低温氮气吸附法研究海绵钯比表面积和孔径分布

采用低温氮吸附法分析了海绵钯在不同除气温度和时间条件下的比表面积,获得了海绵钯的低温吸附脱附等温线,对标准物质Al<,2>O<,3>粉末进行比表面积测定,并评价分析结果的精密性;采用BJH方程对吸附等温线进行孔径分布规律研究.结果认为,当除气时间为3 h时,海绵钯比表面积达到最大值0.38 m<'2>·g<'-1>,当除气时间大于3 h时,比表面积结果趋于稳定.除气时间太长不会对样品比表面积大小产生影响;在相同的除气时间条件下,海绵钯比表面积随除气温度变化趋势不太明显,温度100℃是海绵钯比表面积时较好的除气条件.采用氮气作吸附质对Al<,2>O<,3>标准样品进行比表面积测试,测试结果表明Al<,2>O<,3>标准样品M-BET和S-BET重复性分别为0.05,0.04 m<,2>·g<'-1>,比表面积测量重复性较好.根据海绵钯吸附-脱附等温线确定海绵钯属于第二类吸附等温线类型,在2～160 nm范围其孔径分布较宽.     

化学共沉淀法制备纳米二氧化铈的研究

采用正、反向化学共沉淀法制备了CeO2纳米粉末材料,有机物共沸蒸馏,用XRD、TEM、BET等技术研究粉体的相结构、晶粒大小、比表面积和孔径情况.结果表明,反向制备的纳米CeO2超细粉体粒径在20nm～40nm之间;样品经400℃焙烧3h后粉体的比表面积为123.14m2/g,平均孔径为55.8578(A),总孔容为0.3439cm3/g.     

醇-水基料浆凝胶注模成形制备粉煤灰多孔陶瓷

以工业废料粉煤灰为原料,采用醇-水基料浆凝胶注模成形新工艺制备粉煤灰多孔陶瓷,系统研究预球磨时间和烧结温度对粉煤灰多孔陶瓷显微形貌、物相、抗弯强度、气体渗透速率、密度和开孔率的影响,以及坯体与烧结体的结构继承性。结果表明:随预球磨时间延长或烧结温度升高,粉煤灰多孔陶瓷的密度和强度显著升高,开孔率和气体渗透速率急剧降低;当预球磨时间为8 h时,体积分数为15%的粉煤灰坯体在1 100℃烧结2 h,样品综合性能最佳:密度为0.77 g/cm3,抗弯强度为8.80 MPa,开孔率为71.2%,气体渗透率为100.5 m3/(m2·h·k Pa),最可几孔径为5.56μm,孔径分布均匀,孔隙分布窄,呈三维无规则贯通孔结构。     

聚乙二醇模板对多孔氧化物复合材料的影响

以聚乙二醇(PEG)为模板剂、正硅酸乙酯(TEOS)为硅源,采用溶胶-凝胶法合成了铜掺杂介孔硅铝氧化物复合材料,并通过N2等温吸附-脱附法、X射线衍射、红外光谱等测试对产物进行表征,考察了PEG质量、分子量以及CuO掺杂量对复合材料孔结构的影响.结果表明:加入PEG能够明显增加复合材料的比表面积,随PEG质量增大,介孔孔容增多,孔径分布较均匀,加入24g PEG时比表面积增加一倍达到约500m2·g-1.PEG的分子量为600～2 000时样品以4 nm介孔为主,而分子量为10 000时,样品以小于2 nm的微孔为主.     

粉煤灰复合水泥浆体干燥收缩与孔结构关系的研究

采用氮吸附法研究了不同掺量粉煤灰对水泥浆体孔结构的影响,分析了干燥收缩与孔径分布、孔隙率、比表面积的关系.结果表明:粉煤灰的掺入使复合水泥浆体孔隙率、比表面积增加,细化样品孔结构的同时使较小毛细孔的比例减小,从而一定程度抑制了干燥收缩.     

