超声沉淀法制备纳米Al2O3粉体

将超声辐射应用于以硫酸铝铵 (NH4Al(SO4) 2 ·12H2 O )和碳酸氢铵 (NH4HCO3 )为原料的沉淀法制备Al2 O3 纳米粉体的化学反应工艺过程 ,制备了粒径为 12nm的α Al2 O3 纳米粉体。通过SEM、TEM等分析手段研究了超声辐射对前驱体NH4Al(OH) 2 CO3 沉淀物及最终粉体尺寸、形貌及其团聚行为的影响 ,并探讨了其作用机理。结果表明 :超声辐射由于其自身的空化作用不仅细化了前驱体颗粒、抑制了其间的团聚 ,而且延缓了其向凝胶的转变过程 ,从而有效地细化α Al2 O3 颗粒 ,但过高的频率却易导致颗粒间的进一步聚合     

超声对湿化学法制备Al2O3纳米粉的影响

采用湿化学法在超声场中制备了纳米α-Al2O3粉体,研究了超声辐射作用下前驱体颗粒的成核、长大过程,探索了超声作用下Al2O3晶型的转变.结果表明超声能量能加速前驱体的形核,超声分散可控制晶核的长大和团聚,在超声技术处理下可制备粒径仅为20 nm的NH4A1(OH)2CO3超细前驱体,这一前驱体经8 h陈化后,再经1150℃高温煅烧20 min,可制备得到粒径约为10 nm的α-A1203粉体;研究还发现高频率超声辐射可提高α相Al2O3粉体的结晶度.     

超声场中溶胶凝胶法制备纳米氧化铝粉体的研究

近年来，超声空化处理已被证明是一种制备纳米材料十分有效的技术，当将超声空化作用应用于溶胶凝胶法制备纳米粉体过程时，将为防止团聚体的生成创造一个独特的条件。本文以六次甲基四胺为沉淀剂，研究了超声场下溶胶凝胶法制备纳米Al2O3粉体的工艺，对产物进行了扫描电镜（SEM），X射线衍射（XRD）分析及粒度分析。实验结果表明，超声波的引入可显著提高粉体的性能。超声处理过的前驱体在1100℃煅烧2小时制得了团聚少，平均粒径在30nm左右的α-Al2O3粉体。超声波的辐射作用有利于纳米α—Al2O3粉体的制备，它的作用主要体现在防止胶粒之间的团聚和长大，及破碎团聚体的作用上。     

碳酸铝铵热分解法制备超细氧化铝粉体

以分析纯的NH4Al(SO4)2和NH4HCO3为原料,选择合适的溶液浓度、分散剂及pH值,在合适的工艺条件下,得到NH4Al(OH)2CO3前驱体化合物.前驱体在1100℃下煅烧1h,得到粒径为80～100nm的超细α-Al2O3,Al2O3颗粒基本上呈球形,粒度均匀.研究了溶液浓度、分散剂及pH值对前驱体化合物颗粒细度的影响,用XRD法对前驱体化合物及其煅烧产物进行了表征,并研究了热处理过程中的相变化,对Al2O3多晶转变与热处理温度之间的关系进行了讨论.用SEM对Al2O3粉体的形貌、大小进行了表征.该方法工艺简单,原料易得便宜,综合成本较低,易实现工业化生产.     

碳酸铝铵热解法制备超细Al2O3

以Al2(SO4)3与(NH4)2CO3为原料,采用液相沉淀法,制备出前驱物碳酸铝铵(AACH),并烧结得到Al2O3粉末。通过分析前驱物的热重曲线,确定了前驱物的高温分解过程;并结合对前驱物在不同烧结温度下所得产物XRD图谱的分析,确定了前驱物的高温相变过程为:AACH→AlOOH→Al2O3(无定型)→γ-Al2O3→θ-Al2O3→α-Al2O3。同时,干燥方式对超细Al2O3分散性的影响在本文中也进行了研究。     

共沉淀法制备YAG纳米粉体中团聚的研究

分别在NH4HCO3、氨水溶液中滴加NH4Al(SO4)2和Y(NO3)3的混合溶液,共沉淀生成YAG的前驱体.通过对YAG前驱体组成和结构的表征来讨论2种沉淀剂对前驱体团聚的影响,并且通过对2种前驱体热处理过程中YAG相形成的反应历程分析,来解释最终生成YAG粉体的形貌、尺寸及团聚状态.结果表明,使用氨水作为沉淀剂,生成的YAG粉体团聚严重;使用碳酸盐作为沉淀剂形成的前驱体虽然也有一定程度的团聚,但最终生成分散性好、尺寸较小的YAG纳米粉体.     

