品显示最小的颗粒脱落和积灰。测定每一样品的杨氏模量和最大压缩应力,并总结在图17中。总之,PI气凝胶的增强导致较低的热导率,而以较低的最大压缩应力和较低的杨氏模量为代价。所制备的TD=0.04g/cc的非增强PI气凝胶整块材料的最大压缩强度为57.3psi,且压缩模量为816.7psi。当使用碳毡、和碳组织增强具有相同密度的PI气凝胶时,最大压缩强度为11.7、10.7和11.5psi,且压缩模量为91.8、90.4和182.4psi。碳组织基材在全部纤维中提供最高的压缩强度,部分是由于其独特的纤维不布局。如预期的,经退火的样品显现较高强度,这是密度在加热时增加的反映。
实施例10
相同增强PI气凝胶的机械分析也包括根据遵循ASTMD790设计的3-点挠曲测试。挠曲测试提供了对压缩之外的交变应力的深刻理解。例如,当面板被弯折时,该样品同时遭受侧(x,y)向的拉伸应力和压缩应力。这些应力在仅进行单轴(z向)压缩测试时无法测量。测量未经处理和经退火的TD=0.04g/cc的增强样品的应力-应变曲线(图18),数据总结在图18中。与增强PI气凝胶的压缩强度形成鲜明对比,大多数实例中的挠曲强度超过了非增强PI气凝胶整块材料。碳组织基材显现最大的挠曲强度,该数值为186psi,且杨氏模量为26892psi。挠曲强度与低热导率的组合令CT-4g成为用于进一步研发的首选。
纤维增强PI气凝胶复合材料在10-5托真空中展现优异的热导率。图19显示这一材料与非增强聚酰亚胺气凝胶如何在193K至高达423K(-80℃至150℃)的温度范围内比较。如图中所见,在样品温度为193K(-80℃)测得的这一材料的热导率非常低,为1.5mW/m-K,且当样品温度升至423K(150℃)时,热导率为4.5mW/m-K。对照图19,我们相信,热导率在碳谷(碳组织较少)材料中的急剧下降是由于碳谷增强体的累积不透明化效应,且加入5%碳黑遮光剂进一步改善该结果。通过将这些遮光剂加入聚酰亚胺气凝胶中,热传递的辐射组分大大降低;因此,将整体热导率向下带至193K时的1.5mW/m·K至423K时的4.5mW/m·K范围,如图19中所示。
实施例11
夹层面板复合材料的图形表示和所制造的14”x14”示范面板一起显示于图20中,其中,结构和热学功能并入单一组分中。通过层层结合制程使用粘结剂将具有低热导率(在20℃、10-5托为3.3mW/m-K)和良好机械性质(挠曲强度约700psi,且剪切强度为120psi)的纤维增强聚酰亚胺气凝胶芯材料结合至表皮而制造这种夹层面板,该面板合并有盲嵌和通孔嵌件阵列以及片段式边封封闭***。
下述说明提供制造本发明层状面板的具体实施例的细节。
材料:
待结合的基材是用于夹层样品的PI气凝胶碳纤维复合材料和石墨氰酸酯(Gr/Ce)皮层。该气凝胶可以是单层或多层。在本具体实施例中使用航空品质的密度为0.030lbs./ft2的膜粘结剂FM300-2U。
表面准备:
最初,清洁全部结合表面。Gr/Ce表面打磨至亚光,使用浸有酒精的酒精棉擦拭,直至清洁,并在结合制程中保持清洁。如需要,使用浸有酒精的棉球沾染该结合表面以移除任何引入的表面污染物。如需要,自切割边缘轻柔地移除任何松散的气凝胶碎屑。小心动作,以免敲松额外的碎屑。
夹层结合/固化制程:
1.使用浸有酒精的棉球擦拭Gr/Ce皮层,直至清洁。在室令酒精温挥发10分钟。
2.若需要,移除芯边缘上任何松散的气凝胶碎屑,使用浸有酒精(未饱和)的棉球沾染芯,并令酒精在室温挥发20分钟。这是一个准则;这一材料具有非常多孔的表面,且可需要更长期的高温(120°F,30分钟)以令全部酒精自孔中挥发。对于这一类型的芯,最佳为戴适宜的保护手套并清洁将与该芯材料接触的表面,以防止任何需要在结合前清洁的污染。
3.将膜粘结剂施加至皮层。利用手的热量粘合较小尺寸的样品,或使用真空袋并在完全真空(约12psi)下挤压15分钟。有时,由于膜粘结剂在粘结剂施加制程之前或之后龟裂并剥落,区域将会裸露。可使用相同的膜粘结剂修整这些区域。
