Marangoni convection and weld shape variations in Ar–O2 and Ar–CO2 shielded GTA welding

Increasing the oxygen or the carbon dioxide concentration in the argon-based shielding gas leads to an increase in the weld metal oxygen content when the oxygen or carbon dioxide concentration is to be lower than 0.6 vol.% in the shielding gas. However, when the O₂ or CO₂ concentration is higher than 0.6 vol.% in the Ar-based shielding gas, the weld metal oxygen is maintained around 200 ppm–250 ppm. An inward Marangoni convection mode in the weld pool occurs when the weld metal oxygen content is more than 100 ppm. When it is lower than 100 ppm, the Marangoni convection would change to the outward direction and the weld shape varies from a deep narrow to a shallow wide shape. The effective ranges of O₂ and CO₂ concentrations for deep penetration are same. A heavy layer of oxides is formed when the O₂ or CO₂ concentration in the shielding gas is more than 0.6 vol.%. Based on the thermodynamic calculation of the equilibrium reactions of Fe, Si, Cr and Mn with oxygen in liquid iron for the oxide products, FeO, SiO₂, Cr₂O₃ and MnO and the experimental oxygen content in the weld metal, Cr₂O₃ and SiO₂ oxides are possibly formed at the periphery area of the liquid pool surface under the arc column during the welding process. One model is proposed to illustrate the role of the oxide layer on the Marangoni convection on the pool surface at elevated temperature. The heavy oxide layer inhibited the fluid flow induced by the Marangoni convection and also became a barrier for the oxygen absorption into the molten weld pool.     

Single-Walled Carbon Nanotubes as a Chemical Sensor for SO2 Detection

Single-walled carbon nanotubes (SWNTs) are Introduced as a chemical sensor for the detection of sulfur dioxide (SO₂) molecules. For a single bundle of SWNTs, current-voltage (I-V) curves were measured for a series of different temperatures under adsorption of SO₂ molecules. The I-V characteristics for a "MAT"-type thin film SWNTs, with respect to the amount of SO₂ adsorbed, were measured at room temperature and compared directly with O₂ adsorption. The change in current upon the adsorption of SO₂ is distinctly higher than that of O₂, and is also reversible for adsorption and successive evacuation. Thus, the results strongly suggested that a thin film of SWNTs can be used as a chemical sensor in the nanometer scale devices.     

Ammonia borane-based reactive mixture for trapping and converting carbon dioxide

Ammonia borane (NH₃BH₃) is a reducing agent, able to trap and convert carbon dioxide. In the present work, we used a reactive solid consisting of a mixture of 90 wt.% of NH₃BH₃ and 10 wt.% of palladium chloride, because the mixture reacts in a fast and exothermic way while releasing H₂ and generating catalytic Pd⁰. We took advantage of such reactivity to trap and convert CO₂ (7 bar), knowing besides that Pd⁰ is a CO₂ hydrogenation catalyst. The operation (i.e. stage 1) was effective: BNH polymers, and B−O, C=O, C−O, and C−H bonds (like in BOCH₃ and BOOCH groups) were identified. We then (in stage 2) pyrolyzed the as-obtained solid at 1250 °C and washed it with water. In doing so, we isolated cyclotriboric acid H₃B₃O₆ (stemming from B₂O₃ formed at 1250 °C), hexagonal boron nitride, and graphitic carbon. In conclusion, the stage 1 showed that CO₂ can be ‘trapped’ and converted, resulting in the formation of BOCH₃ and BOOCH groups (possible sources of methanol and formic acid), and the stage 2 showed that CO₂ transforms into graphitic carbon.     

The formation of a SiOx interfacial layer on low-k SiOCH materials fabricated in ULSI application

The characterizations of SiOCH films using oxygen plasma treatment depends linearly on the O₂/CO flow rate ratio. According to the results of Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) analyses, it was found that the carbon composition decreases with increasing O₂/CO flow rate ratio, because more carbon in the Si–O–C and Si–CH₃ bonds on the film surface would be converted by oxygen radicals. It was believed that the oxygen plasma could oxidize the SiOCH films and form a SiO_x interfacial capping layer without much porosity. Moreover, the result of FTIR analysis revealed that there was no water absorbed on the film. A SiO₂-like capping layer formed at the SiOCH film by the O₂/CO flow rate ratio of 0.75 had nearly the same dielectric properties from the result of capacitance–voltage (C–V) measurement in our research.     

