CN108623309A - 一种氧化硅或氮化硅泡沫陶瓷材料的制备方法 - Google Patents

一种氧化硅或氮化硅泡沫陶瓷材料的制备方法 Download PDF

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CN108623309A
CN108623309A CN201810380379.1A CN201810380379A CN108623309A CN 108623309 A CN108623309 A CN 108623309A CN 201810380379 A CN201810380379 A CN 201810380379A CN 108623309 A CN108623309 A CN 108623309A
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foam
silicon
silicon nitride
sintered
slurry
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杨金龙
霍文龙
张笑妍
胡尊兰
任博
席小庆
王亚利
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New Mstar Technology Ltd (tianjin) New Mstar Technology Ltd
Tsinghua University
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Tsinghua University
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Abstract

本发明开发了一种泡沫单质硅及反应烧结低收缩氧化硅或氮化硅纳米纤维泡沫陶瓷材料的制备方法，该方法首次以单质颗粒制备了超稳定泡沫，进而通过反应烧结获得不同泡沫陶瓷产品。主要包括如下步骤：将工业级单质硅粉末球磨至粒径为0.1～4μm，将球磨后的单质硅配制成质量分数为10～40wt％的水基浆料。在上述浆料中添加表面活性剂，并调节悬浮体的pH至4～10。对浆料进行发泡得到超稳定的单质硅泡沫浆料，在常温常压下彻底干燥。将上述所得的硅泡沫坯体分别在含氧气的气氛或氮气气氛下烧结制备氧化硅泡沫陶瓷或氮化硅纳米线泡沫材料。本发明提供了一种泡沫单质硅的制备和应用方法，制备工艺简单，成本低，将泡沫单质硅在不同气氛的反应烧结可以制备多种泡沫陶瓷材料。

Description

一种氧化硅或氮化硅泡沫陶瓷材料的制备方法
技术领域
本发明涉及低收缩泡沫材料、反应烧结陶瓷材料、超稳定泡沫材料、纳米纤维材料的制备方法，具体涉及一种泡沫单质硅及反应烧结低收缩氧化硅和氮化硅纳米纤维泡沫陶瓷材料的制备方法。
背景技术
随着科技的发展，对材料性能要求的不断提高，具有三维纳米结构、超高比表面积、超轻的多孔材料应运而生，诸如碳纳米管气凝胶、聚合物泡沫、微格金属等。在多孔陶瓷制备工艺中，直接发泡法在获得高气孔率、闭孔结构的多孔陶瓷方面具有显著优势，且简便易行。近年来，研究人员采用表面活性剂对颗粒表面进行疏水改性，使其能够稳定吸附在气-液界面上，直接搅拌发泡得到超稳定泡沫，即颗粒稳定泡沫法。这种方法因工艺简单、生产成本低廉、环境友好被认为是一种有发展潜力的轻质高强泡沫陶瓷的制备方法。目前，颗粒稳定泡沫法中通常采用金属氧化物、金属非氧化物颗粒作为泡沫稳定剂，单质颗粒稳定泡沫制备多孔陶瓷研究较少；并且该方法大多用于制备具有闭孔结构的多孔陶瓷，孔壁通常为晶粒紧密堆积形成的微观形貌，一定程度上限制了在催化、过滤等领域的进一步发展。目前所有颗粒稳定泡沫法制备多孔陶瓷的研究都集中于化合物体系，如常见的氧化物体系、氮化物体系陶瓷，而以单质颗粒作为泡沫稳定介质的研究则尚未见报道。
发明内容
针对上述背景技术存在的问题，本发明开发了一种泡沫单质硅及反应烧结低收缩氧化硅或氮化硅纳米纤维泡沫陶瓷材料的制备方法。本发明创新性地采用单质硅颗粒作为泡沫稳定介质，将颗粒稳定泡沫法与反应烧结工艺相结合，以制备具有新型孔结构的高性能三维纳米结构Si3N4泡沫陶瓷以及低收缩氧化硅泡沫陶瓷。
本发明采用技术路线如下：
一种泡沫单质硅及反应烧结低收缩氧化硅或氮化硅纳米纤维泡沫陶瓷材料的制备方法，其特征在于，所述方法包括如下步骤：
(1)将工业级单质硅粉末球磨至粒径为0.1～4μm，将球磨后的单质硅配制成质量分数为10～40wt％的水基浆料，还可以加入铁、镍、铬的氧化物作为促进纳米线生长的催化剂，添加量为单质硅粉质量的0.5～2wt％，得到氮化硅纳米纤维陶瓷材料；
(2)在上述浆料中添加表面活性剂十二烷基三甲基溴化铵、十二烷基三甲基氯化铵、十六烷基三甲基溴化铵、十六烷基三甲基氯化铵中的一种或者任意复配，加入量为浆料质量的0.02～0.40wt％，pH调节至3.0～10.0。
(3)对浆料通过机械搅拌进行发泡得到超稳定的单质硅泡沫浆料，在常温常压下彻底干燥得到干坯。
(4)将上述所得的单质硅泡沫坯体在含氧气的气氛和纯氮气气氛下烧结制备氧化硅泡沫陶瓷或氮化硅泡沫材料。
硅泡沫坯体在含氧气的气氛下烧结时，所述气氛为氧气气氛或者空气气氛，优选纯氧气气氛，烧结制度为：以3～5℃/min升温速率加热至1000℃，然后以1～3℃/min升温速率加热至1300～1450℃，保温1～5h。在该工艺制度下可以制备氧化硅泡沫陶瓷。
硅泡沫坯体在氮气气氛下烧结时，烧结制度为：以10～30℃/min升温速率加热至1000℃，然后以3～10℃/min升温速率加热至1400～1600℃，保温0.3～5h，即可获得纳米线编织成型的氮化硅纳米纤维编织材料。
本发明以单质硅颗粒制备超稳定泡沫，并以此为原料进一步通过反应烧结制备多种泡沫材料，所制备的氧化硅泡沫陶瓷烧结线收缩率＜10％，所制备的氮化硅纳米线直径为40～150nm，长度为20～100μm。
本发明的有益效果是：①本方法通过简单的工艺制备了超稳定泡沫单质硅，通过不同烧结工艺可制备多种产品。②所制备的氧化硅泡沫陶瓷因为硅和氧气的反应产生体积膨胀在一定程度上抵消了烧结收缩，有利于近净尺寸成型。③该发明制备了氮化硅纳米线编织而成的泡沫结构材料，有望应用在过滤和隔热领域，该制备成本低廉。
附图说明
图1是本发明实施例1所用球磨后的单质硅颗粒SEM照片。
图2是本发明实施例1所制备的稳定泡沫坯体的宏观照片。
图3是本发明实施例1所制备的纳米纤维泡沫的SEM照片。
具体实施方式
下面结合实施例和附图，对本发明进一步详细说明。
实施例1
(1)将工业级单质硅粉末通过行星球磨机研磨至平均粒径为0.61μm，如图1所示。将球磨后的单质硅配制成质量分数为30wt％的水基浆料。
(2)在上述浆料中添加浆料质量0.08的wt％十二烷基三甲基溴化铵，pH调节至6.1。
(3)对浆料通过机械搅拌在2000rmp的转速进行发泡10min，得到超稳定的单质硅泡沫浆料，在常温常压下干燥2d得到干坯，如图2所示。
(4)将上述所得的硅泡沫坯体在0.1MPa氮气下烧结，以10℃/min升温速率加热至1000℃，然后以6℃/min升温至1600℃，保温20min，所制备的纳米纤维泡沫如图3所示。
上述实施例对本发明的技术方案进行了详细说明。显然，本发明并不局限于所描述的实施例。基于本发明中的实施例，熟悉本技术领域的人员还可据此做出多种变化，但任何与本发明等同或相类似的变化都属于本发明保护的范围。

