工艺参数对常压烧结制备莫来石晶须的影响

为探索一种常压烧结制备莫来石晶须的工艺方法,采用化学纯原料结合常压烧结法合成莫来石晶须,借助XRD、EDS、SEM探讨了成型压力、烧结温度、保温时间和V2O5添加量对晶须合成质量的影响.结果表明:通过工艺参数调控可以合成莫来石晶须;当成型压力由10 MPa提高至25 MPa时,晶须长径比增加;当烧结温度为1 350℃、保温时间为2 h、V2O5的添加量为4%时,晶须的长径比最大;此外,莫来石晶须优先在试样表面和边缘处生成.     

建筑回收物制备多孔陶瓷材料及其性能表征

以建筑垃圾为主要原料,Al_2O_3为铝源,AlF_3为晶须催化剂,MoO_3为烧结助剂,成功制备了钙长石-莫来石-刚玉多孔陶瓷。采用XRD和SEM分析了多孔陶瓷材料的物相组成及形貌,研究了在烧结温度1 350℃条件下,不同保温时间对多孔陶瓷材料开口孔隙率、孔径分布的影响,以及钙长石-莫来石-刚玉多孔陶瓷的双轴弯曲强度和油水分离性能。结果表明,当AlF_3含量为12%(质量分数)、MoO_3含量为4%(质量分数)时,在烧结温度1 350℃下,保温2 h,制备的钙长石-莫来石-刚玉多孔陶瓷性能最优。孔隙率分析可知,保温时间为2 h时,有利于原料中氧化铝相和玻璃相莫来石化,增加莫来石相的含量;此时多孔陶瓷材料具有46%的开口孔隙率,且样品中莫来石晶须的大量生长造成晶须之间的尺寸较为一致,使得样品的开孔孔隙孔径大小比较集中,比较适合进行油水分离。力学性能分析表明,保温时间为2 h时,样品的双轴弯曲强度为68 MPa,机械性能良好。油水分离性能研究表明,在不同的膜压差下,样品的油乳拦截率均能达到97%～99%,多孔陶瓷膜具有较好的油乳分离性能。     

空心玻璃微珠造孔制备多孔莫来石陶瓷及其性能EI北大核心

以煤矸石和铝矾土为原料,空心玻璃微珠为造孔剂,采用压制成型烧结制备多孔莫来石陶瓷。研究空心玻璃微珠添加量和烧结温度对物相组成、显微结构、抗弯强度和耐酸碱腐蚀性能的影响。结果表明:提高空心玻璃微珠添加量可以增大多孔陶瓷气孔率;空心玻璃微珠的添加可以促进莫来石相的形成,降低烧结温度。在一定温度范围内提高烧结温度可以增大气孔率,但烧结温度超过1350℃后气孔率开始下降。保持Al_(2)O_(3)∶SiO_(2)摩尔比为3∶2,调整空心玻璃微珠添加量至1.68%(质量分数),在1350℃保温2 h烧结条件下可获得气孔率为33.23%、抗弯强度为56.41 MPa的多孔莫来石陶瓷,其耐酸碱腐蚀性能良好。     

硫酸钠熔盐法微硅粉制备莫来石晶须

以微硅粉和Al2(SO4)3为反应原料,硫酸钠为反应介质,反应混料分别在800℃、900℃、1000℃和1100℃下煅烧保温1h后,经溶解、过滤、烘干后得到莫来石晶须。利用XRD和FESEM对合成粉体进行物相分析和显微形貌观察,结果表明:1000℃为莫来石晶须最佳的合成温度,样品在经NaOH溶液碱处理后得到的莫来石晶须长度约为3~4μm,直径约为10~30nm。同时对合成莫来石晶须形成机理进行了探讨。     