Kaolin/ZrO2复合纳米粉体制备及性能研究

以Zr (NO₃)₄·5H₂O为锆源, 利用水热法分别制备ZrO₂和kaolin/ZrO₂复合纳米粉体, 采用扫描电子显微镜、X射线衍射仪、红外光谱仪分析了样品的微观形貌及特性, 使用紫外-可见分光光度计研究了样品的吸光特性, 利用Brunauer-Emmet-Teller (BET)气体吸附法(氮气吸附)测定并计算了样品的比表面积。结果表明, 经过400℃煅烧后, kaolin/ZrO₂表面微球颗粒较纯ZrO₂更加均匀、单一, 不存在成块团聚体; 两种样品均存在介孔结构, ZrO₂主要以无定形形式存在, 但样品中都存在少量的四方相ZrO₂; 在波长190~800nm范围内, kaolin/ZrO₂纳米粉体吸光率均高于纯ZrO₂, 并且其BET比表面积也比纯ZrO₂高19.05m2·g-1, kaolin/ZrO₂纳米粉体在防紫外光特种材料制备及光催化处理工业废水等方面具有更大的优势与潜力。     

孔结构对热电池用氧化镁吸附性能的影响

采用沉淀法制备用于热电池电解质流动抑制剂的氧化镁粉末, 通过调节氨水与镁盐的比例得到不同孔结构的粉末,采用XRD、SEM、TEM、FT-IR和N₂吸附-脱附等方法分析粉末的形貌和孔结构,研究孔结构对电解质漏液率和热电池性能的影响.结果表明:沉淀剂比例能显著改变孔结构,当n(NH₃·H₂O):n(Mg2+)=1.5: 1时,形成大量的介孔,比孔容提高到0.179 cm3/g,比表面积达到30.91 m2/g,氧化镁含量（质量分数）为35 %的电解质粘合板中漏液率仅为6 mg/cm2.适合吸附LiCl-KCl共晶盐的氧化镁孔径应在2~200 nm之间.电解质漏液率高导致热电池平均工作时间变短,氧化镁孔径过小会增加热电池平均激活时间.      

纤维素基多孔碳的制备及其CO2吸附性能研究

以甲基纤维素为原料,改变水热碳化温度得到不同水热产物,随后对其进行化学活化得到多孔碳样品.研究水热温度对多孔碳样品形貌和孔结构的影响,测试了样品在不同压力下的CO2吸附性能.结果表明,水热温度对纤维素基多孔碳的孔结构影响较大.随着水热温度的升高,其比表面积、孔容、微孔比表面积、微孔孔容均呈现出先增大后减小的趋势,平均孔...     

高铝粉煤灰制备拟薄水铝石的比表面积与孔隙特性分析

高铝粉煤灰熟料经预脱硅—碱石灰烧结、溶出、二次脱硅后的溶液经碳分及种分后得到拟薄水铝石产品,并采用低温氮气吸附法分析其比表面积以及孔结构。结果表明,碳分法和种分法制备拟薄水铝石的等温吸附线均属Ⅳ类,晶粒之间的孔隙以中孔为主,等温吸附曲线滞后环类似于H4型,是狭缝孔。碳分产品的BET比表面积略大于种分产品,然而其BJH吸附累积总孔孔容与BJH吸附平均孔径略低于种分产品,两种产品的物化指标均优于普通拟薄水铝石样品。     

水热晶化制备多孔二氧化钛

以工业偏钛酸为原料,利用水热晶化制备多孔二氧化钛光催化剂,考察了不同水热晶化时间对多孔二氧化钛结构和性能的影响。采用XRD、SEM、FT-IR、N2低温吸附-脱附对样品进行表征,并以亚甲基蓝光催化降解体系评价其光催化活性。随着晶化时间的延长,多孔二氧化钛的光催化活性呈现先增大、后减小的趋势。140℃水热晶化2 h所得多孔二氧化钛的光催化活性最佳,反应1 h后对亚甲基蓝的降解率达81.18%,其比表面积SBET=99.59m2/g,孔体积VP=0.271 cc/g,平均孔径DBJH=3.809 nm,晶粒尺寸17.79 nm。     

纯银首饰铸造气孔的形成及防治措施

气孔是铸造纯银首饰的主要缺陷之一,其根本原因是氢、氧等气体在熔融银液与固态银中巨大的溶解度差别而析出造成的。减少或避免纯银首饰中的气孔,熔炼铸造过程中必须采用适当的保护和除气措施,尽量减少进入金属液中的气体,并促使金属液中的气体在浇注前释放出来。实践证明,采用纯净干燥炉料、控制回用料比例、真空回充惰性气体保护、还原性火焰保护、液面覆盖木炭或脱水硼砂、吹氩脱气、多次冷凝和重熔等措施可有效降低气孔的产生。     

