Nd_2Fe_(14)B/α-Fe/非晶Nd-Fe-B三相纳米交换耦合磁体中的结构弛豫

用旋淬法制备了Ｎｄ２Ｆｅ１４Ｂ／α－Ｆｅ基复相纳米交换耦合磁体粉末样品．发现样品由于在室温下的结构弛豫导致磁性能的较大变化．在淬态Ｎｄ－Ｆｅ－Ｂ非晶相和Ｎｄ２Ｆｅ１４Ｂ／α－Ｆｅ纳米晶共存的三相交换磁体中,其效果更为明显．而在淬态完全非晶态或晶态的单相或复相交换磁体中,结构弛豫对磁性能的影响较弱．淬态Ｎｄ１０Ｆｅ８３Ｂ６Ｉｎ磁体粉末经过在室温下置放１年时间后,内禀矫顽力Ｈｃ由刚出炉时的２９６ｋＡ／ｍ增加至３８４ｋＡ／ｍ,剩磁比ｍｒ从０．５５增至０．６２非晶相的存在为晶粒发展完备的晶界提供了可能．应力和缺陷集中的边界区域的结构弛豫和原子调整使得相邻接的相与相、晶粒与晶粒之间的结晶学相关性提高,交换耦合增强．同时完善的晶界也增强磁体的磁硬化．Ｘ射线衍射结果显示结构弛豫的最终结果使得衍射峰宽化,极有可能在晶界处形成了畸变的晶间相．而正是这种畸变的晶间相对磁性能的增强起了关键的作用．     

Nb和Zr对（Nd，Pr）2Fe14B／α-Fe磁体晶化行为和磁性能的影响

采用熔体快淬及晶化退火工艺制备了纳米双相（Nd，Pr）2Fe14B／α-Fe型磁体，研究了Nb和Zr的添加对磁体磁性能、微观结构和晶化行为的影响。结果表明：添加Nb和Zr可提高α—Fe相的晶化温度，抑制α—Fe的析出和长大，避免亚稳相的形成，从而提高硬磁相的体积百分比。Nb和Zr复合添加能细化晶粒，增强硬磁相和软磁相问的交换耦合作用，显著提高纳米晶双相永磁合金的磁性能。合金（Nd，Pr）2Fe14B／α-Fe经过最佳热处理后，磁性能达到Br=1．10T，iHc=534．2kA／m，（BH）max=143．6kJ／m^3。     

动态晶化对纳米晶交换耦合Nd2Fe14B/α-Fe磁性能和显微组织的影响

为改善纳米晶交换耦合Nd2Fe14B/α-Fe永磁合金微结构以提高磁性能，用熔体快淬和动态晶化热处理的方法制备了纳米晶交换耦合Nd2Fe14B/α-Fe永磁体，采用XRD和TEM等方法系统研究了动态晶化热处理对Nd10.5（FeCoZr）83.4B6.1永磁体磁性能和显微组织的影响。结果表明：与传统晶化相比，动态晶化可以在相同的晶化温度下缩短晶化时间，同时能细化晶粒，增强晶粒间磁交换耦合作用，提高磁性能。Nd10.5（FeCoZr）83．4B6.1合金快淬薄带经700℃，10min动态晶化热处理后，制得的粘结磁体获得最佳磁性能，剩磁Br=0．685T，内禀矫顽力Hcj=732kA／m，磁感矫顽力Hcb=429kA／m，最大磁能积（BH）m=75kJ／m^3。     

Cu/Ti复合添加对Nd2Fe14B/α-Fe纳米双相磁体磁性能和相分解的影响

用熔体快淬法制备了高性能纳米双相耦合Nd2Fe14B/α-Fe磁体，研究了Cu/Ti复合添加对Nd2Fe14B/α-Fe纳米双相磁体磁性能和相分解的影响，实验结果表明，Cu和Ti复合添加可提高快淬带的晶化温度，并且改变α－Fe相析出方式，α－Fe直接从TbCu7结构的亚稳相分解中析出，而不是从非晶相中析出，这有利于形成α－Fe相晶粒细小且均匀分布的微结构，其最优磁性能为Hc=384kA/m(4.8kOe),σ＝110Am^2/kg(110emu/g),(BH)max=120kJ/m^3(15MGOe)。     

粉末热挤压制备纳米晶复相Nd2Fe14B/α-Fe永磁体

将球磨后获得的Nd2Fe14B非晶相和α-Fe纳米晶直接进行冷压制坯、真空包套、粉末热挤压来制备近致密的纳米晶复相Nd2Fe14B/α-Fe永磁体.借助于X射线衍射(XRD)、透射电子显微镜(TEM)和振动样品磁强计(VSM)等分析方法研究了挤压温度为950℃时,不同加热时间磁体相对密度、微观组织和磁性能的影响规律.结果表明,随加热时间的延长,Nd2Fe14B及α-Fe的晶粒尺寸逐渐长大.当挤压温度为950℃,加热时间为15 min时,Nd2Fe14B及α-Fe的晶粒尺寸比较细小,分别为60和80 nm,此时磁性能最好,达到Br=0.98T,Hci=305.6 kA/m和(BH)m=89.8kJ/m3.     

