共查询到18条相似文献,搜索用时 62 毫秒
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硒是生物生长所需的微量元素,但是过度摄入对人体是有害的。主要利用X射线光电子能谱仪(X-ray photoelectron spectroscopy, XPS)分析了湿法制备的黄铁矿去除水中Se(Ⅳ)的产物形态。利用X射线衍射仪(X-ray diffraction, XRD)和扫描电子显微镜(scanning electron microscope, SEM)对湿法球磨制备的黄铁矿进行了表征。XRD图谱表明该法制备的黄铁矿纯度较高,图谱中除了FeS2特征衍射峰外基本没有杂峰;SEM观测发现处理后的黄铁矿颗粒形状接近球形,尺寸在80~180 nm范围内。上述相关表征结果表明,湿法球磨制备的黄铁矿具有颗粒粒径更小、比表面积更大、反应活性更高等优点。实验结果表明, 在12 h反应时间内, 该法制备的黄铁矿颗粒对初始浓度为20 mg·L-1的Se(Ⅳ)去除效率达到95%。对该组实验数据进行动力学拟合,其结果满足准一级动力学方程, 表观反应速率常数kobs为0.26 h-1。XPS分析得到如下结论:(1)反应后黄铁矿中铁和硫的结合能均有所降低,即黄铁矿表面出现了新价态的铁元素和硫元素;(2)在反应后的黄铁矿表面有新形态的硒—Se(0)形成,同时也检测到了Se(Ⅳ)形态,但Se(0)的含量占主导优势。由此推测,黄铁矿去除水体中的Se(Ⅳ)以氧化还原为主, 同时伴随着吸附反应。该结果对于利用黄铁矿去除水体中具有高毒性的Se(Ⅳ)具有重要的理论意义和实际应用价值。 相似文献
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膨润土有机改性的FTIR和XRD研究 总被引:4,自引:2,他引:4
研究内容是制备有机膨润土以提高膨润土与有机相的相容性,同时观察膨润土的层状结构在有机化前后的变化情况。以钠基膨润土为原料,并用十八胺试剂作为有机插层剂取代膨润土层间的Na+,制得有机膨润土,且对其结构进行表征。FTIR和DTA-TG都证明有机插层剂已进入膨润土的层间;XRD表明膨润土的层间距由1.4增大到4.3 nm;从实验结果可知,钠化膨润土在各种指标上都比原钙基膨润土有显著的改善,如吸蓝量、膨胀容、胶质价、阳离子交换容量等。改性后的膨润土使其晶片层间的亲水环境改变为疏水环境以及增大晶片层间距离,从而有利于制备综合性能较好的复合材料。 相似文献
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以可溶性淀粉为原料,N,N′-亚甲基双丙烯酰胺为交联剂,采用反相悬浮聚合得到了一种交联淀粉微球(CSM)。为了深入了解交联淀粉微球(CSM)的降解过程,利用傅里叶变换红外光谱(FTIR)和X射线粉末衍射(XRD) 等光谱分析手段,对可溶性淀粉、CSM及其CSM在模拟肠液中不同时间的降解产物进行了分析。FTIR和SEM的研究结果表明, CSM在消化液中3 h内可稳定维持其交联结构,降解后3和12 h之间1 090 cm-1处的C—O—C弯曲振动峰减弱,酰胺的Ⅰ带吸收峰和Ⅱ带吸收峰强度的减弱说明了淀粉分子链被降解, 交联结构开始解聚,12 h后酰胺的Ⅰ带吸收峰和Ⅱ带吸收峰完全消失,说明交联结构已完全被除去;XRD结果表明,CSM在消化液中降解12 h后的情况与可溶性淀粉的降解情况相似,非结晶性部分被分解,结晶度随降解过程的进行而提高,但是仍然小于可溶性淀粉的结晶度。 相似文献
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XRD和FTIR对沸石合成机制的光谱学解析 总被引:1,自引:0,他引:1
以粉煤灰为原料,采用优化的水热晶化一步法合成沸石。比较晶化反应过程沸石产物CEC值及化学成分的变化,推断固液体系中物质转换及元素迁移方式和途径。借助XRD,SEM,FTIR等表征反应过程沸石的晶型变化及成核特性,提出可能存在的沸石生成机制。合成产物主要为NaP1型沸石,反应24h后CEC值最大为135mmol/100g。12h后,产物中初步发现NaP1沸石相特征峰和亚晶结构,48h后出现羟基方钠石的特征弱峰。沸石生成过程涉及到固液体系间的物质流动:碱熔融作用将粉煤灰组分侵蚀进入液相体系,为沸石形成提供了原料组分,而固相体系为沸石生长提供骨架结构,液相体系和固相体系分别为晶化反应的"源"和"汇",这是液相转化机制和固相转化机制的客观反映。 相似文献
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为探究断层构造作用对煤化学结构特征和微晶结构特征的影响,采用傅里叶变换红外光谱(FTIR)和X射线衍射(XRD)分析,对红庆梁矿和段王矿的原生煤及断层构造煤进行分析。结果表明,受断层构造作用影响,红庆梁、段王断层构造煤中苯环二取代、苯环四取代的含量明显大于原生煤,苯环三取代和苯环五取代的含量低于原生煤,断层构造煤中C—O—C伸缩振动、—CH2反对称弯曲振动、—CH3、—CH2和芳环—OH含量均多于原生煤,断层构造煤中醚C—O振动、芳烃CC、—CH和OH—π含量低于原生煤。红庆梁、段王断层构造煤的芳碳率fa是原生煤的1.01和1.03倍,芳环缩合度DOC是原生煤的1.01倍和3.7倍,CH2/CH3值是原生煤样的0.933倍和0.94倍,芳香度I分别是原生煤样的1.01倍和1.34倍。说明断层构造作用促使官能团和脂肪链脱落,增加煤的缩聚程度,降低煤中脂肪侧链的长度,增大芳香结构含量。XRD测试结果表明,原生煤和断层构造煤具有相近的矿物组分,断层构造作用未对煤... 相似文献
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X射线衍射法在泌尿系结石研究中的应用 总被引:3,自引:0,他引:3
欧阳健明 《光谱学与光谱分析》2006,26(1):170-174
泌尿系结石是一种世界范围的常见病、多发病。准确分析尿石的化学成分和物相,有助于了解泌尿系结石的形成机制。X射线衍射法(XRD)是进行泌尿系结石研究的最重要方法之一,用作定性分析时具有可靠性,用作定量分析时具有准确性,且检测简便迅速、灵敏度高、多组分和多晶态可一次性检测。文章综述了XRD在泌尿系结石定性和定量分析中的应用以及XRD与质子激发X射线发射光谱(PIXE)、X射线光电子能谱(XPS)和原子力显微镜(AFM)等联合分析尿石的研究进展。 相似文献
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表面波等离子体沉积类金刚石膜结构的Raman光谱和XPS分析 总被引:6,自引:0,他引:6
本文使用Raman光谱和X 射线光电子能谱 (XPS)的分析方法对表面波等离子体沉积的类金刚石(DLC)薄膜的结构进行了研究。采用 4峰的高斯解谱的方法对不同沉积时间的膜的Raman谱进行处理 ,并由此对膜中sp3键的百分含量PD 进行了定量计算 ;同时还采用 3峰的高斯解谱方法对不同沉积时间的膜的光电子能谱进行处理 ,也对膜中sp3键的百分含量进行了计算。两种方法均得到膜中sp3含量在 2 0 %~ 4 0 %之间 ,且随沉积时间的增加而增加。 相似文献
