不添加烧结助剂制备透明的Y2O3陶瓷

以Y2O3粗粉、碳酸氢铵、硝酸和氨水为原料,通过沉淀法制备了Y2O3纳米粉体.发现沉淀工艺和煅烧温度显著影响Y2O3纳米粉的颗粒大小和尺寸分布,从而影响烧结体的密度和透光性.用X射线衍射分析仪、透射电镜、图像分析仪等研究发现,pH=8时制得的沉淀先驱物经1000℃煅烧,可得到粒度为33 nm,近球形,分散性好,尺寸分布窄的Y2O3粉体.该粉体不加任何添加剂,在1700℃真空烧结4 h可得到透明Y2O3陶瓷.     

复合沉淀法制备(Y,Gd)2O3:Eu纳米粉体及其发光性能

报道了一种采用氨水和碳酸氢铵的混合溶液作为复合沉淀剂来制备(Y，Gd)203：Eu发光粉体的新工艺，采用热分析(TG-DTA)、红外光谱(FT-IR)、X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)等手段对粉体制备过程中的物理化学变化进行了研究．通过X射线激发的发射光谱研究了Eu掺杂浓度和煅烧温度对(Y，Gd)2O3：Eu粉体发光性能的影响．结果表明采用复合沉淀法制备工艺，经过850℃烧2h，可以得到晶粒尺寸为50nm左右，且基本无团聚的(Y，Gd)2O3：Eu粉体，比表面积为23m^2／g，其X射线激发的发光强度较草酸盐沉淀法所得到的相同组分的粉体大大增强．     

Y1.34Gd0.60Eu0.06O3透明陶瓷材料的制备与发光性能

采用复合沉淀法制备了具有良好烧结活性的纳米级Y1．34Gd0．60Eu0．06O3粉体．经850℃／2h煅烧后，得到晶粒尺寸为30-40nm，且基本无团聚的Y1．34Gd0．60Eu0．06O3发光粉体，粉体比表面积为23m^2／g．该粉体经过适当的干压和等静压成型后，于1800℃以上温度烧结6h，可以获得Y1．34Gd0.60Eu0．06O3透明陶瓷．获得的透明陶瓷材料在波长250nm的紫外光激发下发射出较强的红光，发射主峰位于610nm，对应于掺杂Eu^3＋的^5D0-^7F2跃迁．     

氧化钇透明陶瓷的制备

以埔酸钇和碳酸氢铵为原料，通过向碳酸氢铵溶液滴加埔酸钇溶液，制备出了前驱物经950℃煅烧后颗粒尺寸大小为40-60nm的Y2O3粉体。该粉体在添加一定量的添加剂后经真空热压和热等静压成功烧结出红外透过率达82％的Y2O3透明陶瓷。     

低温法制取Y2O3透明陶瓷的研究

发展了一种制备高烧结性Y2O3粉的新途径，并以此为原料，在相对低温下采用普通烧结的办法制备出透明Y2O3陶瓷。以硝酸钇为母盐，氨水为沉淀剂，通过控制反应体系中硫酸根离子的含量，生成树枝状的前驱物晶粒，其轴径比为6，经过1100℃煅烧分解，获得一次颗粒为60nm，颗粒呈球形，低团聚高纯度的Y2O3粉体。该粉体经过模压成型，不加添加剂，于1700℃真空烧结，得到显微组织均匀的透明Y2O3多晶体，其在近红外区的透光率达70％。     

氯离子对氧化镁纳米粉体合成及烧结性能的影响研究

以无水碳酸钠和六水合氯化镁为原料,采用沉淀法,制备了纳米MgO粉体,重点考察了氯离子在粉体合成中的影响.研究表明,在沉淀工艺中掺入氯离子,可以改变先驱物的物相组成,获得以碱式碳酸镁和水合碳酸镁为主要组分的先驱物,在900℃煅烧后可以获得一次颗粒尺寸为40nm的MgO粉体.粉体制备中加入氯离子,烧结时具有促进氧化镁烧结致密化和晶粒长大的作用,同时还有利于获得晶粒尺寸分布均匀的显微组织.掺杂5%(质量分数)氯离子的粉体在空气气氛1200℃烧结3h,样品密度为96.4%,而相同条件下未掺杂氯离子样品的密度只有52.4%.     

