Mn^(2+)掺杂对YAG∶Ce^(3+)荧光陶瓷发光性能的影响

过渡族金属Mn^(2+)掺杂的石榴石荧光陶瓷被认为是实现高显色激光照明的候选材料。然而,由于Mn^(2+)在不同配位环境下离子半径的多样性,Mn^(2+)掺杂石榴石陶瓷体系设计方案尚不明确。本文采用真空烧结技术制备得到不同浓度Mn^(2+)掺杂的YAG∶Ce^(3+)荧光陶瓷,并将Mn^(2+)分别设计进入八面体(OC)和十二面体(DO)格位。通过表征样品物相和显微结构、光致发光、荧光寿命、量子效率等,并通过LD激光器激发对荧光陶瓷的发光性能进行研究。实验结果表明,在添加电荷与体积补偿剂SiO_(2)的前提下,相比Mn^(2+)进入十二面体格位,Mn^(2+)进入八面体后石榴石的晶体结构更加稳定。因此,当Mn^(2+)的浓度控制在0.5%^(6)%(at)范围内,OC系列样品的量子效率高于DO系列样品。此外,OC系列样品的PL谱中位于588 nm和725 nm处的发射峰分别对应于Mn^(2+)占据八面体和十二面体格位的^(4)T_(1)→^(6)A_(1)电子跃迁,而DO系列样品中位于572 nm处的发射峰则源于Mn^(2+)占据扭曲的十二面体格位产生的电子跃迁。得益于Ce^(3+)→Mn^(2+)间高效的能量传递,将浓度为6%(at)的Mn^(2+)设计进入YAG∶Ce^(3+)中八面体格位制得荧光陶瓷,封装得到的激光白光光源的显色指数为70.8,相对色温为5117 K。本文对于Mn^(2+)掺杂的石榴石发光材料的开发研究是有力补充,也为提升YAG∶Ce^(3+)荧光陶瓷光谱中的红光成分,进而提高医疗、显示等领域的激光光源的显色性能提供借鉴。

Continuous wave and active Q-switched operation of Watt-level LED-pumped two-rod Nd,Ce:YAG laser

A high-performance LED-side-pumped two-rod Nd,Ce:YAG laser with continuous-wave(CW) and acousto–optical(A-O) Q-switched operation is demonstrated in this work. A symmetrically shaped flat–flat cavity with two identical LEDside-pumped laser modules is employed for power scalability. In the CW regime, the maximum output average power of laser at 1064 nm is 4.41 W, corresponding to a maximum optical conversion efficiency of 5.3% and a slope efficiency is 12.4%. In the active Q-switched regime, the pulse energy of laser reaches as high as 0.89 m J at a repetition rate of 800 Hz with a pulse width of 457.2 ns, the corresponding highest peak output power is 1.94 k W and the M~2 factor is measured to be about 8.8. To the best of the authors' knowledge, this is the first demonstration and the highest performance of a CW LED-side-pumped two-rod laser Nd,Ce:YAG with Watt-level output reported so far.

激光照明用YAG∶Ce-CaF_(2)荧光陶瓷的冷烧结制备

荧光陶瓷是激光照明的关键材料。为探究低温制备荧光陶瓷的可行性,采用冷烧结工艺在425℃成功制备了致密度高、晶粒尺寸均匀、相界分明的YAG∶Ce-CaF_(2)复合荧光陶瓷。结果表明:发光相与基体之间没有可检测到的界面反应;制备的荧光陶瓷具有较高的量子效率(74.3%)、较好的热导率(室温可达9.4 W·m^(-1)·K^(-1))、优异的热稳定性(在400 K时发光强度仅损失4.3%);在蓝光激光(451 nm)激发下,复合荧光陶瓷表现出良好的黄光发射,并展现出光通量为910.7 lm和流明效率为91.07 lm·W^(-1)的高亮度白色激光照明,其荧光寿命无衰减(66 ns),相关色温为4483~8247 K,显色指数为73.4~83.6。冷烧结工艺是低温条件下制备性能优良荧光陶瓷的新方法。

