新型FeMB系纳米晶软磁材料的成分设计

运用Miedema理论,系统计算Fe,B与Cu,Mo,Ni,Cr,V,Ga,Nb,Hf和Zr等元素形成合金系时的热力学性质。运用理想溶液理论,计算1 600 K时该二元合金系的过剩Gibbs自由能、过剩熵和活度。结果表明,在FeMB体系中,Fe-Zr-B的混合焓最小;1 600 K时Fe-M-B体系的过剩Gibbs自由能与其混合焓相似,其过剩熵趋近于零,活度相对于理想溶液偏差极小,在实际应用中可忽略不计。     

Electrodeposition of Ni-SiC nanocomposite film

The point of zero charge(PZC) of SiC nanoparticles was determined by means of standard potentiometric titration method, while the influences of the main technological parameters on the microstructure of electrodeposited Ni-SiC composite film were studied and optimized. The results show that high bath pH value favors SiC nanoparticles negatively charged and high bath temperature promotes them positively charged. Under the experimental conditions, sodium dodecyl-glycol is proven to be an effective surface modification anionic surfactant for SiC nanoparticles. The results also show that the optimized Ni-SiC composite film is composed of the nanoparticles with the average grain size in the nanometer range (100 nm), and SiC nanoparticles disperse into the nickel matrix uniformly.     

含硼、磷添加剂对电沉积CoNiFe软磁薄膜的影响(英文)

采用循环伏安法制备CoNiFe、CoNiFeB和CoNiFeP软磁薄膜。采用SEM、EDS和XRD进行薄膜形貌、成分及相组成分析,应用振动样品磁强计(VSM)测量其软磁性能,并采用电化学阻抗谱(EIS)及极化曲线研究其腐蚀阻力。结果表明,电沉积CoNiFe、CoNiFeB和CoNiFeP软磁薄膜为晶态和非晶态混合体,含硼、磷添加剂可促进非晶相的形成;CoNiFe和CoNiFeB具有纳米结构;含硼添加剂可提高薄膜的致密度和阻力,并使矫顽力从851.48A/m降低至604.79A/m,而磁饱和强度基本不变。含磷添加剂可增加薄膜粒子的尺寸并降低其耐蚀性,并使CoNiFeP薄膜的矫顽力增加至12485.79A/m,磁饱和强度大幅度降低至1.25T。     

Pitting corrosion of 304ss nanocrystalline thin film

Pitting corrosion behavior of coarse crystalline (CC) 304ss and its nanocrystalline (NC) thin film have been investigated by electrochemical measurement and in situ AFM observation in 3.5% NaCl solution. Results show two effects of nanocrystallization on pitting corrosion behavior: (1) more frequent occurrence of metastable pits, but with lower probability of transition to stable pits, which is attributable to differences in morphologies of sulfur and manganese as well as outstanding repassivation ability of NC thin film; (2) nanocrystallization decreases stable pit generation rate and its propensity to form larger pit cavities, and modifies the morphology of stable pit cavity.     

新型Fe72.7Si17B6.8Nb2.6Cu0.9纳米晶铁芯的磁场热处理工艺与软磁性能

为满足高频变压器对铁芯低损耗的需求,研究了新型Fe_72.7Si₁₇B_6.8Nb_2.6Cu_0.9纳米晶铁芯的热处理工艺,探讨了铁芯动态、静态软磁性能随无磁场退火保温时间与施加不同磁场强度的横磁磁场退火时的变化规律。结果表明,不加磁场时,保温时间为60 min时铁芯的损耗最低,为P_{20 kHz/0.5 T}=11.82 W/kg,而其静态软磁性能在保温30 min处于最优状态,H_{c30 min}=1.86 A/m。施加横向磁场后,其直流磁性能剩磁和矫顽力显著降低,H_{c40 mT}=0.64 A/m,而其损耗在磁场强度为50 mT达到最低,为P_{20 kHz/0.5 T}=10.53 W/kg。高频范围内涡流损耗在铁芯损耗中起主导作用,新型纳米晶铁芯经横向磁场热处理后高频损耗大幅降低,同时磁导率表现优异。     

Crystallization process and soft magnetic properties of nanocrystalline (Fe0.5 Co0.5 ) 86 Hf7 B6 Cu1 alloy used in elevated temperature applications

Nanocrystalline (Fe0.5 Co0.5 )86 Hf7 B6 Cu1 HITPERM alloy was investigated as the candidate of soft magnetic material for high temperature applications, compared with Fe86 Hf7B6 Cu1 NANOPERM alloy. Amorphous alloy ribbons were prepared by single-roller melt-spinning technology. Crystallization process of as-quenched ribbon was investigated using differential scanning calorimeter at different heating rates. The coercivity was determined from quasi-static hysteresis loop measured at room temperature using a computerized hysteresis loop tracer. X-ray diffraction with Cu Kα radiation was used to determine the structure. The vibrating sample magnetometer was usedto measure the magnetization as a function of temperature of the nanocrystllized alloys. That Co substitution for Fein alloy enhances the Curie temperature of amorphous alloy and the magnetization of nanocrystalline alloy at hightemperature. After annealing amorphous precursor, the optimum nanocrystalline alloy obtained shows the local minimum coercivity. The coercivity increases with the increasing annealing temperature corresponding to the formation of ferromagnetic phase in the secondary crystallization.     

