金刚石颗粒表面Cr金属化及薄膜间界面扩散反应的研究

运用直流磁控溅射法可在金刚石颗粒表面沉积150nm的金属Cr层.在超高真空条件下,经300-600℃的热退火处理,可促进Cr膜与金刚石基底间的界面扩散和反应.利用俄歇电子能谱研究了Cr/金刚石颗粒界面的结合状态,发现Cr与金刚石薄膜发生了强烈的界面扩散,Cr元素渗入金刚石层达90nm,并在界面上发生化学反应形成Cr的碳化物层.对界面扩散反应动力学的研究表明,Cr/金刚石界面扩散反应的表观活化能为38.4kJ/mol,界面扩散反应主要由碳的扩散过程控制.热处理温度越高,界面扩散及反应越显著,但不利于碳化物层生成的氧化反应速度也会有所增加,界面反应产物从Cr₂C₃转变为Cr₂C物种.延长热处理时间有利于金属碳化物的生成,同样导致界面反应产物从Cr₂C₃转变为Cr₂C物种.     

不同压力下碳氢体系低压金刚石的非平衡定态系列相图

系统压力是低压金刚石薄膜生长实验中重要的实验参数，如果采用合理的计算方法定量化地预测出压力对金刚石薄膜生长条件的影响，则可以直接用于指导其实验研究。本文报道根据非平衡热力学耦合理论模型绘制了C-H体系金刚石生长投影相图，经与大量实验结果比较相一致，并系统地计算了压力变化的碳氢体系金刚石生长非平衡定态截面相图，得到了金刚石生长区随压力变化的规律。计算得到的相图与经典平衡相图有本质不同，均有金刚石生长区，因而可以合理解决金刚石低压下连续生长而石墨被腐蚀与经典平衡热力学之间的矛盾。本文的计算结果可以为金刚石生长实验提供定量化的压力条件的选择和优化实验条件。     

金刚石表面的氟化作用

金刚石表面的氟化作用Ｓｍｅｎｔｋｏｗｓｉｋ和Ｙａｔｅｓ报道了一种金刚石表面化学功能化的有效方法，该法是用Ｘ光照射金刚石表面覆盖的碘代全氟烃，产生的全氟烃自由基与金刚石表面化学键合，然后热分解使表面形成高熟稳定的强Ｃ－Ｆ健。金刚石表面化学功能化将大大提...     

纳米晶掺钇硬质合金粉末的制备

采用高能球磨法制备了纳米晶掺Y硬质合金粉末。用XRD，SEM和DTA等分析检测手段，研究了纳米晶掺Y硬质合金粉末的结构、形貌和相的变化。结果表明：高能球磨45h，可获得晶粒尺寸约为8nm的掺Y硬质合金粉末；微量Y的加入，有利于硬质合金粉末晶粒的细化；在25～45h范围内，随着高能球磨时间的延长，粉末晶粒尺寸减小，且掺Y硬质合金粉末的晶粒尺寸比未掺Y的硬质合金粉末晶粒尺寸要细一倍；高能球磨25h，粉末中Co的X射线衍射峰消失。高能球磨掺Y硬质合金粉末的DTA曲线在626℃出现了1个尖锐的放热峰。高能球磨掺Y硬质合金粉末固结之后，其合金晶粒细小，机械性能较好。     

去钴深度的测定及其对硬质合金性能的影响

研究了原子吸收光谱法和辉光放电光谱仪定量测定硬质合金去钴深度的新技术。实验得到了腐蚀时间与硬质合金去钴深度、表面显微硬度的关系曲线,分析了去钴深度对硬质合金表面形貌的影响。     

氢气流量对金刚石膜生长的影响研究

研究了电子辅助热灯丝法生长金刚石厚膜过程中氢气流量对沉积速度和膜品质的影响。随氢气流量从100增加到750cm^3/min，金刚石膜的沉积速率单调上升，但金刚石膜品质不断下降，从750到1000cm^3/min，金刚石膜沉积速率下降，但金刚石膜品质随氢气流量增加而提高。拉曼光谱和电子顺磁共振谱研究发现，在所制备的金刚石膜中含有替代形式的氮，氮含量随氢气流量的增加而减小，1000cm^3/min流量下沉积的金刚石膜的含氮量仅为100cm^3/min流量下沉积的金刚石膜的1／40。     

