二乙胺基硫代甲酸钴的合成

制备了配合物 {Co[(C2 H5) 2 NCS2 ]3 } ,经X 射线四圆衍射方法确定了配合物的结构 ,晶体学参数如下 :单斜晶系 ,空间群C2 /c ,C15H3 0 N3 S6Co ,Mr =5 0 3.7,a =1.410 5 (2 ) ,b =1.0 2 99(3) ,c =1.70 5 9(3)nm ,β=110 .15 (1)°,V =2 .32 6 5nm3 ,Z =4.Dc =1.46 6 g/cm3 ,μ =7.77cm-1,F(0 0 0 ) =10 5 6 ,R =0 .0 33,Rw=0 .0 4.中心钴原子由来自二乙胺基硫代甲酸的六个硫原子构成八面体配位结构。Co -S键长和S -Co -S键角分别位于 0 .2 2 6 7(1)～ 0 .2 2 70 (1)nm和 76 .34 (4 )～ 94.48(4 )°之间。     

热分解含氨草酸钴复盐制备纤维状多孔钴粉

以氨为配位剂,通过配位沉淀法制备纤维状钴粉复杂前驱体,并采用XRD,IR,SEM和TGA/DTA研究前驱体粉末的物相、成分与形貌,系统考察前驱体粉末热分解过程中热分解条件如热分解气氛、热分解温度、热分解时间和升温速率对金属钻粉形貌、粒度和比表面积的影响.研究结果表明:在Co(Ⅱ)-C2042——NH3-NH4+-H2O反应体系中得到的前驱体为含氨草酸钴复盐,形貌为纤维状,氨与钴离子配合并生成含氨草酸钴复盐是纤维状形貌形成的内在机制,它是通过含NH3基配合物以链状结构连接[(NH3)M-OX-M(NH3)]2+生长基元以轴向取向连生形成一维形貌;在弱还原性气氛、热分解时间为30～60 min、升温速率为15～20 K/min、热分解温度为623～723 K条件下,热分解含氨草酸钴复盐粉末可以制备比表面积为10.44 m2·g-1的纤维状多孔金属钴粉,其孔结构为两端开放的管状毛细孔且多为中孔.     

用P507萃取分离钴及草酸反萃制备草酸钴

研究锂电池浸出液中钴、镍、锂的P507萃取分离方法,通过直接采用草酸反萃富钴有机相得到草酸钴产品.实验对含有53.8 g/L 钴的料液进行萃取.研究结果表明最佳萃取条件如下:有机相组成(体积分数)为25%P507+5%TBP+70%磺化煤油,萃取剂皂化率为70%,水相初始pH为3.5,常温下萃取10 min,有机相与水相的相比ψ(O)/ψ(A)为1.5:1.0,通过3级错流萃取,钴的萃取率达99.5%,锂和镍的萃取率仅为4.9%和3.1%:P507萃取分离钴、镍、锂过程的焓变分别为: -2.043,-0.812和1.586 kJ/mol;直接使用草酸反萃富钴有机相,得到分相良好的油一水一固3相,最优反萃工艺为:0.03 g草酸/mL富钴萃取剂,温度为40℃,ψ(O)/ψ(A)=1.0:2.5,钴的反萃率达99.5%,反萃后的萃取剂和水相均可再生循环利用.     

丁二酮肟分光光度法测钴方法的研究

以丁二酮肟 (DMG)为显色剂与 Co2＋显色反应,生成二元有色络合物,在二元有色络合物基础上再与碘离子形成三元有色络合物,增大有色物质的对单色光吸收能力,提高显色反应的灵敏度.着重系统研究显色反应的影响因素（络合剂用量、温度、酸度、时间）对显色效果的影响,并确定最佳显色参数：λ max=347 nm,ε =1.4× 104 L× mol－ 1× cm－ 1, pH=5～ 7.线性范围 1.0～ 15 ug/mL,三元有色络合物组成为 Co(DMG)2I2.     

Process and kinetics of the selective extraction of cobalt from high-silicon low-grade cobalt ores using ammonia leaching

An ammonia-based system was used to selectively leach cobalt(Co)from an African high-silicon low-grade Co ore,and the other elemental impurities were inhibited from leaching in this process.This process was simple and environmentally friendly.The results revealed that the leaching ratio of Co can reach up to 95.61%using(NH₄)₂SO₄as a leaching agent under the following materials and conditions:(NH₄)₂SO₄concentration 300 g/L,reductant dosage 0.7 g,leaching temperature 353 K,reaction time 4 h,and liquid-solid ratio 6 mL/g.The leaching kinetics of Co showed that the apparent activation energy of Co leaching was 76.07 kJ/mol(i.e.,in the range of 40-300 kJ/mol).This indicated that the leaching of Co from the Co ore was controlled by an interfacial chemical reaction,and then the developed leaching kinetics model of the Co can be expressed as 1-(1-α)^1/3=28.01×10~3×r_0^-1×C_((NH₄)₂SO₄)^1.5×exp(-76073/8.314 T)×t,whereαis the leaching ratio(%)of Co,r_0 is the average radius(m)of the Co ore particles,T is the temperature(K),and C_((NH₄)₂SO₄)is the initial reactant concentration(kg/m³).     