Segregation of Cu in Cu (Ti) alloys during nitridation in NH3

Cu(Ti 27 at.%) alloys on SiO₂ were reacted in NH₃ for 30 min over the temperature range 400–700 °C. Rutherford backscattering spectrometry in conjunction with high resolution transmission electron microscopy were utilized to investigate reaction products. At 400–450 °C, Ti is observed to segregate to the free surface to react with NH₃, forming an Ti oxynitride layer. Above 500 °C, Ti segregates to both the free surface and to the alloy/SiO₂ interface, leaving relatively-pure Cu layer. Reaction between Ti and SiO₂ results in a TiO/Ti₅Si₃ bilayer structure. By use of high spatial resolution energy dispersive X-ray spcctroscopy, the presence of a Cu-containing layer at the TiO/Ti₅Si₃ interface is observed. This layer may also contain Ti, Si and/or O. We propose a mechanism for Cu segregation to this interface which requires Cu diffusion across TiO and subsequent dissociation of Ti₅Si₃. Thermodynamic calculations support this mechanism.     

Ozone-enhanced molecular beam deposition of nickel oxide (NiO) for sensor applications

For the deposition of nickel oxide (NiO) a molecular beam deposition process in an ozone atmosphere was developed. Pure gaseous ozone is received from a cooling system, which stores only O₃ at −78°C from a O₂/O₃ gas mixture stream, created with an ozone generator. The ozone is released by heating up the system to room temperature. For the deposition process nickel is evaporated while a constant ozone partial pressure is adjusted in the growth chamber. The reactive species of ozone reacts on the substrate surface with the impinging metal atoms to form the compound. This process was carried out in an ultra high vacuum (UHV) chamber to create pure nickel oxide films at room temperature and to study the fundamental layer properties for sensor applications. These films were characterized with respect to their stoichiometric and optical properties by Auger Electron spectroscopy and ellipsometry. The gas sensitivity of the films (as deposited and annealed) on various gases (H₂, NH₃, NO₂, SO₂, CO) was investigated by work function measurements.     

Investigation of a new In2O3-based selective H2 gas sensor with low power consumption

The nanometer-size In₂O₃ was synthesized via a reverse microemulsion. A new catalytic combustion-type In₂O₃-based H₂ gas sensor was developed based on the technology for fabricating the direct-heating-type sensor and a surface-modifying process. A dense SiO₂ layer near the surface of the sensor was formed by chemical vapor deposition (CVD) of hexamethyldisiloxane (HMDS). The SiO₂ layer, which acted as a molecular sieve, reduced the penetration of large molecular, such as C₂H₅OH, CH₄, i-C₄H₁₀, into the sensing layer, resulting in the improvement of selectivity to H₂. The sensitive properties and the working mechanism of the sensor were presented. The In₂O₃ nanoparticles prepared by microemulsion were characterized by transmission electron microscopy and X-ray diffraction.     

Nanostructured Metal Oxide Thin Films for Humidity Sensors

Capacitive humidity sensors were fabricated using countersunk interdigitated electrodes coated with amorphous nanostructured TiO₂, SiO₂, and Al₂O₃ thin films grown by glancing angle deposition. The capacitive response and response times for each sensor were measured. The sensor utilizing TiO₂ exhibited the largest change in capacitance, increasing exponentially from ~ 1 nF to ~ 1muF for an increase in relative humidity from 2% to 92%. Adsorption and desorption response times were measured using flow rates of 2.5 l/min and were between 90 ms and 300 ms for the sensors studied here. A simple model of the capacitive response of the devices has been developed and used to calculate the dielectric constant of the combined system of our films and adsorbed water. The obtained dielectric constants are found to be much higher than bulk or literature values for similar systems.     