Hot-press sintering of MA Fe-based nanocrystalline／amorphous soft magnetic powder

Microstructures and magnetic properties of Fe84 Nb7 B9, Fe80 Ti8 B12 and Fe32 Ni36 (Nb/Ⅴ) 7 Si8 B17 powders and their bulk alloys prepared by mechanical alloying(MA) method and hot-press sintering were studied. The results show that: 1) After MA for 20 h, nanocrystalline bcc single phase supersaturated solid solution forms in Fe84-Nb7 B9 and Fe8o Ti8 B12 alloys, amorphous structure forms in Fe32 Ni36 Nb7 Si8 B17 alloy, duplex microstructure composed of nanocrystalline γ-(FeNi) supersaturated solid solution and trace content of Fe2B phase forms in Fe32 Ni36-V7 Si8 B17 alloy. 2) The decomposition process of supersaturated solid solution phases in Fe84 Nb7 B9 and Fe80 Ti8 B12alloys happens at 710 -780 ℃, crystallization reaction in Fe32 Ni36 Nb7 Si8 B17 alloy happens at 530 ℃ (the temperature of peak value) and residual amorphous crystallized further happens at 760 ℃ (the temperature of peak value), phase decomposition process of supersaturated solid solution at 780 ℃ (the temperature of peak value) and crystallization reaction at 431 ℃ (the temperature of peak value) happens in Fe32 Ni36 V7Si8B17 alloy. 3) under 900 ℃, 30 MPa,0.5 h hot-press sintering conditions, bulk alloys with high relative density(94.7%- 95.8%) can be obtained. Except that the grain size of Fe84 Nb7B9 bulk alloy is large, superfine grains (grain size 50 - 200 nm) are obtained in other alloys. Except that single phase microstructure is obtained in Fe80 Ti8B12 bulk alloy, multi-phase microstructures are obtained in other alloys. 4) The magnetic properties of Fe80 Ti8 B12 bulk alloy(Bs = 1.74 T, Hc = 4.35 kA/m) are significantly superior to those of other bulk alloys, which is related to the different phases of nanocrystalline or amorphous powder formed during hot-press sintering process and grain size.     

频率和磁场强度对非晶及纳米晶合金带材磁性能的影响

研究了频率(f10 kHz)和磁场强度对商业非晶合金1K101和纳米晶合金1K107成品带材铁芯的损耗Pc和幅值磁导率μa的影响。结果表明,两种带材铁芯损耗Pc均正比于磁感应强度B的平方(Pc∝B2)及正比于频率f的平方(Pc∝f2);两种带材铁芯的μa都随B增加到一定值然后下降;当频率f为200 kHz时,1K107合金带材在B为0.4 T时最大幅值磁导率μa=27273.3;1K101合金带材在B=0.7 T时具有最大幅值磁导率μa=6548.9;在相同f、B条件下1K107带材损耗明显小于1K101,即便是f相同、B更大的情况下前者损耗仍可能小于后者,例如P1K107(200 kHz,0.7T)为1302.08 W/kg,P1K101(200 k Hz,0.4T)为2180.36 W/kg,表明纳米晶合金带材的磁性能明显优于非晶合金带材,更适合用于制备高频电力电子变压器铁芯。     

磁控溅射Al-Fe-Sn 薄膜的电输运性能

在电子工业中,为了制备低电阻率的Al合金薄膜,需要对薄膜进行退火。虽然材料的电阻率与其电输运性能密切相关,然而目前为止,对于铝合金薄膜的电输运性能研究甚少。 本文首先利用TEM对于磁控溅射铝合金薄膜的结构,特别是与基底界面处的结构进行了表征。在此基础上,利用霍尔效应测试了解界面状态的变化对于霍尔载流子浓度及迁移率的影响。 我们实验的结果表明, 在退火的过程中,薄膜与下层基底之间通过扩散过程形成紧密接触,从而使得合金薄膜同时具有较高的载流子浓度以及载流子迁移率。最后,利用一个新提出的能带模型,解释所观察到的界面变化对于电导率的影响。     

