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1.
Secondary ion mass spectrometry (SIMS) and glow discharge mass spectrometry (GDMS) were used to determine the impurity concentrations
of hydrogen, carbon, nitrogen, and oxygen elements in Cu films, and the results of SIMS and GDMS were carefully interpreted.
The Cu films were deposited on Si (100) substrates at substrate bias voltages ranging from 0 V to −150 V using a non-mass
separated ion beam deposition method. From the results of SIMS using a Cs− ion beam, as a whole, many high intensity peaks were observed in the Cu films deposited without substrate bias voltage. From
the quantitative GDMS results, these peaks were determined to be signals detected as a cluster state such as CxHx, OxHx, CxOxHx. Therefore, using a combination of these dominant impurities, all the unknown peaks observed in the SIMS results could be
interpreted. Moreover, it was found that the dominant impurities having a great influence on the film purity were hydrogen,
carbon, nitrogen, and oxygen. 相似文献
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黄柱成蔡威易凌云姜雄王林胡程飞肖华荣钟荣海 《中国有色金属学报》2020,30(12):2980-2988
采用钒钛磁铁矿为氧载体对生物质的气化转化行为进行研究,系统考查转化温度、氧载体比例等关键因素的影响。借助热重-差热分析(TG-DSC)、傅里叶红外光谱(FTIR)、气相色谱-质谱联用(GC-MS)、X射线衍射(XRD)等分析测试手段对气化过程产物特性进行表征并揭示生物质转化机制。结果表明:温度升高有利于生物质的气化转化,所得气相产率和气相产物中CO及H2占比皆显著增大;气相产物的释放主要集中在转化过程的前20min,CH4、C2H4和CO2等成分的析出率先达到峰值,CO和H2的析出率达到峰值略有滞后;氧载体的加入可加快生物质各基团的裂解,促进固、液相产物向气相产物的转化。生物质的裂解转化历程可概括为—OH、—C=O、—C=C→—CH3→—CH→—CO,此过程中钒钛磁铁矿逐渐被还原为金属化产品(金属化率可达80%以上)。 相似文献
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目的: 建立HPLC-UV法测定大鼠血浆中S-腺苷蛋氨酸(S-Adenosylmethionine, SAMe)浓度,并用此法研究静脉给药后的大鼠体内药代动力学特征。方法: 色谱柱:大连依利特Kromasil C18 柱(4.6 mm×200 mm, 5 μm),流动相:甲醇∶0.3%三氟乙酸溶液(含1%磷酸二氢钠盐)=2∶98,等浓度洗脱,紫外检测波长:260 nm,流速:0.6 mL/min,柱温:30 ℃。大鼠(n=6)经静脉给予 140 mg/kg SAMe并测定血浆药物浓度,采用DAS 2.0 软件进行药动分析。结果: SAMe能完全分离,线性范围:10~2000 μg/mL,回归方程为Y=30241X+256204,r=0.9991, 日内精密度分别为 2.6%,3.6%,3.9%;日间精密度分别为 6.3%,4.9%,7.9%;回收率分别为107%,101%,98.3%。静脉给予 140 mg/kg SAMe药动学参数,血浆药物浓度-时间曲线下面积AUC(0-t)为(569.52±174.87) mg·L-1·h,半衰期(t1/2)为(2.03±0.96) h,清除率(CL)为(0.21±0.13)L·h-1·kg-1,表观分布容积(Vd)为(0.53±0.31) L/kg。结论: 本实验方法专属性好,灵敏度高,可靠性强,可用于SAMe药动学分析。 相似文献
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A technique including direct acid leaching,vanadium precipitation with alkaline,sodium hydroxide releaching,impurity removing by adjusting pH value,precipitation vanadium with ammonium chloride,and vanadium pentoxide by roasting steps was proposed according to the characteristic of Xichuan clay vanadium mineral.The factors influencing leaching vanadium such as temperature and the concentration of sulfuric acid were investigated and optimized.The experimental results indicate that the extract ratios of V2O5 can reach 94% and 92% at a sodium chlorate ratio of 3% and a manganese dioxide ratio of 3%,respectively.A completely chemical precipitation method was adopted to decontaminate and enrich the vanadium in the acid leaching solution.The X-ray diffraction (XRD) pattern and the purity analysis of vanadium pentoxide indicate that the purity of final vanadium pentoxide can reach 99% and meet the standard specifications.The total recovery can reach about 75%.The technique has the characteristics of simplicity,less investlnent,and more environment safety as compared with the traditional salt roasting method. 相似文献