CO2/O2环境下L320钢在不同流速下的腐蚀行为研究

为了确定L320钢在CO₂/O₂环境中不同流速下的腐蚀行为,通过多相流瞬态模拟仿真软件,模拟目标管道的流动状态,确定室内模拟试验的流速范围,选择L320钢进行CO₂/O₂共存体系下不同流速的高温高压动态反应釜试验,采用扫描电镜、X射线衍射仪对腐蚀产物进行微观形貌表征和成分分析。结果表明:温度和压力随着里程的增加呈现下降的趋势;管道气体流速和壁面剪切力随着里程的增加呈现逐渐上升的趋势。基于Pearson相关系数法,确定了流速是影响腐蚀速率的主控因素。随着流速的增加,L320在CO₂/O₂共存条件下的均匀腐蚀速率逐渐增大。CO₂/O₂共存体系的腐蚀产物为Fe 2 O₃、FeOOH、Fe(OH)3、Fe 3 O 4、FeCO₃等。研究结论可为不同流速下的L320钢在CO₂/O₂共存环境中的防护提供借鉴。     

Effects of p(O2) and p(CO2) on epitaxial growth of BaTiO3 thin films on MgO(100) substrates by using metal organic acid salts

BaTiO₃ thin films were prepared by using metal organic acid salts on MgO(100) substrates, which have large lattice-misfit with BaTiO₃. Amorphous films prefired at 470°C were crystallized to BaTiO₃ phase by heat treatment at higher temperature. Crystallinity and in-plane alignment of the prepared films were found to depend on the heat-treatment conditions. BaTiO₃ films with high crystallinity but poor (100)-orientation were obtained in air at higher than 1200°C. Whereas, (100)-oriented epitaxial BaTiO₃ film was fabricated by annealing at 900°C under low oxygen partial pressure (p(O₂)). Low carbon dioxide partial pressure (p(CO₂)) is also found to be essential for preparation of epitaxial BaTiO₃ films on MgO substrates by using metal organic acid salts.     

Application of decomposed species generated by a heated catalyzer to ULSI fabrication processes

In this paper we report on surface nitridation of SiO₂ and on photoresist removal by using species decomposed from NH₃ or H₂ and generated by a heated tungsten catalyzer. The top surface of SiO₂/Si(100) is nitrided at temperatures as low as 300 °C using species decomposed from NH₃ species. The removal of heavy-doped, as high as 1×10¹⁶ cm⁻², ion-implanted photoresist is realized using atomic hydrogen.     

模板法制备高比表面积的氟化镁及其在HFC-152a脱HF反应中的应用

镁基固体酸催化剂在含氟化学品的合成中具有优异的性能。利用模板法制备了高表面积的氟化镁,并考察了SiO₂模板剂的用量对其结构及催化性能的影响。通过N₂物理吸附、X射线衍射、NH₃-程序升温脱附、透射电镜和X射线光电子能谱等表征手段进行了表征, 以1,1-二氟乙烷(HFC-152a, CH₃CHF₂)脱HF制备氯乙烯(VF,CH₂=CHF)为探针对其催化性能进行了研究。结果表明, SiO₂模板剂用量对氟化镁的比表面积、晶粒度和酸性有较大影响。当SiO₂模板剂用量为14mol%时, 氟化镁比表面积可达304 m²/g, 是不添加SiO₂模板剂的2.5倍, 而且Mg晶粒度更小, 配位数更多。随着Mg配位数增多, MgF₂的酸性位急剧增多, 在以Lewis酸为活性位的1,1-二氟乙烷脱HF反应中, MgF₂的催化活性迅速升高。因此, 以SiO₂为模板是制备高活性MgF₂催化剂的有效方法。     