共沉淀法制备YAG超细粉及透明陶瓷

研究了共沉淀法制备YAG透明陶瓷的工艺。采用Al(NO3)3和Y(NO3)3的混合溶液为母盐,以碳酸氢铵为沉淀剂,采用共沉淀法制备了化学组成为Y2(CO3)3·nH2O+NH4AlO(OH)HCO3的碳酸盐先驱沉淀物。使用透射电镜和X射线衍射对先驱沉淀物的形貌及煅烧过程的相转变进行了研究。结果表明先驱沉淀物在900℃煅烧2h后完全转变为YAG相。1100℃煅烧后得到的YAG粉体具有良好的烧结性能。使用0.5%(质量分数)的TEOS(正硅酸乙酯)作为烧结添加剂,1700℃真空烧结5h后,得到了透明YAG烧结体。     

碳酸铝铵热分解制备α-Al2O3超细粉

研究了以硫酸铝铵和碳酸氢铵为原料合成碳酸铝铵的工艺条件．在实验条件范围内，将硫酸铝铵溶液以低于1．2L．h－1的速度加入到碳酸氢铵溶液中，可合成碳酸铝铵；在其它操作条件下，获得的产物为γ－AlOOHγ－AlOOH升温过程中的物相变化次序为：γ－AlOOH→γ－Al2O3→δ－Al2O3→θ－Al2O3→α－Al2O3;而碳酸铝铵的相变次序为：碳酸铝铵→无定型Al2O3→θ－Al2O3→α－Al2O3碳酸铝铵转变为θ－Al2O3和α－Al2O3的温度均比γ－AlOOH低约100℃γ－AlOOH在1200℃煅烧1h方可完全转变为α－Al2O3，其颗粒尺寸为150um；粉体经1450℃、2h烧结相对密度为84.46％；而碳酸铝铵在1100℃煅烧1h就可完全转变为α-Al2O3，其颗粒尺寸为70um，粉体在相同的烧结条件下相对密度可达97.80％     

醇水共沉淀法制备Yb:YAG透明陶瓷及其性能研究（英文）

Yb:YAG透明陶瓷由于具有宽的吸收带和发射带、高增益、低的热负载、长的荧光寿命、高的量子效率等优点而成为有应用前景的高功率固体激光器用增益介质。本研究优化了粉体的性能并制备了高透明的Yb:YAG陶瓷。以碳酸氢铵为沉淀剂,分别以纯水或乙醇/水混合物为溶剂,采用共沉淀法合成了5at%Yb:YAG纳米粉体。在1250℃下煅烧4h得到的所有粉体均为纯YAG相。与纯水溶剂制备的粉体相比,醇水溶剂制备的粉体具有更小的平均晶粒尺寸和更低的团聚程度。以醇水溶剂制备的粉体为原料,采用真空烧结法在不添加烧结助剂的情况下成功制备了5at%Yb:YAG透明陶瓷,并对1500～1825℃烧结20 h和1800℃烧结10～50 h所得陶瓷的微观结构和直线透过率进行了探究。除在1825℃下烧结20 h所得的陶瓷外,其余的5at%Yb:YAG陶瓷都具有均匀的微观结构。在1800℃下烧结50 h制备的5at%Yb:YAG陶瓷具有最高的光学质量,在1100和400 nm处的直线透过率分别为78.6%和76.7%(样品厚度为2.2mm)。该Yb:YAG透明陶瓷在937nm处的吸收截面为5.03×10~(–21)cm~2,在1031nm处的发射截面为13.48×10~(–21) cm~2。     