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化学复合镀Ni-P-SiO2镀层的XPS和AES分析 总被引:3,自引:0,他引:3
本文运用XEM、AES和XPS分析了Ni-P-SiO2镀层的表面形貌及镀层组成。研究显示:Ni-P-SiO2镀层表面光滑、均匀、光洁度好;其相对原子百分数为Ni74.56%,P12.38%,Si2.77%,Fe2.32%,O6.65%,镀层厚度为6.40um,镀层耐10%NaCl溶液和1%H2S气体的腐蚀能力较强。 相似文献
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俄歇电子能谱(AES)在表面微区元素分析方面优势明显,但是受基体效应的影响,其定量分析,特别是非单质材料表面元素含量分析的准确度差,X射线光电子能谱(XPS)的定量分析准确度较高。为了降低AES定量分析的误差,将XPS和AES两种分析技术联用,选择Pt-Co,Cu-Au和Cu-Ag三种二元合金样品进行了研究,利用样品的XPS定量分析结果对AES的定量分析所用相对灵敏度因子进行修正,将修正后的相对灵敏度因子用于其他不同组分比的样品的定量分析,以验证其分析准确性。结果表明,修正后的灵敏度因子在用于AES定量分析时相对误差明显降低,分析相对误差小于10%。为了解决AES定量分析在积分谱处理形式下选峰困难的问题,将积分谱进行微分化处理,并修正了微分谱的处理形式下的相对灵敏度因子,AES的定量分析相对误差降低到小于9%,表明在两种处理形式下都能得到较为准确的定量结果。修正后的相对灵敏度因子包含了基体效应尤其是背散射效应的影响,从而有助于降低AES定量分析的误差。说明借助XPS提高AES定量分析准确度的研究方法具有一定的可行性。 相似文献
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Samples of the iron oxides Fe0.94O, Fe3O4, Fe2O3, and Fe2SiO4 were prepared by high temperature equilibration in controlled gas atmospheres. The samples were fractured in vacuum and high resolution XPS spectra of the fractured surfaces were measured. The peak positions and peak shape parameters of Fe 3p for Fe2+ and Fe3+ were derived from the Fe 3p XPS spectra of the standard samples of 2FeO·SiO2 and Fe2O3, respectively. Using these parameters, the Fe 3p peaks of Fe3O4 and Fe1−yO are analysed. The results indicate that high resolution XPS techniques can be used to determine the Fe2+/Fe3+ ratios in metal oxides. The technique has the potential for application to other transition metal oxide systems. 相似文献
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Wei Huang Zhijun Zuo Peide Han Zhihong Li Tingdong Zhao 《Journal of Electron Spectroscopy and Related Phenomena》2009,173(2-3):88-95
In the article, the Co/Pd/TiO2, Co/TiO2 and Pd/TiO2 catalysts prepared by the impregnation and sol–gel method are studied by using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The result shows that Co2+ and metal Pd may act as the active center for the direct synthesis of acetic acid from CH4 and CO2 by a two-step reaction sequence. When the catalysts are prepared by the sol–gel, Co2+ can enter the crystal lattice of the TiO2, causing the phase transition from anatase to rutile at lower temperature, but existence of Pd2+ can prevent from the phase transition. When the catalysts are prepared by the impregnation, the phase transition is inhibited not only Co2+ but also Pd2+. 相似文献
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The process of ionic segregation in the surface layer induced by the thermal treatment of the NaNbO3 crystal was studied. The study of the as grown crystal and the crystal heated at 970 K in ambient air was carried out for comparison. The changes in the concentration of the elements within the surface layer were determined using XPS measurements. The AFM technique was applied to determine the surface morphology related to nano-scale transformation. The possibility of appearance of the Ruddlesden–Popper phases was detected by the XRD test. The change in the features of the electric permittivity, the loss tangent, and the electric conductivity was ascribed to the marked participation of the chemically modified surface layer in the measured effective electrical properties. 相似文献
