CN113264771B - 一种快速制备高强度碳泡沫的方法 - Google Patents
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Abstract
一种快速制备轻质高强度碳泡沫的方法,其步骤为:步骤(1)将商用酚醛树脂与2000目粒径的石英粉机械搅拌30 min以上均匀混合;步骤(2)加入少量苯磺酸,作为固化剂,继续搅拌10 min左右混合均匀获得混合浆料;步骤(3)将混合浆料倒入圆柱形模具中,并在100℃的箱式电阻炉中固化2 h;步骤(4)固化后的泡沫胚体置于真空管式电阻加热炉中,真空度为‑0.1MPa,并以5~15℃/min的升温速率升至1000℃,保温3 h之后随炉冷却至室温,以完成泡沫胚体的炭化;步骤(5)炭化后的泡沫胚体置于HF酸中超声刻蚀48 h以上,以滤出石英模板,获得最终的碳泡沫产品。
Description
技术领域
本发明涉及无机多孔材料技术,具体是具低密度高强度特性的碳泡沫的制备技术。
背景技术
碳泡沫因其特殊的组织结构、低的密度、高的孔隙率、低的热膨胀系数、较大的比表面积、抗氧化性能优良、低成本、优异的吸声性能和电磁屏蔽性能等,被广泛应用于航空航天、核工业、超级电容器和催化剂载体等工业领域。
碳泡沫主要存在两种微观结构,一种是开放的网状玻璃态结构,另外一种是球形多孔结构。不同的结构赋予了其不同的特性,如网状玻璃态的碳泡沫一般呈现为开孔结构,开放的孔有利于发挥碳泡沫的吸附作用,此外还有如吸波等特性;而具有球形孔结构的碳泡沫更有利于导热、导电等特性的应用。
目前碳泡沫的发展主要利用它们的功能及结构性质,不论哪种类型的碳泡沫,经过无数次的改进与发展,但它们最显著的缺点是强度普遍较低,不同泡沫碳的结构和密度导致了力学性能的差异性。普通碳泡沫的压缩强度普遍较低,在作为结构或重载材料方面存在着严重的力学性能缺陷。换言之,就是由于多孔结构的特殊性质限制了高强度碳泡沫的发展,它们的广泛应用因此受到限制。此外,现有技术制备碳泡沫往往需要几十甚至上百小时,增加了制备成本。
发明内容
本发明的目的提供一种快速制备轻质高强度碳泡沫的方法。
本发明是一种快速制备轻质高强度碳泡沫的方法,其步骤为:
步骤(1)按照3:1、2:1、1:1和1:2四种比例,分别将商用酚醛树脂与2000目粒径的石英粉机械搅拌30 min以上均匀混合;
步骤(2)加入少量苯磺酸,作为固化剂,继续搅拌10 min左右混合均匀获得混合浆料;
步骤(3)将混合浆料倒入圆柱形模具中,并在100℃的箱式电阻炉中固化2 h;
步骤(4)固化后的泡沫胚体置于真空管式电阻加热炉中,真空度为-0.1MPa,并以5~15 ℃/min的升温速率升至1000℃,保温3 h之后随炉冷却至室温,以完成泡沫胚体的炭化;
步骤(5)炭化后的泡沫胚体置于HF酸中超声刻蚀48 h以上,以滤出石英模板,获得最终的碳泡沫产品。
本发明与现有技术相比有益效果为:
(1)本发明在制备过程中工艺路线简单,仅需要四步,极大的缩短了现有技术的制备周期;且对设备的严苛要求程度较小,仅需要箱式电阻炉和真空加热炉既可制备;制备碳泡沫的原材料成本较低且易于获得,无论在原材料还是工艺路线的设计,还是在设备条件上都极大的减少了制备成本。
(2)不同比例(酚醛树脂/石英模板)的泡沫胚体通过该工艺制备的碳泡沫密度分别为0.947 g/cm3、0.781 g/cm3、0.471 g/cm3和0.306 g/cm3,压缩强度分别为106.4 MPa、76.5 MPa、40.4 MPa和21.6 MPa,显著高于目前国内外现有研究相同密度水平的碳泡沫。
(3)本发明所制备的碳泡沫体积收缩率可控,且在等温炭化环境下样品的几何效应较小,因此可以达到定制产品的要求。
(4)本发明通过在不同树脂胚体中添加不同比重的石英模板,在树脂与固化剂比例一定的条件下,可以改变最终泡沫碳的孔径大小、孔径分布及孔隙率等,达到可控孔的目的。
附图说明