4.堆叠该夹层的层压体。如需要,提供板侧封以保护芯的侧面不受来自真空袋的侧向压力破坏。
5.装袋,进行适宜温度控制下的固化。对夹层堆栈施加完全真空(约12psi),检查气密性并固化。
6.以3°至5°F每分钟匀速固化,直至温度达到250°±10°F,并在此温度范围保持最少90分钟。
7.以3°至5°F每分钟的速率冷却至低于150°F。
8.放空真空并自工具移除。
层压多层芯结合/固化制程:
1.移除芯边缘上任何松散气凝胶碎屑,以及,若需要,以浸有酒精(未饱和)的棉球沾染该芯,并令酒精在室温挥发20分钟。这是一个准则;这一材料具有非常多孔的表面,且可需要更长期的高温(120°F,30分钟)以令全部酒精自孔中挥发。对于这一类型的芯,最佳为戴适宜的保护手套并清洁将与该芯材料接触的表面,以防止任何需要在结合前清洁的污染。
2.将膜粘结剂施加至芯层。这一类型的表面难以粘合,如需要,使用相同的膜粘结剂修整裸露点。保持30分钟的完全真空(约12psi)以确保粘结。
3.堆叠该夹层的层压体。如需要,提供板侧封以保护芯的侧面不受来自真空袋的侧向压力破坏。
4.装袋,进行适宜温度控制下的固化。对夹层堆栈施加完全真空(约12psi),检查气密性并固化。
5.以3°至5°F每分钟匀速固化,直至温度达到250°±10°F,并在此温度范围保持最少90分钟。
6.以3°至5°F每分钟的速率冷却至低于150°F。
7.放空真空并自工具移除。
一种用于将部分穿透的嵌件或“盲(blind)”嵌安装入多层铺层的纤维增强聚酰亚胺气凝胶中的逐步过程(图21)。因为嵌件典型由金属制成,为了消除直接通过该面板z向渗漏的热,研发了一种方法来安全地安装穿透该面板厚度的一部分内的嵌件。这一类型的嵌件与预冲孔的表皮共同固化,并随后作为单一组分安装至已经钻孔的气凝胶芯内。
该边封由分段式设计组成(图22)。在此设计中,该U形密封片段被生产为具有0.25”通风口的2"长片段,其中,该通风口上覆盖有0.5μm颗粒过滤器以防止任何颗粒在升空疏散及/或面板排气过程中自该面板内部逃逸。这些片段随后会以片段末端之间具有2"缝隙的方式结合至外侧表皮。这种2"缝隙随后将会覆盖2-milKapton胶带以完全密封该面板边缘。所形成的这些片段的壁厚为0.010”,以最小化沿着该边封渗漏并传导的热。这一设计提供某些显着的加工优势,其中,所形成的边封的2"长片段可预制,切割为2"长并储存。因为玻璃纤维添加的热渗漏低且重量轻,因此,它是选定用于这一边封设计片段的材料。
实施例12
表2列出了PI气凝胶夹层复合材料的全部机械测试(剪切、挠曲、压缩和拉伸)、样品数、和面板构造。根据ASTMC-393,对各自具有或不具有5cm所需网格图案、包括或不包括石墨氰酸酯表皮、且有无边封或通孔嵌件的3个3”x8”取样片,实施2组4点弯曲挠曲测试。根据ASTMC-273,在5个尺寸为3”x4”x0.75”的仅有气凝胶芯的样品上进行剪切测试。根据ASTMC-297,在2”x2”的仅有气凝胶芯的样品上实施平拉伸测试。也感兴趣的是理解通孔嵌件将如何加入拉伸强度中,故制备3个具有表皮的6”x6”样品,并测试仅有一个通孔嵌件安装在该面板中心的样品。最后,根据ASTMD695,对仅有2”x2”芯的样品进行平压缩测试。
表2.所制备的机械测试取样片和构造
所测试的第一组样品包括3个各自用于4点弯曲(根据ASTMC-393)的取样片,即3个不具嵌件的取样片和3个具有5cm网格的盲嵌的取样片。根据表3中观察到的数据,测量值之间存在小的变动,且盲嵌的安装似乎并不影响取样片大小的面板的挠曲行为。所观察到的最大挠曲荷载为约325与380lbf(挠曲荷载)之间,移位为约-0.23与-0.89吋之间。引发取样片失败所需的移位的量指出,该夹层复合材料的挠曲相当高。全部例子中,失败的方法为在表皮/芯界面剪切脱层(图23)。
表3.4点弯曲挠曲测试的结果
根据ASTMC-297使用无嵌件的0.75吋芯实施平拉伸测试。该测试的结果总结于表4中。所收集的数据间存在大幅变动,最大荷载数据范围是12与45lbf,(3与11psi)之间。对于相同的目标密度0.05g/cc,需要至少25psi的压力来实现层间失败(图24).
