X-ray characterization and phase transformation kinetics of ball-mill prepared nanocrystalline Mg–Zn-ferrite at elevated temperatures

Nanocrystalline Mg–Zn-ferrite is prepared by ball milling the stoichiometric powder mixture of MgO, ZnO and α-Fe₂O₃. A non-stoichiometric ferrite phase is noticed to form after 3 h of milling when particles of starting materials became nano-sized. After 25 h of milling, stoichiometric ferrite phase is formed with 9 nm particle size. Post annealing study of ball-milled sample reveals that the nanocrystalline ferrite phase is stable up to 873 K and then starts to decompose into individual starting phases. However, heat treatment of unmilled stoichiometric powder mixture even at 1473 K for 1 h duration does not result in formation of stoichiometric Mg–Zn-ferrite phase.     

塞曼石墨炉原子吸收光谱法测定粉尘降尘中痕量锡

以KOH熔样,又以KOH作基体改进剂,研究了测定锡的灰化温度、原子化行为和消除干扰及试样前处理的方法,以KOH熔解的粉尘及降尘样液,特别适用于塞曼石墨炉的测定,背景可完全扣除。方法简便、快速、准确,灵敏度和精度高。相对标准偏差为4.0%,回收牢在96.4～110%范围内。     

Pressure-induced phase transitions of multiferroic BiFeO3

Pressure-induced phase transitions of multiferroic BiFeO3 have been investigated using synchrotron radiation X-ray diffraction with diamond anvil cell technique at room temperature. Present experimental data clearly show that rhombohedral （R3c） phase of BiFeO3 first transforms to monoclinic （C2/m） phase at 7 GPa, then to orthorhombic （Pnma） phase at 11 GPa, which is consistent with recent theoretical ab initio calculation. However, we observe another peak at 2θ=7° in the pressure range of 5-7 GPa that has not been reported previously. Further analysis reveals that this reflection peak is attributed to the orthorhombic （Pbam） phase, indicating the coexistance of monoclinic phase with orthorhombic phase in low pressure range.     

Chemical synthesis of p-type nanocrystalline copper selenide thin films for heterojunction solar cells

Nanocrystalline thin films of copper selenide have been grown on glass and tin doped-indium oxide substrates using chemical method. At ambient temperature, golden films have been synthesized and annealed at 200 °C for 1 h and were examined for their structural, surface morphological and optical properties by means of X-ray diffraction (XRD), scanning electron microscopy and UV-vis spectrophotometry techniques, respectively. Cu_2−xSe phase was confirmed by XRD pattern and spherical grains of 30 ± 4 - 40 ± 4 nm in size aggregated over about 130 ± 10 nm islands were seen by SEM images. Effect of annealing on crystallinity improvement, band edge shift and photoelectrochemical performance (under 80 mW/cm² light intensity and in lithium iodide electrolyte) has been studied and reported. Observed p-type electrical conductivity in copper selenide thin films make it a suitable candidate for heterojunction solar cells.     

紫外光电材料ZnO的反应溅射制备及研究

采用直流反应溅射法分别在Si(111),Si(001),及K4玻璃衬底上制备ZnO薄膜,研究了氧氩比、衬底温度以及退火处理对于晶体结晶质量的影响,发现生长过程中的退火处理提高了薄膜质量和晶面取向.通过优化生长条件,在衬底温度为350℃,氧氩比为1:2的条件下生长出了XRD半高宽为01°、C轴取向高度一致的ZnO薄膜.     

BSA-SDS-Ag聚合物纳米微粒的制备及水凝胶性质的研究(Ⅱ)

本文报道用X－射线衍射（XRD），TEM和FTIR光谱考察了在不同的制备条件下BSA－SDS－Ag的SDS－Ag聚合物纳米微粒的结构，形貌以及表面性质，随制备条件的不同，微粒的表面形貌有很大的差异。体系在微也液状态下，用甲醛作还原剂，可把银离子还原为单质，进而聚集成包裹型的团状微粒，微粒粒径32－60nm；微粒表面结构复杂，表明Ag^＋先后与蛋白质中的某些氨基酸残基产生化学键合，再还原为Ag粒，进而聚合成网状结构的聚合物。     

Na2CO3调质钙基脱硫剂硫化机理实验研究

对经Na2CO3溶液调质石灰石煅烧产物CaO的物理结构及硫化特性进行了研究,发现同等条件下调质后石灰石煅烧产物CaO(M-CaO)比未经调质的CaO(N-CaO)具有更高的钙转化率.利用XRD技术对CaO晶体结构进行了测定,通过比较二者的晶胞参数和晶格畸变度等并结合其孔特性,证实M-CaO之所以比N-CaO具有更高的钙转化率,是由于M-CaO比N-CaO具有更高的晶体缺陷浓度,使得在硫化反应过程中通过产物层的扩散具有更高的离子扩散率.     

Structural and electrical properties of lanthanum-substituted lead titanate ceramics

The effect of lanthanum substitution on the structural, dielectric and piezoelectric properties of lead calcium titanate (PCT) ceramics is studied. Samples with compositional formula Pb_{0.76? x} La _x Ca_0.24Ti_0.98Mn_0.02O₃ (PLCT) (x?=?0–0.08, in steps of 0.02) were prepared by the conventional dry ceramic technique. Phase and structural analysis was carried out using XRD and SEM respectively. X-ray analysis confirmed the formation of single-phase compound with tetragonal crystal structure. Dielectric properties were studied in detail as a function of frequency and temperature. The Curie temperature (T _C) and tetragonality (c/a) was found to decrease with increase in lanthanum content. The Curie temperature was also confirmed from the thermal-expansion behaviour of the sintered samples. Piezoelectric coefficients (d ₃₃, d ₃₁, g ₃₃, g ₃₁, g _h, d _h, k _t and k _p) were measured at room temperature. From this study it is found that La³⁺ substitution helps in the improvement of electro-mechanical anisotropy.     

利用红外光谱确定碱法分解粉煤灰的碳酸钠用量的实验研究

利用红外光谱研究了粉煤灰在用碳酸钠碱熔法分解前后的物相变化,发现： 碱熔前,粉煤灰的红外光谱主要显示莫来石和二氧化硅的特征吸收;碱熔后,粉煤灰(后统称熟料)的红外光谱主要表现为霞石的特征吸收。研究还对比了不同配比条件下,莫来石反应的完全程度。发现不同配比的粉煤灰熟料的红外光谱存在很大差异。在一定的碳酸钠用量范围内(粉煤灰∶碳酸钠＞1.2∶1时),其对应熟料的红外光谱主要为霞石的吸收峰,并表现有莫来石吸收残留,说明此配比条件下,莫来石尚未分解完全;当粉煤灰∶碳酸钠＝1.2∶1时,莫来石吸收消失,说明此配比条件下,莫来石可以分解完全,此时熟料的红外光谱中也未出现其他杂峰,证明此时熟料为霞石单一物相;当粉煤灰∶碳酸钠＜1.2∶1时,熟料的红外光谱中出现了碳酸盐的特征吸收,说明碳酸钠过量,同时,硅酸根的特征吸收峰也发生分裂,说明硅酸根的振动吸收峰增加,推测可能是碳酸钠过量后,霞石与碳酸钠发生反应,使霞石吸收过量的Na₂O,导致霞石的晶体结构发生变化。由此可以判定碱熔法分解粉煤灰的最佳配比为粉煤灰∶碳酸钠＝1.2∶1。X射线分析也得到了相同的结论。