图1为碳泡沫的发明工艺流程图,图2为3:1固化后的泡沫生胚宏观形貌,图3为图2黄色方框的放大图,图4为2:1固化后的泡沫生胚宏观形貌,图5为图4黄色方框的放大图,图6为1:1固化后的泡沫生胚宏观形貌,图7为图6黄色方框的放大图,图8为1:2固化后的泡沫生胚宏观形貌,图9为图8黄色方框的放大图,图10为3:1炭后的泡沫胚体宏观形貌,图11为图10的放大图,图12为2:1炭后的泡沫胚体宏观形貌,图13为图12的放大图,图14为1:1炭后的泡沫胚体宏观形貌,图15为图14的放大图,图16为1:2炭后的泡沫胚体宏观形貌,图17为图16的放大图,图18为3:1碳泡沫的微观形貌,图19为图18中黄色方框中的放大图,图20为2:1碳泡沫的微观形貌,图21为图20中黄色方框中的放大图,图22为1:1碳泡沫的微观形貌,图23为图22中黄色方框中的放大图,图24为1:2碳泡沫的微观形貌,图25为图24中黄色方框中的放大图,图26为不同碳泡沫的压缩强度。
具体实施方式
如图1所示,本发明是一种快速制备轻质高强度碳泡沫的方法,其步骤为:
步骤(1)按照3:1、2:1、1:1和1:2四种比例,分别将商用酚醛树脂与2000目粒径的石英粉机械搅拌30 min以上均匀混合;
步骤(2)加入少量苯磺酸,作为固化剂,继续搅拌10 min左右混合均匀获得混合浆料;
步骤(3)将混合浆料倒入圆柱形模具中,并在100℃的箱式电阻炉中固化2 h;
步骤(4)固化后的泡沫胚体置于真空管式电阻加热炉中,真空度为-0.1MPa,并以5~15 ℃/min的升温速率升至1000℃,保温3 h之后随炉冷却至室温,以完成泡沫胚体的炭化;
步骤(5)炭化后的泡沫胚体置于HF酸中超声刻蚀48 h以上,以滤出石英模板,获得最终的碳泡沫产品。
依据GB/T 34559-2017有关规定,测试不同碳泡沫的压缩强度,待测试样几何尺寸为10 mm × 10 mm × 10 mm。
以上所述步骤(1)的机械混合不包括研磨,否则会破坏石英模板的晶型。步骤(1)机械混合为室温环境下搅拌不少于30 min。
以上所述步骤(2)加入固化剂后机械混合时间不宜超过20 min,持续搅拌有利于固化,但搅拌时间过长会导致固化成型不够均匀。
以上所述步骤(3)所述模压之后的混合浆料需在室温下自然静置24 h,使胚体定型。
以上所述步骤(4)炭化过程中的真空压力变化误差为±0.01 MPa。
以上所述步骤(5)超声刻蚀的过程中需要每10个小时更换一次滤出液,高饱和度的滤出液难以滤出残余模板,因此需要及时更换。
从图2~图9的不同比例碳泡沫生胚图可以看出,固化过程中所形成的球形孔随着石英浓度的增大而减小,并且孔径逐渐变的均匀。
图8宏观形貌呈现为红白相间的颜色分布主要是由于石英的浓度增大,导致树脂粘度减小,机械混合难度增大,固化前的生胚浆料不够均匀导致的。
从图13~图19中不同比例炭化后的碳泡沫胚体图可以看出,碳化过程的进行会导致样品均匀收缩,而石英浓度越大,体积收缩率越小,同时球形孔体积也相应减小。
从图18~图25不同比例碳泡沫微观结构可以看出,胚体中石英浓度增大,球形孔孔径减小,孔径分布逐渐均匀,孔壁变薄,柱状韧带变细,镶嵌在韧带内部的球形闭孔减少。
从图26不同比例碳泡沫的压缩性能柱状图可以看出,胚体中石英浓度增大,密度、压缩强度和比压缩强度均呈线性降低,但就任一密度条件下的碳爬模,均有着其独特的性能优势。
本发明工艺流程如图1所示,以下结合具体实例来详细说明本发明的制备工艺。
实施例1:
(1)制备树脂与石英比重为3:1的碳泡沫,首先准备热固性的酚醛树脂15 g(粘度:16000~19000 MP/25℃;残炭率:40~45%;纯度:99%),粒径为2000目的石英粉5 g(主要成分:SiO2,纯度:99%),石英粉在100℃的箱式电阻炉中干燥1 h后备用;
(2)将酚醛树脂倒入研钵中,缓慢加入石英粉,并持续搅拌,搅拌约30 min以上停止搅拌,加入微量的固化剂(苯磺酸),继续搅拌8~10 min至混合浆料为粘稠状,将调配好的混合浆料倒入预制的圆柱形模具中;
(3)将预制的胚体浆料置于室温环境下的空气中,静置24 h至胚体浆料固化定型;
(4)将固化后的泡沫胚体置于箱式电阻加热炉中,并升温至100℃,保持2 h之后随炉自然冷却至室温,完成泡沫生胚的最终固化过程;