非平衡磁控溅射离子镀Cu-Nb纳米晶薄膜的微观结构及性能

研究了Nb含量对纳米晶Cu-Nb薄膜微观结构和性能的影响。使用非平衡磁控溅射离子镀技术,在具有(100)晶面的单晶Si基体和玻璃基体上制备不同Nb含量的Cu-Nb纳米晶薄膜,研究Nb含量对纳米晶Cu-Nb薄膜微观结构和性能的影响。将样品置于卧式真空退火炉中进行400 ℃退火,用配备了能量色散X射线光谱仪的场发射扫描电镜、原子力显微镜、X射线衍射仪、纳米压痕仪和四探针电阻率测试仪等分析了退火前后薄膜的微观结构、力学性能与电学性能。结果表明,沉积态Cu-Nb薄膜表面由致密的纳米晶组成,表面粗糙度最高仅为8.54 nm,且无明显的孔洞和裂纹等缺陷。随着Nb含量的增加,薄膜的平均晶粒尺寸下降5 nm,薄膜的硬度也因细晶强化而有所增加,在靶电流为1.3 A时达到最大值4.9 GPa。退火态样品在硬度、弹性模量、平均晶粒尺寸和表面粗糙度方面与沉积态薄膜相比有较小的变化,Cu-Nb薄膜表现出优良的热稳定性。Nb的加入可有效细化晶粒,达到细晶强化的效果,同时Cu-Nb不互溶的特性使得纳米晶薄膜在高温下也可保持较好的热稳定性。Nb靶溅射电流为0.5 A 时薄膜综合性能最佳,此时沉积态Cu-Nb薄膜的电阻率最低,为3.798×10^-7 Ω/m,硬度和弹性模量高达4.6 GPa和139.5 GPa,薄膜厚度为1050 nm,粗糙度R_a为4.70 nm。     

Influence of electroplating conditions on magnetic properties of Fe-36wt.% Ni alloy film

A Fe-Ni soft magnetic film was prepared in sulphate solution by electroplating. The influences of the molar ratio of n [Fe2+ ]/ n [Ni2+ ], current density, bath temperature, pH and L-ascorbic acid concentration on magnetic properties of Fe-Ni alloy film were investigated. The results show that the saturated flux density(BS) of the film increases initially and decreases after it reaches the specific value with the increase of n [Fe2+ ]/ n [Ni2+ ] molar ratio, current density, bath temperature and pH. However, the relationship between L-ascorbic acid concentration and B S keeps linear. It is observed that the coercive force( Hc) is enhanced with the increase of n [Fe2+ ]/ n [Ni2+ ] molar ratio, current density and pH. By comparison, when the bath temperature increases, Hc always decreases. With the increase of L-ascorbic acid concentration, the coercive force increases initially and then decreases.     

热处理温度对Fe-Ni合金薄膜微结构及磁性的影响

采用直流电沉积法在硫酸盐-氯化物镀液中制备了Fe-44wt%Ni纳米晶合金薄膜.通过原子力显微镜(AFM)、X射线衍射(XRD)、透射电子显微镜(TEM)以及开路磁测量装置,对Fe-44wt%Ni合金薄膜镀态和退火态样品的微结构和磁性能进行测量.结果表明:退火温度升高能够降低薄膜内应力,使薄膜结晶均匀,但对薄膜晶粒尺寸和磁性能影响很大.Fe-44wt%Ni合金薄膜是由γ-(Fe,Ni)相和α-(Fe,Ni)相构成.在250℃真空退火处理1h后Fe-44wt%Ni合金薄膜的晶粒尺寸在20～30 nm之间,且具有良好的软磁性能,饱和磁感应强度BS为1.06T,矫顽力HC为40A/m.     

工艺参数对气膜软接触连铸坯组织性能的影响

研究了气体种类、气体流量、拉坯速度等工艺参数对气膜软接触连铸坯组织性能的影响.结果表明:随气体流量的降低、拉坯速度的增大,铸坯的表面质量变差,宏观组织中的等轴晶比例降低,铸坯的皮下反偏析层厚度增大;气膜软接触连铸坯的力学性能明显高于传统DC连铸坯.     

退火温度对Fe_(52)Co_(26)Nb_6B_(15)Cu_1合金纳米晶软磁特性及微波磁谱的影响

采用熔体快淬法制备了Fe52Co26Nb6B15Cu1合金非晶薄带,使用非晶晶化法在480、500、550、600、650℃对其进行等温退火处理,后采用机械球磨法将其球磨得到Fe52Co26Nb6B15Cu1合金微细磁粉。结合X射线衍射分析、振动样品磁强计等测试技术研究热处理温度对Fe52Co26Nb6B15Cu1合金纳米晶的微结构及软磁相关性能的影响。在此基础上使用矢量网络分析仪测试并分析了热处理温度对该纳米晶复合材料在500 MHz~18 GHz磁谱的影响。结果表明,通过控制热处理温度可以有效的调控Fe52Co26Nb6B15Cu1合金样品的微结构与软磁性能,进而在较大范围内调整样品的复数磁导率(μ′(2.0~4.2),μ″(1.0~2.5))。     

