CN115232341B - 一种兼具低吸收比和高发射率的轻质柔性隔热材料及其制备方法 - Google Patents
一种兼具低吸收比和高发射率的轻质柔性隔热材料及其制备方法 Download PDFInfo
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Abstract
本发明公开一种兼具低吸收比和高发射率的轻质柔性隔热材料,所述隔热材料的结构中包含镀金属聚合物膜和位于其上的聚合物树脂层;所述聚合物树脂层中掺杂有中空微球;所述中空微球为双层球壳结构,其中,内层球壳为硅酸盐玻璃层,外层球壳为由彼此独立的颗粒状二氧化钛形成的层。该隔热材料可克服多层隔热结构的隔热单元中的间隔物自身性能不足的问题。本发明还公开了该隔热材料的制备方法。
Description
技术领域
本发明涉及隔热复合材料技术领域。更具体地,涉及一种兼具低吸收比和高发射率的轻质柔性隔热材料及其制备方法。
背景技术
随着社会的发展和科学技术的进步,人类的能源损耗日渐增大,能源危机逐渐凸显。发展高性能隔热材料无论对于人民日常生产生活和高技术装备都具有重要意义。通常而言,隔热保温(节能)材料包括有机泡沫、无机多孔材料、隔热涂料、隔热粉体、热反射屏等不同形式。尽管综合考虑材料的性能、施工难度、成本和耐候性,不同的应用领域对隔热材料有不同的要求,但在设备轻量化、环境友好和低成本化发展的大趋势下,各领域应用的隔热材料对于隔热性能和密度的协同设计提出了越来越高的要求。尤其对于对材料重量有着更为苛刻要求的航空航天领域更是如此。以航天器为例,航天器在高空甚至深空运行时会在受到太阳光的直接照射是面临高温,同时在远离太阳的深远空又会面对极低的温度。因此,为保障航天器内设备的正常运转和生命体生命活动的进行,须对航天器进行专门的热设计。这其中被动式热控材料和构件以其性能稳定,无需额外能耗等优点获得了广泛应用。
对于真空环境下的应用场合而言,材料的气体对流导热可以忽略,热量传输的主要途径是接触导热和辐射传热。随着人类的脚步迈向更深远的宇宙空间,火箭在太空环境下所运行的时间更长,这对于航天器的有效燃料载荷提出了更高要求。鉴于此,无论对于航天器内部设备和生命体的正常运转,还是航天器低温液体推进剂的高效保存而言,航天器被动式隔热材料都需要一方面保证优异的隔热效果,一方面尽可能降低自身重量。为此,研究人员广泛地将多层隔热结构引入航天器绝热设计中。顾名思义,多层隔热结构是有基本的隔热单元叠加而成,其个人单元由具有高反射能力的反射材料(反射屏)和间隔层材料(间隔物)组成。其中低吸收比和低发射率的反射屏用于对辐射热流的阻隔,而间隔物的作用是将多层反射屏彼此分隔,避免因反射屏的直接搭接导致过大的接触热导。经过长期研究和应用验证,多层隔热结构被认为在太空环境下具有最优的隔热效果。
对于多层隔热结构而言,其隔热效果通常可通过增加反射屏的层数进行增强,但反射屏层数的增加会导致整个隔热结构的重量增大。同时,过多的层数也会增加隔热结构的制作和施工难度。例如,目前,多层隔热结构中的反射屏和间隔物是分开或组合在一起的两部分,制备组件时进行交替叠加;而对于隔热结构的性能调控而言,实现方法通常为调整反射屏的层数以及反射屏和间隔物的比例。然而,隔热材料自身性能的不足限制了多层隔热结构的设计和调控空间。
因此,亟需设计新颖的多层隔热结构以增强隔热效果、降低密度、简化使用难度。目前为止,研究人员已经将多种不同的结构和材料用于多层隔热结构的隔热单元设计和制备中。但是目前报道的材料和结构仍存在密度偏高、制备过程繁琐、性能不佳等问题,因此仍需从个人单元的基础材料入手,设计新材料和新结构以进一步降低密度、增强性能。
