分散的Sm-Co永磁纳米颗粒的机械化学合成及磁性能

通过机械化学合成方法制备了矫顽力分别为2.95×106、2.83×106和8.60×105A/m的分散的单晶纳米Sm2Co7、SmCo5和Sm2Co17硬磁颗粒。研究了球磨时间、原料配比和退火工艺等对所制备的纳米永磁颗粒的微观组织、结构和磁性能的影响。结果表明,机械化学球磨时间至少是4h或更长时才能获得Sm-Co硬磁合金粉末。原料经过高能球磨后、未退火时,由于大部分颗粒为非晶结构,矫顽力较低,随着退火温度的上升,矫顽力增大,当退火温度为600℃时,达到最大值为2.83×106A/m,然后,随着退火温度的进一步升高,矫顽力减小。Sm-Co纳米颗粒的粒径随着退火温度的降低而明显减小。     

分散的Sm-Co永磁纳米颗粒的机械化学合成及磁性能

通过机械化学合成方法制备了矫顽力分别为2.95×106、2.83×106和8.60×105 A/m的分散的单晶纳米Sm2Co7、SmCo5和Sm2Co17硬磁颗粒。研究了球磨时间、原料配比和退火工艺等对所制备的纳米永磁颗粒的微观组织、结构和磁性能的影响。结果表明,机械化学球磨时间至少是4h或更长时间才能获得Sm-Co硬磁合金粉末。原料经过高能球磨后、未退火时,由于大部分颗粒为非晶结构,矫顽力较低,随着退火温度的上升,矫顽力增大,当退火温度为600℃时,达到最大值为2.83×106 A/m,然后,随着退火温度的进一步升高,矫顽力减小。Sm-Co纳米颗粒的粒径随着退火温度的降低而明显减小。     

Fe77Co2Zr9B10Cu2合金的制备及其磁性能

采用单辊快淬法制备了Fe77Co2Zr9B10Cu2合金,在530～750℃等温退火40 min,利用X射线衍射和振动样品磁强计研究了Fe77 Co2 Zr9 B10 Cu2合金的微观结构和磁性能。结果表明:淬态Fe77Co2Zr9B10Cu2合金为非晶、纳米晶双相结构。随着退火温度的升高,α-Fe晶体相从非晶、基体中析出,晶粒尺寸长大,晶化体积分数增加,矫顽力先减小后增大,比饱和磁化强度逐渐增大。实验结果表明,530℃退火后合金的矫顽力最小,在670℃时迅速增大。样品的磁性与其微观结构、晶粒尺寸、晶化体积分数等因素有关.     

Fe掺杂及球磨处理对Sm_2Co_(17)合金结构和磁性的影响

用电弧熔炼法制备Sm2(FexCo1-x)17(x=0,0.3和0.7)母合金锭,均匀化退火后采用球磨方法制备纳米晶合金粉末。研究了Fe掺杂及球磨处理对Sm2(FexCo1-x)17合金结构、居里温度及永磁性能的影响。实验结果表明,随着Fe含量增多,合金中1∶5相逐渐减少,当x=0.7时,形成单相2∶17型化合物,同时居里温度从938℃(x=0)下降到590℃(x=0.7)。球磨处理过程有利于形成单相2∶17纳米合金粉,饱和磁化强度随着球磨时间的增加逐渐增大,同时内禀矫顽力和磁能积与球磨时间的关系呈两头下降的趋势。球磨时间在0.5~1 h时,纳米合金粉末的永磁磁性能达到最佳,Sm2Co17的最佳磁性能为4πMs=0.65 T,iHc=246.8 k A/m,(BH)max=25.5 k J/m3。     

纳米晶Sm_2Co_(17)型块体永磁的制备及磁性能

制备了两种2∶17R型Sm-Co合金:Sm2(Fe,Cu,Zr,Co)17和纯二元Sm2Co17,并利用高能球磨和放电等离子烧结(SPS)制备了致密的纳米晶块体合金,研究了其磁性能和相结构的变化。Sm2(Fe,Cu,Zr,Co)17具有较高的矫顽力,而纯二元Sm2Co17矫顽力基本为零。但高能球磨可快速降低Sm2(Fe,Cu,Zr,Co)17合金的矫顽力。利用放电等离子烧结非晶粉末制备了纳米晶块体合金,纯二元Sm2Co17合金具有较高的矫顽力,并且具有1∶7H相结构。而Sm2(Fe,Cu,Zr,Co)17合金则因为Fe-Co相及Sm2O3相的析出,具有较高的饱和磁化强度和极低的矫顽力。     