邯钢高炉喷吹煤粉的快速热解机制

为了提高邯钢高炉喷吹煤比,模拟煤粉在高炉内的热解。以邯钢喷吹用长治煤(以下简称CL)和大湾煤(以下简称DW)为原料,采用等离子体进行快速热解,计算反应后煤粉的分解率,利用气相色谱仪对气体产物进行分析以及用扫描电镜(SEM)观察反应产物的形貌特征。试验结果表明,CL和DW的分解率分别为43.10%和52.04%,气相产物主要为CO、H2、CH4、C2H2及少量C2H4等气体,热解产物的粒径减小,形貌发生明显变化。在CL煤的基础上配加不同比例的DW后,煤粉颗粒出现了孔状结构,因此可以提高炉内风口回旋区固定碳颗粒的燃烧率,为提高煤粉燃烧率提供理论依据。     

Simulation of Argon Gas Flow Effects in a Continuous Slab Caster

Three-dimensional finite-volume-based numerical models of fluid, heat, and mass transport have been developed and applied to help explain the complex inter-related phenomena of multiphase fluid flow, superheat dissipation, and grade intermixing during the continuous casting of steel slabs. Gas bubbles are simulated using a continuum model, which calculates the volume fraction and velocities of the gas, and its effect on the liquid flow. Turbulence has been incorporated using the standardK-ε turbulence model. Reasonable agreement has been achieved between predicted velocities and corresponding measurements and observations in full-scale water models, both with and without gas injection. The effects of argon gas bubble injection on flow-related phenomena are investigated with simulations of a typical steel slab caster. Argon bubbles alter the flow pattern in the upper recirculation zone, shifting the impingement point and recirculation zones upward. The effect increases with increasing gas fraction and decreasing bubble size. Argon injection also causes superheat to be removed higher in the caster, moves the hot spot upward, lowers the peak heat flux, and increases heat extraction from the wide face and meniscus regions. During a steel grade transition, argon injection slightly affects slab surface composition but has no effect on intermixing in the slab interior.     

气体吸附法测定粉末比表面

简要了静态法和动态法所采用的两类有代表性的仪器。实验表明，两类仪器所得结果是比较一致的。该方法所测量的比表面为总表面积。采用氮吸附质时，可采用单点法。测量小比表面时，应选用低饱和蒸汽压的吸附质，如氩气、氪气等，采用不同的吸附质，所得结果一致。采用氪吸附质，可测量的最小比表面为０．００１ｍ＾２／ｇ。     

脉冲熔融-飞行时间质谱法测定钛中氦和氩

应用气体分析仪开展脉冲熔融-飞行时间质谱法定氦的方法研究和定氩的应用研究,采用气标标定,标定曲线线性良好。选择脉冲-热导法作为参比方法,文中公布的实验结果均为两种方法对比数据。建立了质谱定氦和氩的方法,分析测定科研用充氦钛膜中氦,实际应用于测定粉末冶金钛合金中氩。试验表明脉冲熔融-飞行时间质谱法可以准确测定金属中氦和氩,定量分析结果与现有的脉冲-热导法基本一致。     

金属中气体分析现状与未来

综述了金属中气体分析概况, 提及元素周期表中所有气体元素以及碳和硫。提出常规气体分析已经从氧氮氢碳硫扩大至氦和氩。气体分析所涉及材料种类不断增加, 从金属及合金扩大至冶金炉料、金属氧化物和陶瓷材料等等。气体分析检测极限不断被刷新, 向着更低和更高方向发展。脉冲熔融-质谱新方法应用于金属中气体分析, 可做到氧氮氢氩4元素同时测定, 有可能助推改变气体分析现状。火花源原子发射光谱仪和X射线荧光光谱仪等其他非气体分析专业仪器也正交叉渗入。诸如, 二次离子质谱(SIMS), 离子探针(IM)和电子探针(EP)等微观分析手段一直作为金属中气体分析的辅助手段, 随着未来发展可能转变为主要手段。     

Modeling of molten metal flow in a continuous casting process considering the effects of argon gas injection and static magnetic-field application

