水热法合成FeS2粉晶及其生长热动力学的研究

采用溶胶-凝胶水热法合成了单相黄铁矿结构的FeS2粉晶.用x射线衍射、傅氏变换红外光谱等分析手段对FeS2粉晶进行了表征,以简化的数学模型及相变理论讨论了晶体生长过程.结果表明:FeS2晶粒的生长过程属于相变与扩散的混合机制,符合经时间指数修正的二次方动力学方程,是一个生长速率随时间变化的过程;水热晶化温度高于453 K、反应时间超过18 h且有适量的硫参与反应时,可得到单相的黄铁矿型的FeS2.该过程可分为三个阶段:前期为白铁矿和黄铁矿的成核孕育阶段,中期为FeS2晶核以黄铁矿吞并白铁矿的相变方式逐渐长大的阶段,后期为小晶粒融合而大晶粒继续长大的扩散生长过程.     

纳米TiO2多孔膜的微结构对染料敏化纳米薄膜太阳电池性能的影响

采用溶胶-凝胶方法，在不同的实验条件下获得平均粒径从15到25nm左右的纳米TiO２2颗粒.利用这些颗粒制备出的纳米多孔薄膜，应用于染料敏化纳米薄膜太阳电池. 通过x射线 衍射仪分析，得到TiO２₂颗粒的晶相以及晶粒度大小，用透射电子显微镜观察 了纳米TiO２₂颗粒的形貌和尺寸.应用于太阳电池的纳米TiO２₂多 孔膜，经基于布朗诺尔-埃米特-泰 勒（BET）的多层吸附理论的比表面积测试和孔径分布测试，获得了多孔膜的微 关键词： 溶胶-凝胶法 2')" href="#">纳米TiO２₂ 染料敏化 太阳电池     

非晶钛酸铋的晶化过程

利用差热分析、X射线衍射和透射电子显微镜等技术对溶胶-凝胶法合成的凝胶的晶化过程进行了分析，实验结果表明，Bi₄Ti₃O₁₂非晶凝胶晶化过程经历了四个过程：首先在433℃先形成了Bi₂O₃和TiO₂亚稳相，然后在488℃时TiO₂亚稳相与Bi₂O₃反应形成Bi，Ti复合氧化物亚稳相Bi₂T 关键词： 钛酸铋 铁电材料 溶胶凝胶 非晶 晶化过程     

单轴M型SrFe12-xCrxO19超细粒子结构与磁性研究

采用溶胶-凝胶法制备了单轴M型锶铁氧体SrFe12-x_12-xCrx_xO 19₁₉(x=0—1)超细晶粒.实验结果表明, 随掺杂量x的增大，质量饱和磁化强 度σs_s在x≤04范围内增大，在x=02附近达到极大值.矫顽力Hc_c在x＜05的范围 内单调降低，这对于用作高密度磁记录材料非常有利.当x≤04时，样品是单相结构， 在 x=06以后出现非磁性相α-Fe2₂O3< 关键词： 锶铁氧体 3+')" href="#">Cr3+³⁺ 结构 磁性     

溶胶-凝胶法制备ZnO薄膜的成核-生长和失稳分解研究

采用溶胶-凝胶法在ZnWO₄单晶上制备出透明的ZnO薄膜.通过光学显微镜观察了Z nO薄膜的表面形貌.实验结果表明，ZnO薄膜的形成经历了表面成核，晶粒长大和岛的形成三 个不同的阶段.由于ZnO晶核是在非平衡条件下生长的，在生长过程中不可避免地出现了枝晶 生长和分形生长以及失稳分解. 关键词： 氧化锌薄膜 成核 枝晶生长 分形生长 失稳分解     

