纳米结晶体Ni0.5Zn0.5Fe2O4对高氯酸铵热行为及分解反应动力学的影响

采用差示扫描量热法(DSC)、热重和微分热重(TG-DTG)及固相原位反应池/快速扫描傅立叶变换红外联用技术(hyphenated in situ thermolysis/RSFTIR)研究了纳米结晶体Ni_0.5Zn_0.5Fe₂O₄与高氯酸铵(AP)组成的混合物的热行为和分解反应动力学。结果表明：Ni_0.5Zn_0.5Fe₂O₄使得AP的低、高温分解放热峰温分别提前17.44 K和27.74 K,并使得对应的分解热分别增加3.7 J·g^-1和193.7 J·g^-1。Ni_0.5Zn_0.5Fe₂O₄并不影响AP的晶转温度和晶转热。Ni_0.5Zn_0.5Fe₂O₄使得AP的TG曲线出现3个阶段,并使得后2个失重阶段的初始和终止温度都有所提前。凝聚相分解产物分析表明Ni_0.5Zn_0.5Fe₂O₄加速了凝聚相AP的分解及氨气的释放。含Ni_0.5Zn_0.5Fe₂O₄的AP的高温分解反应的动力学参数E_a=238.88 kJ·mol^-1,A=1018.59 s^-1,动力学方程可表示为dα/dt=10^18.99(1-α)[-ln(1-α)]^3/5e^-2.87×104T。始点温度(T_e)和峰顶温度(T_p)计算得出AP的热爆炸临界温度值分别为:574.83 K和595.41 K。分解反应的活化熵(ΔS^≠)、活化焓(ΔH^≠)和活化能(ΔG^≠)分别为:109.61 J·mol^-1·K^-1、236.49 kJ·mol^-1及172.58 kJ·mol^-1。     

Fe_2O_3/聚糠醛纳米复合材料的制备及光催化性能

以Fe(NO3)3·9H2O和糠醛(FD)为原料,通过聚合-热转化两步法制备了Fe2O3/聚糠醛(PFD)纳米复合材料,用TEM、XRD、XPS和UV-Vis等技术对其尺寸、结构及吸光特性等进行了表征。在自然光、室温条件下,以亚甲基蓝(MB)溶液的催化脱色降解为模型反应,考察了其光催化性能以及热转化温度对催化性能的影响。结果表明,利用该法可以得到纳米级的、相间以强相互相用结合的有机-无机复合材料Fe2O3/PFD,该纳米材料对紫外-可见区的全程光波有强的吸收;热转化条件对复合材料的结构、催化性能等有很大影响,在300℃下处理35min所得的纳米复合材料在自然光条件下具有最佳的催化性能,25min即可使MB溶液完全脱色,并且重复使用3次仍可使MB溶液的脱色率保持在75.0%以上。而在相同条件下,纳米Fe2O3仅能使MB的脱色率达到5.8%。     

针状纳米SrFe12O19的溶胶-凝胶法制备及磁性研究

采用柠檬酸-EDTA的联合络合溶胶-凝胶法制得了针状纳米锶铁氧体磁性微粒。利用XRD对样品的物相进行分析,利用TEM对样品形貌和粒径进行表征,并利用振荡样品磁强计(VSM)对样品进行了磁性能研究。结果表明,相对于柠檬酸法制备的纯锶铁氧体微粒,EDTA加入后制备的SrFe₁₂O₁₉微粒仍保持六方磁铅石型结构,但是粒径减小,形貌向一维发展,且内禀矫顽力H_c显著提高。并直接对凝胶加热,使其发生自蔓延燃烧,省去了凝胶的干燥过程,制备周期缩短1/4以上,同时自蔓延燃烧使SrFe₁₂O₁₉的内禀矫顽力提高10%左右,通过洗涤前驱体使得SrFe₁₂O₁₉纯度得到提高,进而使比剩余磁化强度和比饱和磁化强度提高20%左右,最终制得了粒径为30 nm,长径比为5∶1,内禀矫顽力、比饱和磁化强度与比剩余磁化强度分别为6 446.9 Oe、68.9 emu·g^-1和40.2 emu·g^-1的针状纳米SrFe₁₂O₁₉。     