固相反应法制备MgAl2O4纳米粉体及其烧结行为研究

在800℃下煅烧Al(OH)3和MgSO4混合粉末,冷却后经过水洗得到了结晶良好的MgAl2O4纳米粉体.采用DSC/TG、XRD、TEM和SEM等分析手段研究了混合粉末中Mg/Al原子比对颗粒尺寸及团聚状况的影响,以及MgAl2O4纳米粉体的烧结性能.所制备的MgAl2O4纳米粉体平均颗粒尺寸为12 nm,尺寸分布窄,团聚少.MgAl2O4的生成归因于γ-Al2O3和MgSO4的固相反应.MgAl2O4纳米粉体显示了良好的烧结活性,在1450℃烧结1 h即能获得相对密度为95%的MgAl2O4陶瓷.     

Dependence of photoluminescence (PL) emission intensity on Eu and ZnO concentrations in Y2O3:Eu and ZnO·Y2O3:Eu nanophosphors

Y₂O₃:Eu³⁺ and ZnO·Y₂O₃:Eu³⁺ nanophosphor powders with different concentrations of Eu³⁺ ions were synthesized by a sol-gel method and their luminescence properties were investigated. The red photoluminescence (PL) from Eu³⁺ ions with the main emission peak at 612 nm was observed to increase with Eu³⁺ concentration from 0.25 to 0.75 mol% and decreased notably when the concentration was increased to 1 mol%. The decrease in the PL intensity at higher Eu³⁺ concentrations can be associated with concentration quenching effects. The red emission at 612 nm was shown to increase considerable when ZnO nanoparticles were incorporated in Y₂O₃:Eu³⁺ while green emission from ZnO was suppressed. The increase is attributed to energy transfer from ZnO to Eu³⁺.     

Persistent luminescence of Eu and Dy doped barium aluminate (BaAl2O4:Eu,Dy) materials

Polycrystalline Eu²⁺ and Dy³⁺ doped barium aluminate materials, BaAl₂O₄:Eu²⁺,Dy³⁺, were prepared with solid state reactions at temperatures between 700 and 1500 °C. The influence of the thermal treatments on the stability, homogeneity and structure as well as to the UV-excited and persistent luminescence of the materials was investigated by X-ray powder diffraction, SEM imaging and infrared spectroscopies as well as by steady state luminescence spectroscopy and persistent luminescence decay curves, respectively. The IR spectra of the materials prepared at 250, 700, and 1500 °C follow the formation of BaAl₂O₄ composition whereas the X-ray powder diffraction of compounds revealed how the hexagonal structure was obtained. The morphology of the materials at high temperatures indicated important aggregation due to sintering. The luminescence decay of the quite narrow Eu²⁺ band at ca. 500 nm shows the presence of persistent luminescence after UV irradiation. The dopant (Eu²⁺) and co-dopant (Dy³⁺) concentrations affect the crystallinity and luminescence properties of the materials.     

A novel red phosphor NaLa4(SiO4)3F: Eu

A novel red phosphor NaLa₄(SiO₄)₃F: Eu³⁺ was synthesized by the conventional solid-state reaction at 950 °C for the first time. The luminescence properties of NaLa₄(SiO₄)₃F: Eu³⁺ were investigated, and the critical concentration of the activator concentration (Eu³⁺) was found to be 0.1 mol per formula unit. The phosphor presented red luminescence under the ultraviolet excitation of 254 or 395 nm, attributed to the transitions from ⁵D₀ excited states to ⁷F_J ( J = 0-4) ground states of Eu³⁺ ions. The results indicated that this newly-developed phosphor could find applications in tricolor fluorescent lamp, phosphor-liquid crystal displays and white lighting devices utilizing GaN-based excitation in the near UV.     

