CN106747628B - 一种耐高温泡沫增强SiO2气凝胶绝热材料及其制备方法 - Google Patents
一种耐高温泡沫增强SiO2气凝胶绝热材料及其制备方法 Download PDFInfo
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Abstract
一种耐高温泡沫增强SiO2气凝胶绝热材料及其制备方法,其特征在于,所述的耐高温增强SiO2气凝胶绝热材料包括碳泡沫增强体、网格状碳化硅纳米线、SiO2气凝胶,网格状碳化硅纳米线填充分割碳泡沫内部孔隙空间,SiO2气凝胶均匀填充于碳泡沫增强体,密度为0.05~0.15g/cm3,孔隙率大于90%。碳泡沫增强体为柔性碳泡沫,由三聚氰胺泡沫高温热解得到,网格状碳化硅纳米线,直径为50~20nm。化学气相沉积制备碳化硅‑碳复合泡沫,采用常压干燥技术制备SiO2气凝胶进而得到耐高温泡沫增强SiO2气凝胶绝热材料。本发明具有的优点:1、网状SiC纳米线支撑碳骨架,提高复合材料力学性能;2、碳化硅纳米线降低泡沫孔径,降低材料的热导率;3、复合材料整体密度超低。
Description
技术领域
本发明涉及一种绝热材料及其制备方法,特别涉及一种耐高温泡沫增强SiO2气凝胶绝热材料及其制备方法。
背景技术
气凝胶是近年来受到广泛关注的一类多孔隔热材料。气凝胶的固相骨架由纳米颗粒交联而成,孔径在几纳米至几十纳米之间,具有很高的比表面积,最常见的气凝胶有SiO2、Al2O3及炭气凝胶等。由于气凝胶具有独特的纳米结构,其热传导路径均被明显抑制,具有极低的热导率,目前SiO2气凝胶是导热系数最低的气凝胶材料,因此,SiO2气凝胶的室温热导率可低至0.012~0.020W/m·K,比传统隔热材料的性能优异。虽然SiO2气凝胶材料的热导率很低,但是存在高脆性和低强度缺陷,极大地限制了SiO2气凝胶的实际应用。因此将气凝胶与无机物或有机物进行复合或交联,可以制备具有较好力学和隔热、磁学、催化等性能的复合 SiO2气凝胶材料,但密度和导热系数也会有所增大。
柔性泡沫碳是一种碳素骨架和相互连通的孔腔组成的具有三维网状结构的轻质多孔材料,碳原子之间以一定的成键方式相互连接,密度约为5~10mg/cm3。柔性泡沫碳具有密度低、热性能优异、热导率低等优点,既是一种极具潜力的隔热材料。但柔性泡沫碳抗压强度低,在严苛、复杂的气动环境可靠性难以保证,因此,需要通过改性提高柔性碳泡沫的抗压性能。碳化硅因具有优良的热稳定性和化学稳定性,可在高达1000℃以上温度工作,并且在氧化、还原等高温环境下具有很好的抗腐蚀性、强度保持率。碳化硅晶须由于其特殊尺寸效应,其导热系数比块体低了许多,同时在柔性碳泡沫内部大孔隙填充碳化硅晶须不仅可以提高碳泡沫力学性能,并且内部孔径缩小从而降低导热系数,可以作为SiO2气凝胶的增强体。
申请号为201410157562.7的中国发明专利公开了一种弹性碳泡沫氧气还原催化剂及其制备方法,其特征在于该弹性碳泡沫氧气还原剂是在含微量氧条件下,直接高温碳化三聚氰胺泡沫材料制备而成,通过该方法制备的弹性碳泡沫具有自支撑的三维网络结构、良好的回弹性,优异的氧气还原催化性能,并且其氧气还原性能和弹性可以通过调节微氧的浓度来调控。该专利是采用三聚氰胺泡沫热解得到碳泡沫应用于氧气还原催化剂载体,与本专利应用领域不相同,因此制备工艺以及材料结构存在较大的差异。