发明内容
基于以上问题,本发明的第一个目的在于克服多层隔热结构的隔热单元中的间隔物自身性能不足的问题,提供一种兼具低吸收比和高发射率的轻质柔性隔热材料。该隔热材料中,聚合物树脂层可在作为反射屏的镀金属聚合物膜表面原位成型,获得性能可控的一体化隔热单元。
本发明的另一个目的在于提供一种兼具低吸收比和高发射率的轻质柔性隔热材料的制备方法。
为达到上述第一个目的,本发明采用下述技术方案:
一种兼具低吸收比和高发射率的轻质柔性隔热材料,所述隔热材料的结构中包含镀金属聚合物膜和位于其上的聚合物树脂层;所述聚合物树脂层中掺杂有中空微球;
所述中空微球为双层球壳结构,其中,内层球壳为硅酸盐玻璃层,外层球壳为由彼此独立的颗粒状二氧化钛形成的层。
该隔热材料中,中空微球特有的密闭-颗粒点阵复合球壳结构既可以通过空腔降低密度,又可以通过密闭球壳避免空腔内部气体对流导致传热,还可以通过最外侧的颗粒膜结构减少微球间的接触,增大接触热阻。该中空微球间隔物具有密度低、隔热性能好的特点(间隔物自身密度0.5-1.0g/cm3,导热系数0.06-0.12W/m·K)。
进一步地,所述隔热材料为所述镀金属聚合物膜和聚合物树脂层交替设置的多层结构;优选地,所述镀金属聚合物膜和聚合物树脂层的层数均为2层或以上。
进一步地,所述镀金属聚合物膜为单面或双面镀金属的聚合物膜,膜的厚度为6-30微米。本发明的技术方案中,对镀金属聚合物膜的选择没有其他要求,为镀有金属的聚合物膜即可。示例性的镀金属聚合物膜包括但不限于为镀铝聚酯膜等。
进一步地,所述中空微球的密度为0.3-1.2g/cm3,粒径5-120微米。
进一步地,所述中空微球中,内层球壳的厚度为300-1500纳米,外层球壳的厚度为50-1000纳米。
进一步地,所述隔热材料中,中空微球的体积百分数为30-70%。
进一步地,所述聚合物树脂层为由包含所述中空微球和聚合物树脂的原料经固化后得到。可以理解,固化的方式为采用固化剂进行固化,也即,原料中还包含固化剂。本发明中对具体固化剂的选择没有要求,可根据具体聚合物树脂的种类来进行具体选择。
进一步地,所述聚合物树脂选自可固化的、且固化前为可流动状态,或加溶剂稀释后可流动状态的树脂。
进一步地,所述聚合物树脂选自环氧树脂、不饱和聚酯树脂、酚醛树脂、聚氨酯树脂、聚苯乙烯中的一种或几种。
进一步地,所述原料中,还包含选自偶联剂、选自固化剂、促进剂、表面活性剂、稀释剂中的一种或几种的助剂。
进一步地,当助剂中包含偶联剂时,所述偶联剂的添加量为聚合物树脂含量的0.1-1wt%。
进一步地,所述偶联剂为硅烷偶联剂,包括但不限于选自、KH550、KH560、KH570、KH590中的一种或几种。
具体的助剂例如固化剂、促进剂、表面活性剂的选择和用量本领域技术人员可根据实际情况选择。以环氧树脂为例,所述固化剂包括但不限于为甲基四氢苯酐;所述促进剂包括但不限于为N,N-二甲基苄胺;所述稀释剂包括但不限于为脂肪醇二缩水甘油醚(V22)。
进一步地,所述制备方法包括如下步骤:
将聚合物树脂、助剂混匀,得树脂前驱体;
将树脂前驱体与中空微球混匀,得混合物;
将该混合物施加于镀金属聚合物膜表面;
固化,得所述轻质柔性隔热材料。
进一步地,所述中空微球由包括如下步骤的方法制备得到:
在硅酸盐中空玻璃微球表面包覆二氧化钛前驱体,得前驱体中空微球;