高亮度固态照明用LuYAG∶Ce荧光陶瓷

实现高发光效率、高亮度和良好的热稳定性是固态照明的迫切要求。因此,用于高功率发光二极管或激光二极管(LED/LD)的高性能荧光转换材料具有重要的研究意义。在这项工作中,通过将Lu^(3+)离子引入YAG∶Ce荧光陶瓷中方法作为有效策略来改善YAG∶Ce荧光材料的发光性能。采用固相反应和真空烧结法制Article ID:1000-7032(2023)06-0964^(-1)1收稿日期:2022^(-1)2-31;修订日期:2023-01-30基金项目:中国科学院战略性先导科技专项(XDA22010301)Supported by The Strategic Priority Research Program of The Chinese Academy of Sciences(XDA22010301)第6 HUANG Xinyou期,et al.:LuYAG∶Ce Transparent Ceramic Phosphors for High-brightness Solid-state…备了不同Lu^(3+)含量的(Lu,Y)_(3)Al_(5)O_(12)∶Ce荧光陶瓷(LuYAG∶Ce荧光陶瓷)。随着Lu^(3+)含量的增加,LuYAG∶Ce荧光陶瓷中的Y^(3+)位点被Lu^(3+)位点取代,Ce^(3+)的发射峰呈现从573 nm到563 nm的蓝移现象。当Lu^(3+)含量为60%时,通过将LuYAG∶Ce荧光陶瓷与蓝光LED组合,其发光强度达到最大值,流明效率达到114 lm∙W^(-1)。使用450 nm激光源与LuYAG∶Ce荧光陶瓷构建了透射模式下的激光驱动照明装置。随着功率密度从2.2 W·mm^(-2)增加到39 W·mm^(-2),Lu^(3+)含量为60%的荧光陶瓷光通量从128 lm增加到1874 lm,且没有发光饱和的迹象,最佳发光效率达到128 lm·W^(-1)。因此,LuYAG∶Ce荧光陶瓷有望成为高功率LED/LD照明的潜在荧光转换材料。

Effect of Additive on Microstructure of Transparent YAG Ceramics

Transparent YAG (yttrium aluminum garnet) ceramics were fabricated by solid-state reaction method. Effect of additive (tetraethyl orthosilicate, TEOS) on microstructure of YAG ceramics was investigated. If the addition of TEOS is more than 3% (mass fraction), large amount of liquid phase can be yielded at grain boundaries, resulting in the formation of second phase particles at grain boundaries. If the addition is less than 0.05% (mass fraction), pores are entrapped in the grains. The suitable amount is 0.5% (mass fraction). A fully transparent YAG ceramic was fabricated by vacuum sintering at 1700 ℃ for 5 h. Optical transmittance of the YAG ceramic is 63% in the visible light wavelengths and 70% in the infrared wavelengths.

A high-power high-stability Q-switched green laser with intracavity frequency doubling using a diode-pumped composite ceramic Nd:YAG laser

We successfully obtain a high-average-power high-stability Q-switched green laser based on diode-side-pumped composite ceramic Nd：YAG in a straight piano-concave cavity. The temperature distribution in composite ceramic Nd：YAG crystal is numerically analyzed and compared with that of conventional Nd：YAG crystal. By using a composite ceramic Nd：YAG rod and a type-II high gray track resistance KTP （HGTR-KTP） crystal, a green laser with an average output power of 165 W is obtained at a repetition rate of 25 kHz, with a diode-to-green optical conversion of 14.68%, and a pulse width of 162 ns. To the best of our knowledge, both the output power and optical-to-optical efficiency are the highest values for green laser systems with intracavity frequency doubling of this novel composite ceramic Nd：YAG laser to date. The power fluctuation at around 160 W is lower than 0.3% in 2.5 hours.