硫酸氢铵焙烧粉煤灰提取氧化铝(英文)

采用NH4HSO4焙烧法从粉煤灰中提取Al2O3。首先,通过NH4HSO4焙烧和去离子水浸出法提取粉煤灰中的Al和Fe;然后,加入NH4HCO3溶液沉淀浸出液中的Al和Fe,利用NaOH溶液浸出得到的Al(OH)3和Fe(OH)3混合沉淀,所得铝酸钠溶液经碳酸化分解得到纯净的Al(OH)3;最后,煅烧纯净的Al(OH)3制备α-Al2O3产品。通过实验确定各工艺流程的最佳条件。制备的α-Al2O3产品达到YS/T 274-1998标准的工艺指标。     

尿素均匀沉淀法制备超细α-Al2O3粉体

以Al2（SO4）3和CO（NH2）2为原料,通过均匀沉淀法制备出前驱物Al（OH）3,并煅烧得到超细α-Al2O3粉体。研究CO（NH2）2和Al2（SO4）3的摩尔比、Al2（SO4）3起始摩尔浓度、反应温度、反应时间等对前驱物制备的影响。利用X射线衍射仪、扫描电镜、热重/差示扫描法（DTA/TGA）等多种现代分析检测技术对粉体的性能进行了表征。结果表明：在CO（NH2）2和Al2（SO4）3的摩尔比为10：1、Al2（SO4）3起始浓度为0.05mol/L、反应温度为90℃、反应时间为60min的条件下,能得到分散性能良好、粒径为2μm左右且粒度分布均匀的球形超细α-Al2O3粉体。     

纳米α-Al2O3的制备及其悬浮液分散性的研究

以AlCl3.6H2O和NH4HCO3为原料,采用室温固相化学反应获得前驱体,1100℃煅烧1.5h,制备纳米α-Al2O3粉体,用XRD、TEM、BET及电子衍射等进行表征,通过对粒径和Zeta电位分析,研究了不同pH值、分散剂及其用量对纳米α-Al2O3粉体悬浮液分散性的影响。实验结果表明：产物为α-Al2O3,颗粒粒径为20nm~30nm,粒子尺寸分布较均匀,比表面积为66.32m2/g;悬浮液的分散性能受到pH值、分散剂种类及其加入量的影响,找到了制备高分散的、稳定的α-Al2O3悬浮液的最佳pH值及PEG10000的最佳添加量。     

激光熔覆纳米Al2O3等离子喷涂陶瓷涂层

采用X射线衍射仪、扫描电镜和显微硬度计研究了45#钢表面激光熔覆纳米Al2O3改性Al2O3 13%TiO2(质量分数)陶瓷涂层的相组成、微观结构和显微硬度,同时对涂层的磨损特性进行了考察.结果表明,激光重熔区亚稳相γ-Al2O3转变成稳定相α-Al2O3,熔覆层由粗颗粒α-Al2O3和TiO2以及纳米α-Al2O颗粒组成,在激光的作用下,等离子喷涂层的片层状结构得以消除; 纳米Al2O3颗粒仍然保持在纳米尺度,填充在涂层的大颗粒之间,使涂层致密化程度得以提高,因此纳米Al2O3改性涂层的显微硬度较高,且其耐磨性能明显优于等离子喷涂层.     

X-ray diffraction study of Ba0.985Na0.015Ti0.985Nb0.015O3, Ba0.6Na0.4Ti0.6Nb0.4O3 and Ba0.3Na0.7Ti0.3Nb0.7O3 compositions

The Ba_0.985Na_0.015Ti_0.985Nb_0.015O₃, Ba_0.6Na_0.4Ti_0.6Nb_0.4O₃ and Ba_0.3Na_0.7Ti_0.3Nb_0.7O₃ compositions of the (1 − x) BaTiO₃–xNaNbO₃ (BTNNx) system have been studied by X-ray diffraction and by measurements of dielectric properties. The specimens with composition BTNN (x = 0.015, 0.40 and 0.70) have been refined by the JANA program from X-ray powder diffraction data. Ceramic samples with composition (1 − x) BaTiO₃ + xNaNbO₃ (where x = 0.015, 0.40 and 0.70) were prepared by calcinations from appropriate mixture of BaCO₃, TiO₂, Na₂CO₃ and Nb₂O₅. The calcined powder was sintered at temperature range 1200–1400 °C. As the composition x increased from 0.015 (and 0.70), the ferroelectric ceramics (x = 0.015, FE) with tetragonal phase changed to the ferroelectric relaxors (RFE, x = 0.40). RFE ceramics showed a peculiar diffuse phase transition and dielectric relaxation at the low temperature (down to 180 K) due to a frustration between RFE and FE state. These ceramics present the classical ferroelectric character when 0 ≤ x < 0.075 and 0.55 < x ≤ 1 and relaxor character when 0.075 ≤ x ≤ 0.55.     

