Parametric study of atmospheric-pressure diamond synthesis with an inductively coupled plasma torch

Polycrystalline diamond coatings have been deposited run molybdenum and silicon substrates using an inductively coupled, atmospheric-pressure plasma torch. Growth rates are on the order of 10 hr. The inductively coupled plasma reactor is found to produce a uniform, well-characterized growth environment for experimental and computational .study of the atmospheric-pressure diamond growth regime. Growth morphology is found to be sensitive to reactor conditions such as substrate surface temperature and methane-to-hydrogen feed ratio. An experimental parametric study of these variables is performed and the resultant growth analyzed by scanning electron microscopy, Raman spectroscopy, and X-ray diffraction Spectroscopic analysis of the gas phase is also performed. Results indicate that the, substrate temperature range over which diamond growth occurs shifts toward higher temperatures as the methane-to-hydrogen feed ratio is increased. The growth rate is observed to reach a maximum with varying methane-to-hydrogen feed ratio at constant substrate temperature. Raman analysis of the deposits indicates that higher-quality diamond is achieved at the highest limits of substrate temperature for a given methane-to-hydrogen ratio. Higher-quality diamond is also observed to be, formed at lower methane-to-hydrogen feed ratios.     

On mass- and emission spectroscopic CVD process monitoring of organometallics/O2 discharges

Mass spectroscopic analysis of neutrals and ions from a deposition plasma shows that the decomposition of the organometallic precursor compounds [La(thd)₃, Cu(acac)₂, and Al isopropoxide] in the plasma .starts with the abstraction of complete ligands. The mass spectra of plasma ions sensitively indicate the incomplete oxidation of the organic fragments with increasing organometallic partial pressure. The concentration of carbon-rich ions in the oxygen-based deposition plasma correlates with the carbon content of the deposited oxide films. Specific emissions of the precursor compounds (e.g., Cu atomic lines and LaO bands) can be used to monitor the precursor partial pressure; however, there is some interference with sputter emission from the deposited films. During La₂O₃ deposition, optical emission of oxidation products (e.g., OH, CO, CO₂ bands) was used to regulate the precursor partial pressure in the discharge with a closed-loop control circuit.On leave from Friedrich Schiller University, Institute of Physical Chemistry, Lessingstrasse 10, D-O-6900 Jena, Germany.On leave from California State University, Department of Chemistry, 2555 East San Ramon Avenue, Fresno, California 93740-0070.     

超级微波消解-电感耦合等离子体发射光谱（ICP-OES）法测定土壤中18种元素

为提高土壤多元素同时检测的效率,采用超级微波消解-电感耦合等离子体发射光谱法测定土壤中钾、钠、钙、镁、铜、铁、锰、锌、磷、硫、硼、砷、镉、铬、铅、钴、镓、锂等18种元素含量。比较了超级微波消解、常规微波消解和电热板消解的处理效果,采用超级微波消解法对样品进行前处理,并优化了消解条件。在最优条件下,各元素的检出限在0.05~20 mg/kg,加标回收率在86.2%~107.5%,RSD在0.1%~3.0%,方法准确度及精密度可以满足多元素同时测定的需求,且该方法具有简单、快速、成本低、用酸量少、重现性好等特点。     

气相反应对CVD生长石墨烯的影响

化学气相沉积法(CVD)制备的石墨烯薄膜具有质量高、均匀性好、层数可控且可放大等优点,近年来受到了学术界和工业界的广泛关注。在高温CVD生长过程中,除衬底表面的反应外,气相反应同样会影响石墨烯的生长行为和薄膜质量。本文将综述气相反应对CVD生长石墨烯的影响：首先对CVD体系内的气相传质过程和气相反应进行了详细讨论;随后系统介绍了基于气相调控提高石墨烯的结晶性、洁净度、畴区尺寸、层数和生长速度的相关策略及其机理;最后对气相反应影响CVD生长石墨烯的规律进行总结,并展望了未来可能的发展方向。     

Surface modifications of PET in argon atmospheric pressure plasma: Gas flow rate effect

