Magnetic and morphological characterization of Bi2Fe4O9 nanoparticles synthesized via a new reverse chemical co-precipitation method

Nano-sized Bi₂Fe₄O₉ (BFO) was successfully synthesized using a new reverse chemical co-precipitation method at different pH values of 8–12. These powders were examined by x-ray diffractometery (XRD), thermogravimetrical differential thermal analysis (TG-DTA), field emission scanning electron microscopy (FESEM) and vibrating sample magnetometery (VSM). The XRD analysis showed the formation of pure phase Bi₂Fe₄O₉ at calcination temperature over 700 ℃. The TG-DTA curves indicated the crystallization temperature of 617 ℃ for the Bi₂Fe₄O₉ sample. The FESEM micrographs revealed a precipitates agglomeration, which is related to the nature of the chemical co-precipitation method and free surface energy of nanoparticles. Furthermore, the particle size of the powder samples increased from 43 to 131 nm as the pH value increased from 8 to 12, respectively. Also, the morphological change from nearly cubic to rod-like shape in the nanoparticles was observed by increasing the pH value. The M-H curves of the as-prepared powders confirmed the antiferromagnetic behavior in all samples. Uncompensated spins from the surface led to the appearance of saturation magnetization in the Bi₂Fe₄O₉ nanoparticles. Besides, a decrease in the particles size resulted in more uncompensated spins, thereby improving the saturation and remnant magnetization from M_s = 0.35 emu/g and M_r = 0.010 emu/g for pH = 12 to M_s = 1.15 emu/g and M_r = 0.042 emu/g for pH = 8. Furthermore, as the pH values increase the coercive fields firstly rise up to 196 Oe for pH = 9 and then decrease to 151 for pH = 12.     

Fabrication,microstructure, and optical properties of Yb:Y3ScAl4O12 transparent ceramics with different doping levels

Transparent Yb:Y₃ScAl₄O₁₂ (Yb:YSAG) ceramics with different ytterbium doping concentrations such as 5, 10, 15, 20 at.% have been successfully fabricated by solid-state reactive sintering. All the obtained ceramics are in dense and homogeneous structure after sintering at 1820°C for 30 hours and with a posttreatment by hot isostatic pressing at 1750°C for 3 hours with 200 MPa pressure. We systematically analyzed the influence of Yb³⁺ doping concentration on the microstructure and optical properties of the ceramics. The 10 at.% Yb:Y₃ScAl₄O₁₂ ceramics with a thickness of 3.2 mm show the best transparency as high as 80.9% at 1100 nm. The laser emission of the 10 at.% Yb:YSAG ceramics was tested, resulting in a maximum slope efficiency of 67.6% and a maximum output power of 11.3 W under quasi-continuous wave pump conditions. The tuning range spanned from 990 to 1071 nm.     

纳米Y_2O_2S:Eu~(3+)红色荧光粉的间接法制备及发光性质

用间接法制备纳米级红色荧光粉Y2O2S:Eu3+(物质的量之比为Eu3+/Y3+=0.02)。XRD测试表明,制得纳米级的Y2O2S:Eu3+为单一纯相。透射电子显微镜(TEM)扫描结果显示纳米材料的平均颗粒尺寸为30 nm,与Debye-Scherre公式计算的结果基本一致。荧光光谱中,激发光谱分为3个区域,200-280 nm的区域为Y2O2S基质的激子激发带,峰值为262 nm;280-380 nm的区域属于Eu3+→O2-(S2-)的电荷迁移带,峰值为319 nm;而位于399 nm和472 nm的线状光谱则属于Eu3+的4 f组态内部电子之间的跃迁。     

纳米粉体Y_2O_3:Ti~(3+),Pr~(3+)的光谱性能

采用共沉淀法在氮氢气氛中制备出Y2O3:Ti3+,Pr3+纳米粉体,通过XRD、TEM方法确认了它的晶相与晶粒尺寸,测量了它的激发与发射谱,并与Y2O3:Ti3+纳米粉体的光谱进行了比较。结果显示:共掺Pr3+仅在281nm处产生了激发峰,而在蓝绿光区没有产生激发峰,以致365～480nm的光激发不出Pr3+的特征红荧光。表明:共掺Pr3+的Y2O3:Ti3+用作白光LED荧光粉,难以改善发光性能。     

共沉淀法制备Li[Ni1/3Co1/3Mn1/3]O2及电化学性能研究

采用NH3-NaOH共沉淀法合成了L[Ni1/3Co1/3Mn1/3]O2正极材料,通过改变NH3·H2O浓度及加料方式研究材料的电化学性能.采用XRD、SEM对晶体的结构和形貌作表征.将正极材料Li[Ni1/3Co1/3Mn1/3]O2制成电极极片,组装成电池进行测试.分析测试结果表明,合成的极材料Li[Ni1/3Co1/3Mn1/3]O2具有典型的α-NaFeO2结构,粒径分布较好,呈类球形.     