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《中国有色金属学会会刊》2020,30(6):1687-1696
The effects of CaO content, MgO content and smelting temperature on the vanadium behavior during the smelting of vanadium titanomagnetite metallized pellets were investigated. The thermodynamics of reduction and distribution of vanadium was analyzed and the high-temperature smelting experiments were carried out. The thermodynamic calculations show that the distribution ratio of vanadium between the slag and the hot metal decreases with the increments of CaO and MgO content in the slag as well as the increase of the smelting temperature. The smelting experiments demonstrate that the vanadium content in iron and the recovery rate of vanadium in pig iron increase as the CaO content, MgO content and smelting temperature increase, whereas the vanadium distribution ratio between the slag and iron tends to decrease. Moreover, the recovery rate of vanadium in pig iron has a rising trend with increasing the optical basicity of the slag. The addition of MgO in the slag to increase the slag optical basicity can not only improve the vanadium reduction but also promote the formation of magnesium-containing anosovite, which is beneficial to following titanium extraction. 相似文献
6.
制备V8C7和Cr3C2粉末的传统方法是将V(Cr)氧化物与固体碳球磨混合﹑二次碳化而成,此方法存在碳化温度高﹑粉末粒度粗等缺点。本文介绍了几种国外制备超细V8C7和Cr3C2粉末的制备方法。 相似文献
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目的: 研究盐酸伊伐布雷定片在中国健康志愿者中的单次及连续多次给药药动学特征。方法: 12例受试者采用随机开放二重3×3拉丁方试验设计,研究单次及连续多次给药药动学特征;采用LC-MS/MS法测定血浆中伊伐布雷定及其活性代谢产物S-18982的药物浓度。药动学参数采用WinNonlin软件计算。结果: 单次(5、10、15 mg)给药后伊伐布雷定的主要药动学参数:Cmax分别为(19±10)、(47±24)、(79±41) μg/L,tmax分别为(0.7±0.5)、(0.6±0.3)、(0.5±0.1) h; AUClast分别为(58±32)、(138±83)、(189±115) μg·h·L-1;AUCinf分别为(59±32)、(140±84)、 (191±116) μg·h·L-1;其活性代谢产物S-18982的主要药动学参数:Cmax分别为(3.1±1.2)、(7.9±2.8)、(15.0±5.4) μg/L; tmax分别为(1.1±0.8),(0.8±0.4),(0.6±0.1) h;AUClast分别为(17±8)、 (47±19)、 (76±29) μg·h·L-1;AUCinf分别为(20±8)、(52±21), (85±30) μg·h·L-1。连续多次给药 5 mg 后伊伐布雷定的主要药动学参数:Cmax(20±7) μg/L;tmax(1.0±0.7) h; AUClast( 67±32) μg·h·L-1; AUCinf (69±33) μg·h·L-1;其活性代谢产物S-18982的主要药动学参数:Cmax(4.5±1.3) μg/L;tmax(1.1±0.8) h; AUClast (34±11) μg·h·L-1; AUCinf (39±13) μg·h·L-1。结论: 单次5~15 mg 给药后,伊伐布雷定的体内过程符合一级线性动力学过程,代谢产物S-18982的体内过程呈非线性;连续多次 5 mg 给药后,母药和代谢产物的血药浓度第5天可达稳态,母药在体内无蓄积,代谢产物存在蓄积现象。 相似文献
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Joon Hyung Shim Joong Sun Park Timothy P. HolmeKevin Crabb Wonyoung LeeYoung Beom Kim Xu TianTurgut M. Gür Fritz B. Prinz 《Acta Materialia》2012,60(1):1-7