表4.平拉伸测试的结果
制备总计5个样品用于剪切测试(根据ASTMC-273)。这些样品中不包括嵌件或表皮。结果总结于表5中。5个样品中的3个在测试之前展现了某种形式的脱层。对于样品2和3,在多层堆叠的气凝胶复合材料内造成芯剪切所需的最大荷载出现在568和464lbf(或分别为47和38psi)。与先前使用旧碳纤维絮的0.05g/cc目标密度复合材料上测得的剪切强度相比,最大荷载值为1621与1858lbf(134与153psi)之间。图25中,自芯剪切后的失败图像可证,碳纤维絮的嵌入不规则性可导致初步的机械加工失败。
表5.芯剪切强度测试结果
测量5个2”x2”样品的压缩(根据ASTMD-695)。本组样品中未安装嵌件、边封或表皮。全部5个样品的应力-应变曲线显示在图26中。这些复合材料的单轴压缩分析指出,在较低应变,样品到达一平台,之后为压缩荷载的大幅增加。在该平台过程中,该气凝胶形貌不可逆地崩毁,且只要微孔大小存在窄分布,则平台区域即维持基板水平。随着该微孔在持续应变下完全崩毁,相对侧的微孔壁挤压,且将固体推至固体。这反映在应力的迅速增加中,并往往指代为致密化。这些样品的压缩强度估计为约5psi,且在初始应变处和该曲线的平台部分之前测得。由于不均匀的碳纤维絮不规则性,这些复合材料的强度仍弱于预期。
实施例13
使用TechnicalFibreProductsInc.制造的碳纤维作为用于PI气凝胶的增强体,制备CT-4g。该纤维的原始密度为0.0396g/cc,且厚度为约1/4”。为了获得约3/4”的最终芯厚度,将该PI气凝胶/纤维复合材料叠放为多层。通过首先制备聚(酰胺酸)溶液而制备CT-4g。将均苯四甲酸二酐(PMDA,1mol)溶解于双极性碱性溶剂如N,N-二甲基乙酰胺(DMAc)或N-甲基吡咯烷酮(NMP)(4%固体)中。一旦溶解,则将1,4-苯二胺(PDA,1mol)加入该溶液中,并令其溶解且于室温聚合12小时。在聚(酰胺酸)溶胶已经制备后,它易于被催化并浇铸在碳纤维增强体中。将醋酸酐(3.15mol)加入该聚(酰胺酸)溶胶中,并于室温搅拌1小时。将吡啶(1.26mol)加入该溶液中。在凝胶化点之前(20分钟),将该溶液浇铸于碳纤维增强体中。形成PI凝胶后,将该湿凝胶纤维复合材料在60℃老化16小时,接着以乙醇冲洗以移除全部DMAC、未反应单体和残留催化剂。随后,对该湿凝胶纤维复合材料进行超临界CO2干燥以获得PI气凝胶碳纤维复合材料。
Claims (27)
1.一种气凝胶材料,具有:
a)密度为0.15g/cc或更小;
b)常温常压下的热导率为30mW/m-K或更低;以及
c)挠曲强度为150psi或更大。
2.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料在常温常压下的该热导率为25mW/m-K或更低。
3.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料在常温常压下的该热导率为20mW/m-K或更低。
4.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料具有在常温及10-5托真空下为5mW/m-K或更低的热导率。
5.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料的该挠曲强度为200psi或更大。
6.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料的该挠曲强度为250psi或更大。
7.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料具有5000psi或更大的挠曲模量。
8.如权利要求7所述的气凝胶材料,其特征在于,该气凝胶材料的该挠曲模量为20000psi或更大。