MgO晶须的原位固相合成及其生长机理研究

以AZ91D合金粉末和H3BO3为原料,采用X射线衍射(XRD)、扫描电镜(SEM)及X射线能谱分析(EDS)研究了原料配比和烧结温度对原位固相合成MgO晶须的形貌及其物相变化的影响。结果表明,当Mg/B物质的量比为15∶4时,在惰性气氛条件下采用烧结温度800℃和保温时间2h的工艺可以制备出长度和直径分别为1~3μm和0.1~0.3μm的MgO晶须;探讨了MgO晶须的生长机理,认为MgO晶须的生长符合溶液(Solution)-液(Liquid)-固(Solid)(SLS)机制。     

非水解溶胶-凝胶法制备莫来石晶须

以正硅酸乙酯和无水氯化铝为前驱体,乙醚为氧供体,采用非水解溶胶-凝胶法制备了直径为0.2～20μm,长径比高达60～70的莫来石晶须.借助XRD、SEM和TEM等测试手段研究了莫来石干凝胶粉的活性、矿化剂氟化铝引入方式及其用量、成型压力以及煅烧温度等工艺参数对合成莫来石晶须的影响.结果表明:采用恒压回流工艺制备的莫来石干凝胶粉,在12MPa压力下压制成片状,以外置方式引入3wt%的氟化铝,在1200℃保温1h可制备质量较好的莫来石晶须.     

T-ZnO_w制备过程中工艺参数的影响

采用常压下直接热蒸发锌粉的方法制备了四针状氧化锌晶须(T-ZnOw)。研究了升温速率及保温温度对晶须产量、结构及形态的影响。利用SEM及XRD对产物进行了表征。实验结果表明前期升温速率为3℃/min时,所制备T-ZnOw形貌最为规整,且产率高达95%。随着前期升温速率的提高,产物是不均匀的四针状氧化锌晶须,晶须尺寸增加。随着保温温度的增加,晶须细化,但晶须结构的完整性及产量都有所下降。     

合成工艺对固相法制备高四方性纯钛酸钡粉体的影响

钛酸钡是一种重要的功能陶瓷材料,因具有优异的电学性能而被广泛应用于多层陶瓷电容器(MLCC)等电子元器件。本研究以碳酸钡和二氧化钛为原料,采用固相法制备形貌均匀且四方性高的BaTiO₃粉体,系统研究了合成工艺(合成温度、升温速率和保温时间)对BaTiO₃粉体的影响。通过TG/DTA、XRD和SEM等测试手段对BaTiO₃粉体进行表征,结果表明：合成温度主要影响BaTiO₃粉体的四方性,保温时间和升温速率主要影响BaTiO₃粉体的粒径和粒度分布;原材料经过90 r/min球磨24 h后,在合成温度1050℃、升温速率5℃/min和保温时间3 h的条件下,制备了平均粒径为400 nm、四方性(c/a)为1.009 1的形貌均匀的BaTiO₃粉体。本工作为固相法制备高可靠性MLCC用纯BaTiO₃粉体提供了良好的研究思路。     

8YSZ陶瓷成型与烧结工艺的优化

为了改善8YSZ陶瓷的力学性能,以8YSZ双粒度粉体为研究对象,对其进行干压成型、无压烧结实验。对成型压力、保压时间及黏结剂用量等成型工艺参数进行了优化;利用正交实验对烧结方案进行了设计,讨论了烧结温度、升温速率、保温时间、烧结方式等烧结工艺参数对8YSZ陶瓷烧结性能和力学性能的影响,并优化出其烧结工艺参数。结果表明:选取PVA加入量10%(质量分数)、成型压力10MPa、保压时间30s的成型工艺参数,可压制出相对密度为54.9%的陶瓷坯体;选取烧结温度1500℃,保温时间4h,升温速率5℃/min,烧结方式裸烧的烧结工艺参数,可制备出相对密度为98.3%,抗弯强度为100.3MPa的8YSZ陶瓷。     

用高岭土低温制备莫来石晶须

用高岭土和硫酸铝为原料,硫酸钠为反应介质,研究了在不同温度和不同反应时间对试样产物的影响。结果表明:莫来石晶须生长的最佳温度为900℃,在1000℃开始有氧化铝生成,在1200℃主要物相为氧化铝和硅铝酸钠;在900℃条件下保温2h,制备了直径在0.5μm左右,最大长度大于7μm的莫来石晶须。     