放电等离子烧结Ce、Yb共掺钇铝石榴石稀土荧光粉及其在光伏电池中的应用

通过多场耦合实现快速低温烧结的放电等离子技术具有快速、节能和环保等显著优势,在诸多工业领域中得到广泛应用。利用该技术合成Ce^(3+)、Yb^(3+)共掺钇铝石榴石稀土荧光粉,通过物相结构、形态和光谱特性对稀土荧光粉进行综合分析。结果表明,放电等离子烧结工艺有利于Ce^(3+)和Yb^(3+)嵌入钇铝石榴石的晶格中,晶格常数为1.2005 nm。经研磨后的稀土荧光粉颗粒粒径为1~2μm,YAG:Ce^(3+),Yb^(3+)稀土荧光粉的发射光谱峰值为552 nm和720 nm。具有光转换功能的光伏电池的测试结果表明,光伏电池相对外量子响应在500~1000 nm波长范围内有明显改善,同时短路电流密度高达35.95 mA/cm^(2),增益达0.51 mA/cm^(2),光电转换效率相对提高1.91%。

Novel Phenomenon on Valence Unvariation of Doping Ion in Yb:YAG Transparent Ceramics Using MgO Additives

Yb：YAG nanopowders were synthesized by the alcohol-water co-precipitatlon method adding MgO as sintering additives. Appropriate amount of MgO adding can restrict the agglomeration and reduce the particle size of Yb：YAG powders. When the MgO content was 0.04wt%, well-dispersed Yb：YAG powders with ellipsoidal particles of less than 100 nm diameter were obtained. The experimental results showed the valence variation of doping ion Yb〉 would not appear when adding MgO as sintering additives, so ceramics showed colorless transparent instead of green due to Yb^2＋ color center using traditional SiO2 as additives. The transmission of the sintered Yb：YAG ceramics can reach 80.6% even without annealing. Ceramic morphology showed that the grains had uniform-distribution with the size of 10 iam or so, and no impurity and pore existed in the grain boundary and crystalline while using optimal sintering conditions.

无压烧结制备Y_(2)MgAl_(4)SiO_(12)∶Ce^(3+)荧光陶瓷及光学性能

Y_(3)Al_(5)O_(12)∶Ce^(3+)荧光粉是目前白光LED的主要发光材料,但在使用时存在封装树脂因散热不佳而发生老化等问题。本文采用无压烧结制备了Y_(2)MgAl_(4)SiO_(12)∶Ce^(3+)透明陶瓷荧光体,用于替代荧光粉体和调控发光性能。首先通过化学共沉淀法制备前驱体粉体,经高温煅烧后采用冷等静压成型,最后在马弗炉中1 600℃煅烧制得透明荧光陶瓷。研究了Ce^(3+)掺杂浓度和样品厚度对材料性能的影响,其中掺杂量为0.5%的样品在800 nm处具有56%的透过率,在450 K下发光强度仍能保持室温强度的84%。与蓝光芯片组装成器件测试表明,荧光陶瓷在蓝光LEDs/LDs的激发下发出白光,其CIE色度坐标分别为(0.307 6,0.332 9)和(0.308 0,0.331 6),光效分别为62.6 lm/W和146.3 lm/W。研究结果表明,YMAS∶Ce荧光陶瓷可应用于白光LEDs/LDs领域。

Diode-pumped Kerr-lens mode-locked femtosecond Yb:YAG ceramic laser

We experimentally demonstrated a diode-pumped Kerr-lens mode-locked femtosecond laser based on an Yb：YAG ceramic. Stable laser pulses with 97-fs duration, 2.8-nJ pulse energy, and 320-mW average power were obtained. The femtosecond oscillator operated at a central wavelength of 1049 nm and a repetition rate of 115 MHz. To the best of our knowledge, this is the first demonstration of a Kerr-lens mode-locked operation in a diode-pumped Yb：YAG ceramic laser with sub-100 fs pulse duration.%@ 1674-1056

Structure, Chemical State and Luminescent Properties of Ce,Gd：YAG Transparent Ceramic for Flip-chip White LED Application