The correlation between plasma optical properties and the treated polyethylene terephthalate (PET) surface characteristics have been studied at various Ar flow rate. The rotational T_rot and vibrational T_vib temperatures of APPJ were determined from SPS emission band. The pristine and plasma-treated PET surfaces were characterized by several techniques including X-ray photoelectrons spectroscopy (XPS), Raman spectroscopy, contact angle (CA), and atomic force microscope (AFM). The CA decreased rapidly in the flow rate range 1–3 L/min and weakly dependent as flow rate > 3 L/min. XPS results showed that C 1s % of plasma-treated PET surfaces decreases and has a minimum for samples treated at 3–4 L/min, while O 1s has a maximum at the same flow rate range. The carbon C 1s peak of pristine and plasma treated PET samples resolved into five subcomponents: C–C, C–O, C=O, O–C=O, and π–π bonds with variable percentage ratio accordance to the plasma gas flow rate. Raman data revealed a partial loss in the crystallinity of the treated PET samples and also confirm the incremental of C–O band at Ar flow rate of 3 L/min. AFM images showed that the surface roughness of treated PET films increases as Ar flow rate increases.     

Application of an atmospheric-pressure microwave plasma to the optical fiber manufacturing process

An atmospheric-pressure CVD method is described that uses microwave plasma for manufacturing preforms that are used in the production of optical fibers for telecommunication. The method takes advantage of the very high deposition efficiency and high deposition rates attained when using microwave plasma as well as of efficient glassing of oxide layers by means of the traditional system of burners. A simple theoretical model that allows calculations of close-to-reality plasma temperature profiles is presented.     

Determination of Essential and Toxic Elements in Vegetables from South Korea

This study reports the determination of trace essential (Co, Cr, Cu, Se, and Zn) and toxic (Al, As, Cd, Hg, and Pb) elements in greenhouse tomatoes, peppers, and cucumbers from supermarkets of Seoul, Busan, Gangneung, Daegu, Daejeon, and Gwangju, South Korea using inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectroscopy, and direct mercury analysis. The methods were validated by linearity, limits of detection and quantification, precision, accuracy, and recovery measurements that provided satisfactory results in all cases. Among the essential trace elements, Zn was found to have the highest concentrations (0.84–2.5?mg/kg) followed by Cu (0.21–0.62?mg/kg) and Cr (0.01–0.06?mg/kg). The mean concentrations (mg/kg) of the toxic elements were in the order Al?>?Pb?>?As?>?Cd?>?Hg for tomatoes and cucumbers and Al?>?Pb?>?Cd?>?As?>?Hg for peppers; all were below the permissible limits set by World Health Organization for human consumption. The estimated dietary intake, target hazard quotients (THQs), and hazard indices of the samples were within safe levels. The combined THQ values for the toxic elements in the vegetables were from 0.002 to 0.012 with significant contribution from arsenic, aluminum, cadmium, and mercury. The results of this study show that trace and toxic elements in the analyzed vegetables do not impose any serious health harmful effects for the population upon consumption.     

Process study of thermal plasma chemical vapor deposition of diamond,part II: Pressure dependence and effect of substrate pretreatment

The effect of pressure during thermal plasma chemical vapor deposition of diamond films has been investigated for a pressure range from 100 to 760 Torr. The maximum growth rate in our experiments occurs at 270 Torr for substrate temperatures around 1000°C. The existence of an optimum pressure for diamond deposition may he related to the balance between generation and recombination of atomic hydrogen and carbon-containing active species in front of the substrate. To estimate the concentrations of atomic hydrogen and methyl radicals under thermal plasma conditions, calculations based on thermodynamic equilibrium have been performed. This approximate evaluation provides useful guidelines because rapid diffusion results in a near frozen chemistry within the boundary layer. The effect of substrate pretreatment on diamond deposition depends on the type of substrate used. Two growth modes have been observed-layer growth and island growth of diamond crystals on various substrates. Screw dislocations have been observed in diamond deposition in thermal plasmas, and defects such as secondary nucleations are more concentrated along (III) directions than along (100) directions.     

