Nb2O5掺杂NiFe2O4陶瓷材料的显微结构和导电性能

以NiO、Fe2O3和Nb2O5为原料,采用固相烧结法合成陶瓷粉体,通过等静压-气氛烧结法制备Ni1-xNbxFe2O4(x=0,0.02,0.05,0.07,0.10,0.20)陶瓷试样,并对其进行导电性能测试。通过XRD、SEM、EDX、FTIR和XPS等分析手段对材料的物相组成、显微结构和微区成分进行表征,研究Nb2O5掺杂对陶瓷材料显微结构和导电性能的影响。结果表明:Nb2O5掺杂抑制NiFe2O4基体中NiO相的出现,过量时生成FeNbO4相;适量掺杂(x=0.05)有利于消除晶界孔隙,提高陶瓷的烧结密度;与未掺杂试样相比,掺杂Nb2O5的NiF2O4陶瓷材料的导电性均得到很大改善,其中掺杂量x=0.05的Ni0.95Nb0.05Fe2O4陶瓷试样在1 233 K的电导率较纯NiFe2O4的提高60%。     

Fe2O4催化纤维素水热法制备 Fe2O3/ 碳纳米复合材料

目的在较为温和的条件下制备氧化铁/碳纳米复合材料。方法以纳米Fe3O4粉体为催化剂,水热催化纤维素碳化,并借助扫描电镜、透射电镜、X射线光电子能谱仪和X射线衍射仪对碳化产物进行表征分析。结果获得了粒径约为150 nm的枣核形氧化铁/碳纳米复合材料。结论通过相对温和的水热反应,纤维素被碳化形成了壳核结构的纳米产物,Fe3O4催化剂在反应过程中被氧化并成为壳核结构产物的核心。     

Ag+掺杂ZnWO4纳米棒的微波水热法合成及光催化性能

以硝酸锌(Zn(NO3)2·6H2O)、和钨酸钠(Na2WO4·2H2O)作为起始反应物,利用微波水热法在200℃下合成纳米棒状钨酸锌。利用X-射线粉末衍射、场发射扫描电子显微镜、透射电子显微镜及能谱成分图谱等分析手段对纳米棒状钨酸锌粉体进行表征,并对不同Ag+掺杂量的ZnWO4纳米棒的光催化性能进行了研究。结果表明:Ag+成功的掺入ZnWO4纳米棒中;随着Ag+掺杂量的增加ZnWO4纳米棒的颗粒尺寸也不断增大;Ag+掺杂量2%时纳米棒状钨酸锌粉体的光催化性能最优,但是随着掺杂量的逐渐增加光催化性能反而降低。     

氮掺杂碳包覆Bi2Mn4O10锂离子电池负极材料的制备及其电化学性能(英文)

为抑制高能锂离子电池负极材料Bi₂Mn₄O₁₀容量的快速衰减,通过简单球磨法制备新型高纯Bi₂Mn₄O₁₀/ECP-N(ECP-N为氮掺杂科琴黑)负极复合材料。所合成的Bi₂Mn₄O₁₀/ECP-N复合材料在0.2C倍率下循环100次后可保持576.2m A·h/g的比容量,容量保持率为75%,而纯Bi₂Mn₄O₁₀的容量保持率仅为27%。3C倍率下Bi₂Mn₄O₁₀/ECP-N复合材料的放电容量仍保持在236.1 m A·h/g。引入氮掺杂的科琴黑ECP-N不仅可以有效地提高比表面积以缓冲体积膨胀,增强材料的电导率和可湿性,而且还可以促进离子传输和可逆转化反应。     

SnO2/Zn2SnO4纳米结构的制备及光谱性质

采用自蔓延高温合成-喷射法制备了SnO2纳米线和SnO2/Zn2SnO4纳米结构,利用XRD、SEM、UV-vis和FT-IR对其物相、形貌和谱学性质进行了表征。结果表明:SnO2纳米线凝胶对紫外-可见光的透光度随着SnO2纳米线加入量的增加而增加,但是,SnO2/Zn2SnO4凝胶对紫外-可见光的透光度却随着SnO2/Zn2SnO4的增加而减少;与SnO2纳米线相比,SnO2/Zn2SnO4在1090,1430,1640,3450cm-14个特征波长附近对红外光谱的选择吸收率明显提高,因而对H2O、CH4、CO和CO2等气体的敏感性将显著增强。     

