Co-Sn单相合金深过冷凝固时Co3Sn2 相生长形貌的演变机制

开展了(Co₆₀Sn₄₀)_100-xNb_x (x=0,0.4,0.6,0.8,at%)单相合金的深过冷凝固实验,研究了Co₃Sn₂相生长形貌的演变机制。结果表明,在小过冷度下,Co₃Sn₂相在x=0,0.4以海藻状的模式进行生长,随着添加的Nb含量增加至0.6at%,其生长形貌转变为树枝晶,并在x=0.8进一步转变为分形海藻晶,这主要是由于界面能各向异性和动力学各向异性的变化。随着过冷度的增加,(Co₆₀Sn₄₀)_99.4Nb_0.6合金中Co₃Sn₂相生长形貌在过冷度大于28 K时从树枝晶转变为分形海藻,当过冷度高于143 K时转变为密集海藻。少量的Nb添加在小过冷度和中间过冷度时能提高Co₃Sn₂相的生长速度,但是在大过冷度下会显著降低生长速度。Co₃Sn₂相生长速度随过冷度变化规律的转变对应其生长形貌从分形海藻向密集海藻的转变。     

球磨对Sn-Co合金结构和电化学性能的影响研究

以金属Sn、Co粉末为原料,采用先固相烧结再球磨的方法制备了CoSn2/CoSn和Co3Sn2合金,考察了不同原料配比条件下球磨对合金形貌、结构和电化学性能的影响.结果表明,按照目标产物配比可分别获得单相CoSn2、CoSn和Co3Sn2合金,且合金经过球磨后晶粒细化;球磨可提高Sn-Co合金的电化学性能,对CoSn2的循环性能提升效果显著,经过25次循环后的容量保持率提升了16.5％;对CoSn和Co3Sn2的容量和充放电效率提升效果显著,CoSn的首次放电容量和充放电效率分别提升了167 mAh/g和16.6％,Co3Sn2分别提升了151mAh/g和21.5％.     

Mn1-xZnxFe2O4 (0≤x≤1)纳米粉体的模板辅助溶胶凝胶法制备及其磁性能研究

通过模板辅助溶胶-凝胶法制备了一系列的Mn_1-xZn_xFe₂O₄(0≤x≤1,步长为0.2)纳米粉体。利用XRD和VSM对材料的物相和磁性能进行了表征,主要研究了Mn_1-xZn_xFe₂O₄分子式中Zn含量的变化对样品的微观结构和磁性能的影响。实验结果表明,具有不同Zn含量的Mn_1-xZn_xFe₂O₄样品均为尖晶石结构;随着Zn含量的增加,样品的晶面间距d、平均晶粒尺寸D、饱和磁化强度M_s和居里温度T_c都呈现出下降的趋势,而样品的矫顽力H_c则呈现出先升高后降低的趋势。分析认为,M_s的下降可以用Yafet-Kittel倾角理论解释,T_c的降低归因于晶格中反铁磁性耦合的降低,而H_c的变化则主要是由于材料的磁晶各向异性常数K₁的变化引起的。     

不同锂源对高温固相法制备NCM811正极材料储锂性能的影响

采用4种不同的锂盐(LiOH.H₂O、Li₂CO₃、LiNO₃、CH₃COOLi),以高温固相法制备了LiNi_0.8Co_0.1Mn_0.1O₂正极材料。利用X射线粉末衍射(XRD)和场发射电子显微镜(FESEM)对所制LiNi_0.8Co_0.1Mn_0.1O₂材料的微观结构进行了表征,发现所有合成的LiNi_0.8Co_0.1Mn_0.1O₂样品尺寸均为微米级大小,具有层状结构(R-3m空间群)。电化学测试结果表明采用不同锂源制备的LiNi_0.8Co_0.1Mn_0.1O₂样品的电化学性能差别很大。其中采用LiOH?H₂O为锂源,经500 °C预烧结6 h后,在800 °C下烧结16 h获得的样品锂镍混排程度最低,电化学性能最佳。例如,在0.1 C(1 C=180 mA/g)倍率下其可逆比容量高达206.2 mA.h/g,在10 C大倍率下,其可逆比容量仍保持有80.9 mA.h/g;在0.5 C倍率下100次充放电循环过程中,最高放电比容量为176.2 mA.h/g,平均放电比容量为140.1 mA.h/g。动力学及电极稳定性分析发现,LiOH?H₂O制备的样品的电化学可逆性最好,Li^₊扩散系数最大,充放电循环过程中结构稳定性最好。     