Fabrication of SiO2 Microcantilever Using Isotropic Etching With ICP

This paper reports a new design and microfabrication process for high sensing guard-armed silicon dioxide (SiO₂ ) microcantilever sensor, which can be widely used in chemical, environmental and biomedical applications. One sensor platform consists of two SiO₂ cantilever beams as the sensing and reference elements, two connecting wings, and three guard arms. The guard arms prevent damage to the cantilever beam from collision. To efficiently release the SiO₂ cantilevers from the silicon substrate, an isotropic etch method using inductively coupled plasma (ICP) was developed. The isotropic etching with ICP system provides an advantage in good profile control and high etching rate than wet isotropic etching or conventional RIE (reactive ion etching); however, it has not been gained many attentions. In this work, the effects of chamber pressure, plasma source power, substrate power, SF₆ flow rate relating with Si etching rate, undercutting rate, and isotropic ratio were investigated and discussed. The optimum isotropic etching process achieved a 9.1 mum/min etch rate, 70% isotropic ratio, and 92% etching uniformity. The SiO₂ cantilever sensor was fabricated and the cantilever beam was successfully released using a patterned photoresist layer as an etching mask. This plasma isotropic etching release processing can be also applied to release other SiO₂ or metal suspended MEMS structures, such as bridges and membranes, with a fast etch rate and reasonable isotropic ratio.     

五层纳米SiO2-Al2O3/聚酰亚胺复合薄膜的制备及性能

采用浸胶法制备了一系列SiO₂-Al₂O₃/聚酰亚胺（SiO₂-Al₂O₃/PI）五层耐电晕薄膜A_m A_n PA_n A_m,其中中间层（P）为纯PI薄膜,外层（A_m）、次外层（A_n）分别为SiO₂-Al₂O₃掺杂不同质量分数的纳米SiO₂-Al₂O₃/PI薄膜。采用TEM、FTIR、宽频介电谱仪、电导电流测试仪、耐电晕测试仪、介电强度测试仪和拉伸实验机对五层纳米复合PI耐电晕薄膜的微观结构、介电性能和力学性能进行了表征和测试。结果表明,SiO₂-Al₂O₃/PI复合薄膜掺杂层形成了分布均匀的有机/无机复合结构;SiO₂-Al₂O₃纳米粒子的保护作用是影响复合材料耐电晕性能的主要因素,复合薄膜A₃₂A₁₆PA₁₆A₃₂的耐电晕寿命最大,为23.4 h;外层掺杂量对五层SiO₂-Al₂O₃/PI复合材料的介电强度影响较大,复合薄膜A₂₀A₂₈PA₂₈A₂₀的介电强度最大,为302.3 kV/mm;通过对五层复合结构的设计,可以在兼顾材料力学性能的同时,提高其耐电晕寿命和介电强度。     

Study on the mechanism of NH3-selective catalytic reduction over CuCexZr1--<?Pub Caret?>x/TiO2

Copper--cerium--zirconium catalysts loaded on TiO₂ prepared by a wet impregnation method were investigated for NH₃-selective catalytic reduction (SCR) of NO_x. The reaction mechanism was proposed on the basis of results from in situ diffuse reflectance infrared transform spectroscopy (DRIFT). When NH₃ is introduced, ammonia bonded to Lewis acid sites is more stable over CuCe_0.25Zr_0.75/TiO₂ at high temperature, while Br?nsted acid sites are more important than Lewis acid sites at low temperature. For the NH₃+NO+O₂ co-adsorption, NH₃ species occupy most of activity sites on CuCe_0.25Zr_0.75/TiO₂ catalyst, and mainly exist in the forms of NH₄⁺ (at low temperature) and NH₃ coordinated (at high temperature), playing a crucial role in the NH₃-SCR process. Two different reaction routes, the L-H mechanism at low temperature (<200°C) and the E-R mechanism at high temperature (>200°C), are presented for the SCR reaction over CuCe_0.25Zr_0.75/TiO₂ catalyst.     

Study on the concentration of an enzyme immobilized by Langmuir-Blodgett films

Urease is an enzyme which decomposes urea into NH₃ and CO₂. We can produce a urea sensor by immobilizing urease on the pH sensor, and the Langmuir-Blodgett (LB) method has been expected to be useful as one of the immobilizing methods. We have measured for the first time the amount of urease adsorbed onto the LB film and shown that the relationship between the amount of adsorbed urease and the concentration in the solution can be expressed by an equation similar to the Langmuir adsorption isotherm.     

