Local microstructure and photoluminescence of Er-doped 12CaO·7Al2O3 powder

Er-doped 12Ca0.7Al2O3 （C12A7：Er） powders were prepared using the sol-gel method followed by annealing inorganic precursors. X-ray diffraction （XRD）, Raman and absorption spectra revealed that Er ions existed and substituted Ca^2＋ lattice site in C12A7. The photoluminescence of C12A7：Er at room temperature was observed in the visible and infrared region using 488 nm （2.54 eV） Ar^＋ line as excitation source, respectively. The sharp and intense green emission bands with multi-peaks around 520 nm and 550 nm correspond to the transitions from the excited states ^2H11/2 and ^4S3/2 tO the ground state ^4I15/2, respectively. Furthermore, red emission band around 650 nm was also observed. It was attributed to the electronic transition from excited states ^4F9/2 to the ground state ^4I15/2 inside 4f-shell of Er^3＋ ions. The intensive infrared emission at 1.54 μm was attributed to the transition from the fast excited states of ^4I13/2 to the ground state （^4I15/2）. The temperature dependent photoluminescence of infrared emission showed that the integrated intensity reached a maximum value at near room temperature. The forbidden transitions of intra-4f shell electrons in free Er^3＋ ions were allowed in C12A7 owing to lack of the inversion symmetry in the Er^3＋ position in C12A7 crystal field. Our results suggested that C12A7：Er was a candidate for applications in Er-doped laser materials, and full color display.     

12CaO·7Al2O3 炉渣与合金钢液的反应

 12CaO·7Al2O3炉渣组成为w(SiO2)=6%,w(Al2O3)=46%,w(CaO)=48%,与合金结构钢钢液进行了实验室试验。结果表明,该渣具有很高的碱度,90 min反应结束后钢中w(TO)=0000 6%~0001 3%,w(S)=0000 4%~0001 0%。同时得出为控制钢中总氧含量应将炉渣碱度控制在9左右,钢中生成的夹杂物大都是低熔点、球状、尺寸很小的钙镁铝硅酸盐类夹杂物,这类夹杂物能够避免钢材产生各向异性,并且在轧制时能够稍许变形,能够提高钢材的抗疲劳性能。     

Up-conversion luminescence of Er~(3+)-doped and Yb~(3+)/Er~(3+) co-doped 12CaO·7Al_2O_3 poly-crystals

The optical properties of Er3+-doped and Yb3+/Er3+ co-doped 12CaO·7Al2O3 (C12A7) poly-crystals, synthesized by high temperature solid state method, were investigated in detail. For Er3+-doped and Yb3+/Er3+ co-doped C12A7 poly-crystals, two main emission bands centered around 530/550 nm (green) and 660 nm (red) were observed under 980 nm diode laser excitation via an up-conversion process. The intensity of green up-conversion emission had a strong increase in Er3+ (1.0 mol.%, 1.5 mol.%, 3.0 mol.%), and the i...     

12CaO·7Al2O3预熔渣在精炼过程中的粉化问题

为降低生产成本,拟用较低等级的高铝矾土熟料粉(w(Al2O3)=80%)配料生产12CaO·7Al2O3预熔精炼渣,熔融液态渣冷却凝固后出现粉化问题.分析了粉化原因,研究了几种解决方案,最终提出预熔喷吹造粒生产预熔精炼渣的技术方案.     

Up-conversion luminescence of Er~（3＋）-doped and Yb~（3＋）/Er~（3＋） co-doped 12CaO·7Al_2O_3 poly-crystals

The optical properties of Er3+-doped and Yb3+/Er3+ co-doped 12CaO·7Al2O3 (C12A7) poly-crystals, synthesized by high temperature solid state method, were investigated in detail. For Er3+-doped and Yb3+/Er3+ co-doped C12A7 poly-crystals, two main emission bands centered around 530/550 nm (green) and 660 nm (red) were observed under 980 nm diode laser excitation via an up-conversion process. The intensity of green up-conversion emission had a strong increase in Er3+ (1.0 mol.%, 1.5 mol.%, 3.0 mol.%), and the intensity ratio of red to green up-conversion emission had an increase in Yb3+ (1.0 mol.%, 2.0 mol.%, 10. 0 mol.%)/Er3+ (fixed at 1.0 mol.%). This detailed study of the up-conversion processes allowed us to identify the dominant up-conversion mechanisms in Er3+-doped and Yb3+/Er3+ co-doped C12A7 poly-crystals.     