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V. Venckutė J. Miškinis V. Kazlauskienė T. Šalkus A. Dindune Z. Kanepe 《Phase Transitions》2013,86(5):438-451
LiFeP2O7 and Li0.9Fe0.9Ti0.1P2O7 were synthesised by solid-state reaction and ceramics were sintered. The structure of compounds was studied in the temperature range 300–700 K by X-ray diffraction. Ceramics’ surfaces were investigated by scanning electron microscope. Binding energies of Fe 2p, P 2p and O 1s core levels at ceramics’ surfaces have been determined by X-ray photoelectron spectroscopy and different valence states of Fe and P were detected. Elemental compositions of the compounds were studied by energy dispersive X-ray spectrometer. Impedance spectroscopy was performed in the frequency range 10 Hz–3 GHz and in the temperature interval 400–700 K. The changes of the activation energy of ionic conductivity at 528 and 550 K for LiFeP2O7 and Li0.9Fe0.9Ti0.1P2O7, respectively, were found. The phenomena can be related to disordering in the unit cells of the compounds. 相似文献
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酒石酸钠调控草酸钙晶体生长的SEM,XRD和FTIR研究 总被引:2,自引:0,他引:2
采用扫描电镜(SEM)、X射线衍射(XRD)和傅里叶红外光谱(FTIR)研究了凝胶体系中尿抑制剂酒石酸钠(Na2tart)的浓度和结晶温度对草酸钙(CaOxa)晶体生长的影响。当Na2tart浓度为0.01 mol·L-1时,体系中主要生成棱角尖锐的蔷薇花状一水草酸钙(COM)聚集体,二水草酸钙(COD)含量小于5%,此时XRD图谱上主要为归属于COM的(101),(020)和(202)晶面的衍射峰,FTIR光谱中COM晶体的羧基不对称伸缩振动νas(COO-)和对称伸缩振动νs(COO-)分别为1 618和1 317 cm-1。当Na2tart浓度增加到0.10和0.50 mol·L-1时,COD百分含量分别增加至10%和50%,COM晶体的比表面积减小。COD含量增加后,XRD图谱上归属于COD的(200),(211),(411)和(213)晶面的衍射峰增强。环境温度的影响比浓度的影响更为显著。高温(>47 ℃)有利于COM生成,而低温(<27 ℃)有利于Na2tart诱导COD。FTIR光谱中COD的νas(COO-)和νs(COO-)分别为1 647.6和1 327.7 cm-1。 相似文献
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This work is a comparative study of two FTIR techniques applied to urinary stones analysis: single reflection diamond attenuated total reflection (ATR) and KBr pellet transmission (KPT). We show that the two methods allow the identification of all stone components. The ATR technique is more useful and rapid to identify the species without sample pretreatment. Nevertheless, KPT is more appropriate for components determination in urinary stones. These techniques were applied to the study of a series of 313 calculi. The stone constituents were first identified by ATR, and in a second step, the proportion of each species present in the stone was determined by KPT in whole‐stone mixture. The results obtained showed the presence of 11 different components classified as follows with the frequency of detection in the stones studied: calcium oxalate monohydrate (whewellite), 78.9%; carbapatite, 33.9%; calcium oxalate dihydrate (weddellite), 24%; uric acid anhydrous, 19.2%; ammonium hydrogen urate, 7%; struvite, 4.8%; cystine, 1%; ammonium sodium urate and other phosphates (amorphous carbonated calcium phosphate, brushite, whitlockite), each in less than 1%. 相似文献