Li3-2xB1-xNxO3(x=0.1,0.2,0.3)锂离子固体电解质的制备和性能研究

首次以硝酸锂、碳酸锂、氧化硼为原料,采用固相法制备得到了Li_3-2xB_1-xN_xO₃(x=0.1,0.2,0.3)锂离子固体电解质,通过无压烧结制备得到固体电解质片,并通过x射线衍射(XRD),扫描电子显微镜(SEM),电化学交流阻抗(EIS)对Li_3-2xB_1-xN_xO₃(x=0.1,0.2,0.3)固态电解质进行了表征。结果表明：当x=0.2时,采用无压烧结在600℃烧结10 h制备得到的固体电解质片致密度最高,达到理论密度的90.07%,室温锂离子总电导率也最大,为6.37×10_-6 S/cm,此时激活能值最小,为0.48eV。     

Cr3+掺杂LiNi0.5Mn1.5O4材料的制备及性能研究

采用高温固相法合成了Cr₃₊掺杂的LiNi_0.5Mn_1.5O₄正极材料,研究了掺杂量对材料物理性能和电化学性能的影响。利用XRD、SEM对材料的结构和形貌进行了表征,结果显示样品具有棱边清晰的尖晶石形貌。讨论了不同Cr₃₊掺杂量对LiCr_xNi_0.5-0.5xMn_1.5-0.5xO₄(x=0,0.05,0.1,0.15,0.2)正极材料性能的影响。充放电测试、循环伏安和交流阻抗测试结果表明：当Cr₃₊的掺杂量为x=0.1时(LiCr_0.1Ni_0.45Mn_1.45O₄)正极材料的性能最好,0.1C、0.5C、1C、2C及5C的首次放电比容量依次为131.54mAh g_-1、126.84mAh g_-1、121.28mAh g_-1、116.49mAh g_-1和96.82mAh g_-1,1C倍率下循环50次,容量保持率仍为96.5%。     

网孔结构La2Sn2O7粉体的制备及其在Ag-电接触材料的制备及性能研究

以五水四氯化锡和硝酸镧为原料,采用化学共沉淀法在烧结温度920℃条件下合成了锡酸镧粉体。通过高能球磨法+成型烧结工艺制得Ag-La₂Sn₂O₇电接触复合材料。重点考察了胶凝剂浓度、烧结工艺对La₂Sn₂O₇粉体形貌及物相的影响,并对Ag- La₂Sn₂O₇电接触材料的物理性能进行了分析。研究结果表明：以碳酸氢铵为胶凝剂,于烧结温度920℃,2h条件下获得具有网孔结构的La₂Sn₂O₇粉体;于成型压力1200MPa,烧结温度900℃,6h条件下制得的Ag-La₂Sn₂O₇电接触材料表现出较佳的电阻率和硬度值。经过热挤压工艺,Ag-La₂Sn₂O₇电接触材料发生了大塑性变形,颗粒在热挤压过程中发生流动变形,形成类纤维状结构的排列分布状态,表现出更低的电阻率。     

高容量锂离子电池正极材料LiNi0.5Co0.2Mn0.3O2的制备与工艺优化

采用氢氧化物共沉淀法合成前驱体Ni_0.5Cc_0.2Mn_0.3H(OH)₂,进一步用高温固相法与锂源共混煅烧得到LiNi_0.5Co_0.2Mn_0.3O₂。初步探讨了前驱体与锂源在高温煅烧过程中的质量变化及煅烧工艺对材料结构和性能的影响。热重分析(TGA)表明在煅烧过程中750℃后材料质量几乎没有变化。X射线衍射(XRD)对750℃-900℃的材料进行结构分析,结果表明所有材料具有良好的α-NaFeO₂层状结构和较小的阳离子混排度。扫描电镜(SEM)分析表明材料具有表面光滑,分布均匀的球形结构。横流充放电测试结果表明在850℃煅烧的材料具有最好的电学性能,在0.2C,2.5-4.6V测试条件下,其具有193.7mAh/g的首次放电容量,循环30次后的容量保持率为94.2%,并且具有最好的倍率性能。     