Preparation and characterization of Sr4Al2O7:Eu, Eu phosphors

A new composition of red strontium aluminate phosphor (Sr₄Al₂O₇:Eu³⁺, Eu²⁺) is synthesized using a solid state reaction method in air and in a reducing atmosphere. The investigation of firing temperature indicates that a single phase of Sr₄Al₂O₇ is formed when the firing temperature is higher than 1300 °C and that a Sr₃Al₂O₆ phase is formed as the main peak below 1300 °C. The effects of firing temperature and doping concentration on luminescent properties are investigated. Sr₄Al₂O₇ phosphors exhibit the typical red luminescent properties of Eu³⁺ and Eu²⁺. A comparison photoluminescence study with Sr₃Al₂O₆ phosphor shows that Sr₄Al₂O₇ has higher emission intensity than Sr₃Al₂O₆ as a result of the higher optimum doping concentration of Sr₄Al₂O₇ phosphor.     

Effects of packaging SrI2(Eu) scintillator crystals

Recent renewed emphasis placed on gamma-ray detectors for national security purposes has motivated researchers to identify and develop new scintillator materials capable of high energy resolution and growable to large sizes. We have discovered that SrI₂(Eu) has many desirable properties for gamma-ray detection and spectroscopy, including high light yield of ∼90,000 photons/MeV and excellent light yield proportionality. We have measured <2.7% FWHM at 662 keV with small detectors (<1 cm³) in direct contact with a photomultiplier tube, and ∼3% resolution at 662 keV is obtained for 1 in.³ crystals. Due to the hygroscopic nature of SrI₂(Eu), similar to NaI(Tl), proper packaging is required for field use. This work describes a systematic study performed to determine the key factors in the packaging process to optimize performance. These factors include proper polishing of the surface, the geometry of the crystal, reflector materials and windows. A technique based on use of a collimated ¹³⁷Cs source was developed to examine light collection uniformity. Employing this technique, we found that when the crystal is packaged properly, the variation in the pulse height at 662 keV from events near the bottom of the crystal compared to those near the top of the crystal could be reduced to <1%. This paper describes the design and engineering of our detector package in order to improve energy resolution of 1 in.³-scale SrI₂(Eu) crystals.     

Optical properties of Ba2SiO4:Eu phosphor for green light-emitting diode (LED)

Eu²⁺ activated Ba₂SiO₄ phosphors were synthesized at 1573 K by solid-state reactions under a weak reductive atmosphere and systematically investigated by photoluminescence excitation and emission spectra, diffuse reflectance spectra, concentration quenching process and lifetime. The intensive green LEDs were fabricated by combining the synthesized phosphors with near-ultraviolet InGaN chips (λ_em = 395 nm). The Commission Internationale de I’Eclairage color coordinate of the fabricated LEDs is calculated to be x = 0.1904, y = 0.4751 under 20 mA forward-bias current. The dependence of the green LEDs on forward-bias currents shows that as the current increases, the relative intensity simultaneously increases and the color coordinate presents excellent stability, falling in the standard area of the Institute of Transportation Engineers for traffic lights and the Society of Automotive Engineers for automotive displays. These results indicate that the fabricated phosphor-converted green LEDs show great potential for traffic lights and automotive display applications.     

Synthesis and structural characterization of Eu(III)-doped Zn7Sb2O12

In addition to the lanthanide series elements, Europium is one of the chemical elements of greatest interest for the development of species with oxidation state +3 (III), which leads to interesting electronic transitions. In a general sense, their emission spectrum lines are narrow and sensitive to effects of the ligand field around metallic ions. This property allows the use of Eu(III) as a structural probe. In this work, samples of semiconductor Zn₇Sb₂O₁₂ and of solid solutions based on isoelectronically Eu(III)-doped Zn₇Sb₂O₁₂ with stoichiometry Zn_7−3x Eu_2x Sb₂O₁₂ were prepared. Both Zn₇Sb₂O₁₂ and Zn_7−3x Eu_2x Sb₂O₁₂ were synthesized via a chemical route using Pechini’s method and characterized by Fourier transform infrared absorption vibrational spectroscopy (FTIR) and photoluminescence spectroscopy. In order to perform further spectral analyses, each spectrum was adjusted using a set of Gaussian functions. The FTIR spectrum analysis showed a slight band shift of the vibration mode assigned to the Sb–O bonding ascribed to the [SbO₆] octahedron vibration. The theoretical fitting of the luminescence curves showed a broadening of the most intense emission peaks related to the transition Eu(III) ⁵D₀ → ⁷F₂. As a whole, the results suggest that a less symmetric Eu(III) site occupation in inverse spinel structure may occur in sites close to the antimony octahedron, involving, however, non-substitutional site occupation.     