新型紫外非线性光学晶体KNa5Ca5(CO3)8的合成、表征及性能的研究

采用水热法合成出一种新型碳酸盐非线性光学晶体材料KNa₅Ca₅(CO₃)₈, 该晶体属于六方晶系, 空间群为P63mc, 晶胞参数为a=b=1.00786(4) nm, c=1.26256(8) nm, Z=2。其晶体结构可以看作是由站立的[CO₃]基团连接相邻的两个[CaCO₃]_∞层, 从而沿[010]方向形成了四种不同类型的孔洞, 在这些孔洞中填充着K、Na 和[Na_0.67Ca_0.33]原子。KNa₅Ca₅(CO₃)₈晶体的粉末倍频效应为KDP的1.2倍, 且能够在可见光区实现相位匹配。紫外-可见-近红外漫反射光谱测试结果表明其晶体具有较大的光学带隙, 大概为5.95 eV, 是具有潜在应用前景的紫外非线性光学晶体材料。此外, 第一性原理的计算结果表明, 晶体的非线性系数主要来源于CO₃基团。     

Electronic sensor for the determination of fruit and vegetable respiration

An instrument to measure the respiration rate of whole fruits and vegetables was designed and developed using a pressure variation method. The Motorola MPX-10-DP pressure transducer was used to monitor pressure changes due to respiratory activity. The operating procedures and calculations required to determine respiration rate (RR) in terms of CO₂ produced, RR-CO₂, and O₂ consumed, RR-O₂, with the respirometer were simple. The values of RR-CO₂ and RR-O₂ obtained by the pressure variation method were compared to changes in CO₂ and O₂ concentrations as determined by gas chromatography. The results showed no significant difference (0.05 level) between the two methods.     

The influence of substrate chemistry on the adhesion of electrolessly deposited Ni(P) on metal oxide coated ceramics

The adhesion of electrolessly deposited Ni(P) on alumina ceramic substrates which were coated with thin SiO₂, SnO₂, TiO₂, Al₂O₃, Y₂O₃, ZrO₂ and (In,Sn)O_x (ITO) films was studied. The adhesion was measured with the aid of the 90° peel test. Strong adhesion of Ni(P) was found for the substrates with ZrO₂ and Al₂O₃ coatings and weak adhesion for the substrates with SiO₂, TiO₂, SnO₂, Y₂O₃ and ITO coatings. The fracture path and the type of interfacial bonding were analysed using scanning electron microscopy, energy-dispersive analysis of X-rays and X-ray photoelectron spectroscopy. In the case of the strongly adhering samples, fracture took place through the metal layer and along the interface. In the case of the weakly adhering samples only interfacial failure was observed between the Ni(P) layer and the metal oxide coating. Cross-section transmission electron microscopy studies of the interfaces suggested that the differences in peel energy values are caused by differences in micromechanical interlocking at the metal oxide-Ni(P) interface. In addition, a weak boundary layer which was found to be present at the Ni(P)-alumina interface was absent in the case of the strongly adhering samples with the ZrO₂ substrate coating.     

基于FTIR和RBF网络的二元脂肪酸/SiO2相变储湿复合材料热湿性能优选预测

采用溶胶-凝胶法制备二元脂肪酸（BFA）/SiO₂相变储湿复合材料,既具有相变调温性能,又具有储湿调湿性能,还能满足无机材料的相容性。研究溶液pH值、超声波功率、去离子水用量、无水酒精用量及BFA用量对BFA/SiO₂相变储湿复合材料结构的影响规律,通过FTIR分析BFA/SiO₂相变储湿复合材料的嵌合机制。通过RBF网络,研究BFA/SiO₂相变储湿复合材料的结构参数与热湿性能优选预测模型。结果表明：BFA/SiO₂相变储湿复合材料中BFA与SiO₂仅仅是物理嵌合。最优热湿性能的BFA/SiO₂相变储湿复合材料制备工艺参数：pH值为3.64、超声波功率为120 W、去离子水用量为1.45 mol、无水乙醇用量为0.78 mol和BFA用量为0.079 mol。预测结果：30%相对湿度（RH）~90% RH湿容量为0.1676 g/g、相变焓为41.89 J/g。测试结果：30% RH~90% RH湿容量为0.1653 g/g、相变焓为41.22 J/g。