自生核壳结构MnO2的电磁性能及其生长机理研究

采用水热合成法,以(NH₄)₂S₂O₈作氧化剂,以MnSO₄·H₂O为锰源,制备了自生核壳结构MnO₂粉体。利用X射线粉末衍射、扫描电子显微镜、透射电子显微镜、振动样品磁强计和热重分析对产物进行成分、晶型、形貌、磁性能和热稳定性分析,并通过电磁参数的测试对产物的电磁特性以及电磁波损耗机制进行阐述。结果表明：所制得粉体是直径3～5 μm的核壳结构海胆球形MnO₂,其复介电常数实部在8.40～5.35,虚部在2.66～2.07;复磁导率实部和虚部都很小,分别在1.04～1.14和0.03～0.21范围内。最后分析了核壳结构MnO₂的电磁波损耗机制以及热稳定性能。     

Microwave Synthesized In2S3@CNTs with Excellent Properties inLithium‐Ion Battery and Electromagnetic Wave Absorption

The three‐dimensional nanoflower‐like β‐In₂S₃ composited with carbon nanotubes (CNTs) has been synthesized by a single mode microwave‐assisted hydrothermal technique. The In₂S₃ and CNTs nanocomposites (In₂S₃@CNTs) were investigated as the anode materials of lithium batteries (LIBs) and the electromagnetic wave absorption materials. For LIBs applications, the In₂S₃@CNTs nanocomposite exhibited excellent cycling stability with a high reversible charge capacity of 575 mA⋅h⋅g^–1 after 300 cycles at 0.5 A⋅g^–1. In addition, the In₂S₃@CNTs used as electromagnetic wave absorber displayed a maximum reflection loss of –42.75 dB at 11.96 GHz with a thickness of 1.55 mm.     

Facile Preparation of Snowflake-Like MnO2@NiCo2O4 Composites for Highly Efficient Electromagnetic Wave Absorption

Snowflake-like MnO₂@NiCo₂O₄ composites were successfully fabricated by employing crossed snowflake-like MnO₂ nanorods as cores and one-dimensional (1D) NiCo₂O₄ nanoneedles as shells. Impressively, the MnO₂@NiCo₂O₄ composites exhibited a highly efficient electromagnetic wave (EMW) absorbing capability, and the minimum reflection loss (RL) value reached −58.4 dB at 6.8 GHz for a thickness of 4.0 mm. The reasons for the improved EMW absorption capability of snowflake-like MnO₂@NiCo₂O₄ composites were analyzed. The unique core–shell structure, good impedance matching, and high dielectric loss were all found to be important contributors. Moreover, the interfacial polarization mainly stemmed from the heterostructure, a microcurrent generated from the 1D MnO₂ nanorods and NiCo₂O₄ nanoneedles under alternating electromagnetic fields, and the synergistic effect from the different components were all beneficial to improve the EMW absorption performance. These results demonstrated that snowflake-like MnO₂@NiCo₂O₄ composites could be utilized as promising materials for practical EMW absorbing applications.     

Lightweight,Low-Cost Co2SiO4@diatomite Core-Shell Composite Material for High-Efficiency Microwave Absorption

The porous and biomimetic cobalt silicate@diatomite (Co₂SiO₄@diatomite) was successfully synthesized by a two-step method, including the hydrothermal method and calcination to improve the electromagnetic wave absorption property. Different hydrothermal times were well-tuned for Co₂SiO₄@diatomite composites with different loadings of Co₂SiO₄. Interestingly, the Co₂SiO₄@diatomite composites (6 h, 25 wt%) had a smaller minimum reflection loss. Moreover, the minimum reflection loss (RL_min) could reach −12.03 dB at 16.64 GHz and the matched absorber thickness was 10 mm, while the effective absorption bandwidth (EAB, RL ≤ −10 dB) could be 1.92 GHz. In principle, such findings indicate that Co₂SiO₄@diatomite nanocomposites could be a promising candidate for high-efficiency microwave absorption capability.     