Nd9Fe85.5-xCoxB5.5 (x=0,1,3,5)合金快淬薄带及其热变形磁体的微观组织与矫顽力

以Nd9Fe85.5-xCoxB5.5(x=0,1,3,5)合金快淬薄带(钼辊表面速度V=35 m/s)为原料采用热压/热变形工艺制备了各向同性磁体。微观组织研究表明,含Co合金快淬薄带由大量非晶和少量α-(Fe, Co)和Nd2(Fe, Co)14B相组成,含Co量达到5at%的合金薄带中出现了亚稳相Nd3-(Fe,Co)62B14,它在随后的热压/热变形过程中分解为α-(Fe,Co)和Nd2(Fe,Co)14B;添加Co元素显著减小了热变形磁体的晶粒尺寸,软磁性相与硬磁性相的平均晶粒尺寸分别从无Co合金磁体的61,168 nm减小为含1at%Co合金磁体的24,50 nm。磁性能研究表明,与晶粒尺寸变化相对应,无Co合金以晶间静磁耦合作用为主,含Co合金以晶间交换耦合作用为主,并且随着Co含量的升高,交换耦合作用有所减弱,导致热变形磁体的矫顽力从无Co磁体的151 kA/m单调增大为含5at%Co磁体的218 kA/m。     

快速加热过程中Nd8Fe86B6合金非晶带的晶化及磁性能

利用高频感应加热的快速晶化方法,对Nd8Fe86B6非晶带进行了晶化退火处理.采用X射线衍射和TEM对原淬态和晶化后的薄带进行了微观组织的分析,用VSM对淬态和快速晶化后薄带的磁学性能进行了测量.观察了在不同晶化条件下Nd8Fe86B6非晶的结构变化以及对其磁性的影响.试验结果表明,快速加热可使非晶带迅速晶化.加热速度和加热时间显著地影响薄带的组织及磁性能.随着加热速度的提高,α-Fe与Nd2Fe14B两相的析出越趋于接近,但过高的加热速度亦使α-Fe过快长大.在快速晶化过程中,α-Fe的长大速度仍大于Nd2Fe14B,因此过长的加热时间将使得α-Fe过度长大.因此,一个较理想的磁学性能都应有一个适合的加热条件相配合.     

单相纳米晶Nd12.3Fe79.2Nb2.5B6合金的交换耦合作用与显微组织

采用熔体快淬及晶化退火工艺制备了含铌单相纳米晶Nd12.3Fe79.2Nb2.5B6合金,研究添加Nb对单相Nd2Fe14B纳米晶合金的磁性能、交换耦合和微观结构的影响规律.结果表明:Nb的添加提高了合金的非晶热稳定性,使得合金最佳晶化温度升高;合金晶化退火后,Nb可使晶粒尺寸分布均匀,并得到单一Nd2Fe14B相;晶粒边界比较完整,存在共格、半共格或大角度晶界,但没有观察到晶界相.上述结构可有效提高合金的磁性能,增强交换耦合作用.通过对Nd12.3Fe79.2Nb2.5B6合金磁性能分析可知:650 ℃晶化退火10 min后的合金性能最佳,交换耦合作用最强.     

Fe68Nd5Zr2Y4B21大块非晶合金磁性能的研究

采用铜模吸铸法制备出厚度为0.8 mm的片状Fe68Nd5Zr2Y4B21大块非晶合金.利用X射线衍射(XRD),差热分析(DTA)和振动样品磁强计(VSM)研究了Fe68Nd5Zr2Y4B21大块非晶合金在铸态和不同温度退火后的磁性能.结果表明,Fe68Nd5Zr2Y4B21大块非晶合金在铸态下为软磁性.合金晶化退火后,磁性能转变为硬磁性,得到了块状的纳米晶复合永磁材料.合金硬磁性的产生是由于合金晶化后产生了Nd2Fe14B硬磁性相和α-Fe,Fe3B软磁性相,软、硬磁相间产生了较强的交换耦合作用而造成的.这一方法为制备块体纳米晶复合永磁材料提供了一种新的手段.     

Nb元素对纳米晶（Nd，Pr）FeB／α-Fe复合永磁合金显微结构与磁性能的影响

添加Nb元素会使(Nd,Pr)FeB/α-Fe纳米晶复合永磁合金的平均晶粒尺寸显著减小.用AFM观察快淬(Nd,Pr)10.5Fe81.5-xNbxCo2B6(x(at%,下同)=0.0,0.5,1.0,1.5,2.0,2.5,3.0)合金条带自由表面的显微结构,晶粒平均直径从不含Nb的(Nd,Pr)10.5Fe81.5Co2B6合金的175 nm减小到含2 at%Nb的(Nd,Pr)10.5Fe79.5Nb2Co2B6合金的68 nm,晶粒平均直径细化了61%;当Nb超过2 at%后,Nb含量的增加对晶粒的细化作用明显减弱,含3 at%Nb的合金平均晶粒直径为63 nm,比含2 at%Nb仅细化了7.3%.含2 at%Nb的(Nd,Pr)10.5Fe79.5Nb2Co2B6合金,粘结磁体磁性能达到最佳值,Bτ=0.665 T,Hci=748 kA·m-1,(BH)m=73 kJ·m-3.Nb元素含量在2 at%Nb以下时,合金晶粒粗大,磁性能较低;超过2 at%后,富集在晶界处的富Nb晶间相加厚,晶粒间的交换作用和剩磁增强效应减弱,合金的内禀矫顽力虽然增加,但剩磁Bτ和最大磁能积(BH)m降低.     

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.     

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.     

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。     

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.