Nanostructured yttrium aluminum garnet powders synthesized by co-precipitation method using tetraethylenepentamine

Tetraethylenepentamine(C8H23N5,TEPA) has been used as a novel precipitant to synthesize yttrium aluminum garnet(Y3Al5O12,YAG) precursor from a mixed solution of aluminum and yttrium nitrates via a normal-strike co-precipitation method without controlling the pH value during precipitation process.The original precursor was analyzed by thermogravimetry/differential scanning calorimetry(TG/DSC).The evolution of phase composition and micro-structure of the as-synthesized YAG powders were characterized by X-ray ...     

Effect of Sulfate Ions on YAG Powders Synthesized by Microwave Homogeneous Precipitation

Using Al(NO3)3·9H2O, NH4Al(SO4)2·12H2O, Y(NO3)3 as mother salts, and urea as precipitant, YAG nano-powders were synthesized by microwave homogeneous precipitation. The composition, morphology, and phase transformation of precursor were analyzed by IR, XRD and TEM. The size distribution of YAG powders was characterized using laser diffraction method. The results show that sulfate ions influence the dispersion, composition and morphology of the YAG precursors. The addition of moderate sulfate ions can produce YAG powders with nano size and excellent dispersion at 1100 ℃.     

Study on co-precipitation synthesized Y3Al5O12:Ce yellow phosphor for white LED

A precursor of the Y3Al5O12:Ce (YAG:Ce) phosphor was obtained by co-precipitation of the solution of high purity nitrates with ammonium bicarbonate solution. The precipitation process of the precursor was studied in this work. YAG:Ce yellow phosphors with fine morphology was synthesized by annealing the precursor at a reducing atmosphere. The crystal phase, microstructure of the phosphors and their photoluminescence were investigated. The results indicated that the pure phase of YAG:Ce could be obtained at ...     

Synthesis and characterization of YAG:Ce³⁺ fluorescence powders by co-precipitation method

YAG:Ce3+(Yttrium aluminum garnet) fluorescence powders were successfully prepared by co-precipitation method using aluminum nitrate,yttrium nitrate,cerous nitrate as the starting materials and ammonium carbonate as precipitant.The products were characterized by X-ray powder diffraction,luminescence spectrometer,transmission electron microscope(TEM).The XRD results showed that the obtained YAG:Ce3+ fluorescence powders had the crystalline structures of YAG at calcinations temperature of 900 oC and the TEM results showed that the grain diameters were about 100 nm.The YAG:Ce3+ fluorescence powders,synthesized by co-precipitation method,had the best luminescence property when the Ce doping amount was x=0.06 in the molecular formula of Y3-xCexAl5O12,the calcinations time was 2 h and the calcinations temperature was 1000 °C.     

Microstructural characteristics of Nd:YAG powders leading to transparent ceramics

We reported on the successful synthesis of the Nd:YAG (Nd:Y3Al5O12) nano-powders by using urea as the precipitant with the microwave assisted homogeneous precipitation (MAHP) method. The different microstructural characteristics of the Nd:YAG nano-powders were affected by the concentrations of (Y3++Nd3+) and Al3+ ([Y3++Nd3+]=0.06 mol/L, [Al3+]=0.1 mol/L), aging time (6 d) and aging condition (in vessel). The optimum microstructural characteristics of the high quality Nd:YAG nano-powders leading to transparent Nd:YAG ceramics including the pure YAG phase, the smallest crystallite size, a uniform crystallite size distribution, less density defects, uniform micro-components and the proper molar ratio of (Y3++Nd3+) and Al3+ (0.6148) were discussed.     

Influence of ammonium sulfate on YAG nanopowders and Yb:YAG ceramics synthesized by a novel homogeneous co-precipitation method

Homogeneous and dispersed Y_3 Al_5 O_(12)(yttrium aluminum garnet,YAG) nanopowders were synthesized via a homogeneous co-precipitation method from the mixed solutions of yttrium nitrate,aluminum nitrate and a small amount of ammonium sulfate using hot urea as the precipitant.The method has the superiorities that co-precipitation of cations is ensured and continuous decomposition of the hot urea is achieved to obtain the narrow size distribution particles.The addition of small amount of ammonium sulfate surfactant,although has no influence on YAG garnet phase formation,has significant effect on dispersion,particles distribution and sinterability of the resultant YAG and Yb:YAG powders.Compared with the undoped sample,the green body of Yb:YAG doped with ammonium sulfate has higher total shrinkage,linear shrinkage rate and relative density through sintering at 1600 ℃.The resultant Yb:YAG powders can be sintered into transparent ceramics at 1700 ℃ through vacuum sintering.The influence of the sulfate ions on characteristics of the resultant powders was thoroughly studied.     