Experimental investigation of the parameter dependency of the removal rate of thermochemically polished CVD diamond films

Parameters controlling the removal rate of chemical vapor deposition (CVD) diamond films thermochemically polished on transition metals in a mixed argon-hydrogen atmosphere were investigated. The ambient temperature, the pressure exerted on the diamond film, the angular velocity of the polishing plate, the frequency and the amplitude of the transverse vibrations were among the parameters used in the experiments. Temperature measurements showed that the removal rate was increased exponentially with increasing magnitude of the parameter. An exponential increase in the removal rate was also observed with increasing pressure and hence with increasing contact between the diamond film and the polishing plate. However, an exponential decrease in the removal rate was observed with increasing angular velocity of the polishing plate. The removal rate obtained with the application of transverse vibrations was more than three times that obtained without transverse vibrations. Moreover, the removal rate was seen to be higher at resonant frequencies. An increase in the removal rate with increasing amplitude of the transverse vibrations was also observed. Raman measurements carried out on the films to determine the presence of the non-diamond carbon layer after thermochemical polishing revealed non-diamond Raman lines only for films polished at 1000 °C and 1050 °C for the temperature range 750–1050 °C. Received: 27 October 1999 / Accepted: 2 February 2000     

电感耦合等离子体原子发射光谱法测定稀土钢中微量镧、铈

采用稀王水溶解样品,选择La408.672 nm、Ce456.236nm为分析线,建立了电感耦合等离子体原子发射光谱法(ICP-OES)测定稀土钢中微量镧、铈的方法。结果表明,各元素校准曲线线性良好,相关系数可达0.99999;方法测定范围为：0.0001%～0.10%。检出限为：镧0.00002%,铈0.00006%。按照实验方法测定标样中镧、铈,结果的相对标准偏差RSD(n=8)为2.18%、1.68%。     

Validation of a Method for the Determination of Total Chromium in Rat Feces by Inductively Coupled Plasma Optical Emission Spectrometry

Abstract

The validation of a method for the determination of total chromium in Fischer-344 rat feces by inductively coupled plasma optical emission spectrometry following a rapid, atmospheric-pressure microwave digestion is described. The performance of the method was evaluated over the concentration range of 5.00 to 200 µg Cr/g feces. Data for method linearity, accuracy, precision, digest stability, and storage stability are presented along with limit of detection and limit of quantitation data. Data from a cross-validation method for B6C3F1 mouse feces are also presented. Following validation, the method was applied to analyze samples collected in support of two chronic toxicological investigations.     

Deposition behavior in a low‐temperature cascade arc torch (CAT) polymerization process

Two kinds of hydrocarbon type monomers and three kinds of organosilicons were polymerized by a low‐temperature cascade arc argon plasma torch. Their deposition behaviors were studied as a function of experimental parameters and monomer elemental compositions. It was found that the normalized deposition rate (DR), expressed as deposition yield of DR/(FM)_m, was determined by a composite operational parameter, W*(FM)_c/(FM)_m, where W is the power input, and (FM)_c and (FM)_m are the mass flow rates of carrier gases and monomers, respectively. Experimental results indicated that the deposition yield is highly dependent on the elementary compositions of monomers. Optical emission spectroscopy study on the argon plasma torch showed that the emission intensity of excited argon neutrals was proportional to the value of the parameter W*(FM)_c. These results further certified that excited argon neutrals are the main energy carriers from the cascade arc column to activate monomers in the argon plasma torch. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 967–982, 1999     

电感耦合等离子体原子发射光谱法测定高温合金中低含量钇

建立电感耦合等离子体原子发射光谱法测定高温合金中低含量钇的方法。采用盐酸、硝酸、氢氟酸溶解样品,在优化的仪器条件下,采用基体匹配法配制系列标准工作溶液,选择分析线为360.073 nm。钇的含量在0.0005%~0.050%范围内与光谱强度具有良好的线性关系,相关系数为0.99999,检出限为0.000003%。该方法测定结果的相对标准偏差不大于6.0%(n=8),加标回收率为90.0%~104.0%。该方法简便、快速、准确,可用于高温合金中低含量钇的测定。     

Process study of thermal plasma chemical vapor deposition of diamond,part I: Substrate material,temperature, and methane concentration

Effects of process parameters on diamond film synthesis in DC thermal plasma jet reactors are discussed including substrate material, methane concentration and substrate temperature. Diamond has been deposited on silicon, molybdenum, tungsten, tantalum, copper, nickel, titanium, and stainless steel. The adhesion of diamond film to the substrate is greatly affected by the type of substrate used. It has been found that the methane concentration strongly affects the grain size of the diamond films. Increased methane concentrations result in smaller grain sizes due to the increased number of secondary nucleations on the existing facets of diamond crystals. Substrate temperature has a strong effect on the morphology of diamond films. With increasing substrate temperature, the predominant orientation of the crystal growth planes changes from the (111) to the (100) planes. Studies of the variation of the film quality across the substrate due to the nonuniformity of thermal plasma jets indicate that microcrystalline graphite formation starts at the corners and edges of diamond crystals when the conditions become unfavorable for diamond deposition.     

