Sm5Fe80Cu1Zr3.5Si5B3C2.5非晶合金晶化动力学的研究

利用X射线衍射、透射电镜、振动样品磁强计和差热分析研究了非晶Sm5Fe80Cu1Zr3.5Si5B3C2.5合金中α-Fe/Sm2(Fe,Si)17Cx复合纳米相结构的形成过程、磁性及其晶化动力学.XRD结果表明,随着退火温度的升高,Sm5Fe80Cu1Zr3.5Si5B3C2.5非晶合金先后析出软磁相α-Fe和硬磁相Sm2(Fe,Si)17Cx;当经高温750℃晶化退火后,经Scherrer计算得到合金中α-Fe相和Sm2(Fe,Si)17Cx的晶粒尺寸分别为65.5和22.1nm,其矫顽力增加到58.11kA/m,剩磁为0.967T.晶化动力学分析发现,这种具有较低初始晶化激活能和阶段生长激活能的晶化行为是导致α-Fe相晶粒生长过于粗大和合金中α-Fe和Sm2(Fe,Si)17Cx复合纳米磁体磁耦合性能较差的根本原因.     

低温热处理增强α-Fe/Sm2Fe17Cx纳米复合永磁合金磁性能的机制研究

采用X射线衍射分析、透射电子显微镜、振动样品磁强计研究了经400℃低温热处理前后对Sm5Fe80Cu1Si5B3C2.5Zr<3.5>非晶合金的非晶微结构、晶化后纳米复合永磁体的组织结构及磁性能的影响规律.结果表明,非晶合金直接于750℃退火后软磁α-Fe相和硬磁Sm2(Fe,Si)17Cx相的尺寸分别为50.6和20.6nm,体积分数分别为71.1%和28.9%;而经400℃热处理后复纳米晶组织结构中α-Fe相和Sm2(Fe,Si)17Cx相的晶粒尺寸分别改变为36.5和24.4nm,体积分数分别为76.7%和23.3%,磁交换耦合作用明显增强.径向分布函数计算表明,低温热处理优化了非晶合金的短程有序范围、配位数和最近邻原子间距等微结构参数,改变了原始态非晶合金中α-Fe相和Sm2(Fe,Si)17Cx相的晶化行为,这是细化α-Fe/Sm2(Fe,Si)17Cx复合纳米晶结构和提高磁耦合性能的根本原因.     

Sm12.7Fe86.3Nb1合金的氢处理

Sm12.7Fe86.3Nb1合金在不同温度下氢爆(HD)及氢化-歧化-解吸-再复合(HDDR)处理时,100℃时可氢化形成Sm2(Fe,Nb)17Hy,随着温度升高氢化速度加快,到400℃时单胞体积最大膨胀了3.38%.超过500℃时Sm2(Fe,Nb)17Hy H2→SmHy α-Fe(Nb)发生歧化,直到900℃仍旧存在,故氢爆温度应低于500℃.解吸与再复合过程在超过700℃时可能以SmHy α-Fe(Nb)→Sm2(Fe,Nb)17 H2方式进行.在连续的HDDR处理过程中,吸氢-歧化在升温(400℃/h)的过程中即已完成,而解吸-再复合在保温时与歧化阶段达到平衡,即SmHy α-Fe(Nb)←→Sm2(Fe,Nb)17 H2,抽真空是使该反应向右进行的主要驱动力.在HDDR过程中破坏试样的原颗粒尺寸会残留较多的软磁α-Fe相而恶化氮化后的磁性能,HDDR后残留的α-Fe相含量均高于退火态的残留量,2次循环后磁粉的矫顽力较高.HDDR使粉末颗粒表面产生裂纹,再复合后的Sm2(Fe,Nb)17颗粒细小均匀,尺寸分布在几十纳米到300 nm之间.     