Preparation and characterization of Y3Al5O12:Ln（Ln=Eu,Ce） phosphor powders by ultrasonic atomization and co-precipitation process

A novel technique for YAG:Ln(Ln=Eu,Ce) phosphor powder synthesis with a nanocrystalline structure was developed.Nanocrystalline YAG:Ln powder was prepared by an ultrasonic atomization and co-precipitation method using a mixture solution of ammonium hydroxide(NH3·H2O) and ammonium hydrogen carbonate(NH4HCO3) as precipitant.The as-prepared nano-powders were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),and fluorescence spectrometer.The obtained phosphor powders were homogenous and in size of 50-70 nm.The results demonstrated that by using ultrasonic atomization and co-precipitation process,we could synthesize a good quality YAG:Ln(Ln=Eu,Ce) phosphor powder that had many potential applications.     

Synthesis of Polycrystalline Nd∶YAG Nanopowders Used for Sintering Transparent Ceramics via Gel Combustion

Polycrystalline nano-sized neodymium doped yttrium aluminum garnet (Nd∶Y3Al5O12, Nd∶YAG) powders were synthesized via a gel combustion method using nitrates and citric acid as starting materials. The evolution of phase composition and micro-structure of the powders were characterized by X-ray powder diffraction, thermogravimetry/differential thermal analysis and scanning electron microscopy. Well-crystallized Nd∶YAG nano-sized powders could be obtained at 950 ℃ for 2 h. The resultant powders are well dispersed, have a relatively narrow size distribution with an average particle size of approximately 50 nm, and show excellent sinterability. These powders can be densified to 99.2% of the theoretical density by HP sintering at 1700 ℃ for 3 h under 20 MPa nitrogen pressure.     

Synthesis and Characterization of Er3+∶Y3Al5O12 Nanocrystalline Powders Prepared by Sol-Gel Method

Nano-sized Er3 ∶Y3Al5O12 powders was successfully prepared via a simple sol-gel route at as low a temperature at 800 ℃ whereas a temperature much higher is necessary to obtain this compound by solid state synthesis (about 1500 ℃). The phase purity, composition and microstructural features of the materials were analyzed by means of X-ray diffraction(XRD), infrared spectroscopy(IR) and transmission electron microscopy(TEM), and no other intermediate phase were observed to form in the range of 700～1000 ℃. The luminescence spectra of Er3 substituted for Y3 in YAG in 1% content was characterized on samples at different temperature.     

共沉淀法制备稀土石榴石Ln3Al5O12(Ln=Y, Ce, Yb)

以Y2O3、Yb2O3、Al(NO3)3.9H2O和Ce(NO3)3.6H2O为原料,NH4HCO3、NH3.H2O做复合沉淀剂,用共沉淀法制备纳米稀土石榴石Ln3Al5O12(LnAG,Ln=Y,Ce,Yb)粉体。用TG/DTA、XRD、SEM、TEM等手段对LnAG前驱体及煅烧后的粉体进行表征。结果表明,用上述方法在1 000℃煅烧3h可得到分散性好、形状规则且粒径为50nm左右的Y3Al5O12、Yb3Al5O12、Y2.9Ce0.1Al5O12石榴石粉体,但不能得到Ce3Al5O12石榴石,合成石榴石粉体的最佳煅烧温度为1 050℃以上。     

Citrate sol-gel combustion preparation and photoluminescence properties of YAG:Ce phosphors

Yellow-emitting YAG:Ce3+ nanocrystalline phosphors were prepared by citrate sol-gel combustion method using citric acid as the fuel and chelating agent. The influence of mole ratio of citric acid to metallic ions (MRCM), pH value of the solution, calcination temperature and Ce-doped concentration on the structures and properties of as-prepared powders were investigated in detail. Higher crystallinity and better luminescence performance powders were obtained at MRCM=2, pH=3 and the calcination temperature of 1200 °C. The phosphors exhibited the characteristic broadband visible luminescence of YAG:Ce. The optimum concentration of Ce3+ was 1.0 mol.%, and the concentration quenching was derived from the reciprocity between electric dipole and electric quadrupole (d-q). Especially, the pH value of the solution was a key factor to obtain a stable sol-gel system and then obtain pure and homogeneous rare earth ions doped YAG phosphors at a lower tem-perature. The Y3Al5O12:Ce0.03 phosphor with optimized synthesis-condition and composition had a similar luminescence intensity with the commercial phosphor YAG:Ce.     