热处理对(Fe_(0.52)Co_(0.30)Ni_(0.18))_(73)Cr_(17)Zr_(10)非晶合金的组织结构及磁性能的影响

采用单辊急冷法制备(Fe_(0.52)Co_(0.30)Ni_(0.18))_(73)Cr_(17)Zr_(10)非晶薄带,并对该合金进行等温退火。采用XRD,AFM,VSM研究退火温度对(Fe_(0.52)Co_(0.30)Ni_(0.18))_(73)Cr_(17)Zr_(10)非晶合金的组织结构和磁性能的影响。结果表明:非晶合金晶化过程为Am→α-Fe(Co)+Am′→α-Fe(Co)+Cr_2Ni_3+Fe_3Ni_2+Cr_2Zr+未知相。当退火温度Ti玻璃转变温度Tg时,由于结构弛豫、内应力的释放,合金的饱和磁化强度Ms有所提高;当晶化起始温度TxTi第一晶化峰值温度Tp1时,由于铁磁性α-Fe(Co)相的析出,Ms显著提升;当TiTp1时,由于晶粒长大和第二相的析出,Ms急剧恶化,565℃退火能够获得最好磁性能(Ms=106.8A·m~2·kg~(-1))。490℃和565℃退火后薄带表面的AFM观察表明,AFM图片所呈现的颗粒尺寸要比用Scherrer法测得的α-Fe(Co)纳米晶尺寸大得多,这是典型的包裹晶粒现象。     

纳米TiO2薄膜的制备与表面形貌研究

研究退火温度对薄膜相结构、表面化学组成及形貌的影响。采用射频磁控溅射法在单晶硅片上淀积TiO2薄膜,通过X射线衍射（XRD）、原子力显微镜（AFM）和X光电子能谱（XPS）对其进行表征。结果表明,室温制备400℃以下退火的TiO2薄膜为无定形结构,400℃以上退火的TiO2薄膜出现锐钛矿相,600℃以上退火的TiO2薄膜开始出现金红石相,退火温度在1000℃以上时样品已经完全转变为金红石相;随着退火温度的升高,晶粒尺寸和表面粗糙度逐渐增大,但是当退火温度为1000℃时反而有所减小,晶粒尺寸和表面粗糙度在退火温度为1000℃时发生的这一突变现象,是由该退火温度下的相变导致。     

块状纳米晶Sm2Co17烧结磁体的研究

采用高能球磨和放电等离子烧结技术制备了致密纳米晶Sm2Co17烧结磁体,研究了粉末和烧结磁体的结构和磁性能.球磨粉末在低温退火(<1023K)时,主相为TbCu7结构;高温退火(>1023K)时,主相为Th2Zn17结构.退火温度从923K增加到1223K,粉末的矫顽力从0.99T下降到0.12T.烧结磁体也具有TbCu7结构,磁体平均晶粒尺寸约为35nm.室温时磁体的剩磁为0.65T,矫顽力达0.87T.烧结磁体具有较好的高温性能,573K时的剩磁为0.6T,矫顽力为0.32T.     

放电等离子烧结铁磁性大块非晶的晶化处理及其磁性能研究

采用放电等离子烧结的方法制备出Fe67Co9.5Nd3Dy0.5B20大块非晶合金,且具有很好的非晶性能.用DTA热分析得到合金的第一次晶化结束温度为650℃.在650℃下保温10min退火热处理后,合金出现了较好硬磁性,合金的最大磁能积达61kJ/m3,粉末颗粒的大小对合金的磁性能影响不大.Nd1.1Fe4B4相的析出也对矫顽力有一定影响.     

电沉积制备CuCo颗粒膜微观结构和巨磁电阻效应研究

采用电化学的方法在半导体Si表面沉积了CuCo颗粒膜.研究了膜层电沉积过程中颗粒膜生长的显微结构及热处理过程颗粒膜元素的分布情况.经过450℃退火处理1h后Cu80Co20薄膜GMR达到最大值,随着温度的升高膜层的电阻率也随之下降.面扫描元素分析和XRD分析表明经过退火处理膜层中出现Co粒子的析出,出现了局部富钴的区域.磁阻测量表明此时有利于提高膜层的GMR值.更高温度的退火处理使GMR值降低.磁性能测量发现随着退火温度的提高膜层的饱和磁化强度Ms、矫顽力Hc和剩余磁化强度Mr也随着变大.     

Nanostructured SmCo5 thin films with perpendicular anisotropy formed in a wide range of Sm-Co compositions

In this work, we prepared SmCo5 thin films with (0001) texture exhibiting perpendicular anisotropy in a wide range of Sm(x)Co(100-x) compositions (x = 13.2 approximately 37.0) on Cu/Ta underlayers. At a composition of Sm16.7Co83.3 (SmCo5), the SmCo5 film exhibits a maximum perpendicular coercivity of 18.2 kOe, which is attributed to a good crystallinity and an excellent (000l) texture. The SmCo5 (000l) peaks are shifted to smaller angles compared to the standard powder sample which indicates the formation of a SmCoCu alloy through Cu diffusion. The EDX result for this sample gives a composition of SmCo3Cu2.1 which confirms Cu diffusion into the SmCo5 layer. TEM image shows that SmCo5 film is well crystallized with a grain size of 50 nm.     