孔道Al2O3/SiO2对NaAlH4-Tm2O3体系储氢性能的影响

以机械球磨法制备具有可逆吸放氢性能的NaAlH4-Tm2O3储氢材料体系。利用相同制备方法进一步研究两种不同孔道材料(大孔Al2O3与介孔SiO2)对NaAlH4-Tm2O3体系储氢性能的影响,测试样品的循环吸放氢性能,并对样品吸放氢前后的结构进行表征。结果表明:大孔Al2O3材料的添加并不能明显改善NaAlH4-Tm2O3体系的放氢速率和放氢量,而介孔SiO2的加入使NaAlH4-Tm2O3体系在150℃条件下5 h内的首次放氢量(质量分数)达到4.61%,高于NaAlH4-Tm2O3体系的4.27%,增加了约8.0%。此外,添加介孔SiO2的NaAlH4-Tm2O3体系放氢速率也有所提高。     

La3+、Ce4+掺杂对纳米TiO2-Fe2O3凝胶相变过程的影响

采用sol-gel法制备了掺杂La3+、Ce4+的TiO2-10wt%Fe2O3复合粉体,利用TG-DTA和XRD分析对凝胶的相变过程进行了表征。结果表明:TiO2-10wt%Fe2O3凝胶在450℃发生非晶态向锐钛矿相的转变,而在500℃煅烧2 h后未发现锐钛矿相向金红石相转变;随La3+、Ce4+掺杂量的增加,锐钛矿晶粒呈现细化→长大的趋势;随La3+掺杂量的增加,对Fe2O3微晶的生成作用呈现促进→抑制的趋势,而对Fe3O4微晶的生成呈现抑制→促进的趋势;随Ce4+掺杂量的增加,对Fe2O3微晶的生成作用随掺杂量的增加呈促进→抑制→促进的趋势,而对Fe3O4微晶的生成呈现抑制→促进的趋势;La3+、Ce4+掺杂对TiO2相变过程有重要影响。     

纳米铁氧体NiFe2O4复合材料制备及电磁屏蔽性能

采用溶胶-凝胶法制备纳米镍铁氧体,在凝胶形成之前加入超细可膨胀石墨,生成的干凝胶粉末在马弗炉中灼热一段时间,在纳米镍铁氧体生成的同时微膨石墨发生膨胀,由此合成出纳米铁氧体复合材料。应用X射线衍射仪、扫描电镜、激光粒度分析仪对产物的晶体结构、微观形貌和粒度分布进行了表征分析,并着重对比研究了不同热处理温度对产物粒径分布的影响。利用小型烟箱试验测出产物在军用红外波段质量消光系数大于0.85m2/g;利用矢量网络分析仪测试其在2~18GHz的电磁参数。结果表明:在纳米铁氧体中添加超细微膨石墨,增加了电磁波的损耗,并在红外波段具有显著的消光特性,兼具红外、微波吸波特性,是一种具有潜在应用前景的隐身材料。     

溶胶-凝胶法制备Pt2+掺杂Bi2O3及光催化性能研究

用溶胶-凝胶法制备了Pt2+掺杂的Bi2O3光催化剂(Pt/Bi原子比分别为1/100、2/100、3/100和4/100),以甲基橙为模拟有机污染对催化剂的光催化性能进行了考察。光催化剂用BET、XRD、XPS和紫外-可见漫反射进行了表征,结果表明Pt/Bi原子比为3/100时催化剂的比表面最高;经500℃焙烧后光催化剂晶型为α-Bi2O3;掺杂Pt2+后Bi2O3在可见光区的吸收增强;掺杂Pt2+后Bi 4f7/2和O 1s结合能均向低能端偏移,催化性能测试结果表明Pt/Bi原子比为3/100时的催化剂活性最高。增加的比表面、对可见光响应增强和结合能向低能端偏移均有利于提高Bi2O3光催化活性。     

Co掺杂ZnAl_2O_4纳米颗粒的制备与光学性质

以十六烷基三甲基溴化铵(CTAB)为表面活性剂,采用水热法成功制备了不同掺杂比例的Zn_(1-x)Co_xAl_2O_4(x=0,0.20,0.40和0.60)纳米晶。并对样品的晶体结构、形貌、化学成分、价态和光学性能进行表征。实验结果表明,本方法所制备的不同掺杂浓度的Zn_(1-x)Co_xAl_2O_4纳米颗粒为尖晶石结构,晶化程度良好。根据XRD数据计算了晶胞参数a、晶格间距d_(hkl)、晶粒尺寸D,随着掺杂Co离子浓度的增加,均表现为减小趋势。XPS能谱显示大多数Co离子占据四面体中心位置,但有少量的Co离子占据八面体中心位置。随着掺杂Co离子浓度的增加,紫外吸收光的强度逐渐增加。     