Preparation and Upconversion Luminescence of Y3Al5O12 ： Yb^3＋ , Er^3＋ Trapsparent Ceramics

YAG： 1% （atom fraction） Yb^3＋ , 0.5% （atom fraction） Er3＋ transparent ceramics were fabricated by the solid state reaction method using high-purity Y2O3, Al2O3, Yb2O3, and Er2O3 powders as starting materials. The mixed powder compact was sintered at 1760 ℃ for 6 h in vacuum and annealed at 1500 ℃ for 10 h in an air atmosphere. The ceramics consisted of about 10μm grains and exhibited a pore-free structure. The optical transmittance of the ceramics at 1064 nm was nearly 80%. Upconversion emissions were investigated on the ceramics pumped by a 980 nm continuous wave diode laser, and strong green emission centered at 523 and 559 nm and red emission centered at 669 nm were observed, which originated from the radiative transitions of ^2H11/2→^4I15/2, ^4S3/2→^4I15/2, and ^4F9/2→^4I15/2 of Er^3＋ ions, respectively.     

12 CaO·7 Al2 O3晶体结构及其氧化铝浸出性能

使用分析纯试剂配料,在1350℃保温1 h的条件下合成了A/S=5(Al2O3与Si O2质量比)的铝酸钙熟料.研究了钙铝比C/A(除去与Si O2结合的Ca O后Ca O与Al2O3的摩尔比)对熟料中12Ca O·7Al2O3晶体结构及其氧化铝浸出性能的影响,并通过X射线衍射和X射线荧光等分析手段对其作用机理进行了探讨.结果表明:由于12Ca O·7Al2O3量的增加,C/A=1.0~1.4时,石灰烧结法熟料溶出率随着C/A的提高而提高;在C/A=1.4时,熟料溶出率最高可达93.30%,此时Ca O的缺失形成了有缺陷的12Ca O·7Al2O3,且其中Ca O的物质的量小于11.3 mol;钙铝比提高到1.7时熟料溶出率又出现了下降趋势,这是由于Ca O的饱和导致12Ca O·7Al2O3晶体择优生长取向发生变化,由(211)面开始向(420)晶面转变.     

Synthesis and Spectral Properties of Nd^3＋： Gd3Ga5O12 Nanopowder for Transparent Laser Ceramics

Nd^3＋： Gd3Ga5O12（Nd ： GGG） nanopowder for transparent laser ceramics was synthesized using sol-gel method. XRD, SEM, and fluorescence spectrum were used to study the properties of Nd^3＋ ：Gd3Ga5O12 nanopowder. XRD patterns of samples show that it has a cubic structure. Meanwhile, pure Nd：GGG crystals were obtained at 1000 ℃ for 12 h. SEM photographs show that dispersed, uniform, ball-like Nd：GGG nanopowder is obtained. Both XRD and SEM results show that the crystallization degree and the grain size increase with the increase in calcining temperature. Analysis of fluorescence spectrum shows that fluorescence emission occurs at 1062.7 nm, which is the result of Nd^3＋ （^4F3/2→^4I11/2） transition. Homogenous Nd ： GGG nanopewder with a small grain size synthesized using the sol-gel method is favorable for sintering the transparent ceramic, which proves that the nanopewder obtained is suitable as a precursor for preparing GGG transparent ceramics.     

C12A7炉渣与合金钢液平衡时的Al行为

实验研究得出C12A7炉渣(其组成为:w(SiO2)=6%,w(Al2O3)=46%,w(CaO)=48%)与合金钢液(其化学成分类似42CrMo钢)反应90 min后,钢中w(Al2)=(80～100)×10-6,与之平衡的钢中w(T.O):(6～13)×10-6,生成的夹杂物大都是尺寸很小的低熔点球状钙镁铝硅酸盐类夹杂.从热力学的角度得出了当C12A7炉渣与合金钢液达到平衡时钢中的铝含量以及平衡条件下钢中铝含量较低时也能将钢中氧含量控制在很低范围的原因.     