将所述前驱体中空微球在空气气氛中于600-800℃温度进行热处理,得所述中空微球。进一步地,在硅酸盐中空玻璃微球表面包覆二氧化钛前驱体的方法包括如下步骤:
1)将脲溶于水中溶解,将硅酸盐中空玻璃微球加入到前述溶液中,放入到油浴中加热同时进行机械搅拌;
2)将Ti(SO4)2水溶液滴加入步骤1)中得到的脲与中空微球的混合液中,Ti(SO4)2溶液全部滴加完毕后,继续保持温度并机械搅拌;最后,反应结束后,将中空微球进行过滤并烘干,得前驱体中空微球。
进一步地,将混合物施加于镀金属聚合物膜表面的方式包括3D打印、丝网印刷、辊涂、喷涂、刮涂、点胶、漏印中一种或多种。
本发明的有益效果如下:
本发明中提供的轻质柔性隔热材料中,通过中空微球的外侧球壳结构设计对其热传导性进行控制,并进而提高基于该中空微球的隔热材料的性能;通过中空微球的双球壳双组份复合,降低隔热材料的太阳吸收比和红外发射率;通过选择不同的中空微球粒径和球壳厚度,可以方便地调控所得中空微球的性能;进一步结合对中空微球在复合材料中的体积比例和树脂基体设计,可得到不同密度、力学性能和热性能的系列化隔热材料,进而很好的用于轻质柔性隔热材料领域中。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细的说明。
图1示出本发明中的中空微球的结构示意图。
图2示出本发明中的基于中空微球的复合材料的结构示意图。
图3示出本发明中的隔热材料的制备流程示意图。
图4示出实施例1所用中空复合微球的SEM照片。
图5示出实施例1所用中空复合微球的XRD图。
图6示出实施例1所得基于中空微球的隔热材料的照片。
图7示出实施例1所得基于中空微球的隔热材料的隔热单元。
具体实施方式
为了更清楚地说明本发明,下面结合优选实施例和附图对本发明做进一步的说明。附图中相似的部件以相同的附图标记进行表示。本领域技术人员应当理解,下面所具体描述的内容是说明性的而非限制性的,不应以此限制本发明的保护范围。
实施例1
本实施例的双球壳中空微球制备过程如下:
(1)选用密度为0.25g/cm3的商用中空玻璃微球与水以体积比1:5混合,搅拌均匀,静置分层后取上层漂浮材料,过滤,60℃烘干;秤取30g前述中空玻璃微球,放入1000mL三孔烧瓶中,将0.3mol的脲溶于400ml水中,加入到三孔烧瓶中,然后将烧瓶放入到80℃的油浴中,并进行机械搅拌;将12%的(质量分数)的Ti(SO4)2溶液150mL,转移至恒压分液漏斗中,控制滴加速度,使Ti(SO4)2溶液在50min内加入到脲与中空微球的混合液中,全部滴加完毕后,继续保持温度并持续机械搅拌2h;反应结束后,将得到的中间体中空微球进行过滤,60℃烘干;将复合中空微球放入马弗炉中,在空气气氛中于630℃下热处理8h,得到双球壳中空微球,密度为0.28g/cm3。
(2)所选用的树脂基体为E-51还原树脂,固化剂为聚醚胺。本实施例中双球壳中空复合微球-聚合物复合材料的制备过程如下:称取30g环氧树脂,和13g中空微球,充分混合;另称取70份固化剂,0.5g促进剂N,N-二甲基苄胺,1g偶联剂KH550,33g中空微球,充分混合。然后将上述两种混合物料搅拌均匀,得到复合材料前驱体。将前述前驱体置于模具上,用刮涂方式将前驱体涂布到6微米厚的双面镀铝聚酯膜表面,分别于70℃和110℃热处理2小时,固化。
(3)最后,用水清洗,除去多余的中空玻璃微球及灰尘,并放入真空干燥箱中烘干,即得基于双球壳中空微球的轻质柔性隔热材料。按照上述方法制备的双球壳中空微球-聚合物复合材料内部中空微球的体积占比为56%,隔热材料面密度为17.1g/m2,太阳吸收比为0.12,红外发射率为0.11。