多孔软硬磁Ni0.5Zn0.5Fe2O4/SrFe12O19复合纤维制备及吸波性能

通过静电纺丝技术制备了多孔软硬磁Ni_0.5Zn_0.5Fe₂O₄/SrFe₁₂O₁₉复合纤维,利用综合热重分析仪（TG-DSC）、X射线衍射仪（XRD）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）、X射线能谱仪（EDS）和矢量网络分析仪（VNA）等对复合纤维的晶体结构、微观形貌和电磁性能进行了表征,研究了不同软硬磁质量比对纤维结构和性能的影响。结果表明：900℃下制备的复合纤维具有立体多孔结构,软硬磁质量比为1∶3时,复合纤维的比表面积达到55 m²·g^-1。吸波性能测试结果显示,当吸波剂涂层厚度为3.5 mm时,复合纤维在10.6 GHz处反射损失（R_L）值达到-31.9 dB,在2~18 GHz频率范围内,R_L值小于-10 dB的吸收带宽达到10.5 GHz,覆盖了整个X波段（8.2~12.4 GHz）和Ku波段（12.4~18 GHz）,显示出优异的宽波段吸收性能。     

多孔软硬磁Ni0.5Zn0.5Fe2O4/SrFe12O19复合纤维制备及吸波性能

通过静电纺丝技术制备了多孔软硬磁Ni_(0.5)Zn_(0.5)Fe_2O_4/SrFe_(12)O_(19)复合纤维,利用综合热重分析仪(TG-DSC)、X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线能谱仪(EDS)和矢量网络分析仪(VNA)等对复合纤维的晶体结构、微观形貌和电磁性能进行了表征,研究了不同软硬磁质量比对纤维结构和性能的影响。结果表明:900℃下制备的复合纤维具有立体多孔结构,软硬磁质量比为1∶3时,复合纤维的比表面积达到55 m~2·g~(-1)。吸波性能测试结果显示,当吸波剂涂层厚度为3.5 mm时,复合纤维在10.6 GHz处反射损失(RL)值达到-31.9 dB,在2~18 GHz频率范围内,RL值小于-10 dB的吸收带宽达到10.5 GHz,覆盖了整个X波段(8.2~12.4 GHz)和Ku波段(12.4~18 GHz),显示出优异的宽波段吸收性能。     

可控粒径纳米Fe_3O_4的制备及其磁性研究

本文用空气氧化法,在可见光作用下,添加配合剂(EDTA、柠檬酸、酒石酸、谷氨酸)在室温进行了不同粒径纳米Fe3O4的制备及其磁性能研究。结果表明:在可见光作用下,随EDTA、柠檬酸、酒石酸、谷氨酸等配合剂的添加,得到纳米Fe3O4的粒径有所减小、分散性有所提高;配合剂及可见光共存时,体系反应速率得到提高,高的反应速率使纳米Fe3O4晶粒减小;控制适当的光照度和添加剂的量,室温可得到11.8~29.6nm的Fe3O4颗粒。不同粒径纳米Fe3O4分别呈现出超顺磁性、铁磁性特征。     

聚苯胺/Co_(0.5)Zn_(0.5)Fe_2O_4纳米复合材料的制备及电磁性能

采用高分子凝胶法制备尖晶石型Co0.5Zn0.5Fe2O4,原位聚合法制备纯聚苯胺和聚苯胺/Co0.5Zn0.5-Fe2O4纳米复合材料.使用傅立叶红外光谱(FTIR)、紫外可见吸收光谱(UV-Vis)、X射线衍射仪(XRD)和透射电子显微镜(TEM)对复合材料进行了表征.FTIR和XRD的结果表明样品为纯聚苯胺和聚苯胺/Co0.5Zn0.5-Fe2O4.UV-Vis光谱表明聚苯胺/Co0.5Zn0.5Fe2O4苯环上的π-π*和n-π*分别红移了23nm和5nm.TEM照片可知,聚苯胺和聚苯胺/Co0.5Zn0.5Fe2O4粒子的平均粒径分别约为50nm和70nm.在8.2～12.4GHz测试频率范围内,聚苯胺/Co0.5Zn0.5Fe2O4的ε″数值在9.2～12.3之间,u″数值在0.15～0.16之间;聚苯胺/Co0.5-Zn0.5Fe2O4介电损耗低于纯聚苯胺,而磁损耗高于纯聚苯胺.     