溶胶-凝胶法制备的纳米TiO2结构相变及晶体生长动力学

讨论了采用溶胶-凝胶法经由先驱物钛酸四异丙脂水解而制备的纳米TiO₂粉末的 结构相变 ，并讨论了该纳米粉末的生长动力学机理.结果表明，水解pH值为0.9，当高压釜热处理温度 ＜503K时，粉末晶粒度增长较为缓慢，而当热处理温度＞503K时，粉末粒度明显长大.应用 相变理论计算出了纳米TiO₂颗粒的两阶段的生长激活能，分别是18.5kJ/mol和5 9.7kJ/mol .XRD物相分析表明，高压釜热处理温度达到503K时，样品就开始发生锐钛矿到金红石相的结 构相变，到543K就基本实现了这一结构相变，使得这一相变温度比其他文献中报道的又降低 了许多. 关键词： 2')" href="#">纳米TiO₂ 溶胶_凝胶法 结构相变 晶粒生长动力学     

Dy含量对红色长余辉发光材料Sr3Al2Ｏ6:Eu2＋,Dy3＋性能的影响

采用溶胶凝胶法制备了Sr₃Al₂Ｏ₆:Eu^2＋,Dy^3＋红色长余辉发光材料,利用X射线衍射仪对材料的物相进行了分析,结果表明,1200℃下制备的样品的物相为Sr₃Al₂Ｏ₆,少量的Eu和Dy掺杂没有影响样品的相组成.采用荧光分光光度计、照度计测定了样品的发光特性.结果表明Sr₃Al₂Ｏ关键词： 红色长余辉 3Al₂Ｏ₆')" href="#">Sr₃Al₂Ｏ₆ 溶胶凝胶法     

Ti-Zr-Ni单相准晶合金的室温力学性能研究

以Ti40₄₀Zr40₄₀Ni20₂₀合金为研究对象，用铜 模吸铸法制备出直径为3mm的致密单相准晶棒，通过维氏显微硬度测定和单向压缩实验方 法研究了该合金的室温力学性能 .结果表明：Ti40₄₀Zr40₄₀Ni20₂₀准晶具有良好 的弹性变形能力，室温弹性应 变可达125%.同时，它具有相对高的室温硬度（约55GPa），是普通Ti合金的15倍.T i40_{40 关键词： 准晶 Ti-Zr-Ni合金 解理断裂}     

稀土钇、镧掺杂TiO2薄膜的拉曼谱分析

采用溶胶-凝胶法在石英玻璃衬底上用旋涂法制备了未掺杂、掺杂钇和掺杂镧的TiO₂薄膜样品,对样品在700—1100 ℃范围内进行退火处理,并对样品的拉曼光谱进行了分析.分析表明:随着退火温度的升高,未掺杂TiO₂薄膜发生了从锐钛矿相经混相最终向金红石相的转换,掺杂钇和掺杂镧对TiO₂薄膜的晶相转换起阻碍作用,掺杂镧的阻碍作用更强;稀土掺杂能使TiO₂薄膜晶粒细化,并使晶粒内部应力增大从而阻碍晶格振动,掺杂镧比掺杂钇的效果 关键词： 2薄膜')" href="#">TiO₂薄膜 稀土掺杂 拉曼光谱 溶胶-凝胶     

熔体快淬Pr(Fe1-xCox)2合金的结构和磁性

通过熔体快淬方法获得Pr(Fe_1-xCo_x)₂合金条带,经过X射线衍射、差示扫描量热计和磁性测量对其结构、磁性和热稳定性进行了研究.发现当Co的含量x大于0.2时才可能获得Pr(Fe,Co)₂立方Laves相化合物.对Pr(Fe_0.6Co_0.4)₂合金,在快淬速度为30m/s时,条带由Pr₂(Fe,Co)₁₇,Pr(Fe,Co)₂和富稀土相组成;在速度为40m/s时,获得了几乎单相的Pr(Fe_0.6Co_0.4)₂化合物,其居里温度为305℃;在速度为45m/s时,除了Pr(Fe_0.6Co_0.4)₂化合物外,还存在少量的非晶相.Pr(Fe_0.6Co_0.4)₂化合物在770℃以上发生分解.用40m/s快淬纳米晶粉胶粘磁体有大的磁致伸缩系数（λ_∥-λ_⊥=140×10^-6)和高的硬磁性能（_iH_c=398kA/m). 关键词：     