9.如权利要求7所述的气凝胶材料,其特征在于,该气凝胶材料的该挠曲模量为40000psi或更大。
10.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料包含聚酰亚胺气凝胶或其衍生物。
11.如权利要求1所述的气凝胶材料,其特征在于,该气凝胶材料是纤维增强气凝胶复合材料。
12.一种层压面板,包含:(a)具有至少两个主面的气凝胶层;(b)与该气凝胶层的至少一个主面相邻的表皮;以及(c)与该表皮相邻的反射层。
13.如权利要求12所述的面板,其特征在于,该面板通过至少一个边封在边缘处密封。
14.如权利要求12所述的面板,其特征在于,该面板包括与该气凝胶的第一主面相邻的第一表皮,以及与该气凝胶层的第二主面相邻的第二表皮。
15.如权利要求12所述的面板,其特征在于,该面板包括至少一个通气口,以及至少一个通气过滤器。
16.如权利要求13所述的面板,其特征在于,该边封包括至少一个通气口和至少一个通气过滤器。
17.如权利要求12所述的面板,其特征在于,该气凝胶层具有:
a)密度为0.15g/cc或更小;
b)常温常压下的热导率为30mW/m-K或更低;以及
c)挠曲强度为150psi或更大。
18.如权利要求17所述的面板,其特征在于,该气凝胶层在常温常压下的该热导率为25mW/m-K或更低。
19.如权利要求17所述的面板,其特征在于,该气凝胶层在常温常压下的该热导率为20mW/m-K或更低。
20.如权利要求17所述的面板,其特征在于,该气凝胶层具有在常温及10-5托真空下为5mW/m-K或更低的热导率。
21.如权利要求17所述的面板,其特征在于,该气凝胶层的该挠曲强度为200psi或更大。
22.如权利要求17所述的面板,其特征在于,该气凝胶层的该挠曲强度为250psi或更大。
23.如权利要求17所述的面板,其特征在于,该气凝胶层具有5000psi或更大的挠曲模量。
24.如权利要求23所述的面板,其特征在于,该气凝胶层的该挠曲模量为20000psi或更大。
25.如权利要求23所述的面板,其特征在于,该气凝胶层的该挠曲模量为40000psi或更大。
26.如权利要求17所述的面板,其特征在于,该气凝胶层包含聚酰亚胺气凝胶或其衍生物。
27.如权利要求17所述的面板,其特征在于,该气凝胶层是纤维增强气凝胶。
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WO2014197028A3 (en) | 2015-02-26 |
CN111136987A (zh) | 2020-05-12 |
BR112015021190B1 (pt) | 2021-10-05 |
CA2902538A1 (en) | 2014-12-11 |
AU2014275508A1 (en) | 2015-09-24 |
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US20230357504A1 (en) | 2023-11-09 |
US11760837B2 (en) | 2023-09-19 |
AU2014275508B2 (en) | 2017-02-02 |
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US10246554B2 (en) | 2019-04-02 |
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US20140255642A1 (en) | 2014-09-11 |
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CA2902538C (en) | 2018-05-01 |
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