硅酸盐学报

注射成型结合热等静压制备高性能细晶氧化锆增韧氧化铝陶瓷

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熊新锐 ¹ , 应纪昀 ¹ , 刘子玉 ¹ , 刘鹏 ¹ , 杨现锋 ¹ , 谢志鹏 ²

硅酸盐学报 | 研究论文 2026,54(3): 1032-1041

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硅酸盐学报 |研究论文 2026 , 54 (3) : 1032 -1041

注射成型结合热等静压制备高性能细晶氧化锆增韧氧化铝陶瓷

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熊新锐¹, 应纪昀¹, 刘子玉¹, 刘鹏¹, 杨现锋¹, 谢志鹏²

作者信息

^1．长沙理工大学材料科学与工程学院，长沙 410114

^2．清华大学，新型陶瓷与精细工艺国家重点实验室，北京 100083

通讯作者:

杨现锋（1980—），男，博士，教授。

作者简介:

熊新锐（2000—），男，硕士研究生。

High-Performance Zirconia-Toughened Alumina Ceramics Fabricated by Injection Molding Combined with Hot Isostatic Pressing

Xinrui XIONG¹, Jiyun YING¹, Ziyu LIU¹, Peng LIU¹, Xianfeng YANG¹, Zhipeng XIE²

Affiliations

^1.Changsha University of Science & Technology, College of Materials Science and Engineering, Changsha 410114, China

^2.State Key Laboratory of New Ceramic and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100083, China

Corresponding Author:

YANG Xianfeng (1980-), male, Ph.D., Professor. E-mail: yangxfcsust@csust.edu.cn

XIONG Xinrui (2000-), male, Master candidate. E-mail: 15616222768@163.com

出版时间: 2026-03-20 doi: 10.14062/j.issn.0454-5648.20250277

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摘要

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采用注射成型结合热等静压烧结（HIP）工艺制备了细晶氧化锆增韧氧化铝（ZTA）陶瓷，研究了骨架黏结剂及固相含量对喂料流变性能的影响；使用热重-红外联用技术分析喂料中黏结剂的热分解行为；研究了ZTA陶瓷经过不同温度空气预烧及HIP处理后的微观形貌和力学性能。结果表明：以聚丙烯为骨架黏结剂的喂料呈现典型的剪切稀化流变行为，固相含量为56% （体积分数）时，喂料具有最低非牛顿指数；黏结剂混合未改变其降解顺序及产物，说明黏结剂之间具有良好的工艺兼容性；经过1500 ℃空气预烧结合1450 ℃ HIP处理获得的ZTA陶瓷综合力学性能最优：其相对密度为98.81% （4.15 g/cm³）；硬度为（21.73±0.42）GPa；抗弯强度为（656±24） MPa。采用该工艺制备的陶瓷劈刀具有良好的精度及表面光洁度。

关键词

氧化锆增韧氧化铝陶瓷 / 注射成型 / 热等静压 / 陶瓷劈刀

Abstract

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Introduction

With the increasingly demand of ceramic components in biomedical engineering, microelectronic packaging, and related fields, the requirements for ceramic geometric complexity, accuracy and mechanical properties become popular. Injection molding technology possesses distinct advantages of high dimensional accuracy, superior shape fidelity, and elevated production efficiency for the mass production of geometrically intricate ceramic parts. This study fabricated fine-grained zirconia-toughened alumina (ZTA) ceramics via submicron powder injection molding and hot isostatic pressing (HIP). Furthermore, the rheological behavior of the feedstocks, thermal debinding kinetics, microstructure, and mechanical properties were systematically investigated.

Methods

A ZTA powder with an average particle size of 0.281 μm was used. The binders used consisted of polypropylene (PP, 99% purity; same for subsequent materials), polyethylene (PE, 99%), polystyrene (PS, 99%), ethylene-vinyl acetate (EVA, 98%), paraffin wax (PW 99%), stearic acid (SA 99%) and dibutyl phthalate (DBP, 99.5%). The mass ratio of the binder components m(PP/PE/PS) : m(EVA) : m(PW) : m(SA) : m(DBP) in the feedstock was 30 : 30 : 30:5:5. The ceramic powder and organic binders were fully mixed by an internal mixer (Guangdong C Fine Technology Co., Ltd, China) at 180 ℃ for 90 min, then crushed into granules of less than 5 mm. The solid loading of the feedstocks was 54%, 56% and 58%, respectively. Injection molding was performed using a model VE600Ⅲ-80hs commercial injection molding machine (Zhafir Plastics Machinery GmbH., Germany). Thermal debinding was conducted using a hot air circulation furnace (Wanlong Electric Furnace Co., China). The green bodies were pre-sintered in a muffle furnace (Ruibang Intelligent Technology Co., China) and then HIP post-treated using a model AIP10-30H system (AIP Co., USA). The rheological properties of feedstocks were tested at 190 ℃ by a model Rosand RH2000 capillary rheometer (Malvern Co., UK). The thermal decomposition behavior of binders and green bodies within the temperature range of 30-600 ℃ was examined using a model STA-449C simultaneous thermal analyzer (NETZSCH Co., Germany) coupled with a model TENSOR II FT-IR thermogravimetric-infrared spectroscope (BRUKER Co., USA). The microstructures of ZTA samples were analyzed by a model JSM-6700F field emission scanning electron microscope (SEM, JEOL Co., Japan). The hardness of the samples was measured using a model Instron Wilson VH1150 Vickers hardness tester (BRUKER Co., USA). The flexural strength of the samples was evaluated via the three-point bending method using a model PT-1176 universal testing machine (Baoda instrument Co., Ltd., China).

