纳米晶型MnCo2O4的微波加热法制备及其电催化性能

以Co和Mn的醋酸盐为原料,采用共沉淀法制得草酸盐前驱物,加入一定量微波吸波剂乙炔黑后,用微波进行热处理制得复合氧化物MnCo2O4.X射线衍射和扫描电镜结果表明,产物为纳米晶型,结晶良好,纯度较高,粒径为10~20nm且分布均匀.在室温下、空气气氛中,以6mol/L的KOH溶液为电解液测试了由MnCo2O4制备的空气扩散电极对氧还原反应的催化效果.极化曲线显示,在-0.2V(vsHg/HgO)电位下,氧还原反应电流密度达96mA/cm2.为显示微波加热法的优越性,用马弗炉煅烧制备了MnCo2O4,并对两种热处理方法所得产物的物化性能进行了比较.     

大尺寸电阻加热式碳化硅晶体生长热场设计与优化

大尺寸低缺陷碳化硅(SiC)单晶体是功率器件和射频(RF)器件的重要基础材料,物理气相传输(physical vapor transport, PVT)法是目前生长大尺寸SiC单晶体的主要方法。获得大尺寸高品质晶体的核心是通过调节组分、温度、压力实现气相组分在晶体生长界面均匀定向结晶,同时尽可能减小晶体的热应力。本文对电阻加热式8英寸(1英寸=2.54 cm)碳化硅大尺寸晶体生长系统展开热场设计研究。首先建立描述碳化硅原料受热分解热质输运及其多孔结构演变、系统热输运的物理和数学模型,进而使用数值模拟方法研究加热器位置、加热器功率和辐射孔径对温度分布的影响及其规律,并优化热场结构。数值模拟结果显示,通过优化散热孔形状、保温棉的结构等设计参数,电阻加热式大尺寸晶体生长系统在晶锭厚度变化、多孔介质原料消耗的情况下均能达到较低的晶体横向温度梯度和较高的纵向温度梯度。     

低压供热涂层材料制备及热性能研究

低压供热技术具有安全系数高和节能降耗等优势,因而成为石化稠油长输管线、风力发电叶片冬季防覆冰和室内供暖等领域的研究热点之一。本文制备了一系列低压供热涂层材料,研究不同碳功能填料对涂层发热速率、发热功率及最高发热温度的影响规律,并揭示石墨烯和碳纤维对提升涂层材料热性能的协同作用。其中石墨烯纳米片的还原程度对材料热性能具有重要影响,降低其表面官能团密度对提升涂层供热特性具有促进作用,但是官能团密度过低会导致石墨烯纳米片的团聚现象,引起涂层发热不均匀。加入适量碳纤维可以提高石墨烯的均匀分散性,提升发热速率。优化石墨烯纳米片和碳纤维的比例后,采用24V电压驱动时,涂层材料的发热速率达到7.1℃·s^-1,功率密度为800W·m^-2,最高发热温度为124℃。     

生物质焦油热裂解动力学参数实验研究

基于进样过程中焦油蒸发的不稳定性以及反应温度的测定和控制难度,设计了移动床焦油进样系统,使用样品槽携带焦油进入具有线性温度分布的炉膛空间,以样品槽的运动进样代替焦油流动进样,以获得稳定的焦油蒸发进样和更容易控制的反应温度。在此基础上,研究了不同进样速率下的焦油热裂解及其动力学特性。结果表明,在573~1 123 K,焦油的裂解率随温度的升高而加速升高,并在1 123 K时达到58%的裂解率;焦油热裂解遵循一级动力学反应,其平均活化能为39.5 kJ/mol,指前因子为1.58 min^-1。     

离子热法合成分子筛的研究进展

离子热法是以离子液体或低共熔混合物为介质的一种新型的分子筛合成方法, 它提供了一种离子态的独特合成环境, 为合成新型分子筛及研究分子筛的生成机理提供了机会. 本文综述了离子热法在分子筛合成方面取得的一些进展, 包括合成方法的创新、合成机理的研究、新材料的合成以及新型催化剂的制备等, 并展望了其发展前景.     

