Comparison of ball milling of Fe/Cr powders and Fe-Cr crystalline alloy

Using the mechanical attrition technique (MA), we have prepared a Fe-Cr alloy starting with a mixture of elemental iron and chromium powders with a nominal composition of 28 at% of Fe and 72 at% of Cr. MA was also performed on solid solutions of Fe₂₈Cr₇₂ crystalline alloy. The Mössbauer effect of the mechanically alloyed powder from Cr and Fe metals has been compared with that from crystalline alloy.     

不同样液制备方法电感耦合等离子体原子发射光谱测定人血清铁、锌、铜、铬、镉、铅的比较

３９例血清样品用酸消化和酸稀释制备待测液,ＩＣＰ－ＡＥＳ相同条件下同时测定Ｆｅ、Ｚｎ、Ｃｕ、Ｃｒ、Ｃｄ和Ｐｂ。统计结果表明,消化法测得Ｆｅ、Ｚｎ和Ｃｒ显著高于稀释法,Ｃｄ低于稀释法;Ｃｕ和Ｐｂ两法测得结果无显著差异。相关分析表明,两法测得Ｆｅ、Ｃｕ、Ｚｎ和Ｃｒ正相关;Ｐｂ和Ｃｄ不相关。ＩＣＰ－ＡＥＳ测定动脉粥样硬化和健康对照组间人血清六种微量元素稀释法无显著差异,而消化法测得组间不同程度存在显著性差异。建议采用消化法制备待测液较好。     

不同样液制备方法电感耦合等离子体原子发射光谱测定人血清 …

３９例血清样品用酸消化和酸释制待测液,ＩＣＰ－ＡＥＳ相同条件与此同时地测定Ｆｅ,Ｚｎ、Ｃｕ、Ｃｒ、Ｃｄ和Ｐｂ。统计结果表明,消化法测得Ｆｅ、Ｚｎ和Ｃｒ显著高于稀释法,Ｃｄ低于稀释法;Ｃｕ和Ｐｂ两法测得结果无显著差异。     

Bias voltage effect on the structure and property of chromium copper-diamond-like carbon multilayer films fabricated by cathodic arc plasma

Chromium copper-diamond-like carbon (Cr:Cu)-DLC films were deposited onto silicon and by cathodic arc evaporation process using chromium (Cr) and copper (Cu) target arc sources to provide Cr and Cu in the Me-DLC. Acetylene reactive gases were the carbon source and activated at 180 °C at 13 mTorr, and a substrate bias voltage was varied from −50 V to −200 V to provide the (Cr:Cu)-DLC structure. The structure, interface, and chemical bonding state of the produced film were analyzed by transmission electron microscope (TEM), IR Fourier transform (FTIR) spectra, and X-ray photoelectron spectroscopy (XPS). The results showed that the Cr-containing a-C:H/Cu coatings exhibited an amorphous layer of DLC:Cr layer and a crystalline layer of Cu multilayer structure. The profiles of sp³/sp² (XPS) ratios corresponded to the change of microhardness profile by varying the pressure of the negative DC bias voltage. These (Cr:Cu)-DLC coatings are promising materials for soft substrate protective coatings.     

LDPE phase composition in LDPE/Cu composites using thermal analysis and FTIR spectroscopy

Low-density polyethylene (LDPE) films with different copper contents were prepared from solu-tion. The TGA (thermogravimetric analysis) results show that the presence of copper particles can im-prove the thermal stability of the composite since a maximum increment of 14°C is obtained compared with the pure LDPE in this experiment. The results of DSC (differential scanning calorimetry) in stan-dard conditions show that the Cu content has little influence on the crystallinity, X _c , of LDPE. But a trace of DSC under non-standard conditions suggests that the presence of the copper microparticles has a greater effect on the network phase than on the crystalline long-range-order phase. FTIR spectroscopy was used to study the phase content of LDPE in LDPE/Cu non-oriented composite films prepared from solution with different copper contents by analysis of CH₂ rocking vibrations. A spectral simulation of transmission spectra performed using a two-phase model does not show any variation into the phase composition of the LDPE matrix for all copper contents. When a three-phase model was taken into account, the amount of the orthorhombic phase was found to be constant. However, the fraction of the amorphous and that of the network phase were found to increase and decrease respectively with increase in the copper particle load in the film.     

