惰性介质对煤粉最低着火温度的影响

为了评价惰性介质对煤粉着火爆炸危险性的影响,保证安全生产,采用Godbert-Greenwald恒温炉装置研究分散压力,惰性介质NH4H2PO4、KH2PO4、Ca(H2PO4)2、CaCO3粉体的含量及NH4H2PO4、CaCO3粉体的粒径对煤粉尘云最低着火温度的影响。结果表明:高分散压力对煤粉尘云的影响更显著,最佳分散压力为0.03 MPa,此时煤粉尘云的最低着火温度最低,为594℃;随着惰性介质含量的增大,煤粉尘云的最低着火温度升高,并且存在突变浓度,NH4H2PO4、KH2PO4、Ca(H2PO4)2粉体的突变浓度(质量分数)为28.6%,CaCO3的为33.3%;惰性介质按对煤粉尘云最低着火温度的抑制效果由强到弱的顺序为NH4H2PO4、Ca(H2PO4)2、KH2PO4、CaCO3;煤粉尘云的最低着火温度随惰性介质粒径的减小而升高,CaCO3粉体粒径变化对抑制效果的影响大于NH4H2PO4的。     

环境敏感水凝胶的环境扫描电镜观察

采用环境扫描电镜(ESEM),观察环境敏感水凝胶在自然状态下微观结构.对环境参数进行了优化,观察到温敏水凝胶的真实形貌和多孔结构.改变ESEM成像条件组合包括压力、温度和相对湿度等环境条件,在2℃～50℃和300Pa～600Pa的环境条件下,原位和动态观察分析温敏水凝胶的结构变化和退溶胀响应速度等环境敏感特性.     

中温锌-钙-锰系黑磷化液的制备及膜层性能

已有的高温锰系一步法黑色磷化能耗高,沉渣多,溶液不稳定;中温两步法黑色磷化膜疏松、附着不牢.两者都不适应大生产需要.制备了一种含Zn2+,Mn2+,Ca2+3种离子的中温黑色磷化液,采用环境扫描电镜(ESEM)观察磷化膜表面微观形貌,用X射线能谱仪(EDS)分析磷化膜成分,通过硫酸铜点滴试验评价了磷化膜的耐蚀性能,并考察了ρ(PO430)/ρ(NO3-)、TA/FA、磷化温度和磷化时间对膜层耐蚀性的影响.结果表明,在磷化温度65～75℃,磷化时间30～35 min,TA/FA为9～13,ρ(PO43-)/ρ(NO3-)为2.5条件下,所得磷化膜结晶均匀、致密,呈深黑色,耐蚀性良好.     

石英频率标准日老化率测量结果的不确定度评定

一、概述 1.测量依据 JJG181-2005《石英晶体频率标准检定规程》、JJG180-2002《电子测量仪器内石英晶体振荡器检定规程》。 2.测量环境条件 可处于15℃-30℃范围内任一点,温度最大允许变化范围为±2℃,相对湿度不大于80%。 3.测量标准铷原子频率标准、PO7D频标比对器,输出范围及功能满足被测仪器的要求。 4.测量对象石英频率标准PO16M。     

超临界水热合成法制备TiO_2纳米粉体

采用超临界水热合成法制备TiO_2纳米粉体,研究反应条件包括温度、压力、反应时间对纳米粉体颗粒的粒径大小、形貌及结晶度的影响。结果表明,随着温度从亚临界升高到超临界,TiO_2颗粒粒径急剧减小,且结晶度增大,最终合成10 nm左右结晶度良好的椭球形颗粒。颗粒在26~30 MPa的压力范围内,结晶度随着反应压力的增大而增大,但粉体粒径大小差别不大。在1 min的反应时间内即检测出了TiO_2物相,而在5 min后生成了结晶良好的椭球形晶体,随着反应时间的增加,棒状的颗粒逐渐增多,这是由于发生了溶解-结晶机理。     