The structural and electrical comparison of Y2O3 and Ti-doped Y2O3 dielectrics

A Ti-doped Y₂O₃(Y₂Ti₂O₅) dielectric on polycrystalline silicon followed by rapid thermal annealing results in improved characteristics including a higher effective dielectric constant, higher breakdown electric field, lower electron trapping rate, and larger charge-to-breakdown when compared with Y₂O₃. The performance of high-k Y₂O₃ and Y₂Ti₂O₅ dielectrics were investigated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), capacitance-voltage, and current density-voltage. Incorporating Ti into the Y₂O₃ dielectric imparts improvements in the structural and electrical performance of the material. The Y₂Ti₂O₅ dielectric with 800 °C annealing treatment has the best performance among all the samples tested.     

溶胶-凝胶法制备纳米级Y2O3：Tb^3＋发光材料

采用溶胶-凝胶法合成Y2O3：Tb3＋纳米粒子。用红外光谱（IR）、X射线衍射（XRD）、光致发光（PL）光谱对其进行一系列表征。结果表明所制备的纳材料在400℃还没完全结晶,在1000℃时结晶完全,得到较纯产物且有良好的发光性能。     

Fabrication of high-efficiency Yb:Y2O3 laser ceramics without photodarkening

High-efficiency Yb:Y₂O₃ laser ceramics were fabricated using the vacuum-sintering plus hot isostatic pressing (HIP) without sintering additives. High-purity well-dispersed nanocrystalline Yb:Y₂O₃ powder was synthesized using a modified co-precipitation method in-house. The green bodies were first vacuum sintered at a temperature as low as 1430°C and then HIPed at 1450°C. Finally, the samples were air annealed at 800°C for 10 h. Although no sintering aids were used, full density of the samples with excellent optical homogeneity and an inline transmission of 80% at 400 nm could be obtained. Moreover, photodarkening phenomenon was not detected in the ceramics. Preliminary laser experiment with the fabricated ceramics in a two-mirror cavity has demonstrated 32 W continuous-wave (CW) output at ∼1077 nm with an optical-to-optical conversion efficiency of 58.2%. To the best of our knowledge, this is so far the highest CW output power and optical-to-optical conversion efficiency achieved with the Yb³⁺-doped sesquioxide ceramics in a simple two-mirror cavity.     

Optical and thermal properties of TiO2-doped Y2O3 transparent ceramics synthesized by hot isostatic pressing

Highly transparent Y₂O₃ ceramics using TiO₂ as an additive were synthesized by presintering and hot isostatic pressing (HIP). The effects of TiO₂ contents and sintering conditions on the optical properties of the final transparent ceramics were investigated. A small amount (0.04-0.16 wt%) may decrease the densification temperature by about 200°C. The Y₂O₃ ceramics doped with 0.16 wt% TiO₂ revealed a transparency of 82% in the wavelength range 1-6 μm. The thermal conductivity of the samples is about 11.8 W/m K at 25°C, which is close to that of the undoped Y₂O₃ ceramics.     

草酸沉淀法制备纳米晶Y2O3:Eu3+及粉体评价

报道了草酸作为沉淀剂并添加表面活性剂合成了纳米晶Y2O3：Eu^3 的方法,其一次粒径为20-30nm,团聚尺寸D50=0.53μm。粉体细且分布均匀。与微米晶比较,该纳米晶的发射光谱发生明显蓝移,色座标合荧光粉要求。     

Effect of Y2O3 content on the microstructural characteristics and the mechanical and thermal properties of Yb-doped SiAlON ceramics

