HEMA-TBA凝胶体系制备多孔氧化铝陶瓷

doi:10.15541/jim20160550

摘要/Abstract

摘要：

采用HEMA-TBA凝胶体系制备具有高气孔率, 高强度的多孔氧化铝陶瓷, 研究多孔氧化铝陶瓷的浆料和坯体制备工艺, 并系统研究了分散剂含量和固相体积分数对浆料粘度和悬浮稳定性的影响、干燥和单体含量对生坯性能的影响以及固相体积分数和烧结温度对烧结体微观结构的影响。结果表明: 加入柠檬酸可以使浆料粘度降低, 稳定性提高, 柠檬酸加入量达到2wt%后浆料粘度和稳定性趋于稳定; 固相体积分数的增加会导致浆料粘度和稳定性的增加; 生坯在干燥过程中的收缩比水基体系小很多, 干燥时间也相对更短; 单体含量对生坯强度影响较大, 当单体含量为25wt%时, 生坯强度较高; 通过选择不同的固相体积分数和烧结温度, 可以有效地控制烧结体的微观结构, 气孔率的变化范围在40%~65%, 同时烧结体强度也会随之发生变化, 变化范围在5.7~91.2 MPa。

关键词: 多孔陶瓷, 凝胶注模, 浆料, 流变性能

Abstract:

Porous alumina ceramics with high porosity and high strength were successfully fabricated by HEMA-TBA gelcasting system. Fabrication processes of slurries and ceramic were studied, effects of solid loading and dispersant contents on viscosity and stability of slurries, effects of drying and monomer content on green bodies, and effects of solid loading and sintering temperature on sintered bodies were investigated. The results show that optimum addition of citric acid of 2wt% decreases the viscosity and increases the stability of slurry. The viscosity and stability of the slurries increase with the increase of the solid loading of slurries. Green bodies with low solid loading can be dried with relatively small shrinkage less than 10% and its drying time is also relatively shorter than water based gelcasting system. The amount of monomer has great influence on green body and the strength of green body achieve high value at monomer content of 25%. By choosing the solid loading of slurries and sintering temperatures, ceramic microstructures and the porosity ranging from 40%-65% can be effectively controlled and strength of porous ceramics changes in the range of 5.7-91.2 MPa.

Key words: porous ceramic, gelcasting, slurry, rheological properties

中图分类号:

TQ174

谢雨洲, 彭超群, 王小锋, 王日初, 罗丰. HEMA-TBA凝胶体系制备多孔氧化铝陶瓷[J]. 无机材料学报, 2017, 32(7): 731-738.

XIE Yu-Zhou, PENG Chao-Qun, WANG Xiao-Feng, WANG Ri-Chu, LUO Feng. Porous Alumina Ceramic Prepared by HEMA-TBA Gelcasting System[J]. Journal of Inorganic Materials, 2017, 32(7): 731-738.

图/表 14

表1 实验原料的来源和纯度

Table 1 Manufacture and purity of the raw materials

Name	Abbreviation	Purity	Manufacture
Tert-butanol	TBA	AR	Shanghai Chemical Reagent Co.
2-hydroxyethyl methacrylate	HEMA	AR	Shanghai Chemical Reagent Co.
Methylene-bis-acrylamide	MBAM	AR	Shanghai Chemical Reagent Co.
Benzoyl peroxide	BPO	AR	Shanghai Chemical Reagent Co.
N, N-dimethylaniline	DMA	AR	Shanghai Chemical Reagent Co.
Citric acid	C₆H₆O₇	AR	Shanghai Chemical Reagent Co.
Acetic acid	C₂H₄O₂	AR	Shanghai Chemical Reagent Co.
Alumina	α-Al₂O₃	99.8%	Henan Jiyuan Brother Material Co.

图1 浆料的粘度与分散剂加入量的关系

Fig. 1 Relationship between dispersant amount and viscosity of slurry Solid loading: 10%; O.pH=3

图2 浆料的沉降高度与分散剂加入量的关系

Fig. 2 Relationship between dispersant amount and sedimentation height of slurrySolid loading: 10%; O. pH=3

图3 浆料粘度与固相体积分数的关系

Fig. 3 Relationship between viscosity and solid loading of slurryAmount of citric acid: 2%, O. pH=3

图4 浆料沉降高度与固相体积分数的关系

Fig. 4 Relationship between sedimentation height and solid loading of slurryAmount of citric acid: 2%, O. pH=3

图5 不同固相体积分数的坯体干燥过程中的质量变化

Fig. 5 Mass loss of green body with different solid loadings during the drying process

表2 不同固相体积分数的坯体干燥后的收缩率

Table 2 Shrinkage in green body with different solid loadings after drying

Solid loading	Shrinkage
5%	9.2%-10.1%
10%	5.1%-6.3%
15%	0.9%-1.2%
20%	0.8%-1.0%

图6 不同单体含量的浆料弹性模量随时间的变化

Fig. 6 Storage modulus of slurry with different monomer amount as a function of time Solid loading: 10%

图7 不同单体含量的坯体干燥后的显微形貌

Fig. 7 Microstructures of green body after drying with different monomer amounts(a) 15%; (b) 25%; (c) 35%, solid loading: 10%

表3 不同单体含量的坯体干燥后的抗弯强度

Table 3 Flexural strength of green body after drying with different monomer amounts

Monomer amount	Flexural strength/MPa
15%	3.2±0.2
25%	6.1±0.2
35%	4.2±0.2

图8 1500℃烧结的不同固相体积分数的多孔氧化铝陶瓷的显微形貌

Fig. 8 Microstructures of porous alumina ceramic with different solid loadings sintered at 1500℃(a) 5% ; (b) 10%; (c) 15%; (d) 20%

表4 1500℃烧结的不同固相体积分数的多孔氧化铝陶瓷的气孔率与抗弯强度

Table 4 Porosity and flexural strength of porous alumina ceramic with different solid loadings sintered at 1500℃

Solid loading	Porosity	Flexural strength/MPa
5%	61-65%	5.7±0.2
10%	55-58%	8.3±0.2
15%	47-49%	27.6±1.5
20%	43-46%	48.5±2.1

图9 不同烧结温度条件下多孔氧化铝陶瓷的显微形貌

Fig. 9 Microstructures of porous alumina ceramic sintered at different temperatures(a) 1400℃; (b) 1500℃; (c) and (d) 1600℃

表5 不同烧结温度下多孔氧化铝陶瓷的气孔率和抗弯强度

Table 5 Porosity and flexural strength of porous alumina ceramic sintered at different temperatures

Sintering temperature/℃	Porosity	Flexural strength/MPa
1400	49%-50%	23.7±1.3
1500	43%-46%	48.5±2.1
1600	40%-42%	91.2±4.5

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