以Mn3O4为前驱体制备尖晶石型LiMn2O4及其性能

采用改进的固相反应法合成了高性能的锂离子电池正极材料LiMn2O4。首先,以廉价的MnSO4为原料,通过水解氧化法制备纳米级Mn3O4前驱体;然后,将Mn3O4和Li2CO3混合均匀,在750℃固相反应20 h,得到尖晶石型LiMn2O4。用X射线衍射(XRD)和扫描电镜(SEM)对Mn3O4前驱体和LiMn2O4样品进行表征,用充放电测试和循环伏安技术对LiMn2O4样品进行电化学性能研究。结果表明:所制备的LiMn2O4具有完整的尖晶石型结构,且晶体粒子分布均匀。所制备的LiMn2O4材料在3.0~4.4 V之间,室温(25℃)下,在0.2C倍率下首次放电比容量为130.6 mA.h/g;在0.5C倍率下首次放电比容量为127.1 mA.h/g,30次循环后,容量仍有109.5 mA.h/g,且样品具有较好的高温性能。     

Nb-Cr掺杂原位合成Al2O3/TiAl复合材料的组织与性能

采用原位热压工艺,在Ti-Al-TiO2-Nb2O5体系中加入Cr2O3原位合成Al2O3/TiAl复合材料.借助X射线衍射分析、SEM分析及力学性能分析,研究了Nb-Cr掺杂复合强化Al2O3/TiAl复合材料的反应过程、微观结构及力学性能.结果表明Nb-Cr掺杂原位合成Al2O3/TiAl复合材料能够细化晶粒并通过微合金化增强增韧TiAl复合材料.     

溶胶-凝胶伴随相分离法制备多孔锌铝尖晶石块体

以无水氯化锌和六水氯化铝为前驱体,水和乙醇的混合溶液为溶剂,1,2-环氧丙烷为凝胶促进剂,聚氧乙烯为相分离诱导剂,采用溶胶-凝胶伴随相分离法制备大孔锌铝尖晶石块体材料,并采用差热分析(DTA)、X-射线衍射(XRD)、红外光谱(FT-IR)和扫描电子显微镜(SEM)等 测试技术对所形成的多孔块体的物相和微观结构进行了表征,并研究了高温热处理过程对块体材料的结构以及晶相的影响。结果表明,聚氧化乙烯(PEO) 能诱导体系发生相分离,获得共连续骨架和孔径大小可控的多孔块体。常温下制备出的多孔块体为的锌铝水滑石(ZnAl-LDHs),热处理过程中发生羟基脱除,碳酸根离子分解等反应,最后得到具有单一尖晶石相的多孔块体,该材料在石油化工领域的催化应用具有良好的前景。     

Preparation and electrochemical performance of nanosized Co3O4 via hydrothermal method

The hydrotalcite-type cobalt compounds were prepared through oxidation of Co（OH）2 gel using NH4OH as precipitating agent and H2O2 as oxidant. These hydrotalcite-type cobalt compounds were transformed into Co3O4 through hydrothermal decomposition with nanostructural deformation. The precursor and product were characterized by Fourier-transform infrared（FT-IR） spectrum, X-ray diffractometry（XRD） and transmission electron microscopy（TEM）. The electrochemical performances of as-prepared nanosized Co3O4 as anode materials in lithium-ion batteries were tested by charge-discharge test in the voltage range of 0-3.0 V. The influence of morphology of Co3O4 particle on the capacity and cycling performance was studied. The results show that the shape and size of the final product can be controlled by altering cobalt sources. The irregular cubic Co3O4 with the average particle size of about 10 nm shows the best electrochemical performance. After 10 charge-discharge cycles, the specific charge capacity retains 555 mA.h/g.     

Synthesis, structure and optical properties of CoAl2O4 spinel nanocrystals

CoAl₂O₄ nanocrystals were synthesized by sol-gel method using citric acid as a chelating agent at low temperature. The as-synthesized samples were characterized by thermal analysis, X-ray powder diffraction, infrared spectroscopy and transmission electron microscopy. The results show that CoAl₂O₄ spinel is the only crystalline phase with a size of 10-30 nm in the temperature range 500-1000 °C. The temperature dependence of the distribution of Al³⁺ and Co²⁺ ions in the octahedral and tetrahedral sites in nanocrystals was investigated by X-ray photoelectron spectroscopy (XPS). It is observed that the inversion parameter decreases with increasing annealing temperature. Analysis of the absorption properties indicates that Co²⁺ ions are located in the tetrahedral sites as well as in the octahedral sites in the CoAl₂O₄ nanocrystals. The origin of the green color (300-500 nm absorption band) should be due to the octahedrally coordinated Co²⁺ ions.     