Growth of Fe3O4 Nanorod Arrays on Graphene Sheets for Application in Electromagnetic Absorption Fields

A facial strategy is developed to fabricate a three‐dimensional (3D) Fe₃O₄ nanorod array/graphene architecture, in which Fe₃O₄ nanorods with a length and diameter of about 600 and 100 nm, respectively, are grown on both surfaces of the graphene sheets. The measured electromagnetic parameters show that the 3D architecture exhibits excellent electromagnetic wave‐absorption properties, that is, more than 99 % of electromagnetic wave energy can be attenuated by the 3D architecture if it is added in only 20 wt % of the paraffin matrix, as the thickness of the absorber is in the range from 2.38 to 5.00 mm. The analysis of the electromagnetic (EM) absorption mechanism reveals that the excellent EM absorption properties are related to the special 3D architecture, and therefore, the construction of graphene‐based 3D heteronanostructures is effective in obtaining lightweight EM absorbers with strong absorption properties.     

Metal-Organic Framework Derived Hierarchical Co/C@V2O3 Hollow Spheres as a Thin,Lightweight, and High-Efficiency Electromagnetic Wave Absorber

Developing high-efficiency electromagnetic (EM) wave absorbing materials with light weight, thin thickness, and wide absorption bandwidth is highly desirable for ever-developing electronic and telecommunication devices. Herein, hierarchical metal–organic framework (MOF)-derived Co/C@V₂O₃ hollow spheres were designed and synthesized through a facile hydrothermal, precipitation, and pyrolysis method. The composite exhibits both excellent impedance matching and light weight due to the rational combination of hollow V₂O₃ spheres and porous Co/C. Additionally, multiple components enable a large dielectric and magnetic loss of the composite, giving rise to enhanced EM wave absorption performance with a maximum reflection loss (RL) of −40.1 dB and a broad effective absorption bandwidth (RL < −10 dB) of 4.64 GHz at a small thickness of 1.5 mm. This work provides insights into the design of hierarchical hollow and porous composites as thin and lightweight EM wave absorbers with efficient absorption, which can also be extended to energy storage, catalysis, and sensing.     

A Facile Synthesis of NiFe-Layered Double Hydroxide and Mixed Metal Oxide with Excellent Microwave Absorption Properties

Microwave-absorbing materials have attracted increased research interest in recent years because of their core roles in the fields of electromagnetic (EM) pollution precaution and information security. In this paper, microwave-absorbing material NiFe-layered double hydroxide (NiFe-LDH) was synthesized by a simple co-precipitation method and calcined for the fabrication of NiFe-mixed metal oxide (NiFe-MMO). The phase structure and micromorphology of the NiFe-LDH and NiFe-MMO were analyzed, and their microwave-absorbing properties were investigated with a vector network analyzer in 2–18 GHz. Both NiFe-LDH and NiFe-MMO possessed abundant interfaces and a low dielectric constant, which were beneficial to electromagnetic wave absorption, owing to the synergistic effect of multi-relaxation and impedance matching. The optimum reflection loss (RL) of NiFe-LDH and NiFe-MMO was −58.8 dB and −64.4 dB, respectively, with the thickness of 4.0 mm in the C band. This work demonstrates that LDH-based materials have a potential application in electromagnetic wave absorption.     

钴基钙钛矿氧化物La_(1-x)Na_xCoO_3结构和吸波性能研究

采用溶胶凝胶法制备了钙钛矿型氧化物La1-xNaxCo O3(0≤x≤0.3)超微粉末,用XDR分析该材料的相结构,表明样品为R-3C单相结构。用SEM表征了该材料的微观形貌,观察到样品颗粒尺寸随着掺杂量的增加而增大。用PPMS物性检测仪测量了该材料低温磁滞回线,证明样品存在复杂相结构。用AV3618型微波矢量网络分析仪测试了样品在2~18 GHz范围内的微波吸收特性。当材料涂层厚度为1.8 mm,x=0.1时,La1-xNaxCo O3的吸波性能最佳。在测试频段,最高的吸收峰在11.4 GHz处,峰值高达33.1 d B。     

碳纤维表面羰基铁的原位生长及吸波性能

以Fe(CO)5为前驱体,通过金属有机化学气相沉积(MOCVD),在碳纤维(CF)表面构筑厚度为纳米级的羰基铁(CI)壳层,通过改变沉积温度,调控核壳粉体的形貌结构和吸波性能。用X射线衍射仪、扫描电子显微镜和矢量网络分析仪对粉末的结构及电磁性能进行表征并对其吸波性能进行研究。结果表明:随着沉积温度升高(210~240℃),沉积到CF表面的羰基铁颗粒互相“吞并-融合”,此时CF-CI形成了完整的薄膜包覆型核壳结构;沉积温度太高时(270℃)会造成CF表面羰基铁壳层形貌的恶化。通过调节沉积温度,在纳米尺度上可以有效调控CI壳层的形貌,从而调节CF-CI核壳粒子的电磁性能。以核壳形貌及吸波性能为考察指标,最终确定最佳的沉积温度为240℃。以沉积温度为240℃时所获样品的电磁参数,模拟计算出涂层厚度为0.9 mm时,小于-10 dB的吸波带宽最大为4.6 GHz(13.4~18 GHz);涂层厚度为2.0 mm时,反射率达到最小值为-21.5 dB;厚度为0.9~3.9 mm时,在2~18 GHz均能实现吸波强度低于-10 dB。     

