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人工晶体学报 ›› 2026, Vol. 55 ›› Issue (6): 930-939.DOI: 10.16553/j.cnki.issn1000-985x.2026.0013

• 研究论文 • 上一篇    下一篇

草酸前处理对Y2O3透明陶瓷低温致密化与光学性能的影响

林海宁1,2(), 陈剑1, 黄集权1, 刘欣1,2, 郭旺1,2()   

  1. 1.中国科学院福建物质结构研究所功能晶体与器件国家重点实验室,福州 350002
    2.福建师范大学化学与材料学院,福州 350007
  • 收稿日期:2026-01-27 出版日期:2026-06-20 发布日期:2026-07-07
  • 通信作者: 郭旺,博士,研究员。E-mail:guowang@fjirsm.ac.cn
  • 作者简介:林海宁(2001—),女,福建省人,硕士研究生。E-mail:linhaining@fjirsm.ac.cn
  • 基金资助:
    福建省科技厅引导性项目(2025H0032);功能晶体与器件全国重点实验室自主部署重点项目(GNJT-2025-ZD07)

Effect of Oxalic Acid Pretreatment on Low-Temperature Densification and Optical Properties of Y2O3 Transparent Ceramics

LIN Haining1,2(), CHEN Jian1, HUANG Jiquan1, LIU Xin1,2, GUO Wang1,2()   

  1. 1.State Key Laboratory of Functional Crystals and Devices,Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences,Fuzhou 350002,China
    2.College of Chemistry and Materials Science,Fujian Normal University,Fuzhou 350007,China
  • Received:2026-01-27 Online:2026-06-20 Published:2026-07-07

摘要: 氧化钇(Y2O3)透明陶瓷的高熔点使其通常需要依赖高活性粉体工程或先进烧结技术实现低温致密化。本研究提出一种简便、低成本的草酸液相前处理策略,用于高效活化商业Y2O3粉体,并结合真空无压烧结,在低温条件下制备高性能Y2O3透明陶瓷。草酸处理不仅能有效去除粉体表面吸附杂质,显著细化粉体并改善其分散性,还可通过络合-分解过程在原粉中引入大量30~50 nm的纳米Y2O3颗粒,从而大幅提升烧结活性。在真空无压烧结中,经草酸处理的2%(原子数分数)ZrO2掺杂Y2O3陶瓷致密化温度降低约100 ℃,在1 700 ℃保温5 h即可实现接近完全致密,且显微结构均匀。最终该陶瓷在1 750 ℃烧结后,样品厚度为1 mm时,于600 nm波长处直线透过率最高达75.8%,表现出优异的光学性能。本研究为基于商业粉体,通过简单化学处理实现高熔点氧化物陶瓷的低温、低成本致密化提供了一条有效途径。

关键词: Y2O3透明陶瓷; 草酸前处理; 真空无压烧结; 光学透过率; 微观形貌; 致密化行为

Abstract: Yttrium oxide (Y2O3) transparent ceramics have been widely studied for infrared windows,corrosion-resistant components,solid-state lasers,and scintillator hosts because of their broad optical transparency range,excellent chemical stability,and low thermal expansion coefficient. However,their widespread application is hindered by the high melting point of Y2O3,which necessitates energy-intensive sintering processes at temperatures often exceeding 1 800 ℃ to achieve full densification. Conventional approaches to lower the sintering temperature typically rely on either complex,time-consuming synthesis of ultra-high-purity,nano-sized powders or on expensive advanced sintering techniques like hot isostatic pressing (HIP) or spark plasma sintering (SPS),limiting their scalability and cost-effectiveness. In this study,we report a simple,scalable,and low-cost strategy to dramatically enhance the sinterability of commercial Y2O3 powder through an oxalic acid liquid-phase pretreatment,enabling its low-temperature densification via vacuum pressureless sintering,which is a method that is both industrially favored and economically viable.The method involves treating ball-milled commercial Y2O3 powder with a 1.2 mol/L oxalic acid solution,followed by filtration,washing,and a final calcination at 700 ℃. This treatment is shown to have a profound,multi-faceted activation effect. It not only efficiently removes surface-adsorbed impurities and carbonates,as confirmed by FT-IR analysis,but also refines the average particle size from 1.0~1.3 μm to approximately 300 nm. Crucially,the chelation between Y3+ and C2O42- leads to the in-situ formation of a yttrium oxalate precursor,which upon decomposition generates a substantial population of 30~50 nm Y2O3 nanoparticles. These nanoscale particles act as highly reactive sintering seeds,significantly boosting the overall sintering activity of the powder.The impact of this pretreatment on the sintering behavior and optical quality of Y2O3 ceramics was systematically investigated. For 2.0%(atomic fraction) ZrO2-doped Y2O3,the oxalic acid treatment reduced the densification temperature by approximately 100 ℃. Near-full densification with a uniform,fine-grained microstructure was achieved at just 1 700 ℃ for 5 h under vacuum,a temperature at which untreated samples remained porous and opaque. This low-temperature densification is attributed to the combined effects of improved powder dispersion,and the presence of the nano-sized Y2O3 particles that enhance grain boundary diffusion. The superior sintering activity and microstructural uniformity directly translated into outstanding optical performance. Sintered at 1 750 ℃,the treated Y2O3 ceramics exhibit a maximum in-line transmittance of 75.8% at 600 nm,representing a significant advancement over untreated samples which showed no transmittance at this wavelength under identical conditions.In conclusion,this work introduces a highly effective powder activation strategy that bridges the gap between low-cost commercial precursors and the demanding requirements of high-performance transparent ceramics. By demonstrating that a simple oxalic acid wash can match the sintering efficacy of complex powder synthesis routes,this research provides a new paradigm for the low-temperature,cost-effective fabrication of high-melting-point oxide ceramics.

Key words: Y2O3 transparent ceramics; oxalic acid pretreatment; vacuum pressureless sintering; optical transmittance; microstructure; densification behavior

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