纳米羟基磷灰石粉体的水热合成

采用Ca(NO3)2·4H2O和(NH4)3PO4·3H2O作为反应前驱物,通过水热合成颗粒尺寸在100nm以下的短棒状或针状HA晶体.X射线衍射(XRD)、透射电镜(TEM)和红外光谱(FTIR)分析讨论水热温度、反应时间、表面活性剂和烧结与物相组成、晶粒尺寸和晶体形貌的关系.实验结果表明升高反应温度和延长反应时间有利于HA的生成;表面活性剂有助于改善粉体的分散性能;烧结能提高晶体的结晶程度,但粉体易团聚,当温度高于800℃时HA发生分解.     

聚丙烯发泡珠粒的结晶熔融行为与发泡特性

以CO_2为发泡剂,用高压釜式法制备了发泡聚丙烯(EPP)珠粒。采用差示扫描量热仪和扫描电子显微镜探讨了发泡温度(T_f)和发泡压力(p_f)对EPP结晶熔融行为和发泡特性的影响。结果表明,分别提高发泡温度或压力,EPP的熔融双峰均向高温方向移动,低温晶体与高温晶体的结晶度之比增大,而且温度对双峰的影响比压力更敏感。p_f在2~4 MPa内,EPP的发泡倍率和泡孔密度随p_f增大而增大;T_f在133.6~140℃间,发泡倍率和泡孔尺寸随T_f升高而变大,泡孔密度随T_f升高而变小。在T_f为133.6℃,pf为4 MPa时,EPP的熔融双峰结构比例合适,发泡倍率较大,泡孔密度最大且尺寸分布均匀、表面光滑。     

环境扫描电镜中电荷环境的测量

在环境扫描电镜(ESEM)中,采用高灵敏度的pA-表测试系统,测量法拉第杯,以及Cu-Zn合金、单晶Si、单晶Al2O3三种样品的样品电流(ISP)。ISP值反映出由电子流和离子流控制的ESEM样品室内的电荷环境。法拉第杯的ISP反映出入射电子和离子所控制的电荷环境;样品的ISP反映出入射电子、信号电子和离子所控制的电荷环境。由ISP值可确定ESEM在不同操作和环境条件下的离子化效率、离子化饱和程度,以及气体分子的散射作用。     

磷酸二氢钾粒度对磷酸钾镁水泥性能影响

KH2PO4作为磷酸钾镁水泥主要原材料,与其性能直接相关。研究了KH2PO4粒度对磷酸钾镁水泥的流动性、凝结时间、抗压强度、粘接强度、水化浆体温度和孔隙率等方面的影响。结果表明,随着KH2PO4粒径的减小,磷酸钾镁水泥的凝结时间缩短,流动度先增加后减小;材料抗压强度和粘接强度逐渐增大,中位粒径为45μm时,3h抗压强度达32 MPa,1d粘接强度达4.3MPa;KH2PO4的粒度对磷酸钾镁水泥的水化热有较大影响,对于100mm×100 mm×100mm的试块,成型后中心最高温度逐渐升高,最高可达79.5℃;随着KH2PO4粒径降低,磷酸钾镁水泥的平均孔径降低,孔隙率降低,材料致密程度相应提高。同时,粒径的减小也明显减轻了磷酸钾镁水泥所存在的"泛霜"现象。     

硫酸盐类晶体中[SO_4]~(2-)四面体的结晶方位与晶体的形貌

本文从硫酸盐类晶体中负离子配位多面体的结晶方位和相互联结的稳定性出发，探讨了硫酸盐类晶体中[SO4]2-结晶方位与晶体结晶形貌之间的关系;认为[SO4]2-四面体与金属阳离子（Ba2 、Ca2 、Mg2 …）结合时，由于晶体结构和生长条件（如温度、过饱和度等）的不同，在晶体各族晶面上的叠合速率和取向不同;晶体的结晶形貌迥然有别.晶体的结晶形貌与[SO4]2-四面体在晶体中的结晶方位密切相关，四面体的面和棱的法线（L2）所对向的晶面，生长速率慢，顽强显露，均属晶体的板面;四面体的顶角所指向的晶面，生长速率快，显露面积小，经常消失.     