原位合成莫来石晶须增强碳化硅泡沫陶瓷

以碳化硅粉、氧化铝、高岭土为主要原料,采用有机泡沫浸渍法制备出碳化硅泡沫陶瓷坯体,经原位合成反应法在碳化硅泡沫陶瓷内生成莫来石晶须,研究反应温度对莫来石晶须合成的影响,以及莫来石的理论设计含量对泡沫陶瓷的抗压强度和抗热震性能的影响。结果表明:在1 450℃下形成的莫来石晶须直径约为0.5~1.8μm,长径比约为8~30。当莫来石理论设计质量分数为25%时,泡沫陶瓷的抗压强度为1.76MPa,抗热震性能为15次。     

Synthesis of mullite nanostructured spherical powder by ultrasonic spray pyrolysis

In this paper the synthesis of nanostructured spherical particles of mullite powders by ultrasonic spray pyrolysis is presented. The mullite crystallization and the nanostructure development during heating were examined by infrared spectroscopy, X-ray diffraction, scanning and transmission electron microscope analysis. Comparative analysis of experimentally determined and theoretically calculated particle size distribution, obtained on the basis of three-dimensional (3D) model of spherical/ellipsoidal waves generated by incident ultrasonic field, confirmed that the process of aerosol/powder particle synthesis can be regarded as deterministic process.     

Large-scale synthesis of mullite nanowires by molten salt method

Single-crystalline mullite (3Al2O3 2SiO2) nanowires have been produced in large quantities by a low cost and environmentally benign molten salt synthesis (MSS) method. The raw materials, Al2(SO4)3 and SiO2 powders, react in molten Na2SO4 at 1000 degrees C to produce mullite nanowires without the use of surfactants or templates. After the synthesis, the remaining salts can be easily separated from the products by washing with water. The final products are characterized by X-ray powder diffraction, field emission scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, selected-area electron diffraction, and inductively coupled plasma-atomic emission spectrometry. The thermal and chemical behavior of the raw materials is investigated by heating at a rate of 10 degrees C/min up to 1200 degrees C in air followed by thermogravimetric and differential scanning calorimetry analyses. The single-crystalline mullite nanowires have diameters of 30-80 nm and lengths from several hundreds of nanometers to micrometers and the growth mechanism is discussed.     

硅源对莫来石结合刚玉耐火材料性能的影响

以板状刚玉为骨料,莫来石为结合相,并以高岭土和无定型SiO2微粉作为合成莫来石的硅源,采用反应烧结工艺制备莫来石结合刚玉耐火材料,旨在降低莫来石的烧结成本及获得理想的显微结构.研究表明：以高岭土为硅源,莫来石生成量低于理论量,但生成温度较低,1550℃前已完成莫来石化反应,显微结构较均匀,烧结程度较好,莫来石呈长柱状;...     

Preparation of nanometric titanium hydrous oxide particles by vapour phase hydrolysis of titanium tetrabutoxide

Spherical titanium nanoparticles in the range of 60 to 500 nm have been obtained by a vapour-phase hydrolysis procedure using titanium tetrabutoxide as raw material. In this work, different parameters such as alkoxide temperature, water temperature, carrier gas flow rate, inlet pressure, vacuum and dilution of the raw material were tested. The most important parameters in order to obtain nanoparticles of low mean size were the flow rate, the alkoxide temperature and the inlet pressure. When the temperature decreases the mean size decreases obtaining nanoparticles below 100 nm when the temperature is set up to 125°C. On the other hand, as the flow rate that pass through the alkoxide increases the particle size decreases. Same behaviour is observed when the pressure inlet is increased. In all cases, these results are attributed to a minor concentration of the alkoxide (low amount of alkoxide molecules) in the gas stream. The other parameters, vacuum, water temperature and dilution of the alkoxide did not show any important influence in the particle size as the other ones. Polydispersity (broad or narrow particle size distribution) has the same trend. The alkoxide temperature and carrier flow rate generate narrow distributions while the other parameters produces broad distributions. FT-IR analysis of these nanoparticles showed that for sizes below 100 nm the alkoxide is fully hydrolysed and as the particle size increases the nanoparticle has more alkoxide or alcohol retained inside. The heat treatment of these nanoparticles produces a decreasing in the particle size and in all cases, the spherical shape is retained and no blackening in the nanoparticles of higher size is observed.     