质子交换膜燃料电池气体扩散层的研究进展

气体扩散层在燃料电池中起到支撑催化层、收集电流、传导气体和排出反应产物水的重要作用。本文对气体扩散层的组成、制备方法及参数优化的实验研究现状进行了综述，介绍了现有的气体扩散层性质的各种表征方法，指出了研究中存在的问题，提出了气体扩散层的进一步改进方向。     

液相电化学沉积类金刚石薄膜的研究进展

采用电化学沉积法开展液相中类金刚石薄膜的制备工艺和理论的研究,对于完善类金刚石薄膜的合成技术,开拓类金刚石薄膜的应用领域,具有很重要的理论意义和实用价值。本文概述了液相电沉积技术的基本原理和方法,重点从四个方面介绍了电化学方法制备类金刚石薄膜的研究进展,总结了该方法所制备样品的性能,并对可能的反应机制作了综合性的阐述,最后对液相电沉积类金刚石薄膜的发展前景进行了展望。     

金刚石和类金刚石的常温常压电化学合成

采用线性扫描伏安(LSV)\, X射线粉末衍射和拉曼光谱等方法对电化学还原法从CCl4\|NaCl\|\[BMIM\]BF4体系合成金刚石的可能性进行了研究. LSV研究结果表明, CCl4可在白金研究电极表面直接还原而不需要NaCl作为电子媒介. 采用恒电势电解的方法可在白金研究电极上获得黑色还原产物. 采用X射线粉末衍射和拉曼光谱对研究电极表面形成的黑色产物进行了表征, 在XRD图谱中可观察到金刚石的特征峰, 在拉曼光谱中1 332 cm-1附近可观察到金刚石结构的特征吸收峰, 表明产物中存在金刚石相. 这些结果表明, 采用电化学方法在常温常压下将CCl4转化为金刚石的方法是可行的.     

甲醇在热阴极DC-PCVD方法制备金刚石膜过程中的作用

采用热阴极DC－PCVD方法制备了金刚石膜，研究了甲醇对放电状态和金刚石膜生长特性的影响。结果表明，通入适量的甲醇有利于稳定辉光放电状态，保持阴性清洁，提高膜的生长质量。用扫描电镜和拉曼光谱等测试手段对金刚石膜的生长特性进行了分析。     

High Pressure Behavior of Mercury Cyanamide HgCN2

Using the diamond anvil cell technique, angle‐dispersive X‐ray diffraction and Raman spectroscopy were employed to study the high pressure behavior of mercury cyanamide. Its decomposition under pressure starts at 1.9 GPa and is not completed even up to 10 GPa. The decomposition product α‐Hg transforms to β‐Hg during 7–10 GPa, while the C/N residual is not detectable by X‐ray diffraction. The zero pressure bulk modulus of mercury cyanamide is estimated as 38.5 GPa.     

Microstructure characteristics and shear properties of welding bonding of W/Al dissimilar metals with copper transitional layer

Commercial pure wrought tungsten and 1060 pure aluminum can be joined by using induction‐heat deposition (IHD) welding with commercial pure copper transitional layer. The microstructures of W/Cu/Al interfaces have been studied by means of scanning electron microscope, energy dispersive X‐ray, and X‐ray diffraction. Results show that copper as the transitional metal could form good interfaces with both tungsten and aluminum by IHD under proper processing parameters. The metallic bonding of W/Cu obtained by Cu and W mutual diffusing at a quite limited range without any intermetallic compounds, while eutectic of α(Al)/θ(CuAl₂) makes up Cu/Al interface. The average shear strength of W/Cu and Cu/Al interfaces are about 170 MPa and 55 Mpa, respectively, at room temperature. Copyright © 2012 John Wiley & Sons, Ltd.     