Preparation of Neodymium-Doped Yttrium Aluminum Garnet Transparent Ceramics by Homogeneous Precipitation Method

Neodymium-doped yttriumaluminumgarnet(Nd∶YAG)transparent polycrystalline ceramics,laser ce-ramic matrix materials,are gradually becomingsubsti-tutes for single crystals because they are provided withpredominantly chemical stability,highly doped ionconcentration,excellent optical performance and hightemperature stability[1,2].Presently,the conventionallyused methods to produce Nd∶YAG powders are solid-state processes[3],chemical precipitation methods[4,5]andlowtemperature combustiontechniqu…     

Preparation and characterization of Y3Al5O12:Ln (Ln=Eu,Ce) phosphor powders by ultrasonic atomization and co-precipitation process

A novel technique for YAG:Ln (Ln=Eu, Ce) phosphor powder synthesis with a nanocrystalline structure was developed. Nanocrystalline YAG:Ln powder was prepared by an ultrasonic atomization and co-precipitation method using a mixture solution of ammonium hydroxide(NH₃·H₂O) and ammonium hydrogen carbonate(NH₄HCO₃) as precipitant. The as-prepared nano-powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and fluorescence spectrometer. The obtained phosphor powders were homogenous and in size of 50-70 nm. The results demonstrated that by using ultrasonic atomization and co-precipitation process, we could synthesize a good quality YAG:Ln (Ln=Eu, Ce) phosphor powder that had many potential applications.     

Synthesis of monodispersed nanometer-sized YAG powders by a modified coprecipitation method

Nanometer-sized yttrium aluminum garnet （YAG） powders were synthesized by using the coprecipitation method with ammo- nium hydrogen carbonate as a precipitant. The results indicated that an extremely loose YAG precursor was obtained when iodine was intro- duced in the coprecipitation process on the condition that the initial concentrations of Y^3＋ and Al^3＋ in the solution were set at 0.018 and 0.03 mol/L, respectively, and pH=8. Consequently, the resulting YAG powders after calcination at 1173 K for 2 h were composed of monodispersed particles with an average grain size of 30 nm and better sinterability. The present results indicated that the modified coprecipitation method, with iodine as an additive, was superior to the conventional coprecipitation method, to synthesize ultrafine YAG powders.     

沉淀温度对制备铈掺杂YAG粉体的影响

文中采用共沉淀法来制备铈掺杂YAG前驱体.为获得纯相YAG:Ce3+粉体,实验以CeO₂、Y₂O₃、Al(NO₃)₃·9H₂O和NH₄HCO₃为原料,在不同的沉淀温度下来制备YAG:Ce3+前驱体,将所制得的前驱体经高温煅烧还原得到YAG:Ce3+粉体,并通过TG/DTA、XRD及光谱分析等手段分析了沉淀温度对YAG:Ce3+粉体性能的影响.实验结果表明:沉淀温度为25 ℃时制备出来的YAG:Ce3+粉体发光强度好.      

Study on phosphating treatment of aluminum alloy： role of yttrium oxide

Zinc phosphate coatings formed on 6061-Al alloy, after dipping in phosphating solutions containing different amounts of Y2O3(yttrium oxide), were studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and electrochemical measurements. Significant variations in the morphology and corrosion resistance afforded by zinc phosphate coating were especially observed as Y2O3 in phosphating solution varied from 0 to 40 mg/L. The addition of Y2O3 changed the initial potential of the interface between aluminum alloy substrate and phosphating solution and increased the number of nucleation sites. The phosphate coating thereby was less porous structure and covered the surface of aluminum alloy completely within short phosphating time. Phosphate coating was mainly composed of Zn3(PO4)2-4H2O (hopeite) and AIPO4(aluminum phosphate). Y2O3, as an additive of phosphatization, accelerated precipitation and refined the gain size of phosphate coating. The corrosion resistance of zinc phosphate coating in 3% NaCl solution was improved as shown by po-larization measurement. In the present research, the optimal amount of Y2O3 was 10-20 mg/L, and the optimal phosphating time was 600 s.     