MA法制备Fe83Nb7B9Cu1纳米晶粉末及其热稳定性

利用高能球磨法在Fe Nb B Cu体系中获得纳米晶粉末 ,研究了机械球磨过程中产物的组织结构、α Fe相平均晶粒尺寸及其热稳定性。结果表明 :采用Fe 2 0B中间合金粉末代替B粉并未明显影响机械合金化动力学过程 ;球磨至 5h时 ,即可获得平均晶粒尺寸约 18nm的α Fe单相过饱和固溶体 ,其后延长球磨时间 ,晶粒尺寸缓慢减小 ,至 45h后 ,平均晶粒尺寸减小到 9nm。退火处理后的XRD分析表明 ,α Fe过饱和固溶体从 10 0℃开始发生结构弛豫现象 ,738.8℃后则发生了相转变 :α Fe过饱和固溶体→α Fe固溶体 Fe3 B FeB ,在 5 5 0℃以内退火 ,纳米晶粒长大不明显 ,在 770～ 95 0℃范围内退火 ,晶粒开始明显长大 ,但晶粒尺寸仍处于纳米级范围。     

各向同性Sm2Fe17Nx磁粉及其粘结磁体的制备

采用HDDR工艺制备出了各向同性Sm2Fe17Nx永磁粉，通过XRD，SEM，EDX等手段研究了Sm-Fe合金的凝固，均匀化热处理，氢化-歧化以及脱氢-再化合和氮化等过程中，合金的相及微观结构的变化。结果表明：1050℃，24h的均匀化热处理能有效地消除合金中的杂相，成功地制备出成分均一的单相2：17母合金：800℃氢化-歧化1h后，合金歧化成晶粒为纳米级SmHx和α-Fe，相同温度下脱氢-再化合2h后，合金又再化合为晶粒细小的2：17相，500℃氮化5h后，合金大量吸氮，晶格常数和单胞体积明显增加，体积膨胀量达6．28％；将上述制备的各向同性Sm2Fe17Nx永磁粉用质量分数为3％的环氧树脂粘结剂均匀包缚，获得了密度为6．04g／cm^3，磁性能为：Br=0．6704T，Hcj=015kA／m，（BH）max=73．7kJ/m^3的各向同性Sm2Fe17M粘结磁体。     

快淬SmFe合金的微观结构及相组成

采用SEM、XRD、EDX、AFM等方法分析了快淬Sm-Fe合金的微观结构和相组成。研究表明：Sm-Fe合金铸锭由Sm2Fe17相、富Sm相和大量的α-Fe相组成，经过一定的均匀化热处理后，获得了几乎单一的Sm2Fe17相合金；快淬速度为10m／s时，获得的Sm-Fe合金由Th2zn17，菱形对称结构的Sm2Fe17相及少量的α-Fe组成，合金晶粒尺寸约为100nm，且分布不均匀：当快淬速度为20m／s时，合金仍由Sm2Fe17相和α-Fe相组成，但与10m／s的合金相比，α-Fe相明显增多，同时稳定相Sm2Fe17向亚稳定相Sm10Fe90转变；当快淬速度大于30m／s时，合金完全为ThCu7型六角晶结构的Sm10Fe90相，平均晶粒尺寸在40～50nm，分布均匀。     

Fe84Nb7B9纳米晶粉末热处理特性的研究

通过DTA、SEM和TEM观察对Fe84Nb7B9纳米晶粉末热处理特性进行了研究.结果表明机械合金化可以制备晶粒尺寸在10nm以内的纳米晶粉末,该粉末在100～850℃退火,晶粒尺寸保持在纳米级,并且没有新相生成,表现出良好的热稳定性.其中100～350℃退火纳米晶粒保持在15 nm左右,为后继采用低温压型技术制备块状纳米晶材料提供了理论依据.     