有机纳米颗粒复合Co掺杂ZnO热电性能研究

有机-无机纳米结两端有机材料的离散轨道能级与无机半导体的连续能带差异减小时,使得纳米结界面具有选择性散射不同能量载流子的特征,有利于提高赛贝克系数和热电性能。本文利用溶胶-凝胶法合成了具有有机-无机纳米结结构的聚对苯撑(PPP)纳米复合Zn_1-xCo_xO材料。研究结果表明,较高电导率和赛贝克系数使Zn_0.925Co_0.075O/9 wt% PPP呈现较大的功率因子。另外,有机-无机纳米界面上的界面散射大大降低了热导率。因而,合成的纳米复合材料最大ZT值达到0.22,是Zn_0.925Co_0.075O基体材料的5倍。这一实验结果表明纳米结效应是提高块体热电材料热电性能的有效途径。     

Na_(1.4)Co_2O_4基热电材料的溶胶-凝胶法制备及表征

采用溶胶-凝胶法制备了掺杂Sr, Li和Cu的Na_1.4Co₂O₄基热电材料, 采用XRD分析了Na_1.4Co₂O₄基热电材料的相组成.通过DTA-TG曲线确定材料的预烧结和终烧结温度分别为450和850 ℃. 研究了掺杂量对Na_1.4Co₂O₄基材料电阻率、Seebeck系数和功率因子等热电性能的影响. 结果表明, 掺杂Li可降低Na_1.4Co₂O₄的电阻率, 掺杂 Sr和Cu使材料的电阻率增加; 掺杂Li和Cu可大幅度提高Na_1.4Co₂O₄的Seebeck系数和功率因子; 掺杂Sr的改善效果不显著, 掺杂Li的效果最好; 当Li掺杂量为0.40, Na_1.4Co₂O₄基热电材料的功率因子在15℃时达到最大值 7444.73 μW?m^-1?K^-2.     

Microstructural evolution of intermetallic compounds in Sn–3.5Ag–X (X = 0, 0.75Ni, 1.0Zn and 1.5In)/Cu solder joints during liquid aging

In this paper, the microstructural evolution of IMCs in Sn–3.5Ag–X (X = 0, 0.75Ni, 1.0Zn, 1.5In)/Cu solder joints and their growth mechanisms during liquid aging were investigated by microstructural observations and phase analysis. The results show that two-phase (Ni₃Sn₄ and Cu₆Sn) IMC layers formed in Sn–3.5Ag–0.75Ni/Cu solder joints during their initial liquid aging stage (in the first 8 min). While after a long period of liquid aging, due to the phase transformation of the IMC layer (from Ni₃Sn₄ and Cu₆Sn phases to a (Cu, Ni)₆Sn₅ phase), the rate of growth of the IMC layer in Sn–3.5Ag–0.75Ni/Cu solder joints decreased. The two Cu₆Sn₅ and Cu₅Zn₈ phases formed in Sn–3.5Ag–1.0Zn/Cu solder joints during the initial liquid aging stage and the rate of growth of the IMC layers is close to that of the IMC layer in Sn–3.5Ag/Cu solder joints. However, the phase transformation of the two phases into a Cu–Zn–Sn phase speeded up the growth of the IMC layer. The addition of In to Sn–3.5Ag solder alloy resulted in Cu₆(Sn_x,In_1?x)₅ phase which speeded up the growth of the IMC layer in Sn–3.5Ag–1.5In/Cu solder joint.     