Effect of bonding conditions on conduction behavior of anisotropic conductive film interconnection

This paper presents an investigation on the conduction behaviors of the anisotropic conductive film (ACF) interconnections bonded at various bonding forces. The connection resistance of the ACF joints decreased with increasing bonding force up to 70 N, but subsequently converged to a value of 10 mΩ at bonding forces above 70N. This convergence of the connection resistance in the ACF joints was due to two opposing factors: decreased resistance due to increased contact area and increased resistance due to decreased currentflow path that may have been affected by the delamination of the metal film from the polymeric cores at high bonding forces. During thermal shock testing of the adhesive joints, two different conduction behaviors were observed: increasing connection resistance and the termination of Ohmic behavior. The former was due to decreased contact areas caused by warpage of the package, whereas the latter was caused by delamination at the interface.     

Corrosion behavior of iron thin film in deaerated phosphate solutions by an electrochemical quartz crystal microbalance

The corrosion rates of iron thin film in deaerated phosphate solutions were measured by an electrochemical quartz crystal microbalance as a function of solution pH or phosphorus concentration in solutions. The dependences of corrosion rate and corrosion potential on solution pH and phosphorus concentration have suggested that the corrosion mechanism changes in the vicinity of pH 5 and H₂PO₄⁻ contributes to both anodic dissolution of iron and hydrogen evolution. The corrosion mechanism which contains iron-phosphate-hydroxide complex ion as an adsorbed intermediate was proposed to explain the experimental results.     

Lithium intercalation/de-intercalation behavior of a composite Sn/C thin film fabricated by magnetron sputtering

A tin film of 320 nm in thickness on Cu foil and its composite film with graphite of～50 nm in thickness on it were fabricated by magnetron sputtering.The surface morphology,composition,surface distributions of alloy elements,and lithium intercalation/de-intercalation behaviors of the fabricated films were characterized by X-ray diffraction (XRD),scanning electron microscopy (SEM),electron probe microanalyzer (EPMA),X-ray photoelectron spectroscopy (XPS),inductively coupled plasma atomic emission spectrometry (ICP),cyclic voltammetry (CV),and galvanostatic charge/discharge (GC) measurements.It is found that the lithium intercalation/de-intercalation behavior of the Sn film can be significantly improved by its composite with graphite.With cycling,the discharge capacity of the Sn film without composite changes from 570 mAh/g of the 2nd cycle to 270 mAh/g of the 20th cycle,and its efficiency for the discharge and charge is between 90% and 95%.Nevertheless,the discharge capacity of the composite Sn/C film changes from 575 mAh/g of the 2nd cycle to 515 mAh/g of the 20th cycle,and its efficiency for the discharge and charge is between 95% and 100%.The performance improvement of tin by its composite with graphite is ascribed to the retardation of the bulk fin cracking from volume change during lithium intercalation and de-intercalation,which leads to the pulverization of fin.     

Effect of additional element and heat treating temperature on micro-structure and mechanical behavior of Ag alloy thin film

For Ag alloy film used for the storage media, it is required to have heat-resistance, anti-constant temperature and anti-constant humidity characteristics, corrosion resistance, while high reflectivity over Al is maintained. An Ag alloy thin film （additive element Pd, Cu, P） was created on glass substrates, and various heat treatment was conducted. Then, fine structure was observed on this thin film using AFM, and fine structure evaluation of the inside was carried out by the in-plane diffractometry and X-ray diffraetometry, and in addition, residual stress analysis was carried out. These results were compared and were examined, and fine structure and physical property in a metallic thin film were evaluated, and usefulness of evaluation method was verified.     

Fretting wear behavior of Ti/TiN multilayer film on uranium surface under various displacement amplitudes

Ti/TiN multilayer film was deposited on uranium surface by arc ion plating technique to improve fretting wear behavior. The morphology, structure and element distribution of the film were measured by scanning electric microscopy (SEM), X-ray diffractometry (XRD) and Auger electron spectroscopy (AES). Fretting wear tests of uranium and Ti/TiN multilayer film were carried out using pin-on-disc configuration. The fretting tests of uranium and Ti/TiN multilayer film were carried out under normal load of 20 N and various displacement amplitudes ranging from 5 to 100 μm. With the increase of the displacement amplitude, the fretting changed from partial slip regime (PSR) to slip regime (SR). The coefficient of friction (COF) increased with the increase of displacement amplitude. The results indicated that the displacement amplitude had a strong effect on fretting wear behavior of the film. The damage of the film was very slight when the displacement amplitude was below 20 μm. The observations indicated that the delamination was the main wear mechanism of Ti/TiN multilayer film in PSR. The main wear mechanism of Ti/TiN multilayer film in SR was delamination and abrasive wear.