申请号为201410743407.3的中国发明专利公开了一种耐高温高强度SiC包覆碳泡沫复合隔热材料及其制备方法,其特征在于该耐高温高强度SiC包覆碳泡沫复合隔热材料是一种由碳泡沫和碳化硅气凝胶构成;其空气气氛中耐温性在690~700℃,比纯碳泡沫材料提高了约 100℃,表观密度在0.4~0.6g/cm3,抗压强度在11~15MPa,室温热导率在0.4~0.6W/(m.K)。其制备方法是二氧化硅溶胶注入到碳泡沫材料的孔洞中,经过溶胶-凝胶、老化和干燥得到碳泡沫增强的氧化硅气凝胶复合隔热材料,然后在惰性氛围保护下进行高温热处理,从而制备出一种耐高温高强度SiC包覆碳泡沫复合隔热材料。该发明具有用料简单和工艺简捷的优点,工艺过程操作简单,容易实现规模生产。但是该制备方法得到的SiC包覆材料结构疏松,致密性差,并且导热系数很高,密度较大。
发明内容
本发明要解决的技术问题是克服现有技术的不足,旨在提供一种耐高温泡沫增强SiO2气凝胶绝热材料,其特征在于,所述的耐高温增强SiO2气凝胶绝热材料包括碳泡沫增强体、网格状碳化硅纳米线、SiO2气凝胶,网格状碳化硅纳米线填充分割碳泡沫内部孔隙空间,SiO2气凝胶均匀填充于碳泡沫增强体,密度为0.05~0.15g/cm3,孔隙率大于90%。碳泡沫增强体为柔性碳泡沫,由三聚氰胺泡沫高温热解得到,网格状碳化硅纳米线,直径为50~200nm。
本发明旨在提供一种耐高温泡沫增强SiO2气凝胶绝热材料的制备方法,其特征在于,包括以下顺序步骤:
(1)将三聚氰胺泡沫热解得到的柔性泡沫碳浸入无水乙醇中,超声振荡清洗10~30min,取出后烘箱中100~120℃烘干备用;
(2)将六水硝酸镍、无水乙醇按照1∶(10~50)的摩尔比配制硝酸镍溶液;
(4)碳泡沫浸入硝酸镍溶液中,浸渍4~10h;
(5)浸渍结束后烘干,放入气相沉积炉中,化学气相沉积碳化硅纳米线,以三氯甲基硅烷为碳化硅气源,氢气为载气,氩气作为稀释气体,沉积温度900~1100℃,沉积时间为1~3h,形成碳化硅-碳复合泡沫材料;
(6)采用氧化硅质量分数含量为10~20%的硅溶胶为SiO2气凝胶硅源,将去离子水∶无水乙醇∶硅溶胶按体积分数比为(1~1.5)∶(0.5~1)∶1混合搅拌,将碳化硅-碳复合泡沫浸入混合液中,调节PH至6~8进行胶凝反应;
(7)胶体进行老化,老化液为正硅酸乙酯与无水乙醇的混合液,正硅酸乙酯与无水乙醇体积比为1∶2~5,老化时间30~50h;
(8)经过溶剂置换-表面修饰-溶剂置换后,得到复合泡沫增强的SiO2湿凝胶;
(9)常压下梯度干燥,梯度干燥工艺为60~80℃保温1~2h,90~100℃保温1~2h,120~140℃保温1~2h,即可得到耐高温泡沫增强SiO2气凝胶绝热材料。
本发明具有的优点:1、网状SiC纳米线支撑碳骨架,提高复合材料力学性能;2、碳化硅纳米线降低泡沫孔径,降低材料的热导率;3、复合材料整体密度超低。
附图说明
图1为耐高温增强SiO2气凝胶绝热材料结构示意图
[10]为柔性碳泡沫;[20]为碳化硅晶须;[30]为SiO2气凝胶。
具体实施方式
下面结合具体实施例,进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定。
实施例1
(1)将三聚氰胺泡沫热解得到的柔性泡沫碳浸入无水乙醇中,超声振荡清洗30min,取出后烘箱中100℃烘干备用;
(2)将六水硝酸镍、无水乙醇按照1∶20的摩尔比配制硝酸镍溶液;
(4)碳泡沫浸入硝酸镍溶液中,浸渍10h;
(5)浸渍结束后烘干,放入气相沉积炉中,化学气相沉积碳化硅纳米线,以三氯甲基硅烷为碳化硅气源,氢气为载气,氩气作为稀释气体,沉积温度1100℃,沉积时间为2h,形成碳化硅-碳复合泡沫材料;
(6)采用氧化硅质量分数含量为15%的硅溶胶为SiO2气凝胶硅源,将去离子水∶无水乙醇∶硅溶胶按体积分数比为1.5∶1∶1混合搅拌,将碳化硅-碳复合泡沫浸入混合液中,调节PH至7进行胶凝反应;
(7)胶体进行老化,老化液为正硅酸乙酯与无水乙醇的混合液,正硅酸乙酯与无水乙醇体积比为1∶2,老化时间40h;
(8)经过溶剂置换-表面修饰-溶剂置换后,得到复合泡沫增强的SiO2湿凝胶;