丁二酮肟沉淀分离-EDTA滴定法测定镍钴锰三元氢氧化物中镍

镍钴锰三元氢氧化物为制备锂离子电池正极材料镍钴锰酸锂的主要原料,Ni含量是其比较重要的质量指标。若直接采用EDTA滴定法测定镍钴锰三元氢氧化物中Ni含量,共存的Co和Mn会对测定结果存在干扰。试验首先将镍钴锰三元氢氧化物样品用盐酸溶解,在微氨性的溶液中,以丁二酮肟为沉淀剂,Ni²⁺与丁二酮肟生成红色沉淀并实现与Co²⁺、Mn²⁺的分离;再将沉淀溶解,用EDTA滴定法测定Ni²⁺,从而建立了丁二酮肟沉淀分离-EDTA滴定测定镍钴锰三元氢氧化物中Ni含量的方法。对实验条件进行优化,确定沉淀剂用量为理论用量的1.9倍,沉淀初始pH值为8~9,陈化时间为30min,陈化温度为80℃,沉淀洗涤次数为6次。通过对模拟样品溶液测定表明,样品中Mg、Fe、Cu、Zn、Cr、Cd等微量杂质元素对Ni测定的干扰可忽略。对NCM111型、NCM622型、NCM811型镍钴锰三元氢氧化物中的Ni进行准确度考察,测定结果的相对标准偏差(RSD,n=11)在0.29%~0.48%之间,测定值与电感耦合等离子体原子发射光谱法(ICP-AES)结合EDTA滴定法的结果相一致。对NCM523型、NCM811型镍钴锰三元氢氧化物的加标回收率在96.9%~102.5%之间。     

掺钕氧化钪激光透明陶瓷纳米粉体的合成及研究

研究了化学共沉淀法合成Nd:Sc2O3纳米粉的工艺.以Sc2O3为基质材料,掺杂0.5％(原子分数)的Nd3+,添加适量聚乙二醇(PEG)和(NH4)2SO,作为分散剂,以氨水(NH3·H2O)和碳酸氢铵(NH4HCO3)混合溶液作复合沉淀剂,采用化学共沉淀法获得了碱式稀土碳酸盐前躯体,在1100℃下煅烧该前躯体4h,制备出性能良好的Nd:Sc2O3纳米粉.采用热重-差热分析仪(TG/DSC)、红外光谱分析仪(IR)、X射线衍射仪(XRD)、透射电子显微镜(TEM)等测试手段对Nd:Sc2O3前躯体和煅烧后的粉体进行表征.实验结果表明:在室温下,用氨水和碳酸氧铵混合溶液作为复合沉淀剂合成出的前躯体为碱式稀土碳酸盐.通过XRD和EDS能谱分析,Nd3+完全固溶于Sc2O3的立方晶格中,这将有利于制备激光透明陶瓷.在1100℃的温度下煅烧此前躯体得到的Nd:Sc2O3纳米粉具有颗粒粒度小(约50 nm)、分散性好、团聚程度轻、结晶良好的性能.因此,采用此工艺合成的粉体将有可能制备出的Nd:Sc2O3透明陶瓷.     

超细氧化铝的高分子网络凝胶法制备与研究

以硝酸铝溶液为原料,聚丙烯酰胺为单体,N,N′-亚甲基丙烯酰胺为网络剂,硫酸铵为引发剂,采用高分子网络凝胶法制备了超细氧化铝粉体。研究了沉淀剂种类,单体、网络剂及引发剂的质量比,和单体质量对合成氧化铝凝胶的影响。实验结果表明:以氨水为沉淀剂,当单体质量为0.05 g,单体、网络剂、引发剂质量比为5:1:1,聚合温度达到65℃时,可获得均匀、稳定的氧化铝凝胶;经900℃煅烧2 h后可获得的粒径细小,分散性好的氧化铝粉体。     

Synthesis and characterization of YAG: Ce3+ fluorescence powders by co-precipitation method

YAG:Ce³⁺(Yttrium aluminum garnet) fluorescence powders were successfully prepared by co-precipitation method using aluminum nitrate, yttrium nitrate, cerous nitrate as the starting materials and ammonium carbonate as precipitant. The products were characterized by X-ray powder diffraction, luminescence spectrometer, transmission electron microscope (TEM). The XRD results showed that the obtained YAG:Ce³⁺ fluorescence powders had the crystalline structures of YAG at calcinations temperature of 900 °C and the TEM results showed that the grain diameters were about 100 nm. The YAG:Ce³⁺ fluorescence powders, synthesized by co-precipitation method, had the best luminescence property when the Ce doping amount was x=0.06 in the molecular formula of Y_3-xCe_xAl₅O₁₂, the calcinations time was 2 h and the calcinations temperature was 1000 °C.