SiAlON ceramics are primarily employed in ceramic cutting tools, which exploit their stable physical properties in high-temperature cutting environments due to their excellent mechanical properties. Here, Yb/Y-co-doped SiAlON ceramics are prepared by adding Yb and Y rare-earth (RE) ions in the RE_xSi_12-(m+n)Al_m+nO_nN_16-n (m = 0.4, n = 1.0) composition. Yb₂O₃, the RE oxide, is the main sintering additive. For RE_x composition design with (Yb_1-y + Y_y)_x, Yb₂O₃ is replaced by Y₂O₃ (y = 0.00, 0.25, 0.50, 0.75, 1.00). While Yb₂O₃ has excellent high-temperature stability, it is limited by its microstructural characteristics, that is, the β-SiAlON morphology and limited fracture toughness due to the small cation sizes. Thus, the changes in the above properties are investigated for various Y₂O₃ additive contents substituting for Yb₂O₃. The average grain width decreases, and the equiaxed β-SiAlON grains are elongated with increasing Y₂O₃ content. Regarding the mechanical properties, the hardness and fracture toughness are evaluated using the indentation fracture method. The hardness decreases with increasing Y₂O₃ content; however, the fracture toughness exhibits a significant increase (～53.6%) from 4.6 to 7.0 MPa?m^1/2. Regarding crack propagation, intergranular fracture is mainly observed in the Yb/Y-co-doped SiAlON ceramics, whereas transgranular fracture is primarily observed in the Yb-single-doped SiAlON ceramic. Y₂O₃ substitution increases the α/β-SiAlON phase ratio, and the grain boundary phase exhibits increasing vitrification with increasing Y₂O₃ content. Moreover, the thermal properties of the Yb/Y-co-doped compositions are analyzed and discussed regarding intrinsic properties such as phonon scattering. The microstructural characteristics and improved fracture toughness derived from the Yb/Y-co-doped system designed in this study suggest considerable potential for the future composition design of ceramic cutting tools.     

Y2O3-Bi2O3催化剂制备及其可见光催化降解2,4-二氯苯酚的研究

采用高温固相法合成一系列不同质量比的Y2O3-Bi2O3复合可见光复合催化剂,在日光色镝灯照射下,以2,4-二氯苯酚的可见光催化降解为目标反应,研究了Bi/Y质量比及焙烧温度对Y2O3-Bi2O3复合催化剂的结构及活性的影响.结果表明,复合光催化剂Y2O3-Bi2O3的最佳焙烧温度1023 K,焙烧时间2.5 h,最佳...     

水热法制备Y2O3:Eu3+微米棒及其荧光性能表征

利用水热法制备了Y2O3和Y2O3:Eu3+,探讨了反应温度、反应时间及氢氧化钠溶液浓度对产物晶型的影响,确定了生成较好晶型的反应条件为：反应温度180℃,反应时间24 h,氢氧化钠溶液浓度2 mol/L. 研究了Y3+和Eu3+的配比对Y2O3:Eu3+荧光性能的影响. 结果表明,当n(Y3+):n(Eu3+)的比例为100:5时,其荧光强度最佳. TEM分析表明,Y2O3:Eu3+粉末具有直径约0.2~0.6 mm、长度为几到十几微米的棒状结构.     

Effect of powder milling routes on the sinterability and optical properties of transparent Y2O3 ceramics

In ceramic processing, the size distribution of the starting powder to a certain degree is inevitable. It is prerequisite to control the size distribution, which influences the fabrication of a sound green body featuring both smaller pores and a narrower pore structure for full-density sintering facilitated by the easier elimination of pores. The milling process was systematically investigated here to elucidate the effect of powder characteristics on the sinterability and transmittance of Y₂O₃ ceramics. Three types of powder sets having different width of particle size distribution (W_PSD) while keeping the same median size (D₅₀) were prepared by changing the milling condition. By means of narrowing the W_PSD in this research, pore free transparent polycrystalline Y₂O₃ with average grain size of 730 nm was successfully fabricated by hot-pressing at 1500℃, which is 100℃ lower than the previously lowest known sintering temperature.     

TiO2对Y2O3-ZrO2系统显微结构和机械性能的影响

研究了利用水热技术合成TiO2-Y2O3-ZrO2系统微粉，实验测定了粉料的相组成和晶粒尺寸，单斜和四方ZrO2是主要晶相，在含高TiO2的结构中，发现了ZrTiO4。测量了在1300℃烧结样品的断裂韧性，这类四方氧化锆晶体显示出了良好的机械性质。     

Structural and electrical properties of ZnO:Ag core-shell nanoparticles synthesized by a polymer precursor method