Ce,Gd：YAG transparent ceramic was prepared by tape casting and solid state reaction method. Meanwhile, its crystal structure, chemical state and luminous properties were discussed. The prepared samples are identified as pure garnet structure by the XRD results. The valence states of tetravalent and trivalent Ce ions were identified distinctly by X-ray photoelectron spectroscopy. A strong broad band yellow emission was found in photoluminescence（PL） spectra. The quantum yield reached 90.2% at room temperature. When collaborated with a 1.0 mm × 1.0 mm flip-chip, a luminous efficiency（LE） as high as 116.5 lm/W with a correlated color temperature（CCT） of 6627 K at a power dissipation of 1.13 W at 350 m A was demonstrated, indicating that Ce,Gd：YAG transparent ceramics had a promising potential for high power white light-emitting diodes.

Effect of Heat Treatment on Crystallization of Nd:YAG Ceramics

（Nd0.01Y0.99）3Al5O12 nano-sized powders were synthesized by low temperature combustion （LCS）, using Nd2O3, Y2O3, Al（NO3）3.9H2O, ammonia water and citric acid as starting materials. The powders were characterized by TG-DTA, XRD, FT-IR, ICP and TEM, respectively. The grain sizes were calculated by the Scherrer＇s formula using the full width at half maximum （FWHM） of YAG （420） crystal plane diffraction lines. The study focused on crystallization of ceramics at different heat treatment temperatures. The experimental results show that crystallizing temperature of YAG is 850 ℃, and the intermediate crystal phase YAP, appearing during heat treatment, transforms to YAG cubic crystal phase at the temperature of 1 050℃. The particle size of the powders synthesized by LCS is nano-sized. With the temperature increasing, the mean grain sizes raise, the stand deviations keep almost at the value of 2.0 and the lattice parameters decrease. The grains mainly grow by grain boundary diffusion. The lattice parameter expansion is caused by an increase of the repulsive dipolar interactions on surfaces of crystallites,

Sr_(0.5)Zr_(2)(PO_(4))_(3)-(Ce,Sm)PO_(4)复相陶瓷核废物固化体的制备及化学稳定性

为同时固化高放废物中的模拟放射性核素Sr、Ce和Sm,采用一步微波烧结工艺成功制备了Sr_(0.5)Zr_(2)(PO_(4))_(3)-(Ce,Sm)PO_(4)复相磷酸盐陶瓷固化体,采用XRD、Raman、SEM-EDS和密度表征研究了其物相组成、微观结构以及致密性,并利用PCT法评估了化学稳定性。结果表明:Sr_(0.5)Zr_(2)(PO_(4))_(3)相和(Ce,Sm)PO_(4)独居石相兼容性好,两相间不发生相互反应;所制备的复相陶瓷固化体晶粒尺寸小,相对密度高于96%,改变Sm/Ce比对固化体的微观结构和致密性无明显影响;PCT测试结果表明Sr、Ce和Sm的元素归一化元素浸出率都较低,与单相磷酸盐陶瓷固化体相比,复相磷酸盐陶瓷固化体具有较为优异的化学稳定性。

Preparation of Yb:YAG Transparent Laser Ceramics with Urea Co-Precipitation Method

YAG phosphor doped with Yb (3+) for transparent ceramics was prepared by the co-precipitation method with urea used as precipitant. DTA-TG,XRD,SEM and IR spectrum analyzers were used to investigate the structure and morphology of the precursor and the sintered poly-crystal. The results indicates that the weight loss is about 40% as the powder calcined at 1200 ℃,and well-crystallized YAG powder is obtained with particle size in the range of 100～150 nm. The SEM analysis of the fracture surface of the sintered body shows that the grain size is about 1～2 μm and the pore volume is very low. The ceramics body with favorite optical properties is obtained by sintering at 1700 ℃.