Formation and Evolution Mechanism of the Inclusions of Al2O3·SiO2·CaO and Al2O3·SiO2·CaO·MgO in Seamless Steel Tube Steel

Herein, the formation and evolution mechanism of inclusions of Al₂O₃·SiO₂·CaO and Al₂O₃·SiO₂·CaO·MgO in seamless steel tube steel are investigated. In the long strip defects on the longitudinal cross section of the steel tube after the rolling bar piercing, the defect is mainly formed by Al₂O₃·SiO₂·CaO·MgO inclusions and Al₂O₃·SiO₂·CaO·inclusions dotted with·CaS inclusions after the rolling. The typical inclusions in the different steelmaking stages are mainly composed of CaS, Al₂O₃·(SiO₂), CaO·(SiO₂), MnS·(TiN), Al₂O₃·SiO₂·CaO·(CaS)·(MnS), Al₂O₃·SiO₂·CaO·MgO·(MnO), Al₂O₃·SiO₂·CaO·MgO·(CaS)·(MnS), etc. In the billet, the average sizes of Al₂O₃·SiO₂·CaO-based and Al₂O₃·SiO₂·CaO·MgO-based inclusions are much larger than those of the other types of inclusions. Part of SiO₂ in the deoxidized products SiO₂ can be reduced by [Al], resulting in the formation of the Al₂O₃·SiO₂ composite inclusions. The SiO₂ in Al₂O₃·SiO₂ inclusions can continuously be reduced by the dissolved [Ca] to form the Al₂O₃·SiO₂·CaO composite inclusions. The SiO₂ in the Al₂O₃·SiO₂·CaO inclusions can be reduced by the dissolved [Mg] to form the Al₂O₃·SiO₂·CaO·MgO composite inclusions. Another formation process of Al₂O₃·SiO₂·CaO·MgO inclusions is the entrapment of ladle slag in the vacuum degassing (VD) stage, due to the strong agitation of the rising Ar bubbles in the vacuum condition of the VD stage.     

12CaO·7Al2O3基精炼渣脱硫试验

在试验室用MoSi₂井式电阻炉试验研究了12CaO·7Al₂O_O3的预熔工艺和含10%～20%BaO、2%～6%MgO、1%～3%Li₂O,（12CaO·7Al₂O₃）/SiO₂=8～10的12CaO·7Al₂O₃基精炼渣对成分为（%）0.23C、1.29Mn、0.44Si、0.026P、0.023S、0.04Mo、0.02Cr、0.06Cu的低碳钢的脱硫能力。结果表明,12CaO·7Al₂O₃基预熔精炼渣具有较好的脱硫能力,在1 590℃加入量为3%的条件下,能将钢液中的硫含量从0.030%降低到0.006%,脱硫率80.00%。通过运用正交方法对渣成分进行优化,得出12CaO·7A国₂O₃基精炼渣的优化渣系为:15%BaO,4%MgO,3%Li₂O,（12CaO·7Al₂O₃）/SiO₂=9。     

Investigation of Chemical Bond Properties and Moessbauer Spectroscopy in YBa2 Cu3O7

Chemical bond properties of YBa2Cu3O7 were studied by using the average band-gap model. The calculated resuits show that the covalency of Cu(1)-O bond is 0. 406, and one of Cu(2) -O is 0.276. Moessbauer isomer shifts of ^57Fe in Y-123 were calculated by the chemical surrounding factor h,defined by covalency and electronic polarizability.The charge-state and site of Fe were determined. The relation between the coupling constant of electron-phonon interaction and covalency is employed to explain that the Cu(2)-O plane is more important than the Cu(1)-O chain on the super-conductivity in the Y-123 compounds.     

12CaO·7Al2O3炉渣与合金钢液的反应

12CaO·7Al2O3炉渣组成为w（SiO2）-6％,w（Al2O3）-46％,w（CaO）=48％,与合金结构钢钢液进行了实验室试验。结果表明,该渣具有很高的碱度,90min反应结束后钢中w（TO）=0．0006％～0．0013％,w（S）=0．0004％～0．0010％。同时得出为控制钢中总氧含量应将炉渣碱度控制在9左右,钢中生成的夹杂物大都是低熔点、球状、尺寸很小的钙镁铝硅酸盐类夹杂物,这类夹杂物能够避免钢材产生各向异性,并且在轧制时能够稍许变形,能够提高钢材的抗疲劳性能。     