Determination of total phosphorus and nitrogen in turbid waters by oxidation with alkaline potassium peroxodisulfate and low pressure microwave digestion, autoclave heating or the use of closed vessels in a hot water bath: comparison with Kjeldahl digestion

The evaluation of the use of alkaline peroxodisulfate digestion with low pressure microwave, autoclave or hot water bath heating for the determination of total phosphorus and nitrogen in turbid lake and river waters is described. The efficiency of these digestion procedures were compared to a Kjeldahl digestion procedure with sulphuric acid-potassium sulfate and copper sulfate. The final solution before digestion was 0.045 M in potassium peroxodisulfate and 0.04 M in sodium hydroxide. Procedures were evaluated by the analysis of suspensions of two reference materials, National Institute of Environmental Science, Japan, no. 3 Chlorella and no. 2 pond sediment and natural turbid waters. Best recoveries of phosphorus and nitrogen by microwave heating were obtained when solutions were digested at 95 °C for 40 min. Quantitative recoveries of phosphorus from Chlorella suspensions up to 1000 mg/l were obtained by all three heating procedures, but incomplete recoveries of nitrogen occurred above 20 mg N/l in the digested sample. Good recoveries of phosphorus and nitrogen from suspended sediment suspensions were obtained only from solutions containing <150 mg/l of suspended sediments. Recoveries of phosphorus from phosphorus compounds containing COP and CP bonds added to distilled water were quantitative (94-113%) except for polyphosphates (microwave, 34±8; autoclave, 114±6; water bath, 96±4) and aluminium phosphate (8-23%). Recoveries of nitrogen compounds containing CN bonds added to distilled water were quantitative (94-96%). The analysis of a range of natural turbid water samples by alkaline peroxodisulfate and microwave, autoclave and water bath heating gave similar total phosphorus and nitrogen results. All procedures using alkaline peroxodisulfate underestimate phosphorus concentrations at high suspended sediment concentrations (>150 mg/l) and are only suitable for the analysis of very turbid samples when the turbidity is due to organic matter (algal cells, plant detritus). Underestimation of nitrogen occurs when samples contain more than 20 mg N/l.     

微波消解ICP-AES法测定玩具塑料中镉

采用微波加压消解溶样，ICP-AES法测定玩具塑料中镉含量，选择最佳工作条件，方法简便、快速、可靠。适用于各类玩具塑料中镉含量的分析。     

MICRO-PHASE SAEPARATION IN EPOXY RESIN WATERBORNE PARTICLES DURING CURING PROCESS

Sub-micron sized phenolic epoxy resin waterborne particles were prepared by phase inversion emulsification. Micro-phase separation occurred during the curing process at high temperature. The as-prepared samples possessed one glass transition temperature （Tg） and two exothermal processes during DSC heating scannings. After being thermally treated above the exothermal peak temperature, they possessed two glass transition temperatures with the disappearance of exothermal peaks, whilst a core/shell structure was formed. This was likely related with the outward diffusion of reactive oligomers to the outer layer of particles.     

微波场对SrTiO3化学合成中热过程的影响

在分析微波场中SrTiO3化学合成体系与电磁场相互作用的基础上,探讨合成体系在微波场中的加热机制和影响升温的主要因素（如合成体系的介电性质、保温材料的结构、生还的致密度等）,结果表明,TiO2和SrCO3在低温阶段对体系的升温速率的贡献相接近;高温阶段体系升温主要是TiO2的贡献,同时产物对升温有较大的影响。微波合成与常规合成再加热方式上的明显不同,对合成过程、合成时间等影响较大。     

红外吸收法测定碳化铪粉末中的氧含量

应用氧氮分析仪建立碳化铪粉末中氧的测定方法。针对碳化铪熔点极高的特性,对加热功率、称样量和空白值等测定条件进行探讨,选择适合的助熔剂和高温石墨坩埚,确定了最佳测试条件。将该方法用于实际样品测定,测定结果的相对标准偏差小于2.0%(n=9),样品的加标回收率为98.1%～102.6%。