无支撑优质金刚石膜研制中的相关问题探讨

无支撑优质金刚石膜在微波真空器件和光学器件中的广泛应用,有赖于制备成本的下降和工艺的完善。结合微波等离子体化学气相沉积(MPCVD)金刚石膜的工艺研究结果,本文就沉积速率、晶面取向以及内应力的相关问题进行了初步探讨。对于给定的设备,沉积速率与多种因素有关,包括膜的质量、膜厚均匀性和有效沉积面积、以及形核的密度。在通常情况下,金刚石膜呈(111)择优取向,而样品位置下移5mm后,观察到(100)取向。对内应力的初步研究表明,CH4/H2比例较低(1.5)时,金刚石膜的内应力趋向于压应力,而(100)取向的出现则有助于使内应力降到最低。     

Unusual Nano-Microcrystals of Natural Diamond

Described are unusual nano-microcrystals of natural diamond found in a meteorite crater of Ukraine and advised about the earlier unknown mechanism of diamond polyhedra growth—the formation by globules. It was revealed that diamond nano-microcrystals in a meteorite crater are very similar to globular crystals, and at the same time have octahedral faceting. The morphology and composition of diamond nano-microcrystals are studied by scanning electron microscopy and with an energy dispersive X-ray analyser. These tiny crystals are grown on the grains of impact apographitic diamond from the Bilylivka meteorite crater (Zapadnaya impact crater) on the Ukrainian Shield. Their surface morphology indicates that the nano-microdiamonds are grown, most probably, by a vapor deposition process immediately after the formation of the impact diamond–transformation of the graphite into diamond and lonsdaleite.     

12Cr2MoWVTiB钢高温再热器管氧化膜的特征

电厂的12Cr2MoWVTiB钢高温再热器管实际运行中易出现氧化失效,为了对其实施有效的监督,采用扫描电镜、电子探针和X射线衍射对高温高压水蒸气下运行5.0×10~4h形成的氧化膜形貌、结构、成分及物相进行了分析.结果表明:氧化膜蒸汽侧形貌呈丘状或蘑菇云状,氧化膜基体侧呈方解石状,氧化膜横断面呈石状;氧化膜结构明显分为3层,外层、中间层和内层氧化膜均由粗大的柱状晶构成,各柱状晶层间有大量孔洞,而内层氧化膜与基体结合处氧化膜晶粒为细小等轴晶;O元素含量从外层氧化膜到靠近基体处,存在正的浓度梯度分布,而Fe,Cr,Mo元素含量存在负的浓度梯度分布,Cr,Mo元素在紧靠基体的氧化膜侧产生富集,含量均高于钢基体中的含量;氧化膜物相为Fe_3O_4和FeCr_2O_4.     

Analysis of the structural changes of a phosphate glass during its dissolution in simulated body fluid

The structural changes of two calcium–sodium metaphosphate glasses during its dissolution in simulated body fluid (SBF) have been analyzed by Fourier transform Raman spectroscopy (FT-Raman), scanning electron microscopy (SEM) and environmental scanning electron microscopy (ESEM). The results showed that no structural changes could be detected during the first week of dissolution. However, after approximately 4 weeks of dissolution the analysis of the glass surface revealed the presence of a thin orthophosphate layer. The elemental analysis of this layer by X-ray dispersive energy showed the presence of calcium phosphate ions, while almost no sodium was detected. The observation of the glasses by ESEM showed the formation of small crystals when the water vapor pressure of the chamber was decreased. This indicates that the layer analyzed by SEM and FT-Raman was related to a hydrated calcium phosphate layer.     