四酸微波消解-电感耦合等离子体发射光谱(ICP-OES)法测定土壤和沉积物中全硼含量

土壤和沉积物的结构特点决定了全硼分析时存在消解不完全、易挥发损失等问题,为了提高全硼检测的效率和可靠性,利用微波消解仪对土壤和沉积物样品进行消解,选择分析谱线为208.957 nm,比较了不同酸体系消解的处理效果,并优化了赶酸温度,建立了一种四酸微波消解结合电感耦合等离子体发射光谱(ICP-OES)法测定土壤和沉积物中全硼含量的方法。在最优条件下,全硼含量在0.01~1.00 mg/L浓度范围内具有良好的线性关系,线性相关系数大于0.999,方法检出限为0.7 mg/kg,回收率为89.3%～96.5%,相对标准偏差为1.1~3.0%。方法可为土壤和沉积物中全硼的含量测定提供参考。     

A magnetically excited microwave plasma source for atomic emission spectroscopy with performance approaching that of the inductively coupled plasma

A novel magnetically excited microwave plasma emission source was developed and tested. Unlike previous microwave plasma sources which couple energy from the microwave electric field, this source couples energy from the magnetic field. The resultant plasma shape allows easy entrainment of wet sample aerosol, such as is produced by a conventional inductively coupled plasma (ICP) nebulizer and spray chamber, into the core of the plasma. Plasma support gas can be either nitrogen or air although better sensitivity is achieved using nitrogen. Good stability of operation was observed for both aqueous and organic solvents over a wide range of sample flows. The measured performance when used as a spectroscopic source in conjunction with an echelle polychromator showed detection limits approaching those of commercial ICP sources.     

Determination of boron in boron-alloyed steels by inductively coupled plasma atomic emission spectrometry

An inductively coupled plasma atomic emission spectrometry (ICP-AES) procedure has been developed and examined for the determination of boron content (0.01 up to about 2% B) in boron-alloyed steels such as POLDI ATA BOR (65% Fe, 19%Cr, 12% Ni, 1.5% Mn, 1% B), POLDI ATA BOR EXTRA (62% Fe, 18% Cr, 13% Ni, 2.5% Mo, 1.5% Mn, 1% B) and POLDI ATA BOR-R (75% Fe, 18% Cr, 3.5% Ti, 1.8% B). The steel sample is dissolved with a mixture of hydrochloric, nitric, sulfuric and phosphoric acids in a quartz vessel. Borides of alloyed metals, especially of iron and chromium, are quantitatively decomposed. The presence of phosphoric acid in a sample solution reduces the volatility of boric acid with water vapour.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

电感耦合等离子体发射光谱法测定二硼化锆中26种杂质

建立微波消解样品,电感耦合等离子体发射光谱法测定二硼化锆中26种杂质元素含量的方法。根据二硼化锆的化学组成对杂质检测的影响,确定了各元素最佳分析线;通过考察不同浓度的锆基体对待测元素的影响来确定最佳锆基体浓度;通过萃取法分离硼元素,消除硼对杂质检测的干扰;采用基体匹配法、多谱拟和技术消除了锆基体的干扰。在选定的仪器工作条件下,各待测元素的质量浓度与信号强度成良好的线性关系,线性相关系数均大于0.999。测定结果的相对标准偏差不大于6%(n=11),样品加标回收率为94%~101%。该方法操作简便,测定结果准确,可用于二硼化锆中26种杂质元素的测定。     

电感耦合等离子体发射光谱法测定高纯铝中硅

建立电感耦合等离子体发射光谱(ICP-AES)法测定高纯铝中硅元素的分析方法。样品采用碱溶法进行预处理,以氢氧化钠溶液溶解,再加入盐酸、硝酸酸化。选取了硅251.611 nm分析谱线进行分析。硅的质量分数在0.001%~0.01%范围内与光谱强度具有良好的线性关系,线性相关系数为0.9991。该方法检出限为0.00012%,测定结果的相对标准偏差不大于10.2%(n=8),加标回收率为93.2%~104.2%。该方法操作简便,测定结果准确、可靠,适用于快速检测高纯铝中硅元素,具有推广价值。