Zinc Coordination Complex for use in Uniform ZnS Microflowers Synthesis

Uniform snowball zinc sulfide (ZnS) microflowers with nanosheet covering were synthesized using the one step reaction of zinc coordination compounds with thiourea at 160 °C for 24 h. X‐ray single crystal diffraction, electron microscopy, energy‐dispersive X‐ray spectrometry, and X‐ray diffraction were used to characterize the products. The flower‐like ZnS crystals may have some application in catalyst or solar cell devices. This work is also expected to be applied in the fabrication of other transition metal sulfide crystals with special morphology.     

Extraction of phenolic compounds from water samples by dispersive micro‐solid‐phase extraction

In this article, the use of magnetically separable sorbent polyaniline/silica‐coated nickel nanoparticles is evaluated under a dispersive micro‐solid‐phase extraction approach for the extraction of phenolic compounds from water samples. The sorbent was prepared by in situ chemical polymerization of aniline on the surface of silica‐modified nickel nanoparticles and was characterized by Fourier transform infrared spectroscopy, transmission electron microscopy, X‐ray powder diffraction, scanning electron microscopy, energy‐dispersive X‐ray spectrometry, and vibrating sample magnetometry. Effective variables such as amount of sorbent (milligrams), pH and ionic strength of sample solution, volume of eluent solvent (microliters), vortex, and ultrasonic times (minutes) were investigated by fractional factorial design. The significant variables optimized by a Box–Behnken design were combined by a desirability function. Under the optimized conditions, the calibration graphs of analytes were linear in a concentration range of 0.02–100 μg/mL, and with correlation coefficients more than 0.999. The limits of detection and quantification were in the ranges of 10–23 and 33–77 μg/L, respectively. This procedure was successfully employed in the determination of target analytes in spiked water samples; the relative mean recoveries ranged from 96 to 105%.     

Effect of temperature on CO2 corrosion of carbon steel

This work investigates the effect of temperature on the corrosion product layer of carbon steel exposed to a CO₂‐containing solution. The measurement techniques, such as scanning electron microscopy with energy dispersive spectrometry, X‐ray diffraction, and X‐ray photoelectron spectroscopy, were used to systematically characterize the morphology and composition of the corrosion product layer. The corrosion rates were calculated by weight loss method. The corrosion mechanisms as a function of temperature are studied and discussed. The results showed that temperature is an important factor in the corrosion rate of carbon steel. Copyright © 2009 John Wiley & Sons, Ltd.     

Effect of pressure on the growth of boron and nitrogen doped HFCVD diamond films on WC–Co substrate

Boron and nitrogen compounds are added in the acetone/hydrogen gas mixture to deposit hot filament chemical vapor deposition (HFCVD) diamond films on the cobalt cemented tungsten carbide (WC–Co) substrate under the pressure of 1–4 kPa. The as‐deposited diamond films are characterized by field emission scanning electron microscope (FESEM), atomic force microscopy (AFM), X‐ray diffraction (XRD) spectroscopy and Raman spectroscopy. The results reveal that the surface morphology, growth rate, structure and quality of the diamond films vary with the pressure and the type of the impurity addition. The diamond grains tend to develop into the nanometer scale with the decrease of the pressure. However, adding of boron or nitrogen impurities in the gas mixture will weaken the nanocrystallization effect by reducing the carbon supersaturation. Density functional theory (DFT) calculations indicate that co‐adsorption of B and N containing radicals can favor the adsorption of CH₃ on diamond (100) surface. Thus, at low pressure of 1 kPa, large grained cubic (100) facet diamond rather than typical nanometer diamond is produced for B–N co‐addition gas mixture. The present results appear to be useful to efficiently synthesize high quality doped diamonds with desirable properties for mechanical application. Copyright © 2015 John Wiley & Sons, Ltd.     