A mathematical model has been developed to analyze molten metal flow, considering the effects of argon gas injection and static magnetic-field application in the continuous casting process. The k-ɛ turbulence model is used to calculate the turbulent variables. A homogeneous fluid model with variable density is employed to tackle the molten metal-argon gas flow. The electromagnetic force is incorporated into the Navier-Stokes equation, and the effects of boundary conditions of the magnetic field on the velocity distribution near the mold wall are included. A good agreement between the numerically obtained flow-field results and measurements is obtained. The argon gas injection changes the molten metal flow pattern, mainly in the upper portion of the mold. By applying the magnetic field, values of the averaged velocity field in the bulk decrease significantly, and, especially at the top free surface, they become very small, which can cause meniscus freezing. When magnetic-field application and argon gas injection are used together, the external flow field out of the gas plume is significantly suppressed; nevertheless, flotation of gas bubbles is still active and is not affected directly by the magnetic field. Although the penetrating length of the gas plume is shortened, the argon gas bubbles in molten steel still cause fluctuation at the top free surface, which prevents the occurrence of freezing.     

Mathematical Model of RH Blow Argon Mode Affecting： Decarburization Rate in Ultra-Low Carbon Steel Refining

 A mathematical model in present study has been established to investigate the effect of Rheinstahl Heraeus (RH) blow argon mode on the decarburization rate in ultra-low carbon steel refining based on the RH equipment of Shougang Qian′an Iron and Steel Co Ltd (SQISCO). The calculated results show that the increase of argon flowrate promotes the carbon elimination from argon gas bubble surface, molten steel free surface in vacuum as well as splash droplet surface, while reduces that from the interior of liquid steel. It has been found the critical turning point of flowrate ascension is at the 5th minute and the optimum blow argon flowrate in later stage is 2100 L/min in accordance with the 2 stages argon blow mode, which have been confirmed in the commercial production in SQISCO.     

8-羟基喹啉锗印迹聚合物合成及选择性吸附锗研究

以8-羟基喹啉和四氯化锗为模板,采用杂化沉淀聚合法制备了8-羟基喹啉锗印迹聚合物微球MIPs,并对其微观结构及孔径分布进行表征,推测了8-羟基喹啉锗印迹聚合物合成过程,对MIPs对锗离子的吸附性能进行了研究。结果表明,MIPs具有大比表面积(170.32m~2/g)、微观多孔的纳米微球结构。吸附时间延长、溶液中初始锗含量提高,MIPs对锗离子的选择性吸附能力提高,当吸附时间2h、溶液中初始锗浓度为0.5mg/mL时,MIPs对锗的吸附率达到最大96.84%,MIPs对锗离子具有显著吸附选择特性。     

Influence of atomising gas on particle characteristics of Al,Al–1 wt-%Li,Mg, and Sn powders

Abstract

The influence of physical and flow properties of atomising gas on the particle characteristics of gas atomised Al, Al–1 wt-%Li, Mg, and Sn powders was investigated in a pilot plant gas atomiser with IN4/ON18/3·5–4·0 type ‘confined design’ nozzle. In the tests, Al powders were produced under high and low pressures of argon, under air, (N₂ + O₂ ) mixture, nitrogen, and helium; Al–1 wt-%Li binary alloy powders were produced under argon and helium; Mg powders were produced under high and low pressures of argon and helium; and finally Sn powders were produced under argon, nitrogen, and helium. The morphology, size, size distribution, and surface features of the powders used in the present study were examined under SEM together with dry and wet sieving, used for sizing the powders. It was observed that high gas velocities and/or low atomising gas densities not only affect powder particle size, but also shape and surface texture. The oxygen content of the atomising gases also has an influence on the powder particle shape. In this context, powders produced under helium are finer in size owing to efficient secondary breakup; more spherically shaped in their fine size fraction in non-oxidising or difficult to oxidise atomising liquids (such as Sn and Al), because the time to breakup is shorter than that for solidification; and more irregularly shaped in their coarse size fraction in oxidising atomising liquids (such as Mg and Al–Li) owing to oxygen (the time to breakup is longer than that for solidification) compared with other atomising gases such as argon, air, (N₂ +O₂ ) mixtures, and pure nitrogen.