MgAl2O4:Eu3+荧光粉的制备及其光谱特性

采用水热辅助固相法合成一系列Eu³⁺掺杂MgAl₂O₄:Eu³⁺荧光粉。主要考察粉体的物相结构、形貌、颗粒尺寸及电/磁偶极跃迁强度随Eu³⁺摩尔分数的变化规律。结果表明:当Eu³⁺不等价取代Mg²⁺后并未影响基质材料的晶体结构,产物全部为立方相MgAl₂O₄,但间隙O^2?的存在会影响被取代离子Mg²⁺的配位关。当Eu³⁺掺入时,其会与溶液中的NH₄⁺共同参与调控样品的形貌和尺寸,以致片状颗粒的厚度减小、不规则程度加剧。基于J-O理论认为,在248 nm紫外和395 nm近紫外光激发下,Eu³⁺在MgAl₂O₄中所处格位的对称性差异是引起电偶极(⁵D₀→⁷F₂)和磁偶极(⁵D₀→⁷F₁)跃迁相对强度不同的主要原因。     

Low-voltage cathodoluminescence properties of green-emitting ZnAl2O4:Mn nanophosphors for field emission display

A low-cost ZnAl₂O₄:Mn²⁺ green nanophosphor for field emission display (FED) was successfully synthesized by the coprecipitation method and a two-step firing, firstly calcining at 1200 °C for 2 h in air and then annealing at 900 °C for 3 h in flowing NH₃ gas. The effects of the preparation process and the Mn²⁺ concentration on optical properties of ZnAl₂O₄:Mn²⁺ were investigated. The phase composition, particle morphology, photoluminescence (PL) spectra of the ZnAl₂O₄:Mn²⁺ phosphor as well as low-voltage field emission properties of the FED device prepared by using the synthesized ZnAl₂O₄:Mn²⁺ phosphor were examined. Similar to ZnGa₂O₄:Mn²⁺, Mn²⁺-doped ZnAl₂O₄ showed two green emission bands centered at 508 and 517 nm, respectively, which originate from ⁴T₁(⁴G)→⁶A₁(⁶S) transitions of Mn²⁺ on T_d and O_h sites. The PL intensity reached the maximum at 0.5 at.% Mn²⁺. Under the low-voltage excitation, the FED device exhibited bright green emission, high voltage brightness saturation, and high color purity.     

Induced crystallization and physical properties of Li2O–CaF2–P2O5:TiO2 glass system: Part II. Electrical, magnetic and optical properties

The results of various physical properties namely, dielectric properties (dielectric constant, loss tan δ, ac conductivity σ, over a wide range of frequency and temperature and dielectric breakdown strength in air medium at room temperature), optical absorption, electron spin resonance (ESR) at liquid nitrogen temperature and magnetic susceptibility at room temperature of Li₂O–CaF₂–P₂O₅:TiO₂ glass-ceramics have been reported. The optical absorption and magnetic susceptibility studies indicated that the titanium ions exist in Ti³⁺ state in addition to Ti⁴⁺ state in these samples. However, the reduction seems to be the lowest in the sample containing 0.6 mol% of TiO_2. The dielectric constant and loss variation with the concentration of TiO₂ have been explained on the basis of space charge polarization mechanism. The dielectric relaxation effects exhibited by these samples have been analyzed by a pseudo Cole–Cole plot method and the spreading of dielectric relaxation has been observed. The ac conductivity in the high temperature region seems to be related both with electronic and ionic movements. The low temperature (or the nearly temperature independent) part of conductivity could be explained on the basis of quantum mechanical tunneling model. The studies on dielectric breakdown strength indicated the highest insulating strength for the sample containing 0.6 mol% of TiO₂.     

Spectroscopic and dielectric studies on MnO doped PbO–Nb2O5–P2O5 glass system

PbO–Nb₂O₅–P₂O₅ glasses containing different concentrations of MnO ranging from 0 to 2.5 mol% were prepared. A number of studies viz., differential thermal analysis, infrared, optical absorption, luminescence, Raman and ESR spectra, magnetic susceptibility and dielectric properties (constant ′, loss tan δ, ac conductivity σ_ac over a range of frequency and temperature) of these glasses have been carried out. The results have been analyzed in the light of different oxidation states of manganese ions. The analysis indicates that when the concentration of MnO is around 1.0 mol%, manganese ions mostly exist in Mn²⁺ state, occupy network forming positions with MnO₄ structural units and increase the rigidity of the glass network. When MnO is present in higher concentrations, these ions seem to exist mostly in Mn³⁺ state and occupy modifying positions.