实施例2-9中的隔热膜具体实施步骤按实施例1进行,具体区别条件及得到的复合材料的性能参数如表1所示:
表1实施例2-9中基于中空复合微球间隔物的隔热膜的制备条件和性能参数
注:
(a)中空玻璃微球为商品微球或参照专利201210056295.5“一种空心玻璃微球软化学制备方法和所制空心玻璃微球及其应用”自制;
(b)太阳吸收比参照标准GJB 2502.2-2006“航天器热控涂层试验方法第2部分:太阳吸收比测试”测试;
(c)红外发射率参照标准GJB 5023.2-2003“材料和涂层反射率和发射率测试方法第2部分:发射率”测试。
显然,本发明的上述实施例仅仅是为清楚地说明本发明所作的举例,而并非是对本发明的实施方式的限定,对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动,这里无法对所有的实施方式予以穷举,凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (6)
1.一种兼具低吸收比和高发射率的轻质柔性隔热材料,其特征在于,所述隔热材料的结构中包含镀金属聚合物膜和位于其上的聚合物树脂层;所述聚合物树脂层中掺杂有中空微球;
所述中空微球为双层球壳结构,其中,内层球壳为硅酸盐玻璃层,外层球壳为由彼此独立的颗粒状二氧化钛形成的层;
所述中空微球的密度为0.3-1.2g/cm3,粒径5-120微米;
所述中空微球中,内层球壳的厚度为300-1500纳米,外层球壳的厚度为50-1000纳米;
所述隔热材料中,中空微球的体积百分数为30-70%;
所述中空微球由包括如下步骤的方法制备得到:
在硅酸盐中空玻璃微球表面包覆二氧化钛前驱体,得前驱体中空微球;
将所述前驱体中空微球在空气气氛中于600-800℃温度进行热处理,得所述中空微球;
在硅酸盐中空玻璃微球表面包覆二氧化钛前驱体的方法包括如下步骤:
1)将脲溶于水中溶解,将硅酸盐中空玻璃微球加入到前述溶液中,放入到油浴中加热同时进行机械搅拌;
2)将Ti(SO4)2水溶液滴加入步骤1)中得到的脲与中空微球的混合液中,Ti(SO4)2溶液全部滴加完毕后,继续保持温度并机械搅拌;最后,反应结束后,将中空微球进行过滤并烘干,得前驱体中空微球;
所述聚合物树脂层由包含所述中空微球和聚合物树脂的原料经固化后得到;
所述聚合物树脂为硅橡胶和酚醛树脂中的一种。
2.根据权利要求1所述的轻质柔性隔热材料,其特征在于,所述镀金属聚合物膜为单面或双面镀金属的聚合物膜,膜的厚度为6-30微米。
3.根据权利要求1所述的轻质柔性隔热材料,其特征在于,所述原料中,还包含选自偶联剂、促进剂、表面活性剂、稀释剂中的一种或几种的助剂。
4.根据权利要求3所述的轻质柔性隔热材料,其特征在于,当助剂中包含偶联剂时,所述偶联剂的添加量为聚合物树脂含量的0.1-1wt%。
5.如权利要求1-4任一项所述的轻质柔性隔热材料的制备方法,其特征在于,包括如下步骤:
将聚合物树脂、助剂混匀,得树脂前驱体;
将树脂前驱体与中空微球混匀,得混合物;
将该混合物施加于镀金属聚合物膜表面;
固化,得所述轻质柔性隔热材料。
6.根据权利要求5所述的制备方法,其特征在于,将混合物施加于镀金属聚合物膜表面的方式包括3D打印、丝网印刷、辊涂、喷涂、刮涂、点胶、漏印中一种或多种。
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