Study of solid-solution hardening in binary aluminium-based alloys

Solid-solution formation in binary aluminium-based alloys is due essentially to the combined effects of the size and valence of solvent and solute atoms, as expected by the four Hume-Rothery rules. The lattice parameter of aluminium in the solid solution of the sputtered Al?Fe films is [Al-a (Å)=4.052?6.6×10^?3Y]. The increasing and decreasing evolution of the lattice parameter of copper [Cu-a (Å)=3.612+1.8×10^?3Z] and aluminium [Al-a (Å)=4.048?1.6×10^?3X] in the sputtered Al-1.8 to 92.5 at. % Cu films is a result of the difference in size between the aluminium and copper atoms. The low solubility of copper in aluminium (<1.8 at % Cu) is due to the valences of solvent and solute atoms in contrast with other sputtered films prepared under similar conditions, such as Al?Mg (20 at. % Mg), Al?Ti (27 at. % Ti), Al?Cr (5at. % Cr) and Al?Fe (5.5 at. % Fe) where the solubility is due to the difference in size.     

Synthesis and magnetic properties of Cu-coated Fe composite nanoparticles

The Fe/Cu nanocomposites with iron as core and copper as shell have been successfully synthesized by a two-step reduction method. A spherical nanoparticle of γ-Fe was first fabricated by the reduction of ferrous chloride, and then the Fe particle was coated by nanocrystalline Cu through the reduction of copper sulfate. The thickness of copper shell has been tuned by varying the initial concentration of copper sulfate. The morphology, crystalline structure, chemical composition and magnetic properties of the products were investigated by using transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS) and vibrating sample magnetometer (VSM). It was found that the saturation magnetization (M_s) values of the Fe/Cu core–shell particles are varied owing to the different thickness of copper layer. Though the M_s value of the Fe/Cu nanocomposite is lower than that of pure iron nanoparticles, the higher M_s value (22.411 emu/g) of the Fe/Cu composites is also investigated. The result of the thermogravimetric analysis (TGA) showed the enhanced antioxidation capacity of the Fe/Cu nanocomposites. This kind of nanocomposites combined the excellent magnetism of iron and the electronic, thermal conductivity of copper, suggesting potential application as a novel electromagnetic material.     

Surface modification of polyvalent element-containing glasses

Seven soda-lime silicate glasses, each of which contains one of the following polyvalent metals: Fe, Mn, Cu, Ce, Ti, V, and Cr, are oxidized in air and reduced in H₂/N₂ (1/99) at their respective glass transition temperature for some period. A crystalline oxide surface layer is created on the glasses (except the vanadium-bearing glass) under the oxidizing condition, since the metallic ions are oxidized from lower to higher valence state, and thereby calcium ions diffuse outward and react with oxygen ions. In contrast, a silica-rich surface layer is created on the glasses under the reducing condition, since sodium and calcium ions diffuse inward. It is found that the extents of both outward and inward diffusions strongly depend on the type of the polyvalent ions for the same conditions of heat-treatment. Out of the seven polyvalent metals studied in this work, copper induces the highest extent of both the inward and outward diffusion, and hence, the thickest surface layer of both amorphous silica and crystalline alkaline earth oxides. The oxide layer lowers the onset temperature of the primary crystallization. The silica-rich surface layer enhances the chemical resistance of the glass in a hot basic solution.     