Magnetic, electrical and plastic properties of Fe76Nb2Si13B9, Fe75Ag1Nb2Si13B9 and Fe75Cu1Nb2Si13B9 amorphous alloys

Influence of 1 h annealing in vacuum on magnetic, electrical and plastic properties of Fe₇₆Nb₂Si₁₃B₉, Fe₇₅Ag₁Nb₂Si₁₃B₉ and Fe₇₅Cu₁Nb₂Si₁₃B₉ melt spun ribbons were carefully investigated. It was shown that in all cases soft magnetic properties can be significantly enhanced by applying 1-h annealing at characteristic temperatures T_op. This optimization annealing causes that permeability increases more than 15-times and magnetic losses (tangent of loss angle) achieves a minimum in relation to the as quenched state. Using structural examinations (X-ray and HRTEM) it was shown that for the Fe₇₅Cu₁Nb₂Si₁₃B₉ alloy the optimized microstructure corresponds to a nanocrystalline αFe(Si) phase whereas in other alloys to a relaxed amorphous phase free of iron nanograins. As a consequence of this fact the Fe₇₆Nb₂Si₁₃B₉ and Fe₇₅Ag₁Nb₂Si₁₃B₉ alloys show higher plasticity in comparison to the nanocrystalline Fe₇₅Cu₁Nb₂Si₁₃B₉ alloy. Temperatures of the first stage of crystallization, and related diffusion parameters were determined using measurements of resistivity versus temperature with different heating rates.     

Fe2+-Ni2+-NH3-NH4+-C2O42-H2O体系的沉淀配合平衡热力学

针对草酸盐配位共沉淀热分解还原法制备超细铁镍合金粉过程中Fe2+-Ni2+-NH3-NH4+-C2O42--H2O体系的溶液平衡建立热力学分析模型,并根据模型进行相关计算,揭示反应体系中各物质随pH值、氨及草酸浓度的变化关系。结果表明:溶液中的Fe主要以[Fe(C2O4)n]2 2n络合物形式存在,而铁氨络合物含量很低。当氨含量较低时,溶液中的Ni主要以[Ni(C2O4)n]2 2n存在;氨含量较高时,在酸性条件下,溶液中的Ni主要以[Ni(C2O4)n]2 2n存在,在碱性条件下,则主要以[Ni(NH3)n]2+存在。低pH值下,Ni的沉淀率较Fe的高,而高pH值下,Ni的沉淀率则较Fe的低。     

New Zr6CoAs2-type compounds: Y6CoBi2, Ho6CoBi2 and Tm6CoBi2

Results of a powder X-ray diffraction investigation of new ternary compounds are reported. The compounds Y₆CoBi₂ [a=0.8312(1) nm, c=0.4144(1) nm], Ho₆CoBi₂ [a=0.8246(2) nm, c=0.4095(1) nm], and Tm₆CoBi₂ [a=0.8155(2) nm, c=0.4066(1) nm] crystallize in the hexagonal Zr₆CoAs₂-type structure (space group P6b2m No. 189). The Zr₆CoAs₂-type structure is a superstructure of the Fe₂P-type structure.     

Thermodynamics and phase diagrams in the binary systems Na2O-SiO2, Na2O-GeO2, Na2O-B2O3, Li2O-B2O3, CaO-B2O3, SrO-B2O3, and BaO-B2O3

We applied our model to the enthalpy of mixing data of the binary systems Na₂O-SiO₂, Na₂O-GeO₂, Na₂O-B₂O₃, Li₂O-B₂O₃, CaO-B₂O₃, SrO-B₂O₃, and BaO-B₂O₃. The most stable composition in the liquid, that is where the enthalpy of mixing is most negative, is with a metal-oxygen ratio of 4 to 3, for monovalent metals (Na and Li) and 3 to 4 for divalent metals (Ba and Ca) in liquid silicates or borates. The same applies to the CaO-SiO₂, CaO-Al₂O₃, PbO-B₂O₃, PbO-SiO₂, ZnO-B₂O₃, and ZnO-SiO₂ systems. The oxygen to metal ratio, its constant value in various types of systems, reflects and describes the structure of the liquid. Using the analyzed enthalpies of mixing data and the available phase diagrams, we calculated the enthalpies of formation of the various binary compounds. The results are in excellent agreement with data in the literature that were obtained from direct solid-solid calorimetry.     