(5)固化后的泡沫胚体通过砂轮机和砂纸等将毛边和表面打磨平整,之后将胚体置于管式电阻加热炉中,以10 ℃/min的升温速率从室温快速加热至1000℃,保持3 h,之后结束升温程序随炉冷却至室温,完成胚体的炭化过程;
(6)将炭化后的泡沫胚体表面打磨平整,完全浸入滤出液HF酸中,浸泡约48 h以上,其中每隔6 h更换一次HF酸,并在超声波清洗仪中超声振荡15 min;
(7)完成滤出工艺的碳泡沫首先通过无水乙醇超声清洗15 min,并反复操作3次,最终制备出3:1(酚醛树脂:石英粉)的碳泡沫。
经测试,采用该工艺制备的碳泡沫密度为0.947 g/cm3,压缩强度为106.4 MPa,比压缩强度为112.35 MPa·cm3/g。
实施例2:
(1)制备树脂与石英比重为1:1的碳泡沫,首先准备热固性的酚醛树脂10 g(粘度:16000~19000 MP/25℃;残炭率:40~45%;纯度:99%),粒径为2000目的石英粉10 g(主要成分:SiO2,纯度:99%),石英粉在100℃的箱式电阻炉中干燥1 h后备用;
(2)将酚醛树脂倒入研钵中,缓慢加入石英粉,并持续搅拌,搅拌约30 min以上停止搅拌,加入微量的固化剂(苯磺酸),继续搅拌8~10 min至混合浆料为粘稠状,将调配好的混合浆料倒入预制的圆柱形模具中;
(3)将预制的胚体浆料置于室温环境下的空气中,静置24 h至胚体浆料固化定型;
(4)将固化后的泡沫胚体置于箱式电阻加热炉中,并升温至100℃,保持2 h之后随炉自然冷却至室温,完成泡沫生胚的最终固化过程;
(5)固化后的泡沫胚体通过砂轮机和砂纸等将毛边和表面打磨平整,之后将胚体置于管式电阻加热炉中,以10 ℃/min的升温速率从室温快速加热至1000℃,保持3 h,之后结束升温程序随炉冷却至室温,完成胚体的炭化过程;
(6)将炭化后的泡沫胚体表面打磨平整,完全浸入滤出液HF酸中,浸泡约48 h以上,其中每隔6 h更换一次HF酸,并在超声波清洗仪中超声振荡15 min;
(7)完成滤出工艺的碳泡沫首先通过无水乙醇超声清洗15 min,并反复操作3次,最终制备出1:1(酚醛树脂:石英粉)的碳泡沫。
经测试,采用该工艺制备的碳泡沫密度为0.471 g/cm3,压缩强度为40.4 MPa,比压缩强度为85.77 MPa·cm3/g。
本发明未详细说明部分属于本领域技术人员公知常识。
Claims (6)
1.一种快速制备高强度碳泡沫的方法,其特征在于,其步骤为:
步骤(1)分别按照3:1、2:1、1:1、1:2四种比例,将商用酚醛树脂与2000目粒径的石英粉机械搅拌30 min以上均匀混合;
步骤(2)加入少量苯磺酸,作为固化剂,继续搅拌10 min混合均匀获得混合浆料;
步骤(3)将混合浆料倒入圆柱形模具中,并在100℃的箱式电阻炉中固化2 h;
步骤(4)固化后的泡沫生胚置于真空管式电阻加热炉中,真空度为-0.1MPa,并以5~15℃/min的升温速率升至1000℃,保温3 h之后随炉冷却至室温,以完成泡沫胚体的炭化;
步骤(5)炭化后的泡沫胚体置于HF酸中超声刻蚀48 h以上,以溶解沥出石英模板,获得最终的碳泡沫产品。
2.根据权利要求1所述的快速制备高强度碳泡沫的方法,其特征在于,所述步骤(1)的机械混合不包括研磨。
3.根据权利要求1所述的快速制备高强度碳泡沫的方法,其特征在于,所述步骤(1)机械混合为室温环境下搅拌不少于30 min。
4.根据权利要求1所述的快速制备高强度碳泡沫的方法,其特征在于,所述步骤(2)加入固化剂后机械混合时间不超过20 min,持续搅拌有利于固化。
5.根据权利要求1所述的快速制备高强度碳泡沫的方法,其特征在于,步骤(3)将混合浆料倒入圆柱形模具后,将其置于室温环境下的空气中,静置24h至胚体浆料固化成型。
6.根据权利要求1所述的快速制备高强度碳泡沫的方法,其特征在于,步骤(5)所述超声刻蚀的过程中需要每10个小时更换一次溶解液。
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