Fabrication and laser output of transparent Nd:YAG ceramics from microwave synthesized precursors

We report the laser output of transparent Nd：YAG （Nd：Y3Al5O12） ceramics fabricated from Nd：YAG precursors through the microwave-assisted homogenous precipitation （MAHP） method. Pure phase and uniform Nd：YAG nano-powders with average sizes less than 100 nm were obtained by heating treatment of.the Nd：YAG precursor particles aged for 6 d in vessel with humidity of 30%-50% at 25℃. Transparent Nd：YAG ceramic pellets were obtained by vacuum sintering at 1730℃ for 10 h. Laser output （305 roW） with a slope efficiency of 5.1% was realized through an end-pumped configuration. Our results indicate that the MAHP method could potentially be used for the fabrication of laser ceramic products,

High-Power Dual-End-Pumped Actively Q-Switched Ho:YAG Ceramic Laser

We present a high-power Ho：YAG ceramic laser pumped at 1908nm. Using a dual-end-pumped structure, the maximum continuous-wave output power of 48 W is obtained, corresponding to a slope efficiency of 70.4% with respect to the absorbed pump power. At actively Q-switched mode, the maximum average output power of 46 W and the minimum pulse width of 21 ns are achieved at a pulse repetition frequency of 20 kHz, corresponding to a peak power of approximately 109.5kW. In addition, the beam-quality M2 factor is found to be 1.4 at the maximum output power.

Damage characteristics of YAG transparent ceramics under different loading conditions

YAG (Y_(3)Al_(5)O_(12)) transparent ceramics have attractive application prospects for transparent armor protection modules because of their excellent light transmittance and anti-ballistic capability. Understanding the fracture behavior and damage mechanism of YAG is necessary for armor design. To explore the damage characteristics of YAG under compression and tension, shock compression and shockless spalling experiments with soft recovery technique are conducted. The spall strength of YAG is obtained and the recovered samples are observed by CT and SEM. It is shown that the macroscopic damage characteristic of YAG under compression is vertical split cracks with oblique fine cracks distributed in the entire sample, while that under tension is horizontal transgranular cracks concentrated near the main spall surface. The cracks generated by macroscopic compression, tension and shear stress extend in similar tensile form at the microscale. The proportion of transgranular fractures on spall surfaces is higher than that of cracks induced by macroscopic compression. Meanwhile, higher loading rate and longer loading duration increase the transgranular fracture percentage.

Comparative spectroscopic investigation of Yb-doped YAG,YSAG and YLaO_3 transparent ceramics

Transparent Yb doped YAG, YSAG and YaLaO3 ceramics are fabricated by using the co-precipitation method. The spectral properties and thermal parameters of these Yb doped cubic phase transparent ceramics are compared, and their different and potential applications are also analysed. The absorption cross-section and the emission cross-section of these ceramics are measured and calculated. The essential properties of these materials especially for the rep-rated pulsed high-energy diode-pumped solid-state lasers are investigated. The results show that Yb doped YAG, YSAG and YaLaO3 are all suitable materials used for diode-pumped solid-state lasers.

A Mid-IR Optical Parametric Oscillator Pumped by an Actively Q-Switched Ho:YAG Ceramic Laser

We demonstrate a mid-IR ZnGeP2 （ZGP） optical parametric oscillator （OPO） pumped by a dual-end-pumped actively aeoasto-optie Q-switched Ho：YAG ceramic laser. The maximum average output power of 35 W is obtained at a pulse repetition frequency of 20 kHz from the Ho：YAG ceramic laser. Under the maximum incident pump power of Ho：YAG ceramic laser, the maximum output power of 14 W is obtained from the ZGP OPO, corresponding to the slope efficiency of 49.6% with respect to the incident pump power. The wavelength can be tuned from 3.5 μm to 4.2μm （signal）, corresponding to 5.24.1 μm （idler）. The beam quality M2 is less than 2.3 from the ZGP OPO.

Investigation on the scattering effect of ceramic Nd:YAG

This paper investigates the scattering effect of domestic 0.5 at% ceramic Nd：YAG. An effective method has been utilized to measure the scattering and absorption coefficients. An end-pumped continuous wave （CW） Nd：YAG ceramic laser was also demonstrated. A maximum output power of 6.7 W at 1064 nm was obtained at an 808-nm pump power of 32.9 W. Conversion efficiency and slope efficiency have been achieved. This indicates that scattering has an important effect on the optical performance of ceramic Nd：YAG.