Effect of sputtered Cu film’s diffusion barrier on the growth and field emission properties of carbon nanotubes by chemical vapor deposition

Growth of carbon nanotube (CNT) films with good field emission properties on glass is very important for low cost field emission display (FED) applications. In addition to Ni, Co and Fe, Cu can be a good catalyst for CNT growth on glass, but due to diffusion into SiO₂ it is difficult to control the CNTs density and uniformity. In this paper, four metal barrier layers (W, Ni, Cr, Ti) were deposited by dc magnetron sputtering on glass to reduce the Cu diffusion. As-grown CNT films showed various morphologies with the use of different barrier metals. CNTs with uniform distribution and better crystallinity can be synthesized only on Ti/Cu and W/Cu. Voltage current measurements indicate that better field emission properties of CNT films can be obtained on titanium and tungsten barriered Cu, while chromium and nickel are not suitable barrier candidates for copper in CNT-FED applications because of the reduced emission performance. PACS 81.05.Uw; 61.46.Fg; 85.45.Db; 66.30.-h     

XAFS spectra from X-ray fluorescence Kβ line using conventional energy-discriminating detector

X-ray fluorescence spectra of copper (Cu) metal, copper monoxide (CuO), and potassium chromate (K₂CrO₄) were recorded as a function of incident X-ray energy near the Cu K-edge and chromium (Cr) K-edge, respectively, using a conventional silicon drift detector. The spectra contained components due to elastic, inelastic, and multiple scattering, in addition to the Kα and Kβ lines. Cu and Cr K-edge X-ray absorption fine structure (XAFS) spectra of Cu, CuO, and K₂CrO₄ were obtained by an intensity analysis of the Kα and Kβ lines. The intensity of the Kβ line for the different incident photon energies was obtained by numerically removing the additional scattering components using the MUSCAT program. These spectra exhibited a jump near the K absorption edges, which reproduced the spectral features obtained in transmission mode for both Cu, CuO, and K₂CrO₄. A chemical shift was also clearly identified in the X-ray absorption near edges structure using the X-ray fluorescence Kβ line. In addition, the Cr K-edge extended XAFS spectrum of K₂CrO₄ was clearly observed using the Cr Kβ fluorescent line. The XAFS measurements on the Kα and Kβ lines are possible, and they carry equally valuable information.     

永磁性Pr55Al12Fe30Cu3 大块金属玻璃

报道一个新的Pr55Al12Fe30Cu3 大块金属玻璃.采用铜模吸铸法制备了直径为5 mm、长度达100 mm的Pr55Al12Fe30Cu3 大块金属玻璃.差示扫描量热分析结果表明在该Pr基大块金属玻璃体系具有宽达64 K左右的过冷液相区，而且该合金呈非晶态时的熔化温度要比相应晶态样品的熔化温度高约140 K.磁滞回线测量表明非晶态Pr55Al12Fe30Cu3 块体合金在室温下呈现永磁特性，而完全晶化后样品在室温下呈现软磁特性. 关键词： 大块金属玻璃 玻璃转变 晶化 永磁性     

高压密封微波消解-ICP-AES法测定五种蒙药中无机元素

采用HNO3-HClO4消解体系分别对额日敦-乌日勒、德都红花七味丸、通拉嘎-5、乌珠目-7、给旺-9等五种蒙药样品进行高压微波消解制样,利用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定了镁、铝、钙、铬、锰、铁、钴、镍、铜、锌、砷、硒、锶、钼、银、镉和铅等17种无机元素的含量。通过添加标准回收实验,回收率均在97.25%~106.35%之间,验证了分析数据的可靠性。所有元素测定结果的相对标准偏差均小于3.3%,具有良好的准确度和精密度。实验结果表明,其中常量元素Ca,Mg和Fe,Mn,Zn,Cu的含量较高,测定结果可为开发研制蒙药新制剂、研制蒙药的质量控制标准和提高蒙药药效提供理论依据。     