In Situ Synthesis of C-N@NiFe2O4@MXene/Ni Nanocomposites for Efficient Electromagnetic Wave Absorption at an Ultralow Thickness Level

Recently, the development of composite materials composed of magnetic materials and MXene has attracted significant attention. However, the thickness and microwave absorption performance of the composite is still barely satisfactory. In this work, the C-N@NiFe₂O₄@MXene/Ni nanocomposites were successfully synthesized in situ by hydrothermal and calcination methods. Benefiting from the introduction of the carbon-nitrogen(C-N) network structure, the overall dielectric properties are improved effectively, consequently reducing the thickness of the composite while maintaining excellent absorption performance. As a result, the minimum reflection loss of C-N@NiFe₂O₄@MXene/Ni can reach −50.51 dB at 17.3 GHz at an ultralow thickness of 1.5 mm, with an effective absorption bandwidth of 4.95 GHz (13.02–18 GHz). This research provides a novel strategy for materials to maintain good absorption performance at an ultralow thickness level.     

测定钛铁矿中TFe、TiO2、SiO2、Al2O3、CaO、MgO的含量

以粉末压片法制样,采用X射线荧光光谱(XRF)法测定钛铁矿中TFe、TiO2、SiO2、Al2O3、CaO、MgO的含量。对样品的矿物效应、样品粒度、分析谱线等条件进行优化。利用不同产地的质控样品制作工作曲线,验证矿物效应影响不大;通过样品粒度小于74 μm,很好地解决了颗粒粒度效应的影响。 精密度实验表明,待测组分的相对标准偏差均低于3.6%(RSD,n=10),能满足钛铁矿中各组分的测定要求。     

光催化材料Cu/Fe2O3-TiO2的结构和性能

光催化材料Cu/Fe2O3-TiO2的结构和性能;复合半导体;Cu/Fe2O3-TiO2;光催化材料;光响应性能     

Determination of Manganese(II) with Preconcentration on Almond Skin and Determination by Flame Atomic Absorption Spectrometry

Almond skin was used as a biosorbent by solid-phase extraction for the preconcentration of manganese(II) before the determination by flame atomic absorption spectrometry. Characterization of almond skin was performed by infrared spectroscopy. The functional groups of the almond skin surface were shown to be beneficial for the adsorption of manganese(II). At pH 6.0, the manganese(II) ions were retained on the almond skin and afterward quantitatively eluted using 1.5?mol?L^?1 nitric acid. The pH, flow rate and volume of sample, concentration, and flow rate of eluent and interfering ions were characterized. Using a sample size of 30?mL, a linear dynamic range of 1–120?µg?L^?1 was obtained. A detection limit of 0.24?µg?L^?1 manganese(II) and a relative standard deviation of 1.6% at 30?µg?L^?1 were achieved. The accuracy of the present procedure was evaluated by the determination of manganese(II) in a certified reference material (GSB07-1189-2000). The protocol was also used for the determination of manganese(II) in wastewater. The fortified recoveries were from 99.0 to 99.4%.     

ChemInform Abstract: Crystal Structure and Properties of the Manganese Containing Swedenborgite YBaMn3AlO7.

Small crystals of the title compound are grown from BaAl₂O₄, Y₂BaO₄, and MnO in a floating‐zone mirror‐image furnace.     