液氮球磨Sm-Fe合金的组织演变

利用低温液氮球磨技术制备了Sm-Fe合金粉体,采用XRD、HRTEM和惰性气脉冲-红外-热导等方法对Sm2Fe17合金粉体在液氮球磨过程中的组织演变进行了研究。结果表明,液氮球磨可加速细化Sm-Fe合金粉体。球磨5 h后,Sm-Fe合金的晶粒尺寸约为10 nm,9 h后晶粒尺寸约为5 nm。Sm-Fe合金中的氮含量随着球磨时间的延长而增加,主轴转速150 r/min球磨9 h后,氮含量达1.62% (质量分数, 下同)。随着球磨时间的延长,Sm2Fe17相向非晶态转变,降低球磨转速可以延缓非晶的形成过程     

熔体快淬非晶Fe-Si-B-Cu合金的晶化行为

采川筹热扫描量热分析(DSC)、x射线衍射分析(xRD)以及透射电镜技术(TEM)对熔体快淬非晶薄带Fe75.5Si13.5B9Cu2的晶化行为进行研究.结果表明:在不同升温速率下的DSC曲线中出现两个放热峰,晶化表现激活能分别为369.177和430.162kJ/mol;经500～680℃、1h等温退火后,发现晶化时发生a-Fe(Si)相的形核长大以及Fe3B和Fe2B相的析出;在500℃退火后获得的a-Fe(Si)平均晶粒尺寸最小;a-Fe(Si)的晶格常数起初增大,在560℃达到最大值后缓慢降低;在500℃等温退火,随着时间的延长,a-Fe(Si)的晶粒尺寸及晶格常数逐渐增大,在等温退火1h时,晶粒尺寸约为20nm.     

高比表面积磁性-荧光介孔磷灰石纳米纺锤体的制备(英文)

以单十二烷基磷酸酯为模板剂制备了Sm3+和Fe3+共掺杂的兼具磁性和荧光特性的纺锤形介孔纳米羟基磷灰石。利用XRD、SEM、TEM、VSM、PL及氮气吸附-脱附曲线等手段对产物进行了表征与研究。掺杂的Sm3+和Fe3+以固溶和镶嵌氧化物纳米粒子2种形式存在于羟基磷灰石基体中。煅烧前后,Sm3+和Fe3+共掺杂的羟基磷灰石试样均具有良好的超顺磁性。煅烧使试样的比饱和磁化强度从13.45(A·m2)·kg-1增加至19.51(A·m2)·kg-1。煅烧后,Sm3+和Fe3+共掺杂羟基磷灰石呈纳米纺锤体形貌,长200~350 nm,直径50~100 nm。其中分布有大量的双孔介孔,孔径分别为3.64和9.01 nm。大量双孔分布的介孔使产物具有大的比表面积和高的孔体积比,分别为153.52 m2/g和0.3286 cm3/g。产物具有生物靶向性、生物标识性及高的载药容量,在药物载体中具有大的应用潜力。     

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。     

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.     

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.     

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.     

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。     

Synthesis and electrochemical properties of LiNi0.4Mn1.5Cr0.1O4 and Li4Ti5O12

Spinel compound LiNi_0.4Mn_1.5Cr_0.1O₄ (LNMCO) and Li₄Ti₅O₁₂ (LTO) were synthesized by the sol-gel method and the solid-state method, respectively. The particle sizes of the products LiNi_0.4Mn_1.5Cr_0.1O₄ and Li₄Ti₅O₁₂ were 0.5 to 2 um and 0.5 to 0.8 um, respectively. All samples exhibited excellent electrochemical properties. A LiNi_0.4Mn_1.5Cr_0.1O₄/Li₄Ti₅O₁₂ (LNMCO/LTO) cell was fabricated and was demonstrated to exhibit good electrochemical properties at the high current rate of 1 C. When the specific capacity was determined based on the mass of the LNMCO cathode, the LNMCO/LTO cell delivered 125 mAh g⁻¹ at 1 C and 77 mAh g⁻¹ at 5 C. The capacity retentions after 30 cycles were 94.4 % and 83.1 %, respectively.