(9)常压下梯度干燥,梯度干燥工艺为80℃保温1h,100℃保温2h,120℃保温2h,即可得到耐高温泡沫增强SiO2气凝胶绝热材料。
实施例2
(1)将三聚氰胺泡沫热解得到的柔性泡沫碳浸入无水乙醇中,超声振荡清洗30min,取出后烘箱中100℃烘干备用;
(2)将六水硝酸镍、无水乙醇按照1∶10的摩尔比配制硝酸镍溶液;
(4)碳泡沫浸入硝酸镍溶液中,浸渍10h;
(5)浸渍结束后烘干,放入气相沉积炉中,化学气相沉积碳化硅纳米线,以三氯甲基硅烷为碳化硅气源,氢气为载气,氩气作为稀释气体,沉积温度1100℃,沉积时间为2h,形成碳化硅-碳复合泡沫材料;
(6)采用氧化硅质量分数含量为15%的硅溶胶为SiO2气凝胶硅源,将去离子水∶无水乙醇∶硅溶胶按体积分数比为1.5∶1∶1混合搅拌,将碳化硅-碳复合泡沫浸入混合液中,调节PH至7进行胶凝反应;
(7)胶体进行老化,老化液为正硅酸乙酯与无水乙醇的混合液,正硅酸乙酯与无水乙醇体积比为1∶2,老化时间40h;
(8)经过溶剂置换-表面修饰-溶剂置换后,得到复合泡沫增强的SiO2湿凝胶;
(9)常压下梯度干燥,梯度干燥工艺为80℃保温1h,100℃保温2h,120℃保温2h,即可得到耐高温泡沫增强SiO2气凝胶绝热材料。
上述仅为本发明的两个具体实施方式,但本发明的设计构思并不局限于此,凡利用此构思对本发明进行非实质性的改动,均应属于侵犯本发明保护的范围的行为。但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何形式的简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (4)
1.一种耐高温泡沫增强SiO2气凝胶绝热材料,其特征在于,所述的耐高温泡沫增强SiO2气凝胶绝热材料包括碳泡沫增强体、网格状碳化硅纳米线、SiO2气凝胶,网格状碳化硅纳米线填充分割碳泡沫内部孔隙空间,SiO2气凝胶均匀填充于碳泡沫增强体,密度为0.05~0.15g/cm3,孔隙率大于90%。
2.根据权利要求1所述的耐高温泡沫增强SiO2气凝胶绝热材料,其特征在于,所述的碳泡沫增强体为柔性碳泡沫,由三聚氰胺泡沫高温热解得到。
3.根据权利要求1所述的耐高温泡沫增强SiO2气凝胶绝热材料,其特征在于,所述的网格状碳化硅纳米线,直径为50~200nm。
4.一种耐高温泡沫增强SiO2气凝胶绝热材料的制备方法,其特征在于,包括以下顺序步骤:
(1)将三聚氰胺泡沫热解得到的柔性碳泡沫浸入无水乙醇中,超声振荡清洗10~30min,取出后烘箱中100~120℃烘干备用;
(2)将六水硝酸镍、无水乙醇按照1∶(10~50)的摩尔比配制硝酸镍溶液;
(4)碳泡沫浸入硝酸镍溶液中,浸渍4~10h;
(5)浸渍结束后烘干,放入气相沉积炉中,化学气相沉积碳化硅纳米线,以三氯甲基硅烷为碳化硅气源,氢气为载气,氩气作为稀释气体,沉积温度900~1100℃,沉积时间为1~3h,形成碳化硅-碳复合泡沫材料;
(6)采用氧化硅质量分数含量为15%的硅溶胶为SiO2气凝胶硅源,将去离子水∶无水乙醇∶硅溶胶按体积分数比为(1~1.5)∶(0.5~1)∶1混合搅拌,将碳化硅-碳复合泡沫浸入混合液中,调节pH 至6~8进行胶凝反应;
(7)胶体进行老化,老化液为正硅酸乙酯与无水乙醇的混合液,正硅酸乙酯与无水乙醇体积比为1∶2~5,老化时间30~50h;
(8)经过溶剂置换-表面修饰-溶剂置换后,得到复合泡沫增强的SiO2湿凝胶;
(9)常压下梯度干燥,梯度干燥工艺为60~80℃保温1~2h,90~100℃保温1~2h,120~140℃保温1~2h,即可得到耐高温泡沫增强SiO2气凝胶绝热材料。
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