用φ20mm离心萃取器两步法制取高纯钇

本文研究了中钇富镧稀土的氧化物溶液在环烷酸中的萃取行为，测定了镧钇组成、温度变化与分离系数的关系；在Ｐ＿（５０７）体系中研究了ｐＨ值与分配比的关系；提出用环烷酸、Ｐ＿（５０７）两种萃取剂制备高纯钇的工艺流程。用８４台φ２０ｍｍ离心萃取器进行了一个月的台架试验，结果证明两种萃取剂有很好的互补性，在满足钇的纯度要求下有较高收率。离心萃取器具有易分相、体系存留量少、液流密闭性好等优点，它更适宜于粘度大、级数多、产品纯度要求高的体系。     

Mechanism for the Peritectic Reaction and Growth of Aligned Grains in YBa2Cu3O6+x

It is experimentally observed that the peritectic reaction, 211 + liquid → 123, can be driven essentially to completion in 1 h at an undercooling of only ∽30°C. The kinetic data, together with the observed microstructures, are inconsistent with the normal mechanism of the peritectic reaction. It is proposed that the mechanism of the reaction involves dissolution of 211 particles into the liquid and precipitation of solid 123. The aligned grain structure is explained through sympathetic nucleation of new 123 grains on existing grains.     

钇、钪分离工艺的新进展

本文简要介绍中国科学院长春应用化学研究所近年来在钇、钪分离工艺研究方面的新进展。     

Effect of Ca2+ and Mg2+ ions on the sintering and spectroscopic properties of cr-doped yttrium aluminum garnet ceramics

In this work, we investigated the effects of Ca²⁺ and Mg²⁺ ions and annealing temperature on the spectroscopic parameters of chromium-doped yttrium aluminum garnet ceramics (Cr:YAG). Samples were obtained with either a separate or a simultaneous addition of calcium and magnesium oxides. To achieve this, aqueous suspensions were prepared using Y₂O₃, Al₂O₃, Cr₂O₃, MgO, and CaO high-purity powders as raw materials. The obtained suspensions were freeze-granulated, pressed into pellets, debinded, and subjected to reactive sintering in vacuum at 1715°C for 6 h. Each material was annealed in air with temperatures between 1300 and 1700°C. Samples were also compared to Cr:YAG ceramics with the addition of silica as a sintering aid. All the materials obtained were then exposed to 445 nm excitation, and emission spectra in the visible and infrared wavelengths were recorded. The results showed that the emission spectra of Cr:YAG ceramics varied according to the annealing conditions: as-sintered samples exhibited strong emissions of around 680 nm and, after air annealing, of around 1400 nm. This phenomenon is attributed to the Cr³⁺→Cr⁴⁺ transition. Samples doped solely with MgO exhibited the highest emission intensity in the infrared region. Thus, Mg²⁺ ions provided the best conversion efficiency of chromium ions.     

稀土镧、钇对蓝色氧化钨氢还原的影响

借助于ＳＥＭ、Ｘ射线衍射技术及ＩＰＰ粉末粒度仪等系统地研究了稀土镧、钇对蓝色氧化钨（ＢＯ）氢还原的影响。结果表明：稀土元素镧、钇在蓝色氧化钨的还原钨粉中以氧化物及钨酸盐形式存在；还原后所得的钨粉颗粒大多为规则形状的多面体；稀土镧、钇和铝相似，强烈地抑制ＢＯ氢还原钨粉颗粒的长大，而且钇的作用更为显著。     

Spherical Yttrium Aluminum Garnet Embedded in a Glass Matrix

Containerless processing was used to investigate the glass-forming behavior of Al₂O₃–Y₂O₃ glass. The amorphous bulk samples were obtained at compositions with 25–37.5 mol% yttria when the melt was cooled at a cooling rate of ∼250 K/s. Although small spherical particles (∼10 μm) with the same composition of the matrix were detected in the amorphous samples with 32.5–37.5 mol% yttria, the microfocus X-ray diffraction result indicated that the small spherical particles were crystalline Y₃Al₅O₁₂ garnet (YAG), rather than being amorphous. This observation suggested that small YAG particles could not grow larger after their nucleation, because of the high viscosity at high undercooling and the high cooling rate, which would graze the nose of the continuous cooling temperature diagram of YAG.     

好氧颗粒污泥对钇离子的吸附/解吸性能

为实现稀土尾水中钇离子（Y3+）的回收，探究了好氧颗粒污泥（AGS）对Y3+的吸附-解吸附效果。考察了混合方式、初始Y3+浓度、pH、盐度、铅离子及粒径对AGS吸附效果的影响。相比于搅拌及振荡，曝气混合下AGS具有更好的吸附效果，80%以上的吸附在前10 min完成。当初始Y3+浓度<50 mg/L时，AGS能完全吸附废水中Y3+离子，此后吸附率随着Y3+浓度的增大而减小。H+、Na+和Pb2+会与Y3+竞争AGS上的吸附位点，导致吸附率减小。0.6～1.0 mm的AGS吸附容量最大，2.4～3.0 mm的AGS经人工破碎后吸附容量增大15%。对吸附过程进行动力学和热力学拟合。动力学符合伪二级模型（R2=0.9999），表明化学吸附起主导作用；Webber-Morris方程分析表明颗粒内扩散是影响吸附速率的主要因素。热力学符合Langmuir模型（R2=0.9849），表明吸附过程是一个单分子层吸附过程，拟合得到最大吸附量为Qmax=24.39 mg/gSS。利用XPS对吸附前后AGS进行表征，发现参与吸附官能团有酯基、羧基、氨基，同时与K+进行离子交换，钇在AGS表面的主要化学态是Y2(CO3)3。探究了硝酸及氯化铵对吸附饱和AGS的解吸效果。HNO3的单次解吸附率（99%）明显高于NH4Cl（64%），但五次吸附-解吸附循环后，HNO3组解吸附率降至10%，NH4Cl组解吸附率仍维持在50%。     

石油亚砜树脂分离稀土的性能研究

应用石油亚砜萃取树脂与ＮＨ＿４ＣＮＳ体系，测定了稀土元素的分配比（Ｋｄ）、分离因素（β）和分离度Ｒｓ），讨论了ＮＨ＿４ＣＮＳ的浓度、稀土进样量和温度等对稀土分离的影响。应用于混合稀土的分离和测定，分析了６０．３２％的氧化钇，相对标准偏差为±１．４７％。     

苯丙烯酸邻菲罗啉铕钇配合物的合成及荧光特性

在乙醇介质中，合成了标题化合物，测定了其组成，红外光谱及荧光光谱，结果表明，羧酸的羟基氧及邻菲罗啉中的氮原子均与稀土离子配位，铕钇配合物的荧光强度值高于铕配合物。     

固相反应法制备YAG透明陶瓷

研究了固相反应法制备钇铝石榴石(yttrium aluminum garnet，YAG)透明陶瓷的工艺。采用高纯Y2O3和Al2O3超徽粉为原料，在1300℃煅烧2h，制备出YAG粉末。YAG相生成温度比常规温度大约低200℃。加入0．5％(质量分数)正硅酸乙醑烧结助剂后，YAG坯体在1700℃真空烧结5h，得到了高透光的YAG陶瓷，其在可见光区最大透光率为63％，在红外光区的透光率接近70％。YAG陶瓷具有均匀的微观结构，晶粒尺寸大约为10～30μm。