Phase Transformation and Magnetic Properties of Mechanically Alloyed PrCo5-based Magnets

PrCo5-based nanograin Pr=CO100-x （x=14-22） alloys with high coercivity were synthesized by mechanical alloying and subsequent annealing. The crystallization, phase components and magnetic properties of the alloys were investigated systematically. The main phase of the alloy for x=14 is Pr2CO17 with rhombohedral Th2Zn17-type. The amount of the Pr2CO17 phase decreases with increasing Pr content, and a nearly single phase PrCo5 with hexagonal CaCu5-type is formed in Pr18Co81 alloy. Further increase in the Pr content leads to the formation of another magnetically hard Pr2Co7 phase with its Curie temperature about 350℃. Remanences decrease monotonously with increasing Pr content, whereas the coercivities increase, reaching a maximum of 2040 kA/m （25.6 kOe） in Pr19CO81 powders milled for 5 h and annealed at 973 K for 2 min, and then decrease for higher Pr content. The high coercivity is attributed to the high anisotropy field of the PrCo~ phase and its nanoscale grain size.     

Exchange Coupling and Magnetic Behavior of SmCo_(5-x)Sn_x Alloys

Exchange coupling and magnetic properties of SmCo5 alloys containing different amounts of Sn were investigated in sintered magnets.X-ray diffraction analysis revealed the formation of Sm2Co17 and Sm2Co7 phases in SmCo5 matrix.Exchange coupling mechanism was evaluated by switching field distribution,dcdemagnetization and magnetization curves as function of reverse applied field.Energy product of 59.2 kJ/m 3(7.4 MGOe),remanent magnetization to maximum magnetization ratio of 0.97 and remanence coercivity to intrinsic coercivity ratio of 1.75 were achieved for 0.2 at.% Sn.     

晶粒尺寸对氧化钒薄膜电学与光学相变特性的影响

采用直流对靶磁控溅射方法制备氧化钒薄膜,通过改变热处理温度获得了具有不同晶粒尺寸的相变特性氧化钒薄膜,对氧化钒薄膜相变过程中电阻和红外光透射率随温度的突变性能进行研究.结果表明:经300℃和360℃热处理后,薄膜内二氧化钒原子分数达到40%,氧化钒薄膜具有绝缘体-金属相变特性,薄膜的晶粒尺寸分别为50nm和100nm;...     

X-ray and Magnetoresistance Measurements of Electrodeposited Cu-Co Granular Films

Granular CoxCu1-x alloy films were prepared by electrodeposition at room temperature directly onto semiconducting Si substrate. X-ray diffraction (XRD) revealed that the as-deposited films formed single phase metastable fcc alloy structure. The fcc lattice parameter αwas found to decrease linearly with increasing Co concentration x in the studied range. The giant magnetoresistance (GMR) of the films was improved after annealing. Pure Co fcc diffraction peaks were observed in the diffractogram of the annealed sample, indicating phase separation occurred upon annealing. The optimal annealing temperature was 450℃. The maximum of magnetoresistance (MR) ratio 8.21% was obtained for the Co20Cu80 thin film after annealing at 450℃for 1 h. The saturation field decreased upon annealing in the MR curves of Co20Cu80 film.     

Structural Stability and Magnetic Properties of the TbCu$_{7}$ -Type SmCo$_{x - 0.4}$Ti$_{0.4} (x = 5.0hbox{–}8.5)$ Alloys

We have studied the composition dependence, thermal stability, long-term stability at 500°C, and magnetic properties of the nanostructural TbCu₇-type (1:7) Sm-Co-Ti alloys. We prepared the SmCox-0.4Ti_0.4 alloys with a wide composition range from x = 5.0 to x = 8.5 by high-energy ball-milling, followed by annealing at 700-1100°C for 2 h. After annealing at 700°C, the powders with x = 7.0-8.5 showed a single 1:7 structure, while the powders with x = 5.0-6.5 presented the 1:7 plus CaCu₅-type (1:5) structure. At an annealing temperature higher than 800°C, a minor Th₂Zn₁₇-type (2:17) phase precipitated in the matrix of the 1:7 phase. Intrinsic coercivity iHc exhibits a maximum of 2.3 T at room temperature and 0.4 T at 500°C in the x = 7.0 samples annealed at 700°C. The temperature coefficient of iHc seems stable as the Sm/Co ratio changes from 1/6.5 to 1/7.5. The coercivity decreased with increasing annealing temperature Ta, from 2.3 T at Ta = 700°C to 1.3 T at Ta = 1100°C, which is mainly attributed to the grain growth from 35 nm for Ta = 700°C to 1 ?m for Ta = 1100°C. After holding at 500°C for up to 360 h, the microstructure and magnetic properties of the 1:7-type nanograin alloys remained almost unchanged, indicating a structurally and magnetically long-term stabilization at the potential high-temperature application environment.     

Hierarchical assembly of Sm2Co7/Co magnetic nanoparticles into highly stable and uniform nanospheres

Hierarchical assembly of colloidal Sm2Co7/Co clusters in the form of nanospheres has been processed through a polyol process. The SmCo nanospheres are found to be robust, uniform ( 100 nm) and tend to self-assemble in the form of ordered superstructures. Each nanosphere consists of large number of discrete fine particles ( 6.0 nm), having two-phase structure of both Sm2Co7 and Co-phases. Upon annealing, these phases transform into Sm2Co17 phase with very high magnetization (169 emu/g). A possible mechanism on the formation of nanospheres from the individual Sm2Co2o7 and Co nanoparticles is also discussed.