LIU Ziyu (1991-), female, Ph.D., Lecturer. E-mail: ziyuliu@csust.edu.cn
Lutetium oxide (Lu2O3) transparent ceramics have a great potential in high-power or high-efficiency solid-state laser applications due to the excellent thermal-mechanical properties, low fabrication temperature, high absorption and emission cross-sections when doped with trivalent rare earth laser ions. Among them, Lu2O3 doped with Yb3+ stands out as the best combination for applications in high-efficiency and high-power lasers, considering a high thermal conductivity due to the similar ionic radii and bonding forces of lutetium and ytterbium ions. The combination of vacuum pre-sintering with HIP post-treatment, along with the powder synthesized by a co-precipitation method, highly favors to fabricate highly transparent sesquioxide ceramics. Some previous reports demonstrated the high efficiency and high power laser outputs of Yb:Lu2O3 transparent ceramics. Thermal properties of Yb:Lu2O3 ceramics are significant for the high-efficiency and high-power laser applications. In ceramic gain media, the significant factors affecting the thermal conductivity include the doping content of active ions, porosity and grain size. Although increasing Yb3+ concentration could not cause a decrease in thermal conductivity in theory, little work has reported the related experimental investigations yet.
The commercial oxide powders (i.e., Lu2O3 and Yb2O3) were utilized as raw materials. Ammonium bicarbonate (NH4HCO3) and ammonium sulfate ((NH4)2SO4) were used as a precipitant and a dispersant, respectively. The precursors of Yb:Lu2O3 were synthesized by a co-precipitation method. All the precursors with different Yb3+ doping contents were calcined at 1050 ℃ to obtain Yb:Lu2O3 powders, which were dry-pressed at a low pressure in a steel die and then cold-isostatically pressed at 250 MPa. All the green bodies were vacuum sintered at 1500 ℃ for 2 h to fabricate pre-sintered ceramics that then were HIP post-treated in Ar atmosphere pressure of 176 MPa at 1750 ℃ for 3 h. Finally, the HIP post-treated ceramics were annealed in air at 900 ℃ for 10 h and then polished on the both sides to a thickness of 1.3 mm for the coming optical characterizations. Some annealed transparent ceramic disks were then machined to the sizes of (Φ = 10.0 mm, d = 1.3 mm) and (Φ=5.5 mm, d<1.0 mm) for measuring the thermal diffusivity and specific heat, respectively.
The phase compositions of the synthesized precursors and powders were identified by X-ray diffraction (XRD, Cu Kα1 radiation, λ = 0.154 18 nm). The microstructures of all the powders and ceramics were determined by field emission scanning electron microscopy (FESEM, SU8220, Hitachi, Japan). The in-line transmittance and absorption spectra of Yb∶Lu2O3 transparent ceramics were characterized by ultraviolet-visible-near infrared spectroscopy (UV-VIS-NIR, Carry-5000, Varian, USA). The thermal diffusivity was measured by a laser-flash method, and the specific heat was measured by differential scanning calorimetry (DSC).
Pure Lu2O3 precursor consists of spherical particles with various sizes, which range from tens of nanometers to hundreds of nanometers in diameter, but the micro-morphology of the precursor with Yb3+ is made of thin stacked layers with nano-sized thickness, indicating that Yb3+ doping has a great impact on the morphologies of Lu2O3 precursor, but its concentration level does not affect the morphologies of the precursors apparently. The particles of Yb3+-doped nano-powders agglomerate in two-dimensional space and are in the shape of regular polyhedra. The phases of all the calcined nano-powders are consistent with those of cubic Lu2O3. The lattice parameters of Yb:Lu2O3 nano-powders are 10.384 4、10.389 4、10.390 2、10.394 9 Åand 10.396 5 Å, respectively, with increasing the Yb3+ concentration. The corresponding average gain sizes are 57.7, 51.9, 53.6, 61.8 and 51.4 nm, respectively. The relative densities of all the Yb:Lu2O3 pre-sintered ceramics are 95.3%, 96.1%, 95.6%, 95.4% and 95.7%, with average grain sizes of 0.92, 0.97, 0.99, 1.09 μm and 1.14 μm, respectively, as Yb3+ concentration increases. 3% Yb:Lu2O3 transparent ceramic sample has the maximum in-line transmittance with the values of 83.0% at 1080 nm and 78.8% at 600 nm. The absorption coefficients at 948 nm of these ceramics are linearly correlated to Yb3+ doping content, which follows the Lambert-Beer Law. Four main emission peaks are located at 948, 976, 1033 and 1079 nm, respectively, among which the largest emission cross-section is at 976 nm with a value of 1.148×10-20 cm2. The laser emission wavelengths include 1079 nm and 1033 nm. The maximum thermal conductivity of 3% Yb∶Lu2O3 ceramics is 13.1 W·m-1·K-1 at room temperature, which is similar to the value of Yb:Lu2O3 single crystal, while the thermal conductivity of 15% Yb∶Lu2O3 ceramics is 11.6 W·m-1·K-1, which is greater than that of pure YAG material. The result indicates that Yb:Lu2O3 transparent ceramics are a gain medium with a high thermal conductivity, even doped with a high Yb3+ doping content, demonstrating a great application potential in high-power solid-state lasers.
Yb:Lu2O3 transparent ceramics with Yb3+ doping content of 0-15% were fabricated by vacuum sintering and HIP post-treating from co-precipitated nano-powders. The nano-powders calcined at 1050 ℃ had the similar particle sizes with different morphologies as the precursors. 3% Yb∶Lu2O3 nano-powder showed a better dispersivity, and the corresponding transparent ceramics possessed the maximum optical quality with the in-line transmittance of 83% at 1080 nm. The spectral characteristics of all the Yb:Lu2O3 transparent ceramics were calculated. At β of > 0.059, there were two main lasing emission wavelengths, peaked at 1033 nm and 1079 nm, respectively. 3% Yb:Lu2O3 transparent ceramics possessed better thermal properties rather than others, with the room-temperature thermal conductivity of 13.1 W·m-1·K-1. The results indicated a great application potential of Yb:Lu2O3 transparent ceramics in high-power solid-state lasers.
| 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 |