中非铜钴矿带某尾矿浸钴工艺还原剂比选研究

中非铜钴矿带某尾矿中的钴资源具有较高的回收价值.为充分开发回收利用其中的钴资源,本文开展了钴浸出工艺中SO_2和焦亚硫酸钠(SMBS)两种还原剂比选研究.研究结果表明,在尾矿粒度-0.074 mm占73.2%,液固比3∶1,终点pH 1.5,硫酸浸出时间为1 h,还原剂浸出时间4 h的优化条件下,SO_2的用量为10 kg/t-矿,而SMBS的用量为3.5 kg/t-矿,且钴的浸出率都能达到84%左右.考虑到SO_2及SMBS的用量和它们的当地价格,认为SMBS作为浸钴工艺的还原剂更具经济性.     

钴结壳开采装置及方法

海底钴结壳的开采,需要一种能适应海底特殊条件、针对钴结壳特殊性能的开采方法.作者根据现有钴结壳开采方法,提出了激振破碎开采法,并研究了相关机电技术:通过调节激振频率及振幅以适应厚度差距较大的钴结壳分布状况;激振作业不需反力以适应高低不平、悬崖遍布的海底地形;通过比例电液减压阀来改变液控变量马达的排量以改变激振频率;通过结合比例电液减压阀、密封氮气压力位移转换器和机液伺服阀以实现对独立回转的2个偏心体进行等偏心距控制,以消除侧向振动.研究结果表明:该开采方法装备能使破碎设备在海底斜坡上作业,即使悬吊于悬崖堑沟之中也能正常作业;设备能根据钴结壳自身特点进行参数最优调节,实现高效共振剥落.     

水射流辅助刀具切削钴结壳

为了减小钴结壳切削过程中产生的冲击载荷,提高集矿机的行走安全性,提出了水射流辅助刀具切削钴结壳的切削方法.分析了单个截齿切削钴结壳时的受力情况,建立了水射流辅助刀具切削钴结壳的力学模型,通过仿真计算获取了水射流压力和刀具在钴结壳表面产生初始裂纹所需最小切削力的作用规律.仿真结果表明:与纯刀具切削相比,当水射流作用点和刀具作用点重合时,刀具在钴结壳表面产生初始裂纹所需的最小切削力明显下降;随着水射流压力的增加,刀具所需的最小切削力急剧下降.开展了水射流辅助刀具切削钴结壳模拟料实验.实验结果表明:与纯刀具切削钴结壳相比,水射流辅助刀具切削钴结壳时,切削过程中冲击载荷的最大值明显下降,当射流压力为5 MPa时,冲击载荷的最大值下降约50%,有效值下降约10%.     

电沉积制备氮化钴纳米片超级电容器

采用一种简单的电化学沉积和退火方法,实现了在碳布基底上碳氮结构修饰氮化钴(CC@Co2 N@CN)材料的制备,并将其用于高性能超级电容器.氮化钴表面修饰的碳氮结构不仅可以提高整个电极的电容,而且可以缓解氮化钴的氧化,从而提高整体的导电性能.同时,CC@Co2 N@CN表现出极长的寿命,在10000次循环后容量仍能保持其初始值的77％.在电流密度为1 m A·cm-2时,该电极的面积电容最高可达429.4 m F·cm-2.因为具有较大的面积电容和良好的循环稳定性能,此类基于碳布基底的氮化钴碳氮结构超级电容器在储能领域具有广阔的应用前景.     

Synthesis and characterization of carbon-coated cobalt ferrite nanoparticles

Cobalt ferrite nanoparticles (CFNPs) were prepared via a reverse micelle method. The CFNPs were subsequently coated with carbon shells by means of thermal chemical vapor deposition (TCVD). In this process, acetylene gas (C₂H₂) was used as a carbon source and the coating was carried out for 1, 2, or 3 h at 750°C. The Ar/C₂H₂ ratio was 10:1. Heating during the TCVD process resulted in a NP core size that approached 30 nm; the thickness of the shell was less than 10 nm. The composition, structure, and morphology of the fabricated composites were characterized using X-ray diffraction, simultaneous thermal analysis, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area diffraction. A vibrating sample magnetometer was used to survey the samples’ magnetic properties. The deposited carbon shell substantially affected the growth and magnetic properties of the CFNPs. Micro-Raman spectroscopy was used to study the carbon coating and revealed that the deposited carbon comprised graphite, multiwalled carbon nanotubes, and diamond- like carbon. With an increase in coating time, the intensity ratio between the amorphous and ordered peaks in the Raman spectra decreased, which indicated an increase in crystallite size.     