Si内标-X射线衍射法定量测定铁矿中Fe3O4、Fe2O3和SiO2

铁矿物相的准确定量对矿物价值评价及选冶工艺研究有重要作用,现有化学法流程复杂效率低,X射线衍射全谱拟合法可溯源性差,结果准确性难以评价和验证。本研究建立了以Si为内标,以Cu靶X射线为辐射光源,步进扫描方式获得衍射谱图,以待测相含量为横坐标,待测相与内标相峰面积比值为纵坐标建立校准曲线,以曲线对铁矿中Fe3O4、Fe2O3和SiO2物相进行定量的方法。试验对制样条件、扫描参数、内标物选择、积分方式、重叠峰校正等进行了优化选择,结果表明,试样全部通过45 μm标准筛,Si内标比例为10%,步进长度0.01°,步进时间30S,选择对Fe3O4（311）、Fe2O3（104）、SiO2（011）和Si（111）的衍射峰进行积分强度计算,可获得最优结果。在选定工作条件下,Fe3O4在1.07～100%范围内线性相关系数(R2)为0.9953,相对标准偏差(RSD)1.1%～13.2% (n=6),加标回收率99.7 %~114.8 %,检出限(LOD)4.29%;Fe2O3在1.51～100%范围内线性相关系数(R2)为0.9991,相对标准偏差(RSD)2.8%～10.6% (n=6),加标回收率87.1%~112.2%,检出限(LOD)2.56%;SiO2在0.79～29.72 %范围内线性相关系数(R2)为0.9957,相对标准偏差(RSD)3.2%～10.3% (n=6),加标回收率86.6%~98.9%,检出限(LOD)0.68%。方法易溯源、准确性易评价和验证,适合开展标准化检测和应用。     

锂离子电池LiMn2O4正极材料的高温改性

锂离子电池LiMn2O4正极材料的高温改性;锂离子电池;正极材料;尖晶石;LiMn2O4;包覆     

掺杂Co2+和Sm3+对纳米ZnFe2O4铁氧体的电磁损耗性质的影响

采用NaHCO3与FeCl3?6H2O,ZnSO4?7H2O,Co(NO3)2?6H2O和Sm(NO3)3?6H2O进行室温固相反应制得碱式碳酸盐和氢氧化铁混合前驱物,先微波加热,再热分解分别制得复合氧化物ZnFe2O4,Co0.5Zn0.5Fe2O4和Co0.5Zn0.5Fe1.95-Sm0.05O4.由激光粒度分析仪、XRD和SEM表征:获得了颗粒分布均匀、平均粒度为62nm左右的立方晶系尖晶石结构的纳米铁氧体粉体.并测试样品的相对介电常数和相对磁导率,研究了它们的电磁损耗特性.结果表明:在ZnFe2O4中,掺入Co2 ,Sm3 元素可以在100～1800MHz测试频率范围内不同程度提高材料的电磁损耗特性.     

X射线荧光光谱法测定萤石中CaF2、CaCO3、S、Fe及SiO2

X射线荧光光谱法分析是目前快速分析方法之一,精密度受基体效应、均匀性、元素间干扰等影响。采用粉末压片法制备样品,用X射线荧光光谱法直接测定F、Ca元素,得出CaF_2及CaCO_3含量,并同时分析萤石中S、Fe、SiO_2的含量。精密度实验表明,待测元素的相对标准偏差均低于0.66%(RSD,n=10),能满足萤石中各元素的检测要求。     

SiO2包覆Gd2O3:Er3+,Yb3+纳米粉的制备、结构及发光性能

用微乳液法合成出SiO2包覆的Yb3+,Er3+离子舣掺杂的Gd2O3粉体,X射线衍射结果表明所制备粉体为立方Gd2O3结构.透射电镜照片显示其颗粒形状近似为球形,粒径为10～40 nm;该粉体在波长为980 nm的半导体激光器激发下发射出中心波长为562 nm的绿色和660 m的红色上转换荧光,分别对应于Er3+离子的4S3/2/2H11/2→4I15/2跃迁和4F9/2→4I15/2跃迁.发光强度和激发功率关系的研究揭示其均为双光子过程,能量传递和激发态吸收是上转换发光的主要机制.由于其具有高效的上转换发光性能,而经过纳米复合后制成的纳米Gd2O3(核)/SiO2(壳),容易溶于水并易于和有机物结合,能与生物分子结合.     

球形SiO2-Al2O3的制备、结构和性能

将Na2SiO3·9H2O 溶液通过强酸性阳离子树脂进行离子交换得到酸性硅溶胶,再将硅溶胶与铝溶胶及六次甲基四胺混合后采用油柱成型法制备了球形SiO2-Al2O3复合氧化物. 通过XRD、BET 及TPD等手段对样品进行测试和表征, 结果表明, 600 ℃焙烧得到的SiO2-Al2O3中SiO2以无定型形式存在, 其比表面、孔容与表面酸性随SiO2含量的增加而提高, 孔径、堆密度随SiO2含量的提高而减小, 压碎强度基本保持不变.