Influence of growth parameters on the fabrication of high-quality colloidal crystals via a controlled evaporation self-assembly method

A controlled evaporation self-assembly method with multiple controllable parameters was used to synthesize high-quality colloidal crystals. The environmental parameters, such as the relative humidity, evaporation temperature and pressure, were studied for the quality controls of colloidal crystals during the formation. In the experimental results, we show how these parameters influence the quality of colloidal crystals significantly. Moreover, it is found that, under the case of the relative humidity of 70%, evaporation temperature of 35 °C and pressure of 6.0 kPa, the fabricating high-quality colloidal crystals is optimal from aqueous solution of monodisperse polystyrene spheres with a diameter of 260 nm in a short time (less than 10 h). Highest possible crystal quality may be obtained after the natural drying in the vacuum chamber.     

真空蒸发冷凝制备超细铜粉的研究

借助激光粒度分析仪、扫描电镜、辉光放电质谱仪和X射线衍射仪等手段研究了真空蒸发冷凝制备超细Cu粉的方法及规律。实验表明,金属Cu的蒸发速率受蒸发温度和真空度的影响较大,所得Cu粉为面心立方晶体,形状规则,平均粒径小于2μm,分散性好,而且在真空条件下有利于制备高纯Cu粉。考察了蒸发温度、真空度、保温时间和冷凝条件四个因素对超细Cu粉粒度和形貌的影响规律,并用成核理论进行了分析。     

Electron beam-induced formation of nanosized α-Fe crystals

Focused electron beam induced chemical vapor deposition was performed in a scanning electron microscope with a field emission gun using a precursor of iron carbonyl. Due to the longer deposition time and higher gas pressure than those of our previous electron beam-induced deposition method, a new type of deposition occurred. A large amount of nanosized crystals were produced around the focused beam irradiation point on a carbon substrate at room temperature. The nanocrystals were systematically characterized using transmission electron microscopy with electron energy loss spectroscopy (EELS), and were identified to be single crystals of α-Fe.     

Characterization of Mixed Neodymium Lanthanum Heptamolybdate Crystals Grown by Gel Encapsulation Technique

Crystals of mixed NdLa heptamolybdates (max. size0.75×0.75×0.75 mm3) grown by silica gel technique were characterized using EDAX, IR, optical and scanning electron micrscopies.X-ray as well as electrn diffraction. The composition of the crystals was determined as (Nd1/2 La1/2 )2 Mo7O24·35H2O.The crystals exhibit varied morpholgies including square and octagonal platelets, cuboids, multifaceted crystal in coalesced and aggregated forms and spherulites.The XRD results indicate crystallinity of the grown material. Electron diffraction results suggest thermal instability of the material. IR results show the presence of peaks due to water and metal-oxygen bonds     

Synthesis of Ba-doped CeO(2) nanowires and their application as humidity sensors

Ba-doped CeO(2) nanowires were obtained from CeO(2) particles through a facile composite-hydroxide-mediated (CHM) route. The products were characterized by x-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscope (HRTEM). The formation process of the product was discussed. Humidity sensors based on the source material CeO(2) particles, Ba-doped CeO(2) nanowires grown for 12 and 72?h, were fabricated. The responses to humidity for static and dynamic testing proved that both doping Ba into CeO(2) and converting morphology into a nanowire can improve the humidity sensitivity. The resistance changes from 465 to 3.9?MΩ as the relative humidity (RH) increases from 25% to 88%, indicating promising applications of Ba-doped CeO(2) nanowires in environmental monitoring.     

温度、湿度和拉伸取向对聚丙烯薄膜透湿性能的影响

研究了环境相对湿度和温度对3种不同取向聚丙烯(PP)薄膜的水蒸汽透过率的影响。试验结果表明:随着温湿度的增大,聚丙烯薄膜的水蒸汽透过率也增大;聚丙烯薄膜的水蒸汽透过系数受温度的影响要显著于相对湿度;在一定的温湿度条件下,双向拉伸聚丙烯(BOPP)、单向拉伸聚丙烯(OPP)和未拉伸聚丙烯(CPP)3种薄膜的透湿系数值依次增加,说明拉伸取向操作可提高PP薄膜的阻湿性能。