纳米CuFe_2O_4-rGO复合材料的制备及电化学性能

采用溶剂热法成功制备了纳米CuFe_2O_4-rGO复合材料。通过X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和电化学工作站对样品的结构、形貌及电容特性进行表征。结果表明,CuFe_2O_4纳米粒子均匀地分散在石墨烯片层间,其中CuFe_2O_4-20%rGO复合材料具有最优的电化学性能,当电流密度1 A·g~(-1)时,其比电容为1 952.5 F·g~(-1),当电流密度为1 A·g~(-1)时,CuFe_2O_4-20%rGO复合材料经1 000次充放电后的比电容保持率为86.17%。     

多孔朵状Fe_3O_4纳米微球的制备及其性能研究

<正>众所周知,纳米材料的尺寸大小、晶型、形貌构型等结构特征对材料的化学物理性能有重要的影响[1],由于特殊形貌的新材料所具有独特、新颖、高效的化学物理等方面的性质以及在众多领域中的潜在应用[2],特别是3D花状空心纳米结构新物质[3-4],新形貌物质的纳米材料的制备方法和应用特性已经吸引了世界上材料领域的广泛兴趣和关注[5]。目前为止,合成3D纳米结构的方法有自组装法、三维导向连接法以及水热法等,即通过使用有     

纳米Fe_3O_4及钴离子掺杂Fe_3O_4:有机碱共沉淀制备和磁性质

以有机碱四甲基氢氧化铵(TMAH)为沉淀剂合成了纳米Fe3O4和Co2+掺杂的纳米Fe3O4粒子。分别讨论了碱用量,铁盐溶液浓度,反应温度,有机碱及PEG-4000的分散性等因素对纳米Fe3O4的形貌影响。结果表明,所合成的纳米Fe3O4为30nm左右的反尖晶石型面心立方结构,有机碱除了起沉淀剂作用,还能够提高纳米Fe3O4的分散性。本文还讨论了不同Co2+掺入量的纳米Fe3O4粒子的磁性质,结果表明Co2+掺杂的纳米Fe3O4粒子的矫顽力在不同掺入量的下有较大的改变。当Co2+掺入量为10.0%时,纳米Fe3O4的矫顽力达到最大值,为1628Oe。     

Ultrasonic-assisted synthesis of PMMA/Ni0.5Zn0.5Fe2O4 nanocomposite in mixed surfactant system

PMMA/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite with superparamagnetic behavior was synthesized by in situ emulsion polymerization of methylmethacrylate (MMA) monomer in the presence of Ni_0.5Zn_0.5Fe₂O₄ colloidal suspension assisted by ultrasonic irradiation. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). XRD and FT-IR spectra confirmed the formation of PMMA/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite. TEM images showed that Ni_0.5Zn_0.5Fe₂O₄ nanoparticles with the particle sizes of about 12 nm were well dispersed in the polymer matrix. The nanocomposite at room temperature exhibited superparamagnetic behavior under applied magnetic field. The formation mechanism of PMMA/Ni_0.5Zn_0.5Fe₂O₄ nanocomposite was proposed as well.     

Bi2Fe4O9纳米粉体:水热法制备及表征

Bi₂Fe₄O₉ nanoparticles were prepared at low temperature via a facile, one-step hydrothermal synthesis process using iron(Ⅲ) nitrate nonahydrate(Fe(NO₃)₃·9H₂O) and bismuth nitrate pentahydrate (Bi(NO₃)₃·5H₂O) as starting materials and sodium hydroxide (NaOH) as the precipitant and mineralizer. XRD results indicate that the as-prepared nanoparticles are pure Bi₂Fe₄O₉. SEM images reveal that the as-prepared Bi₂Fe₄O₉ nanoparticles have a sheet-like morphology. The Bi₂Fe₄O₉ nanoparticles thus obtained are paramagnetic at room temperature as shown by magnetic measurements.     

纳米微孔NixZn(1-x)Fe2O4的水热合成研究

０引言尖晶石型铁酸盐是一类重要的磁性材料，它可用于防止电磁波辐射设备以及隐身材料中的吸波剂犤１，２犦，具有价格低廉、吸波性能优良的特点。同时尖晶石型铁酸盐也是一类重要的催化剂，９０年代初又发现了氧缺位的该类化合物具有将CO２还原为C的优良催化性能犤３犦。因此，有关铁酸盐的制备及性能研究一直是化学工作者和材料科学工作者感兴趣的领域。随着新的合成方法的不断涌现，对传统铁氧体材料进行结构改造以提高其性能是一个重要的研究发展方向，本文采用模板剂造孔技术，首次在NixZn（１－x）Fe２O４水热合成中选用模板剂，…     

