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人工晶体学报 ›› 2024, Vol. 53 ›› Issue (11): 1918-1926.

• 激光晶体/ 透明陶瓷 • 上一篇    下一篇

Yb∶CaF2透明陶瓷的压力辅助烧结及其性能研究

刘强1, 李想1,2, 郭礼豪2,3, TOCI Guido4, PIRRI Angela5, PATRIZI Barbara4, VANNINI Matteo4, 吴俊林2,3, 李江2,3   

  1. 1.江苏大学材料科学与工程学院,镇江 212013;
    2.中国科学院上海硅酸盐研究所,透明陶瓷研究中心,上海 201899;
    3.中国科学院大学,材料与光电中心,北京 100049;
    4.意大利国家研究委员会国立光学研究所,佛罗伦萨 50019;
    5.意大利国家研究委员会“Carrara”应用物理研究所,佛罗伦萨 50019
  • 收稿日期:2024-09-09 出版日期:2024-11-15 发布日期:2024-12-09
  • 通信作者: 李 江,博士,研究员。E-mail:lijiang@mail.sic.ac.cn
  • 作者简介:刘 强(1964—),男,江苏省人,教授。E-mail:lq88611338@163.com
  • 基金资助:
    国家重点研发计划(2023YFB3812000);中国科学院国际伙伴计划(121631KYSB20200039)

Pressure-Assisted Sintering and Properties of Yb∶CaF2 Transparent Ceramics

LIU Qiang1, LI Xiang1,2, GUO Lihao2,3, TOCI Guido4, PIRRI Angela5, PATRIZI Barbara4, VANNINI Matteo4, WU Junlin2,3, LI Jiang2,3   

  1. 1. College of Materials Science and Engineering, Jiangsu University, Zhenjiang 212013, China;
    2. Transparent Ceramics Research Center, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 201899, China;
    3. Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China;
    4. National Institute of Optics, Italian National Research Council, Florence 50019, Italy;
    5. Institute of Applied Physics “Nello Carrara”, Italian National Research Council, Florence 50019, Italy
  • Received:2024-09-09 Online:2024-11-15 Published:2024-12-09

摘要: 本文采用化学共沉淀法合成了5%(原子数分数,下同)Yb∶CaF2纳米粉体。经过冷冻干燥后,粉体的团聚程度有所减轻,粉体呈立方片层状,平均颗粒尺寸约为40 nm。以冷冻干燥后的粉体为原料,通过热压烧结结合热等静压(HIP)烧结后处理制备了高光学质量的5%Yb∶CaF2透明陶瓷。分析了热压烧结过程中样品的致密化行为,并对陶瓷的显微结构、直线透过率、吸收光谱及激光性能进行测试与表征。结果表明,陶瓷坯体在热压烧结时的保温阶段存在致密化驱动力的激活阈值,同时HIP后处理能够进一步压缩和排除热压陶瓷内残留气孔,有效提高陶瓷的光学质量。通过热压烧结(625 ℃×2 h,50 MPa)结合HIP后处理(600 ℃×3 h,100 MPa Ar)制备的5%Yb∶CaF2透明陶瓷在400和1 200 nm处的直线透过率分别为72.6%和92.2%(厚度2 mm),其在976 nm处的吸收截面为0.52×10-20 cm2。使用波长为930 nm的光纤耦合二极管激光器(LD)端面泵浦Yb∶CaF2透明陶瓷,获得了最大输出功率为0.81 W、斜率效率为9.7%的准连续激光输出。

关键词: Yb∶CaF2透明陶瓷, 热压烧结, 热等静压烧结, 显微结构, 激光性能

Abstract: The 5%(atomic fraction) Yb∶CaF2 nano-powders were synthesized by chemical co-precipitation method. Following freeze-drying, the agglomeration degree of the powders reduces, and the powders exhibit cubic lamellar structures with an average particle size of approximately 40 nm. High optical quality 5%Yb∶CaF2 transparent ceramics were subsequently fabricated through hot pressing, supplemented by hot isostatic pressing (HIP) sintering as a post-treatment, utilizing the freeze-dried powders. The densification behaviour of the samples during the hot pressing process was investigated. The microstructure, in-line transmittance, absorption spectra, and laser performance of the ceramics were assessed and analyzed. The findings indicate that activation threshold of densification driving force occurs during the holding stage of the hot pressing process, and the HIP post-treatment effectively compresses and removes residual pores within the hot pressed ceramics, thereby significantly enhancing their optical quality. The in-line transmittance of the 5%Yb∶CaF2 transparent ceramics, produced through hot pressing (625 ℃×2 h, 50 MPa) followed by HIP post-treatment (600 ℃×3 h, 100 MPa Ar), is 72.6% and 92.2% at 400 and 1 200 nm, respectively, with a thickness of 2 mm. Additionally, the absorption cross-section at 976 nm is determined to be 0.52 ×10-20 cm2. A fiber-coupled diode laser (LD) with a wavelength of 930 nm served as the pumping source for end-face pumping of the Yb∶CaF2 transparent ceramics, obtaining a quasi-continuous laser output with a peak power of 0.81 W and a slope efficiency of 9.7%.

Key words: Yb:CaF2 transparent ceramics, hot pressing sintering, hot isostatic pressing sintering, microstructure, laser performance

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