Sol-gel processed Ce^3＋, Tb^3＋ codoped white emitting phosphors in Sr2Al2SiO7

Sr2Al2SiO7：Ce^3＋, Tb^3＋ white emitting phosphors were fabricated using the sol-gel method. X-Ray Powder Diffraction （XRD） analysis confirmed the formation of Sr2Al2SiO7：Ce^3＋, Tb^3＋. Scanning Electron Microscopy （SEM） observation indicated that the microstructure of the phosphor consisted of regular fine grains with an average size of about 0.5-1 μm. Luminescence properties were analyzed by measuring the photoluminescence spectra. The Ce^3＋, Tb^3＋-codoped Sr2Al2SiO7 phosphors showed four main emission peaks： one at 414 nm for Ce^3＋ and three at 482, 543, and 588 nm for Tb^3＋. The emission spectra of the samples with different doping concentrations showed that the Tb^3＋ emission was dominant because of the persistent energy transfer from Ce^3＋. The decay characteristic was better than that prepared by the solid-state process in the comparable condition. The codoped phosphor displayed long persistent white phosphorescence.     

硼氧酸盐(K2O·CaO·4B2O3·12H2O)的合成与表征

以氯化钙、四硼酸钾为原料,以水为溶媒,采用易于工业化、无污染的水溶液法制备一种新型硼酸钾钙复盐.该方法工艺条件为:去离子水450ml,四硼酸钾和氯化钙的质量比65:7.5,搅拌转速400 r/min,45℃反应3 h.通过化学分析、红外光谱、X射线衍射、扫描电镜等分析测试方法,对所合成的复盐进行了分析和表征.考察了反应温度对晶体形貌的影响.结果表明:所采用的工艺条件是合适的,制备的K2O·CaO·4B2O3·12H2O硼酸钾钙复盐晶型发育良好、形貌规整.反应温度的不同会使硼酸钾钙复盐的形貌发生改变.     

Luminescent properties of amorphous phosphor 1.4YeO3·2.5Al2O3·0.1Tb2O3 prepared by sol-gel method

Amorphous phosphor 1.4YeO3·2.5Al2O3·0.1Tb2O3 （the same composition as Y2.8Tb0.2Al5O12） was prepared via a sol-gel method at relatively low temperature （i.e., below 650℃）, which is much lower than that for the preparation of polycrystalline Y3Al5O12：Tb^3＋ （above 1400℃）. The amorphous phosphor prepared in the optimized conditions showed a bright green-yellowish luminescence, the intensity of which was comparable with that of polycrystalline sample and the emissions of which were assigned to 5D4 → 7Fj transitions of Tb^3＋. Besides the emissions of Tb^3＋, the amorphous samples prepared at temperatures below 500 ℃ presented a weak blue emission band around 420 nm.     

Preparation and photoluminescence of Tb^3＋ doped SrAl2O4 phosphor by composite combustion method

High-efficient Tb^3＋ activated SrAl2O4 phosphor was synthesized by a combined combustion-solid-state reaction method. The precursor of SrAl2O4：Th^3＋ phosphor was prepared via a combustion process, and then the as-prepared powder was heated in a reductive ambient of activated carbon at 1250 ℃ for 1 h. The results of X-ray diffraction, scanning electron microscopy, and photoluminescence spectra revealed the influence of the dosage of urea and heated process on the crystallinity, morphology, and photoluminescence of the phosphor. Comparing with traditional solid-sate reaction, the crystallinity and emission intensity of the SrAl2O4：Tb^3＋ phosphor were improved by this two-step process.     

[C4H7N2]3·PMo12O40配合物晶体的形貌模拟及其最佳纳米化计算的探讨

采用量子化学计算软件Material Studio的Morphology模块BFDH法则模拟了[C4H7N2]3·PMo12O40配合物晶体生长稳定外形,以晶体模拟形貌为基础,运用纳米计算方法通过对[C4H7N2]3·PMo12O40的不同纳米微粒总晶胞数、总原子数、比表面积、单颗粒表面原子数、单颗粒表面晶胞数及表面活性原子比例的计算,得出了[C4H7N2]3·PMo12O40纳米微粒的最佳纳米尺度为135 nm,认为晶体纳米化过程中[C4H7N2]3·PMo12O40制备到该尺度范围,理论上[C4H7N2]3·PMo12O40的活性和稳定性会达到均衡的最佳状态.