The quantitative determination of FeS2 phases in coal by means of57Fe Mössbauer spectroscopy

A knowledge of the concentration of pyrite and marcasite in coals can provide important insight into the genesis of coal deposits. Determinations of the relative amounts of pyrite and marcasite by traditional methods of coal analysis are, however, beset with many difficulties. Using⁵⁷Fe Mössbauer spectroscopy and a mild chemical treatment with hydrofluoric acid, a technique has been devised for the quantitative determination of the relative concentrations of pyrite and marcasite in samples of whole coals or their low-temperature ashes. The sample preparation procedure is comparable to less accurate methods. Good qualitative agreement has been obtained between ore microscopic and Mössbauer spectroscopic techniques for a series of extensively investigated whole coal samples.     

拉曼光谱研究天然FeS_2晶须结构及其相变规律

利用显微激光拉曼技术研究了山西耿庄天然纳-微米FeS2晶须的结构.发现FeS2晶须中有白铁矿和黄铁矿两种结构类型.较粗的藕节状、粗柱状、串珠状等不规则形貌为白铁矿相,直线状、平直、表面光滑的品须为黄铁矿相.耿庄FeS2晶须结晶生长早期以白铁矿相为主,中期是白铁矿和黄铁矿型结构共存,晚期以黄铁矿相为主.晶须生长过程有早期白铁矿结晶向晚期黄铁矿结晶转变的趋势.而且有黄铁矿包覆白铁矿的生长现象.FeS2晶须结构相变规律与形貌、形成时间和成分特点具有关联性.     

Hydrothermal synthesis of FeS2 for lithium batteries

Nanocrystalline FeS₂ cathode material of lithium cell was synthesized from cheap materials of FeSO₄, Na₂S₂O₃, and sulfur by a hydrothermal process. The scanning electron microscopy analysis showed the obtained material was nano-sized, about 500 nm. The X-ray powder diffraction analysis showed that the synthetic FeS₂ material had two phases of the crystalline structure, pyrite and marcasite. The phase of marcasite seems to have no negative effect on the electrochemical performance of the material. The synthetic FeS₂ showed a significant improvement of electrochemical performance for Li/FeS₂ cells.     

Electrical resistivity and band gap of marcasite (FeS2)

For a natural crystal of marcasite, an energy gap of 0.34 eV and an acceptor level at 0.052 eV are determined from temperature-dependent (53–370 K) electrical resistivity measurements. Magnetic susceptibilities and dielectric constants of marcasite and pyrite are compared in view of the large difference in their energy gaps.     

An ab initio study of 5d noble metal nitrides: OsN2, IrN2, PtN2 and AuN2

The crystal structure, phonon stability, elasticity and electronic properties of four noble metal nitrides (PtN₂, IrN₂, OsN₂ and AuN₂) with three structural types (pyrite, marcasite and CoSb₂ structure) were studied by first principles calculations. In agreement with experiments and previous theoretical predictions, it is found that the most stable structure for OsN₂ is marcasite, for PtN₂ is pyrite, and for IrN₂ is the CoSb₂ structure. It is found that these three compounds are thermodynamically metastable with respect to solid N₂ and the metal at zero pressure. The structures are mechanically and dynamically stable. The lowest energy structure of AuN₂ is the CoSb₂ structure. The formation energy of AuN₂ is found to be very high compared to the other three nitrides studied here. This underlies the experimental difficulty in the synthesis of this compound. OsN₂ is found to be metallic, while IrN₂ and PtN₂ are both semiconductors.     

Magnetic properties of iron marcasite FeS2

The magnetic susceptibility, χ, of a natural single crystal of marcasite, FeS₂, has been measured between 300K down to 4K. At room temperature χ=0.3×10^?5 emu/g and it is temperature independent down to 10K. Below 10K it increases up to 1.3×10^?5 emu/g. It is concluded that iron in marcasite is in the Fe²⁺ low spin state, and that the 6d electrons occupy the t_2g ground state. Consequently iron in marcasite (FeS₂) is not magnetic in agreement with our Mössbauer spectra recorded at 4.2K in an external magnetic field up to 39.9 kOe. The small value of χ is explained in terms of contributions from ppm impurities. i.e., diamagnetism and Van Vleck paramagnetism.     