Preparation of MnxNi0.5-xZn0.5Fe2O4 Nanorods by the Co-precipitation Method

Mn_xNi_0:5-xZn_0:5Fe₂O₄ nanorods were successfully synthesized by the thermal treatment of rod-like precursors that were fabricated by the co-precipitation of Mn²⁺, Ni²⁺, and Fe²⁺ in the lye. The phase, morphology, and particle diameter were examined by the X-ray diffrac-tion and transmission electron microscopy. The magnetic properties of the samples were stud-ied using a vibrating sample magnetometer. The results indicated that pure Ni_0:5Zn_0:5Fe₂O₄ nanorods with a diameter of 35 nm and an aspect ratio of 15 were prepared. It was found that the diameter of the Mn_xNi_0:5-xZn_0:5Fe₂O₄ (0≤x≤0.5) samples increased, the length and the aspect ratio decreased, with an increase in x value. When x=0.5, the diameter and the aspect ratio of the sample reached up to 50 nm and 7～8, respectively. The coercivity of the samples first increased and then decreased with the increase in the x value. The coer-civity of the samples again increased when the x value was higher than 0.4. When x=0.5,the coercivity of the Mn_xNi_0:5-xZn_0:5Fe₂O₄ sample reached the maximal value (134.3 Oe)at the calcination temperature of 600 oC. The saturation magnetization of the samples first increased and then decreased with the increase in the x value. When x=0.2, the satura-tion magnetization of the sample reached the maximal value (68.5 emu/g) at the calcination temperature of 800 oC.     

添加Al2O3对Ni0.5Zn0.5Fe2O4纳米纤维结构和磁性能的影响

采用静电纺丝技术制备了添加0～20wt%Al2O3的Ni0.5Zn0.5Fe2O4纳米纤维。通过XRD、FESEM、TEM和VSM对样品的物相结构、形貌和磁性能进行了表征。结果表明,所合成的复合纳米纤维的直径都分布在40～150 nm之间,添加到纤维中的Al2O3主要以非晶态形式分布于铁氧体晶粒边界;随着Al2O3添加量的增加,可观察到γ-Fe2O3相逐渐析出,Ni-Zn铁氧体的晶格常数单调减小,说明有一些Al2O3进入到尖晶石晶格中取代了B位的Fe3+离子,Ni-Zn铁氧体的平均晶粒尺寸先增大后减小,在Al2O3添加量为8wt%时达到最大值39.2 nm;比饱和磁化强度和矫顽力随Al2O3添加量的增加呈现出相同的变化规律,先减小后增大,当Al2O3添加量超过5wt%时又开始变小。     

流变相法制备LiNi0.5Mn1.5O4锂离子电池正极材料及其电化学性质

LiNi_0.5Mn_1.5O₄ was prepared by rheological method using CH₃COOLi, Ni(CH₃COO)₂ and Mn(CH₃COO)₂ as raw materials. XRD and SEM results show that LiNi_0.5Mn_1.5O₄ synthesized at 850 ℃ has cubic spinel structure with clearly defined shape and particle size of 0.2～0.4 μm. Electrochemical tests show that the LiNi_0.5Mn_1.5O₄ presents a plateau near 4.7 V and delivers the maximum discharge capacity of 140.5 mAh·g^-1. After 100 cycles, the capacity loss per cycle was only 0.015% discharged at 0.2C and the capacity retention was more than 76.3% discharged at 2.0C at room temperature and the capacity loss per cycle was only 0.32% discharged at 0.2C at 55 ℃.     

Sol-Gel Template Synthesis of Highly Ordered LiCo0.5Mn0.5O2 Nanowire Arrays and Their Structural Properties

Highly ordered LiCo_0.5Mn_0.5O₂ nanowire arrays were prepared using porous anodic aluminum oxide (AAO) template from sol-gel solution containing Li(CH₃COO), Co(CH₃COO)₂, and Mn(CH₃COO)₂. Electron microscope results showed that uniform length and diameter of LiCo_0.5Mn_0.5O₂ nanowires were obtained, and the length and diameter of LiCo_0.5Mn_0.5O₂ nanowires are dependent on the pore diameter and the thickness of the applied AAO template. X-ray diffraction and electron diffraction pattern investigations demonstrate that LiCo_0.5Mn_0.5O₂ nanowires are a layered structure of LiCo_0.5Mn_0.5O₂ crystal. X-ray photoelectron spectroscopy analysis indicates that the most closely resembling stoichiometric layered LiCo_0.5Mn_0.5O₂ material has been obtained.