The microstructure of the base oxide on 304L steel

304L stainless steel specimens were subjected to 168 h of oxidation in dry oxygen at 600°C. The composition and microstructure of the oxide as well as the steel near the steel–oxide interface were investigated using SEM and TEM in conjunction with EDS analysis. It was found that the first oxide layers, referred to as the base oxide, consisted of 50–100 nm-sized corundum-type grains. Each grain contained oxides of chromium, iron plus a small amount of manganese in a solid solution with the chemical formula (Cr,Fe,Mn)₂O₃. In the oxide regions closest to the steel–oxide interface, the grain center compositions varied laterally from grain to grain, with the cation balance ranging between very chromium-rich (Cr:Fe=4:1) and very iron-rich (Cr:Fe=1:8). Within each oxide grain, the chromium level was generally higher in the center than near the boundary. This was due to the much quicker diffusion of iron (compared to chromium) at and through the oxide grain boundaries than in the bulk of the oxide grains, creating iron enrichment near the oxide grain boundaries. Compositional variation with respect to the distance from the steel–oxide interface was also noted. Chromium was richer in the oxide regions closer to the steel–oxide interface than farther out in the oxide and depleted from the steel regions bordering the steel–oxide interface. Manganese was also depleted in those steel regions although hardly enriched in the oxide just outside the steel–oxide interface. Nickel was less reactive than chromium, iron or manganese and hence was virtually absent from the oxide.     

激光诱导击穿光谱定量分析中的分析线自动选择方法

为了实现激光诱导击穿光谱分析中的分析线自动选择,定义了元素发射谱线的相对强度比(RDTIR)、波长偏差(WDDT)两个参数,并据此对检测谱线进行筛选,通过设定合理的阈值,剔除自吸收和干扰严重的谱线。通过对高合金钢(GBW01605)实验数据的分析,分别选定了样品中主要元素铁、铬、镍、锰、铜的分析线,选线结果符合谱线的选取原则。     

吸光度比值-导数光谱法同时测定铜(Ⅱ)和铬(Ⅲ)的研究

提出了运用吸光度比值-导数光谱法同时测定Cr(Ⅲ)与Cu(Ⅱ)含量的新方法。在pH 5.7的HAc-NaAc的缓冲溶液中,Cr3+,Cu2+与铬天青S(CAS)和溴化十六烷基三甲胺(CTMAB)可分别形成蓝色三元络合物。其摩尔吸光系数分别为2.52×105 L·mol-1·cm-1和1.01×105 L·mol-1·cm-1。Cu2+和Cr3+的浓度分别在0.08～1.2 μg·mL-1和0.05～0.52 μg·mL-1范围内符合比尔定律,其检测限分别为0.014和0.013 μg·mL-1。此方法应用于环境水中Cr(Ⅲ),Cu(Ⅱ)的同时测定,取得了满意的结果。     

微波消解ICP-MS法测定啤酒废酵母中的微量金属元素

建立了微波消解-电感耦合等离子体质谱法(ICP-MS)同时测定啤酒废酵母粉中铜、铅、锌、铁、锰、镉、铬和砷等八种微量元素的方法。在实验中,对仪器的最佳工作参数进行了优化,选择适当的同位素,并用铑作内标元素,有效地抑制了分析信号的漂移及分子和多原子离子的质谱干扰;探讨了混合酸消解体系、消解液用量、微波消解功率及时间对测定结果的影响。以HNO₃-H₂O₂(2∶1)作为消化试剂,在0.5 MPa压力下2 min,1.0 MPa压力下3 min,1.5 MPa压力下5 min,4 mL HNO₃和2 mL H₂O₂能完全消解样品。在选定的实验条件下,对五种啤酒废酵母粉样品进行了精密度和回收率实验,方法相对标准偏差在0.94%～3.26%(n=9)之间,加标回收率在98.4%～102.6%之间。     

基于团簇模型设计的Cu-Cu_(12)-[M_(x/(12+x))Ni_(12/(12+x))]_5(M=Si,Cr,Cr+Fe)合金抗高温氧化研究

文章在稳定固溶体团簇模型的指导下,对白铜合金进行微合金化,将Cu元素在合金中的含量固定为72.22 at.%,改变Ni与M(M为Si,Cr,Cr+Fe)的比例,设计了系列合金成分,并对其抗高温氧化性能及其机制进行了研究.同时加入基体中的Ni-Si元素可以从两方面提高合金的抗氧化性能:以团簇形式加入,形成稳定固溶体结构,可以降低Cu-Ni-Si合金的化学反应活性;Si/Ni比增大后,合金在少量固溶的基础上能析出抗氧化性能优于基体的析出相,且析出越多,抗高温氧化性能越好.所以其抗氧化能力的来源并不是形成致密Si氧化物薄膜.Ni-Cr的同时加入可以明显抑制Cu合金在800?C以下的中温氧化,但其抗高温氧化能力主要与外氧化层中是否形成连续的Cr氧化层有关,因而该系列合金的抗高温氧化能力与Cr/Ni比有密切联系,合理选择团簇内Cr/Ni比例,才能够提高Cu合金的抗高温氧化能力.第四组元Fe和第三组元Cr相比较,不能够起到优先氧化、生成保护性氧化皮的作用,所以Cr,Fe同时添加只能抑制Cu在800?C以下的中温氧化,却不能够提高Cu合金的抗高温氧化能力.     