This study reports spectrometric and spectroscopic evidence indicating a pronounced role of surface grain boundaries in enhancing oxygen incorporation on oxide ion conducting ceramic yttria stabilized zirconia (YSZ). Oxygen isotope exchange measurements were carried out using high spatial resolution (50 nm) secondary ion mass spectrometry (SIMS) under cathodically biased conditions as well as on bare YSZ surface. Surface mapping of the 18O distribution by SIMS clearly shows high activity at surface grain boundaries, suggesting that these boundary regions provide preferential pathways for oxygen incorporation into YSZ in both cases, albeit the effect is less pronounced without bias. The results are supported by a.c. impedance spectroscopy measurements conducted on polycrystalline YSZ membranes with surface grains engineered for different sizes, which indicate that smaller grains (i.e. higher grain boundary densities) exhibit lower electrode impedances. These results open up the possibility of engineering nanostructured YSZ surfaces containing a high density of grain boundaries to achieve enhanced performance of electrochemical devices, particularly for solid oxide fuel cells operating at low temperatures. 相似文献
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Comparative study of LNO, LSCO and LSMO as electrode layers for microelectronic capacitors by dynamic SIMS 总被引:1,自引:0,他引:1
Chemical solution-deposited multilayer systems of SrTiO3 (STO)/X/Pt/TiO2/SiO2/Si [where X=LaNiO3 (LNO), La0.5Sr0.5CoO3 (LSCO), La0.7Sr0.3MnO3 (LSMO)] were investigated by dynamic secondary-ion mass spectrometry (SIMS). The STO layer is intended to serve as a dielectric layer for a capacitor, the conducting layers ‘X’ are a buffer layer intended to eliminate fatigue effects, which usually occur at the Pt/STO interface. Depth profiles of the main components were obtained, revealing intense diffusion processes, which must have occurred during the deposition/crystallisation processes. Furthermore, Al impurities from the substrate, most probably originating from the Pt-sputter process, are preferentially found at the interfaces. Ti is found to diffuse from the (isolating) STO layer into the conductive ‘X’ oxide layers, where a region of constant concentration is observable in all three sample systems. 相似文献
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钒钛磁铁矿提钒尾渣浸取钒 总被引:1,自引:0,他引:1
采用硫酸−氢氟酸−次氯酸钠组合浸出体系浸取钒钛磁铁矿提钒尾渣中的钒,研究浸出过程中试剂浓度、浸出液固比、浸出温度、浸出时间、物料粒度对钒浸出率的影响。结果表明:钒的浸出率随试剂浓度、液固比、温度和时间的升高而增大;当矿物粒度小于0.20 mm时,钒浸出率有随矿物粒度变小而减小的趋势。在物料粒度0.15~0.25 mm、初始硫酸浓度150 g/L、初始氢氟酸浓度30 g/L、次氯酸钠加入量为矿量1.5%、矿浆液固比6:1、浸出温度90 ℃、浸出时间6 h、搅拌速度500 r/min的条件下,钒的浸出率可达85%以上。 相似文献
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为了提高转炉钒渣提钒回收率,提出钙镁复合焙烧-酸浸提钒新工艺,研究MgO/(CaO+MgO)摩尔比、焙烧和浸出工艺参数对钒回收率的影响。结果表明:当焙烧添加剂CaO完全被MgO取代时,钒浸出率降低,由88%降至81%;然而,采用CaO/MgO复合焙烧却能强化钒的浸出。当MgO/(CaO+MgO)的摩尔比为0.5:1时,钒浸出率达到94%。XRD和SEM-EDS结果表明,CaO/MgO复合焙烧添加剂能强化焙烧过程中可溶性钒酸盐的生成,并通过减少硫酸钙沉淀的生成改善浸出过程的动力学条件。 相似文献