Monodispersed core-shell type ZnO:Ag nanoparticles were synthesized by a polymer precursor method and their structural and electrical properties were reported in detail. The synthesis technique involves a sol-gel type chemical reaction between aqueous solutions of poly-vinyl alcohol (PVA), sucrose and Zn²⁺ salt. The Zn²⁺-PVA-sucrose polymer precursor powders so obtained after the reaction was further explored for the synthesis of ZnO:Ag nanoparticles. The key part of the work lies in the use of polymer coated ZnO nanoparticles as templates to obtain the ZnO core-Ag shell type nanostructures. Structural and spectroscopic analyses of the derived samples were performed with X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The XRD patterns of the ZnO:Ag nanoparticles consist of distinct peaks corresponding to the hexagonal wurtzite type (space group P63mc) crystal structure of ZnO along with the typical peaks of face centered cubic crystal structure of metallic silver. EDS and XPS analyses confirmed the chemical composition and surface structure of the core-shell nanoparticles. Microstructural analysis revealed the monodispersed platelet shaped ZnO nanoparticles with a thin layer of Ag coating on the surface. UV–visible diffuse reflectance studies revealed the effects of Ag coating on the optical properties of the samples. Detail analysis of the dielectric properties of the samples were performed as a function of frequency (1 Hz to 10 MHz) and temperature (300–528 K) to investigate the electrical conduction mechanism in the samples.     

热处理对Al2O3/PSZ(3Y)陶瓷材料结构和性能的影响

将烧结的Al2O3/PSZ(3Y)陶瓷材料在不同温度和时间下进行热处理,对不同热处理制度下的试样致密性能和力学性能进行了测试,用X射线衍射分析了热处理前后材料中的各晶相的变化情况。结果表明:1560℃烧结的Al2O3/PSZ(3Y)陶瓷材料,经1100℃热处理6小时后其抗弯强度达到680MPa,比未处理试样的强度提高了近30%。热处理后基体中出现的不同晶格常数的四方氧化锆晶相对提高材料的力学性能有利。     

Yb2O3 and Y2O3 co-doped zirconia ceramics

A suspension stabilizer-coating technique was employed to prepare x mol% Yb₂O₃ (x = 1.0, 2.0, 3.0 and 4.0) and 1.0 mol% Y₂O₃ co-doped ZrO₂ powder. A systematic study was conducted on the sintering behaviour, phase assemblage, microstructural development and mechanical properties of Yb₂O₃ and Y₂O₃ co-doped zirconia ceramics. Fully dense ZrO₂ ceramics were obtained by means of pressureless sintering in air for 1 h at 1450 °C. The phase composition of the ceramics could be controlled by tuning the Yb₂O₃ content and the sintering parameters. Polycrystalline tetragonal ZrO₂ (TZP) and fully stabilised cubic ZrO₂ (FSZ) were achieved in the 1.0 mol% Y₂O₃ stabilised ceramic, co-doped with 1.0 mol% Yb₂O₃ and 4.0 mol% Yb₂O₃, respectively. The amount of stabilizer needed to form cubic ZrO₂ phase in the Yb₂O₃ and Y₂O₃ co-doped ZrO₂ ceramics was lower than that of single phase Y₂O₃-doped materials. The indentation fracture toughness could be tailored up to 8.5 MPa m^1/2 in combination with a hardness of 12 GPa by sintering a 1.0 mol% Yb₂O₃ and 1.0 mol% Y₂O₃ ceramic at 1450 °C for 1 h.     

共沉淀法制备Ni/Al2O3催化剂的研究

油脂加氢催化剂是以金属镍为活性组分、氧化铝为载体制备的Ni/Al2O3催化剂。在制备催化剂过程中,其合成条件直接影响着催化剂的最终活性。以工业硝酸镍、碳酸钠和自制氧化铝粉为原料,利用共沉淀的方法制备加氢催化剂,考察了反应温度、反应时间、反应液pH及反应过程中搅拌转速对催化剂活性的影响。通过实验数据汇总分析,最终确定制备Ni/Al2O3油脂加氢催化剂的最佳条件：反应温度为85 ℃、反应结束时溶液pH=8.0、反应时间为1.5 h、搅拌转速为600 r/min。在此条件下制备的Ni/Al2O3催化剂,经棕榈油加氢评价后测定的碘值最低。     

柠檬酸凝胶燃烧法制备Nd3+,Yb3+:Y2O3多晶原料及其相组成和荧光特性的研究

本文采用柠檬酸凝胶燃烧法合成了性能优良的Nd3+,Yb3+:Y2O3多晶原料。XRD、IR和SEM测试结果表明样品在900℃煅烧可获得纯相的Nd3+,Yb3+:Y2O3,平均粒径约为40 nm;TG-DTA测试结果表明样品在30～600℃之间失重约为49.28%;从荧光光谱上可以看出两个主要发射峰位于970～1100 nm之间,最强发射峰位于1030nm,对应Yb3+的2F5/2→2F7/2能级跃迁。