多弧离子镀TiN与不同金属基材间的接触界面与表面特性

用多弧离子镀技术在不同金属基材上进行TiN镀膜实验 ,制备了TiN/Fe、TiN/Cu和TiN/Cr/Cu复合膜 .借助扫描电子显微镜 (SEM)、X射线衍射仪 (XRD)和光电子能谱 (XPS) ,研究了TiN与Fe、Cu和Cr/Cu三种不同衬底接触界面的形貌、结构及其表面特性 .SEM观察发现 ,在一定离子镀膜条件下 ,TiN涂层可与Fe、Cu和Cr/Cu金属基材形成均匀平整的接触界面 ,在铜基上TiN界面清晰 ,在Fe与Cr/Cu界面有明显的层状晶界微结晶分布 .XRD分析显示 ,Fe、Cu和Cr/Cu表面生成的薄膜都包含TiN、Ti2 N等多晶相 ,在Cr/Cu界面还包含Ti-Cr的金属间化合物 .XPS结果表明 ,表面除了TiN膜外 ,还生成TiO2 和TiOxNy 等氧化膜 .Ar+ 刻蚀 5min后 ,TiO2 消失 ,TiOxNy 减少 ,TiN则呈增加趋势 .TiN与Cr/Cu界面形成明显的Ti-Cr和Cr-Ni互扩散层 ,这有助于增强薄膜附着力 ,形成较牢固的TiN涂层 .     

ICP-AES法测定广西产中药广豆根及千斤拔中的金属元素含量

采用湿法消解制样,运用ICP-AES法对广西产中药广豆根和千斤拔中的常最及微量金属元素的含量进行了测定.研究了仪器的工作条件,各元素的分析线和检测限,元素的含量平均值和标准差.结果表明广豆根中含Cu,Zn,Fe,Mn,Cr等微量金属元素和Ca,Mg,Na,K常量金属元素;千斤拔中含Cu,Zn,Fe,Ni,Mn,Cr等微量金属元素和Ca,Mg,Na,K常最金属元素;两者都不含Sn,Pb,Cd等对人体有害的元素.相对标准偏差值均小于5%.研究中还发现广豆根和千斤拔中Zn/Cu值分别为6.4和5.7左右,呈锌高铜低的现象,与癌症患者血清中锌低铜高的现象相反,而与抗癌中药中微量元素的含量锌高铜低的现象一致,这对理解这些抗癌中药的药理作用有一定的启示作用.     

Copper and copper oxide nanoparticles in a cellulose support studied using anomalous small-angle X-ray scattering

Microcrystalline cellulose is a porous natural material which can be used both as a support for nanoparticles and as a reducer of metal ions. Cellulose supported nanoparticles can act as catalysts in many reactions. Cu, CuO, and Cu₂O particles were prepared in microcrystalline cellulose by adding a solution of copper salt to the insoluble cellulose matrix and by reducing the copper ions with several reducers. The porous nanocomposites were studied using anomalous small angle X-ray scattering (ASAXS), X-ray absorption spectroscopy, and X-ray diffraction. Reduction of Cu²⁺ with cellulose in ammonium hydrate medium yielded crystalline CuO nanoparticles and the crystallite size was about 6–20 nm irrespective of the copper concentration. The size distribution of the CuO particles was determined with ASAXS measurements and coincided with the crystallite sizes. Using sodium borohydrate or hydrazine sulfate as a reducer both metallic Cu and Cu₂O nanoparticles were obtained and the crystallite size and the oxidation state depended on the amount of reducer.