Results and discussion

At 190 ℃, the shear viscosity of the raw material decreases with increasing shear rate, demonstrating the pronounced shear-thinning characteristics advantageous for injection molding. The feedstocks utilizing polypropylene as a skeletal binder exhibit a typical shear-thinning rheological behavior and a homogeneous microstructural morphology. At a shear rate of 100 s^-1, the shear viscosities of raw materials with solid contents of 54%, 56%, and 58% are 466.79 Pa·s, 900.90 Pa·s, and 2352.54 Pa·s, respectively. The non-Newtonian index reaches its minimum value (i.e., n=0.47) for the material at 56% solid-content. The TG and TG (DSC)-FTIR analyses reveals that the mixing process of binders does not affect the decomposition products, but affects the degradation process. The mixing of binders leads to an eutectic melting. Furthermore, a winding structure is formed between the straight chain part of DBP and other binder components due to a physical or chemical adsorption of binders on the surfaces of ceramic particles. Therefore, the initial degradation temperature increases. The ZTA ceramics with a high relative density of 98.81% and fine grains can be fabricated via air pre-sintering and HIP post-treatment technology. The ZTA ceramics pre-sintered at 1500 ℃ and HIP-ed at 1450 ℃ have superior comprehensive properties with a hardness of (21.73±0.42) GPa and a flexural strength of (656±24) MPa. Based on the optimized process, the fabricated ceramic capillary bonding tools exhibit excellent dimensional accuracy and superior surface finish.

Conclusions

In this work, fine-grained ZTA ceramics were fabricated via submicron powder injection molding combined with HIP. The feedstocks with polypropylene (PP) as a skeletal binder exhibited characteristic shear-thinning rheological behavior and homogeneous microstructure. At a solid content of 56%, the feedstocks demonstrated the minimum non-Newtonian index (n=0.47). During mixing, degradation products of the binder system remained stable, while preserving the mixing sequence, indicating partial processing compatibility among binder components. The ZTA ceramics pre-sintered at 1500 ℃ and HIP-ed at 1450 ℃ exhibited superior comprehensive properties (i.e., a relative density of 98.81% (4.15 g/cm³), hardness of (21.73±0.42) GPa, and flexural strength of (656±24) MPa). This study could realize the preparation of fine-grained, high-density ZTA ceramic capillary bonding tools, providing an effective pathway for manufacturing precision ceramic components with micro-scale structures.

Key words

zirconia-toughened alumina ceramics / injection molding / hot isostatic pressing / ceramic capillary bonding tool

引用本文

熊新锐, 应纪昀, 刘子玉, 刘鹏, 杨现锋, 谢志鹏. 注射成型结合热等静压制备高性能细晶氧化锆增韧氧化铝陶瓷. 硅酸盐学报, 2026 , 54 (3) : 1032 -1041 . DOI: 10.14062/j.issn.0454-5648.20250277

Xinrui XIONG, Jiyun YING, Ziyu LIU, Peng LIU, Xianfeng YANG, Zhipeng XIE. High-Performance Zirconia-Toughened Alumina Ceramics Fabricated by Injection Molding Combined with Hot Isostatic Pressing[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (3) : 1032 -1041 . DOI: 10.14062/j.issn.0454-5648.20250277

基金

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国家自然科学基金(52172063)

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2026年第54卷第3期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250277

接收时间：2025-04-14
首发时间：2026-10-27
出版时间：2026-03-20

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出版历史

收稿日期：2025-04-14
修回日期：2025-05-15

基金

国家自然科学基金(52172063)

作者信息

^1．长沙理工大学材料科学与工程学院，长沙 410114

^2．清华大学，新型陶瓷与精细工艺国家重点实验室，北京 100083

通讯作者:

杨现锋（1980—），男，博士，教授。

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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