Composition dependences of thermodynamical properties associated with Pb-free ternary,quaternary, and quinary solder systems

In the present study, Chou’s General Solution Model (GSM) has been used to predict the enthalpy and partial enthalpies of mixing of the liquid Ag–In–Sn ternary, Ag–In–Sn–Zn quaternary, and Ag–Au–In–Sn–Zn quinary systems. These are of technical importance to optimize lead-free solder alloys, in selected cross-sections: x_In/x_Sn = 0.5/0.5 (ternary), Au–In_0.1–Sn_0.8–Zn_0.1, Ag–In_0.1–Sn_0.8–Zn_0.1 (quaternary), and t = x_Au/x_In = 1, x_In = x_Sn = x_Zn (quinary) at 1173, 773, and 773 K, respectively. Moreover, the activity of In content in the ternary alloy system Ag–In–Sn has been calculated and its result is compared with that determined from the experiment, while the activities of Ag contents associated with the alloys mentioned above have been calculated. The other traditional models such as of Colinet, Kohler, Muggianu, Toop, and Hillert are also included in calculations. Comparing those calculated from the proposed GSM with those determined from experimental measurements, it is seen that this model becomes considerably realistic in computerization for estimating thermodynamic properties in multicomponent systems.     

x(Mg0.7Zn0.3)0.95Co0.05TiO3-(1−x)(La0.5Na0.5)TiO3 ceramic at microwave frequency with a near zero temperature coefficient of resonant frequency

Dielectric properties of x(Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃-(1?x)(La_0.5Na_0.5)TiO₃ ceramic were investigated at microwave frequencies. A nearly 0 ppm/°C temperature coefficient of resonant frequency was realized at x = 0.9. A two-phase system was confirmed by XRD analysis. A dielectric material applicable to microwave devices with a Q × f of 20,000–87,000 GHz and a dielectric constant of 21.27–26.2 was obtained at 1100 °C after 4 h of sintering. The microwave dielectric material 0.9(Mg_0.7Zn_0.3)_0.95Co_0.05TiO₃-0.1(La_0.5Na_0.5)TiO₃ sintered at 1150 °C for 4 h has a dielectric constant of 24.56, a Q × f of 68,000 GHz, and a τ_f value of 0 ppm/°C. It is proposed as a candidate dielectric for GPS patch antennas.     

(Sn1-xZnx)57(In0.78Bi0.22)43低熔点无铅焊料的微观结构表征(英文)

为了寻求一种应用于三维集成电路低温焊接的无铅焊料，基于多组元混合的概念设计并表征(Sn_1-xZn_x)₅₇-(In_0.78Bi_0.22)₄₃ (x=0.10,0.15,0.20，摩尔分数，%)四元合金。采用扫描电子显微镜、X射线衍射仪和差示扫描量热仪研究合金的显微组织、热性能和润湿性。结果表明，合金由金属间化合物BiIn₂、In_0.2Sn_0.8和富Zn固溶体组成。随着Zn添加量的增加，BiIn₂和富Zn相的体积分数增加。合金的熔点低至70℃，源自低熔点金属间化合物In_0.2Sn_0.8和BiIn₂的形成；合金具有良好的润湿性，润湿角约为40°。在合金和Cu板的界面结合处形成一种薄而坚韧的Cu₅Zn₈层，提高焊点可靠性。研究表明，通过多组元混合概念设计合金可以有效提高...     

Phase diagram of the Sn–Zn–Ti system

Equilibrated Sn–Zn–Ti alloys and (Sn + Zn)/α-Ti diffusion couples have been studied by scanning electron microscopy, metallography, and differential scanning calorimetry. For the first time an isothermal section, at 600 °C, of the ternary Sn–Zn–Ti system has been constructed. A previously unknown ternary phase with approximate formula Ti₃Sn₂Zn₆ (probable homogeneity interval in the range Ti₅Sn₄Zn₁₁ to Ti₅Sn₃Zn₁₂) has been found.The solubility ranges of the titanium based solid solutions and the intermetallic phases have been looked for. As far as we could detect and in agreement with theoretical considerations, zinc dissolves more in Ti–Sn phases than tin into Ti–Zn compounds. Titanium additions of 3 and 4 at.% Ti do not influence significantly the Sn–Zn eutectic temperature. The experimentally determined melting enthalpies of the nearly eutectic alloys have values around 100 J g⁻¹.     