微波法制备纳米氧化锌及其光催化性能研究

以硫酸锌和尿素为原料,采用微波加热法制备纳米氧化锌,比较了不同工艺条件下制备的纳米氧化锌的性能,结果表明,不同反应时间制备的纳米氧化锌均为六方晶系的纤锌矿结构,颗粒大小平均为52．14nm,反应时间、反应物浓度及焙烧温度对纳米氧化锌的光催化性能均有一定的影响。反应时间1．5h、硫酸锌的浓度0．25mol／L、焙烧温度450℃时,纳米氧化锌的光催化效果较好。     

Synthesis of silver nanoparticles using the polyol process and the influence of precursor injection

Spherical silver nanoparticles with various sizes and standard deviations were synthesized by the polyol process. Two different synthesis methods were compared in order to investigate the influence of reaction parameters on the resulting particle size and its distribution. In the precursor heating method, wherein a solution containing silver nitrate was heated to the reaction temperature, the ramping rate was determined to be a critical parameter affecting the particle size. In contrast, in the precursor injection method, in which a silver nitrate aqueous solution was injected into hot ethylene glycol, because of rapid nucleation, the injection rate and the reaction temperature were important factors in terms of reducing the particle size and attaining monodispersity. Silver nanoparticles with a size of 17 ± 2?nm were obtained at an injection rate of 2.5?ml?s(-1) and a reaction temperature of 100?°C.     

燃烧合成氮化硅粉体的超细粉碎

采用燃烧合成氮化硅原始粉料,用球磨的方法进行颗粒超细粉碎,探讨了球磨时间与粉料粒度的关系。结果表明,随着研磨时间的增长,平均粒径减小,但研磨时间的延长到一定时,粒径基本不再减小。该粉料经过24h的球磨后,其平均粒径可降低一个量级,由微米级细化到亚微米级0.5μm左右。粒度分布由原来双峰分布变成了狭窄的单峰分布,颗粒细而均匀。测试了粉体超细粉碎前后的粒度及比表面积,并对其形貌进行了显微形貌观察,讨论了超细过程中的一些现象,对不同球磨机的研磨效果进行了对比。     

烧结方式对LiFePO4/C复合正极材料电化学性能的影响

对LiFePO4/C复合前驱体,分别采用静态氮气气氛,动态氮气气氛及静态真空三种烧结方式进行碳热还原合成LiFePO4/C复合正极材料.采用XRD、SEM、CV和充放电循环测试等方法分析和表征材料的结构、形貌和电化学性能.结果表明,烧结方式对所得材料的结晶度、晶粒大小、碳含量、合成温度以及电化学性能均有显著影响.真空烧结所得材料结晶度高,而动态气氛烧结对材料颗粒细化及均匀化都有积极影响,同时也能有效促进锂离子扩散动力学.动态气氛烧结可将材料的烧结温度降低到500℃,且所得材料表现出优异的电化学性能.0.5C倍率下循环首次放电比容量达到163.4 mAh/g,50次循环后容量保持率为99.02%.     

含氢硅油制备SiC晶须的研究

以高含氢硅油为原料,在石墨基体上生长出SiC晶须。主要研究石墨基体的表面状态和加热温度对SiC晶须生长的影响,探究SiC晶须形成过程。影响SiC晶须形核和生长的主要因素为热处理温度,随着热处理温度的升高,SiC晶须的结晶产量也相应增高。石墨基体的表面状态对SiC晶须的形成也有一定的影响,随着石墨基体缺陷提供形核点的增多,SiC晶须的结晶产量提高,并且出现相互搭接的现象。SiC晶须的形成过程分为形核和生长两个部分,低温形核,高温生长,遵循VLS(气-液-固)生长机理。