Energy dispersive X-Ray fluorescence determination of thorium in phosphoric acid solutions

Energy dispersive X-ray fluorescence studies on determination of thorium (in the range of 7 to 137 mg/mL) in phosphoric acid solutions obtained by dissolution of thoria in autoclave were made. Fixed amounts of Y internal standard solutions, after dilution with equal amount of phosphoric acid, were added to the calibration as well as sample solutions. Solution aliquots of approximately 2–5 µL were deposited on thick absorbent sheets to absorb the solutions and the sheets were presented for energy dispersive X-ray fluorescence measurements. A calibration plot was made between intensity ratios (Th Lα/Y Kα) against respective amounts of thorium in the calibration solutions. Thorium amounts in phosphoric acid samples were determined using their energy dispersive X-ray fluorescence spectra and the above calibration plot. The energy dispersive X-ray fluorescence results, thus obtained, were compared with the corresponding gamma ray spectrometry results and were found to be within average deviation of 2.6% from the respective gamma ray spectrometry values. The average precision obtained in energy dispersive X-ray fluorescence determinations was found to be 4% (1σ). The energy dispersive X-ray fluorescence method has an advantage over gamma ray spectrometry for thorium determination as the amount of sample required and measurement time is far less compared to that required in gamma ray spectrometry.     

Ag/Au Alloy LSPR Engineering by Co‐deposition of RF‐Sputtering and RF‐PECVD

Silver‐Gold alloy/diamond like carbon (Ag‐Au/DLC) nanocomposite films were prepared by co‐deposition of RF‐sputtering and RF‐PECVD on glass substrates by using acetylene gas and silver‐gold target. The deposition process was carried out at room temperature in one minute with the variable parameters of initial pressures and RF powers. X‐ray diffraction analysis demonstrated the formation of Ag/Au alloy nanoparticles with a face‐centered cubic (FCC) structure. Localized surface plasmon and optical properties of Ag‐Au alloy nanoparticles were studied by UV‐visible spectrophotometry which showed that increasing RF power and initial pressure cause a redshift in all samples. Moreover, the effect of RF power and initial pressure on the size and shape of nanoparticles were studied by 2D Atomic force microscopy images. Energy dispersive X‐ray spectroscopy revealed the formation of Ag‐Au/DLC nanoparticles and the percentages of C, Ag, Au and O in all samples. The applied method for Ag/Au alloy preparation is the one step and low‐cost method which makes the samples ready for sensing application.     

Novel nano molten salt tetra‐2,3‐pyridiniumporphyrazinato‐oxo‐vanadium tricyanomethanide as a vanadium surface‐free phthalocyanine catalyst: Application to Strecker synthesis of α‐aminonitrile derivatives

Efficient and recyclable novel nano tetra‐2,3‐pyridiniumporphyrazinato‐oxo‐vanadium tricyanomethanide, {[VO(TPPA)][C(CN)₃]₄}, as a vanadium surface‐free phthalocyanine‐based molten salt catalyst was successfully designed, produced and used for the Strecker synthesis of α‐aminonitrile derivatives through a one‐pot three‐component reaction between aromatic aldehydes, trimethylsilyl cyanide and aniline derivatives under neat conditions at 50 °C. This catalyst was well characterized using Fourier transform infrared, UV–visible, X‐ray photoelectron and energy‐dispersive X‐ray spectroscopies, X‐ray diffraction, scanning and high‐resolution transmission electron microscopies, inductively coupled plasma mass spectrometry and thermogravimetric analysis. The catalyst can be simply recovered and reused several times without significant loss of catalytic activity.     

Synthese und Untersuchung von kohlenstoff‐ und stickstoffzentrierten (Z) trigonal‐prismatischen Wolframclustern des Formeltyps A[W6ZCl18]

Synthesis and Characterization of Carbon‐ and Nitrogen‐Centered (Z) Trigonal Prismatic Tungsten Clusters of the Formula Type A[W₆ZCl₁₈] Solid state reactions of tungsten(IV) chloride and carbodiimides (cyanamides) of lithium, sodium, calcium and silver yielded black crystalline powders of centered (Z) trigonal‐prismatic tungsten cluster compounds having the general formula A[W₆ZCl₁₈] with A = Li, Na, Ca, Ag and Z = C, N. Crystal structures of the corresponding compounds were investigated by powder and single‐crystal X‐ray diffraction. The nature of the central atom was studied by mass spectrometry and nuclear magnetic resonance spectrometry. It turned out that the central atom can be C (in the case of the lithium and sodium compound) or N (in the case of the sodium and calcium compound).