Ultrafine eutectic Ti x Sn y /TiNi composites with high damping capacity

Three kinds of bulk-type ultrafine Ti _x Sn _y /TiNi (Ti _x Sn _y represents Ti₃Sn, Ti₂Sn, and Ti₅Sn₃ or Ti₆Sn₅) composites with homogeneous eutectic microstructure were prepared by arc melting. The composites exhibit high damping capacity (tanδ greater than 1 × 10^?2) and enhanced mechanical strength (the highest fracture strength is 2.15 GPa). The damping capacity originates from TiNi and Ti₃Sn, while the eutectic contributes to the mechanical strength.     

The effect of Zn on the microstructure and electrical properties of Mn1.17−xNi0.93Co0.9ZnxO4 (0 ≤ x ≤ 0.075) NTC thermistors

As-sintered Mn_1.17?xNi_0.93Co_0.9Zn_xO₄ (0 ≤ x ≤ 0.075) bodies consisted of two phases: a major Mn-rich phase with a cubic spinel structure and a minor NiO phase with a cubic structure. The Mn_1.17?xNi_0.93Co_0.9Zn_xO₄ ceramics were highly dense, ranging from 96 to 98% of the theoretical density and were microscopically homogeneous. The addition of Zn did not cause much change in the grain size and porosity. The obtained ρ₂₅, B_25/85 constant, and activation energy of the negative temperature coefficient (NTC) Mn_1.17?xNi_0.93Co_0.9Zn_xO₄ thermistors were in the range 1145–3696 Ω cm, 3218–3550 K, and 0.277–0.306 eV, respectively. This means that the electrical properties can be adjusted to desired values, depending on their Zn content. In particular, the resistivity and sensitivity were substantially enhanced with increasing Zn content.     

Isothermal Section of the Co-Gd-Sn Ternary System Between 0 and 55 at.% Sn at 500 °C

The isothermal section of the Co-Gd-Sn system between 0 and 55 at.% Sn at 500 °C was investigated by means of powder x-ray diffraction. Five ternary phases were identified or confirmed: Gd₆Co₂Sn, Gd₃Co₈Sn₄, Gd₃Co₆Sn₅, Gd₄CoSn₈, and Gd₃Co₄Sn₁₃. A new ternary phase Gd₁₁₇Co₅₇Sn₁₁₂ with Dy₁₁₇Co₅₇Sn₁₁₂-type structure, space group Fm[`3]m Fm\bar{3}m , and lattice parameter a = 3.0023 (4) nm was found. The ternary rare earth compound Gd₃Co₈Sn₄ presents a homogeneity range of 20 to 27 at.% Sn along the 20 at.% Gd iso-concentration line. Comparison of this section with those of the Co-Gd-Sn system reported in the literature was made and the differences were discussed.     

锌对SnxZn/Cu界面微空洞的影响

通过向锡钎料中添加不同含量的Zn元素,系统研究了锌对SnxZn/Cu(x=0,0.2,0.5,0.8(质量分数,％))界面处柯肯达尔空洞形成的影响.结果表明,经热老化处理后,纯Sn/Cu接头中的Cu3 Sn层和Cu3 Sn/Cu界面出现了大量柯肯达尔空洞.然而随着Zn元素含量的增加,反应界面处的Cu3Sn层逐渐变薄甚至消失,柯肯达尔空洞也随之显著减少或消失;锌在反应界面处的富集现象越来越显著.锌参与了界面反应,形成了(Cu,Zn)6Sn5相、Cu6(Sn,Zn)5相和Cu-Zn固溶合金,其中Cu-Zn固溶合金层可以显著影响铜的界面扩散.Zn元素直接参与了界面扩散,在很大程度上缓和铜和锡的不平衡扩散,从而有效抑制了柯肯达尔空洞的形成.