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Ferritic steels in steam turbines for the power industry operate without coatings in the temperature range of 590–600 °C. For higher operation temperatures the substrate has to be replaced or coated, otherwise the ferritic substrate at a temperature of 650 °C develops thick oxide scales that promote sudden turbine blade failure. The advantage of the use of coatings is that coated ferritic steels are much less expensive than austenitic stainless steels or nickel base superalloys. In order to go forward to coatings design, the Thermo‐Calc code was used as a base for the mass spectrometry (MS)‐data. Thermogravimetry (TG)–MS experiments were conducted in a closed steam loop in order to obtain information about the oxyhydroxides formation as reaction between coatings and steam. From those results the role of the different coating element could be established and optimized for the coating durability. An oxidation mechanism based on the TG–MS results is given. 相似文献
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钒是重要的战略金属,萃取法是当前溶液中钒分离富集的主要方法之一。本文从含钒溶液的特点及溶液中钒的存在形态出发,阐述了溶液中钒分离富集的难点所在,综述了含钒溶液萃取分离富集钒的研究进展,对萃取机理及工艺影响因素等进行了总结分析,展望了萃取法的发展趋势。有机磷类萃取剂、有机胺类萃取剂、长链醇萃取剂、羟肟类萃取剂等传统的有机溶剂萃取体系应用相对成熟,但有机溶剂萃取体系普遍存在易挥发、有毒有害、易燃易爆等问题;近年来,双水相、三液相、离子液体等新型绿色萃取体系受到越来越多的关注;乳状液膜、微乳液、支撑液膜、聚合物包容膜等液膜萃取在缩短萃取流程、降低生产成本、提高钒分离效率及钒产品质量等方面有较大发展空间。 相似文献
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目的: 建立LC-APCI-MS/MS法测定大鼠胆汁、尿液和粪便中维氨酯的浓度,对该药在大鼠体内的排泄规律进行研究,为临床试验提供依据。方法: 生物样本经处理后,采用Agilent TC C18色谱柱,甲醇-水-甲酸(93∶7∶0.1)为流动相,辛伐他汀为内标,在三重四极杆串联质谱仪上,采用大气压化学离子化(APCI)、正离子方式选择性离子监测模式,维氨酯和内标的检测离子分别为m/z448283和m/z419285,分别测定尿液、胆汁和粪便中原型物的含量。结果: 胆汁、尿样、粪便中维氨酯的回收率均大于89%,日间和日内的变异系数均小于10%。胆汁和尿液中维氨酯在0.0808~40.4ng/mL浓度范围内线性关系良好(r=0.9972和0.9949),粪便中维氨酯在0.2525~101ng/mL浓度范围内线性关系良好(r=0.9990),维氨酯的定量下限为0.2pg,方法符合生物样品分析要求。维氨酯在粪便中72h内、在尿液中96h内、在胆汁中24h内原型药的平均累积排泄量分别为12.9%、0.003%、0.0001%。结论: 该方法灵敏度高,专属性强,样品前处理简便,分析速度快,可满足大鼠排泄研究中药物浓度测定的要求,大鼠灌胃给药(5mg/kg)后维氨酯从尿液和胆汁中排泄的原型药物很少。 相似文献
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K. K. Soni D. B. Williams J. M. Chabala R. Levi-Setti D. E. Newbury 《Oxidation of Metals》1992,37(1-2):23-37
Oxidation behavior of Al-Li alloys, containing a high volume fraction of Ferich second-phase particles, was studied at 530°C and 200°C. Morphological studies showed enhanced growth of Li-rich oxides in the vicinity of the insoluble second-phase particles. Microanalytical depth profiling of the oxide layer with a high resolution scanning ion microprobe indicated rapid diffusion and subsequent oxidation of Li at the free surface. Examination of the alloy surface after removal of the oxide layer suggested that the initial oxide growth occurred in the lateral direction. Secondary ion image depth profiling of the alloy surface after oxide removal revealed Li segregation to the alloy/second-phase interface, supplying Li for accelerated oxidation. A microstructural model of the oxidation process in this case is presented. 相似文献