Luminescent properties of Eu-activated nanophosphors Ca3Y0.8Gd0.2(VO4)2.4(PO4)0.6: Eu for light-emitting diodes

Eu³⁺-doped Ca₃Y_0.8Gd_0.2(VO₄)_2.4(PO₄)_0.6 nanophosphors have been prepared by modified solid-state reaction. X-ray powder diffraction, transmission electron microscopy (TEM), photoluminescence excitation and emission spectra were used to characterize the resulting samples. X-ray powder diffraction (XRD) analysis confirmed the formation of YVO₄. Photoluminescence (PL) results showed that the phosphor could be efficiently excited by UV-visible light from 350 to 550 nm, exhibiting bright orange-red emission(excited by 397) and red emission(excited by 467), which has potential application as a phosphor for UV and blue GaN-based light-emitting diodes (LEDs). TEM images show that the grain size of Ca₃Y_0.45Eu_0.35Gd_0.2(VO₄)_2.4(PO₄)_0.6 is about 39 nm, which is in full agreement with the theoretical calculation data from the XRD patterns.     

Photoluminescence properties of NaGd(MoO4)2:Eu nanophosphors prepared by sol-gel method

NaGd(MoO₄)₂:Eu³⁺ (hereafter NGM:Eu) phosphors have been prepared by sol-gel method. The properties of the resulting phosphors are characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), photoluminescence (PL) spectra and decay curve. The excitation spectra of NGM:Eu phosphors are mainly attributed to O → Mo charge-transfer (CT) band at about 282 nm and some sharp lines of Eu³⁺ f-f transitions in near-UV and visible regions with two strong peaks at 395 and 465 nm, respectively. Under the 395 and 465 nm excitation, intense red emission peaked at 616 nm corresponding to ⁵D₀ → ⁷F₂ transition of Eu³⁺ are observed for 35 at.% NGM:Eu phosphors as the optimal doping concentration. The luminescence properties suggest that NGM:Eu phosphor may be regarded as a potential red phosphor candidate for near-UV and blue light-emitting diodes (LEDs).     

Novel blue-emitting phosphor NaMg4(PO4)3:Eu, Ce with energy transfer

A blue-emitting phosphor of NaMg₄(PO₄)₃:Eu²⁺, Ce³⁺ was prepared by a combustion-assisted synthesis method. The phase formation was confirmed by X-ray powder diffraction measurement. Photoluminescence excitation spectrum measurements show that the phosphor can be excited by near UV light from 230 to 400 nm and presents a dominant luminescence band centered at 424 nm due to the 4f⁶5d¹ → 4f⁷ transition of Eu²⁺ ions at room temperature. Effective energy transfer occurs in Ce³⁺/Eu²⁺ co-doped NaMg₄(PO₄)₃ due to large spectral overlap between the emission of Ce³⁺ and excitation of Eu²⁺. Co-doping of Ce³⁺ enhances the emission intensity of Eu²⁺ greatly by transferring its excitation energy to Eu²⁺, and Ce³⁺ plays a role as a sensitizer. Ce³⁺-Eu²⁺ co-doped NaMg₄(PO₄)₃ powders can possibly be applied as blue phosphors in the fields of lighting and display.