电弧喷涂制备Fe65Cr20Mo7B3.5SiMn1.5W3涂层

在Q235低碳钢板上利用电弧喷涂工艺进行喷涂,以制得Fe65Cr20Mo7B3.5SiMn1.5W3涂层。喷涂材料为自行配制的丝材,按照35%的填充率将配好的粉填充到U型不锈钢外皮中,经过多道拉拔、挤压工艺制成Φ2mm的粉芯丝材。采用X射线衍射仪、扫描电镜、能谱分析仪、透射电镜对涂层的物相和组织形貌及成分进行了表征;采用差示扫描量热仪、显微硬度仪等设备对涂层的热稳定性及显微硬度进行了检测和分析。试验结果表明:涂层组织形貌呈典型的层状组织结构,由变形良好的带状粒子相互搭接堆积而成。涂层含有50.63%的非晶相,同时含有纳米级的晶相。涂层组织均匀、结构致密、孔隙率低,并且涂层硬度高达1040.5HV0.3,属硬质涂层,具有良好的热稳定性。     

Al2O3-Sm2O3-CeO2电解质的性能（英文）

采用溶胶-凝胶法和低温燃烧技术制备Ce1-xSmxO2（x=0,0.1,0.2,0.3）和掺杂Sm和（2%-8%）Al2O3的二氧化铈;研究其合成、结构、致密化、导电性和热膨胀等性能,并利用XRD研究其结构和相组成。结果表明,于1300°C烧结球团,获得致密的陶瓷,于1250°C在Ce0.8Sm0.2O0.2中加入2%和4%的Al2O3以促进烧结。利用扫描电子显微镜观察烧结后球团的表面形貌,使用双探针交流阻抗谱研究总离子电导率。     

Zur Kenntnis von RbBa3Ca4Cu3V7O28

Single crystals of RbBa₃Ca₄Cu₃V₇O₂₈ were prepared above the melting point of the reaction mixture. It crystallizes with hexagonal symmetry, space group C_6V⁴-P6₃mc, a 11.1751, c 12.434 Å, Z = 2. RbBa₃Ca₄Cu₃V₇O₂₈ is the second member of a new structure type of the copper-oxovanadates. Ba²⁺ shows an unusual 12-fold coordination. The two calcium positions are coordinated by trigonal prisms and octahedra respectively. The copper coordination is characterized by a stretched square pyramid. The Cu²⁺ ions are outside the centre nearly in plane of the pyramids.

Zusammenfassung

Einkristalle von RbBa₃Ca₄Cu₃V₇O₂₈ wurden oberhalb des Schmelzpunktes der Reaktionsmischung erhalten. Die Verbindung kristallisiert hexagonal, Raumgruppe C_6V⁴-P6₃mc, a 11.1751, c 12.434 Å, Z = 2. RbBa₃Ca₄Cu₃V₇O₂₈ ist das zweite Beispiel für einen neuen Strukturtyp der Kupfer-Oxovanadate, mit 12-fach koordinierten Ba²⁺ -Ionen. Die zwei Calciumpositionen sind trigonal prismatisch bzw. oktaedrisch koordiniert. Die Koordination der Cu²⁺-Ionen ist durch eine gestreckte Pyramide charakterisiert. Cu²⁺ ist auβerhalb des Polyederzentrums nahezu in der quadratischen Fläche der Pyramide angeordnet.     

Sinterability and dielectric properties of Ba0.55Sr0.4Ca0.05TiO3-CaTiSiO5-Mg2TiO4 composite ceramics

The composite ceramics of Ba_0.55Sr_0.4Ca_0.05TiO₃-CaTiSiO₅-Mg₂TiO₄ (BSCT-CTS-MT) were prepared by the conventional solid-state route. The sintering performance, phase structures, morphologies, and dielectric properties of the composite ceramics were investigated. The BSCT-CTS-MT ceramics were sintered at 1100 °C and possessed dense microstructure. The dielectric constant was tailored from 1196 to 141 as the amount of Mg₂TiO₄ increased from 0 to 50 wt%. The dielectric constant and dielectric loss of 40 wt% Ba_0.55Sr_0.4Ca_0.05TiO₃-10 wt% CaTiSiO₅-50 wt% Mg₂TiO₄ was 141 and 0.0020, respectively, and the tunability was 8.64% under a DC electric field of 8.0 kV/cm. The Curie peaks were broadened and depressed after the addition of CaTiSiO₅. The optimistic dielectric properties made it a promising candidate for the application of tunable capacitors and phase shifters.