Claims (8)

1.一种氧化硅或氮化硅泡沫陶瓷材料的制备方法，其特征在于，所述方法包括如下步骤：
(1)将工业级单质硅粉末球磨至粒径为0.1～4μm，将球磨后的单质硅配制成质量分数为10～40wt％的水基浆料；
(2)在步骤(1)所得浆料中添加表面活性剂，并将pH调节至3.0～10.0；
(3)在机械搅拌条件下对步骤(2)所得浆料进行发泡，得到单质硅泡沫；
(4)将步骤(3)所得浆料进行干燥，得到单质硅泡沫坯体；
(5)将步骤(4)所得单质硅泡沫坯体进行烧结得到氧化硅泡沫陶瓷或氮化硅纳米纤维陶瓷材料。
2.按照权利要求1所述的方法，其特征在于，步骤(2)中所述表面活性剂为十二烷基三甲基溴化铵、十二烷基三甲基氯化铵、十六烷基三甲基溴化铵、十六烷基三甲基氯化铵中的一种或者任意复配，加入量为浆料质量的0.02～0.40wt％。
3.按照权利要求1或2所述的方法，其特征在于，步骤(4)中所述干燥在常温常压下进行。
4.按照权利要求1或2所述的方法，其特征在于，步骤(5)中所述烧结在含氧气的气氛下进行，所述气氛为氧气气氛或者空气气氛，烧结工艺为：以3～5℃/min升温速率加热至1000℃，然后以1～3℃/min升温速率加热至1300～1450℃，保温1～5h，得到氧化硅泡沫陶瓷。
5.按照权利要求4所述的方法，其特征在于，所述氧化硅泡沫陶瓷的线收缩率＜10％。
6.按照权利要求1所述的方法，其特征在于，步骤(5)中所述烧结在氮气气氛下烧结，所述烧结工艺为：以10～30℃/min升温速率加热至1000℃，然后以3～10℃/min升温速率加热至1400～1600℃，保温0.3～5h，得到氮化硅纳米纤维陶瓷材料。
7.按照权利要求1或6所述的方法，其特征在于，步骤(1)中还添加铁、镍、铬的氧化物作为促进纳米线生长的催化剂，添加量为单质硅粉质量的0.5～2wt％，得到氮化硅纳米纤维陶瓷材料。
8.按照权利要求7所述的方法，其特征在于，所述氮化硅纳米纤维陶瓷材料的直径为40～150nm，长度为20～100μm。
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