酞菁钴的合成、性能及应用研究

文章比较了单核、双核、三核磺化酞菁钴(s-CoPc、b-CoPc、t-CoPc)和1,2-二羧基酞菁钴(CobcPc)的UV-Vis、IR光谱,分析了s-CoPc/CobcPc和顺二硫氰根-双(2,2'-联吡啶-4-羧酸-4'-羧酸四丁基铵)合钌(Ⅱ)(N719)协同敏化的纳米TiO2薄膜的UV-Vis吸收性能,利用循环伏安法研究了s-CoPc、CobcPc的氧化还原行为.结果表明,s-CoPc在Q带的最大吸收峰位于655 nm,b-CoPc、t-CoPc最大吸收峰分别红移至658 nm和663 nm,先吸附N719后吸附s-CoPc的纳米TiO2薄膜以及共吸附CobcPc和N719的纳米TiO2薄膜的协同敏化效果好.     

磷酸钴纳米粒子的微波辐射制备法

介绍用微波辐射法对磷酸钴纳米粒子的制备方法和分离方法.并对磷酸钴纳米粒子进行了结构和组成的测试,讨论了影响粒子形成的主要因素.通过实验得到了平均粒径为50.64nm的球形微粒的磷酸钴纳米粒子.     

回收废旧锂离子电池制备镧掺杂钴铁氧体

以废旧锂离子电池为原料,柠檬酸为凝胶剂,通过溶胶-凝胶自蔓延燃烧法制备出镧掺杂钴铁氧体,用X射线衍射仪(XRD)、场发射扫描电镜(SEM)、透射电镜(TEM)、振动样品磁强计(VSM)和磁致伸缩性能自动测量仪分析所制备样品的晶型、形貌、磁性和磁致伸缩性.结果表明,镧掺杂的钴铁氧体具有尖晶石结构,性能较纯钴铁氧体有所改变,随着La元素掺杂量的增加,样品的饱和磁化强度,磁致伸缩系数,应变导数逐渐减小.当掺杂量x=0.025时,应变导数在较低的磁场下取得最大值-1.18×10-9 m/A,这有利于氧化铁系的磁致伸缩材料在非接触式传感器和执行器方面的应用.     

Optical properties of cobalt xanthate films on different substrates

Cobalt isopropyl xanthate thin films (CXTFs) were deposited via chemical bath deposition onto different substrates: commercial glass (CG), indium tin oxide (ITO), and poly(methyl methacrylate) (PMM). Isopropyl xanthate was synthesized according to a method described in the literature. The cobalt nitrate and isopropyl xanthate were mixed in a beaker, which allowed the thin films to be deposited via a simple ion-ion mechanism. The transmission, reflectivity, refractive index, dielectric constant, and optical conductivity were investigated for various thin films coated onto different substrates. An ultraviolet-visible spectrophotometer was used to measure the optical properties of the thin films. The lowest value of the transmission and the highest value of the refractive index were observed for the thin films deposited onto PMM. The structure of the cobalt xanthate was characterized by Fourier transform infrared (FTIR) spectroscopy, which was measured using a Perkin-Elmer Spectrum 400 spectrometer. The stretching vibration of the Co-S bonds was observed at 359 cm-1 in the FTIR spectrum of the CXTFs.     

纳米钴粉的制备及其在乙醇中的分散性能

针对高性能硬质合金的制备基础研究,通过直流电弧等离子体蒸发法制备纳米级钴粉,利用X线衍射(XRD)、X线荧光分析(XRF)、振动磁强计(VSM)、透射电子显微镜(TEM)和相应的选区电子衍射(SAED)等测试手段对样品进行表征。在测定样品粉体于无水乙醇中pH-Zeta电位的基础上,研究超声时间和特定的分散剂及其加入量对分散效果的影响。研究结果表明:直流电弧等离子体蒸发法制备的纳米钴粉为立方晶体结构,纯度(质量分数)达99.923%,粒径分布窄,颗粒呈现球形。随着超声时间和分散剂浓度的增加,纳米钴粉在无水乙醇中的分散效果呈现先增大后减小的趋势;不同分散剂分散效果从优到劣的顺序为:PVP,SHMP,TEA,CTAB和STAN-80。纳米钴粉在无水乙醇中较好分散工艺为:在pH=7的情况下,PVP加入量(质量分数)为2%,超声时间为30 min,超声功率为560 W。     

电沉积法制备Co(OH)_2薄膜及其电化学性能研究

在硝酸钴溶液中,通过电沉积在镍箔基底上制备出了Co(OH)2薄膜.用X射线衍射仪(XRD)和场发射扫描电子显微镜(FESEM)表征了产物的结构和形貌,用红外光谱(FT-IR)对所制样品的组分进行了分析,用循环伏安和恒电流充放电等测试方法对其电化学性能进行了研究.结果表明,具有均匀片状网络形貌的Co(OH)2表现出优良的电化学性能,其单电极比电容值达1042F.g-1,有望成为电化学电容器电极材料.     

钴铁氧体复合纳米颗粒的制备及其磁性

通过溶胶凝胶法制备尖晶石CoFe2O4/α-Fe复合纳米颗粒体系,用X射线衍射仪、振动样品磁强计对样品的结构和磁性进行了研究.这种新型材料具有较高的饱和磁化强度Ms(51.44 A.m2/kg)和矫顽力Hc(10.8×104 A/m),最大磁能积(BHmax)相比同样方法制备的纯CoFe2O4有较大的提高.磁性能的改善可能来源于处于内层的CoFe2O4与外壳层的α-Fe之间的交换耦合作用.