注浆成型结合真空发泡法制备梯度多孔氮化硅陶瓷

doi:10.15541/jim20160077

无机材料学报 ›› 2016, Vol. 31 ›› Issue (8): 865-868.DOI: 10.15541/jim20160077

注浆成型结合真空发泡法制备梯度多孔氮化硅陶瓷

邓健^{1, 2}, 姚冬旭¹, 夏咏锋¹, 左开慧¹, 尹金伟¹, 曾宇平¹

(1. 中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海200050; 2. 中国科学院大学, 北京100049)

收稿日期:2016-02-01 修回日期:2016-03-28 出版日期:2016-08-20 网络出版日期:2016-07-20
作者简介:邓健(1989–), 男, 硕士研究生. E-mail: djmengwu@student.ustc.edu.cn
基金资助:
中国科学院上海硅酸盐研究所高性能陶瓷和超微结构国家重点实验室主任青年基金(SKL201401);青年科学基金(51501215)

Gradient Porous Silicon Nitride by Slip Casting and Vacuum Foaming

DENG Jian^{1, 2}, YAO Dong-Xu¹, XIA Yong-Feng¹, ZUO Kai-Hui¹, YIN Jin-Wei¹, ZENG Yu-Ping¹

(1. State Key Laboratory of High Performance Ceramics and Superfine Microstructures, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China; 2. University of Chinese Academy of Sciences, Beijing 100049, China)

Received:2016-02-01 Revised:2016-03-28 Published:2016-08-20 Online:2016-07-20
About author:DENG Jian. E-mail: djmengwu@student.ustc.edu.cn
Supported by:
Science Foundation for Youth Scholar of State Key Laboratory of High Performance Ceramics and Superfine Microstructures, Shanghai Institute of Ceramics, Chinese Academy of sciences (SKL201401);Youth Science Foundation (51501215)

摘要/Abstract

摘要：

通过注浆成型结合真空发泡制备出具有明显梯度结构的多孔氮化硅陶瓷。该工艺在浆料中加入发泡剂, 然后注入底部为石膏的模具中, 抽真空保压并恒温保存, 浆料在低压下会形成孔径梯度结构。研究发现, 气压对样品的梯度结构有较明显影响, 随着气压由80 kPa降低到9 kPa, 样品气孔率由59.01%提高到80.85%, 当气压为80 kPa时, 样品无宏观梯度结构, 随着气压的降低, 梯度结构趋于明显。压汞法测试表明, 9 kPa气压制备的样品孔径分布比较分散, 具有0.5、20、30、40、60、100和200 μm等多种气孔孔径值。该工艺具有简易、廉价, 孔径分布和气孔率可调的优点, 可实现大尺寸、复杂形貌材料的制备, 为梯度多孔材料的制备方法提供了新思路。

关键词: 梯度, 发泡, 多孔, 氮化硅

Abstract:

Gradient porous silicon nitride was fabricated by a combination method of slip casting and vacuum foaming. Firstly, foaming agent was added into Si₃N₄ aqueous slurry, then the uniformly stirred slurry was poured into the mold with plaster as base. Under low pressure and steady temperature, a green body with gradient pores was formed. Based on our research, the gradient structure and porosity were greatly influenced by the vacuum pressure. With the pressure decrease from 80 kPa to 9 kPa, the porosity increased from 59.01% to 80.85% and the gradient structure became more noticeable. When the pressure was 80 kPa, the sample obtained a uniform pore structure. After the pressure being decreased to 9 kPa, the sample obtained dispersed pore size distribution including values of 0.5, 20, 30, 40, 60, 100 and 200 μm measured through mercury intrusion method. Gradient porous ceramics with adjustable porosity and pore size distribution, as well as achievable complex shape and large scale, may fabricate through this simply and low cost method.

Key words: gradient, foaming, porous, silicon nitride

中图分类号:

TQ174

邓健, 姚冬旭, 夏咏锋, 左开慧, 尹金伟, 曾宇平. 注浆成型结合真空发泡法制备梯度多孔氮化硅陶瓷[J]. 无机材料学报, 2016, 31(8): 865-868.

DENG Jian, YAO Dong-Xu, XIA Yong-Feng, ZUO Kai-Hui, YIN Jin-Wei, ZENG Yu-Ping. Gradient Porous Silicon Nitride by Slip Casting and Vacuum Foaming[J]. Journal of Inorganic Materials, 2016, 31(8): 865-868.

图/表 7

图1 注浆成型结合真空发泡制备梯度多孔氮化硅工艺流程图

Fig. 1 Flow chart of slip casting and vacuum foaming method for gradient porous silicon nitride

图2 梯度形成原理图

Fig. 2 Process of forming gradient structure

图3 30 kPa气压下制备的样品坯体(a)和烧结后样品(b)的XRD图谱

Fig. 3 XRD patterns of green body (a) and sample prepared under 30 kPa atmosphere pressure (b)

表1 不同气压下制备样品密度和气孔率测试值

Table 1 Densities and porosities of samples prepared under different atmosphere pressures

Samples	1	2	3	4
Pressure /kPa	80	50	30	9
Density /(g﹒cm^-3)	1.41	0.84	0.61	0.66
Porosity /%	59.01	75.50	82.20	80.85

图4 不同气压下制备样品光学显微照片

Fig. 4 Optical microscopy morphologies of samples prepared under different atmosphere pressures(a) 80 kPa; (b) 50 kPa; (c) 30 kPa; (d) 9 kPa

图5 不同样品的SEM照片

Fig. 5 SEM images of different samples(a, b, c) Sample1; (d, e, f) Sample 4. The arrow in (e) shows the “window” forming on the foam surface

图6 不同气压下制备样品孔径分布

Fig. 6 Pore diameter distribution of samples prepared under different atmosphere pressures

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注浆成型结合真空发泡法制备梯度多孔氮化硅陶瓷

Gradient Porous Silicon Nitride by Slip Casting and Vacuum Foaming

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