Sulphur L2,3 and L1 XANES investigations of pyrite and marcasite

S L_2,3 and L₁ XANES of the polymorph minerals pyrite (FeS₂) and marcasite (two different cleavage planes) were measured in total electron yield mode using synchrotron radiation. Small but distinct differences were found in the fine structure of these spectra. Calculations with the FEFF-8 code were performed to reproduce the experimental data. Ex situ UV–ozone oxidation of the samples reveals different reactivity. Sulphate was identified on the pyrite and one marcasite cleavage planes whereas the second plane normal to the first one oxidises with changing quanta of sulphate and sulphite.     

Influence of ferric iron on the electrochemical behavior of pyrite

The electrochemical behavior of a pyrite electrode in a sulfuric acid solution with different concentrations of ferric iron (Fe³⁺) was investigated using electrochemical techniques including measurements of open circuit potential, cyclic voltammetry, Tafel polarization curves and electrochemical impedance spectroscopy (EIS). The results show that the pyrite oxidation process takes place via a two-step reaction at the interface of the pyrite electrode and the electrolyte, and that a passivation film composed of elemental sulfur, polysulfides, and metal-deficient sulfide is formed during the process of the first-step reaction. Ferric iron plays an important role in the dissolution of pyrite by enhancing the direct oxidation. The Tafel polarization curves indicate that the polarization current of the pyrite electrode increases with an increase in Fe³⁺ concentration. It has also been shown that the higher concentration of Fe³⁺, the more easily the pyrite can be transformed into the passivation region. Moreover, the EIS response is found to be sensitive to changes in Fe³⁺ concentration.     

Pressure induced phase transition in MnTe2

Energy dispersive high-pressure powder X-ray experiments have been performed for MnTe₂ up to a pressure of 20 GPa. MnTe₂ undergoes a discontinuous transformation from the cubic pyrite type structure to the orthorhombic marcasite type structure at 7.0±0.5 GPa upon increasing pressure. The transformation is accompanied by a large reduction in the specific volume (ΔV/V=0.18) which probably reflects different magnetic properties of the two modifications of MnTe₂.     

Investigation of Virgin Coals and Coals Subjected to a Mild Acid Treatment

A quantitative determination of the relative marcasite/pyrite contents in virgin coals is possible by means of ⁵⁷Fe Mössbauer spectroscopy. Complications arise, however, when iron-containing silicates, carbonates, or other salts are present. The application of a mild chemical treatment involving hydrofluoric acid has been employed to remove these Fe-containing phases while leaving the iron-disulfide phases unaffected. Several South African coal samples with non-iron disulfide, Fe-containing phases ranging from 18 to 30 weight percent have been subjected to a hydrofluoric acid leaching at room temperature. The loss of mineral matter with HF leaching correlates well with the mineral matter residue following low temperature ashing. The ⁵⁷Fe Mössbauer spectra of the resulting coal samples, collected at 297K, indicate that only FeS₂ phases are present. The Mössbauer parameters for these samples (0.619 ≤E_Q≤0.622 mm s^?1; 0.306≤δ≤0.309 mm s^?1) indicate the absence of appreciable quantities of marcasite in the coals. These Mössbauer parameters differ slightly, but systematically, from those of pyrite for which a quadrupole splitting of 0.6110 ± 0.0020 mm s^?1 has been established. On the basis of previous studies, these increased E_Q values suggest the presence of As substitution in the pyrite phases. ⁵⁷Fe Mössbauer spectra of virgin coals exhibit phase assemblages comparable to those observed by x-ray diffraction (XRD), e.g. pyrite and (Ca,Fe)CO₃, even though the presence of pyrite is less definite in the XRD data.