水解FeCl_3制备单分散P(St-co-AA)/Fe_2O_3亚微核壳粒子

用液相沉积法制备了壳层均匀、包裹致密的单分散P(St-co-AA)/Fe2O3亚微核壳粒子。用XRD、TEM和FESEM表征了该类粒子的物相、形貌及微观结构。结果表明用该法制备的核壳粒子,其壳层为Fe2O3晶粒,且均匀地包裹在乳胶粒子表面形成草莓状结构;改变FeCl3溶液的用量和重复包裹次数能方便地调节P(St-co-AA)/Fe2O3亚微核壳粒子的壳层厚度。可通过煅烧法用该核壳粒子来制备形状完整的单分散亚微中空磁球。     

ZnS包覆 SiO2核壳和空腔结构纳米球制备研究

ZnS包覆SiO2三维核壳结构或空腔结构纳米球可用于光子晶体的组装.本实验采用层层自组装法,利用二氧化硅模板表面的静电作用吸附纳米晶粒子,生成纳米晶包覆层,制备核壳结构的SiO2@ZnS和SiO2@ZnS：Mn^2＋纳米球.控制氢氟酸对二氧化硅的蚀刻程度,制备了空腔型硫化锌纳米球.采用XRD、UV、PL、TEM、SEM、AFM等测试手段对核壳结构和空腔型硫化锌纳米球进行了表征.结果表明ZnS纳米晶包覆SiO2后,在其表面形成了包裹紧密、形貌规整、粒径均一的ZnS壳层;经5%氢氟酸蚀刻得到的空腔纳米球结构完好、厚度均匀.     

Al_2O_3/Ni包裹粉体的制备、烧结行为及其显微结构研究

利用非均相沉淀包裹技术,在铝无机盐溶液中制备出氧化铝前驱体包裹纳米镍颗 粒的复合粉体,并通过能量发散能谱（ＥＤＳ）以及俄歇电子能谱（ＡＥＳ）研究包裹粉体的成分构 成,发现镍纳米颗粒表面均匀地包裹一层氧化铝的前驱体．煅烧后的包裹粉体在氩气氛中进行 热压烧结．结果表明,与溶胶－凝胶法制备的粉体相比,包裹粉体可以在较低的温度下达到致 密化．烧结后的材料其显微结构明显不同于球磨粉体烧成的材料,不论在氧化铝晶界或晶内, 镍颗粒与氧化铝之间都有孔隙,这是由于镍的热膨胀系数比氧化铝的热膨胀系数大引起的． Ａｌ２Ｏ３／Ｎｉ复合材料的断裂方式以沿晶断裂为主.     

SiO_2@Ag核壳粒子表面形貌及壳层厚度影响因素的研究

用溶胶-凝胶法制备单分散的亚微米二氧化硅,经表面巯基化改性后,采用自组装化学镀法在其表面包Ag,得到SiO2@Ag核壳复合粒子,研究还原剂的种类、浓度和反应温度对核壳结构SiO2@Ag亚微米颗粒形貌及表面Ag壳层厚度的影响规律。结果表明:还原剂的种类对SiO2@Ag核壳复合粒子表面形貌影响较大,还原性太弱很难在二氧化硅表面形成致密均匀的银层,还原性太强则容易形成散银;还原剂浓度增加使二氧化硅表面银颗粒的粒径增大,银壳层厚度增大,但是当还原剂浓度到达一定的值后,浓度对银粒径大小和银壳厚度的影响变弱;反应温度对SiO2@Ag核壳复合粒子表面形貌也有较大影响,0~30℃时,银粒子随温度升高尺寸变大,银壳厚度也相应增大,若温度继续增加到50℃后则开始出现散银,包覆效果变差。     

中空CdS/ZnS纳米核壳材料的制备及其光催化性能探究

采用化学浴法制备聚苯乙烯(PS)/CdS纳米核壳材料,在超声波的作用下采用化学浴法制备PS/CdS/ZnS纳米核壳材料,最后溶液刻蚀除去中心模板,得到中空的CdS/ZnS核壳材料。利用SEM、TEM、EDX、XRD和UV-Vis等测试手段对样品的形貌、成分、粒度、微观结构和吸光度等进行了表征。结果表明:该方法制备的CdS/ZnS纳米材料具有空心双壳层结构,颗粒大小均匀,内壳层厚度为85~100nm,外壳层厚度约为40nm,在可见光下具有良好的稳定催化效能,能够多次回收循环利用。     

低对称性SiO2/Ag核壳复合纳米结构的银镜反应制备及表面增强拉曼散射活性研究

利用银镜反应在自组装的SiO2纳米粒子单层膜上制备了低对称性的SiO2/Ag核壳复合纳米结构.通过透射电镜(TEM)、扫描电镜(SEM)和紫外-可见分光光度计(UV-Vis)对核壳复合纳米结构的表面形貌和光学性质进行了表征.以亚甲基蓝作为探针分子,研究了低对称性SiO2/Ag核壳复合纳米结构的表面增强拉曼散射(SERS)活性.     

SiO2纳米壳的厚度对羰基铁/SiO2核壳复合粒子的性能影响

以聚乙烯毗咯烷酮作表面改性剂，用溶胶-凝胶法，通过控制反应时间，在羰基铁粒子表面均匀快速地包覆不同厚度的SiO2纳米壳层，并研究了SiO2纳米壳层厚度对羰基铁／SiO2核壳复合粒子的抗热氧化性能、静磁性能、微波介电常数和吸波性能的影响．结果表明：增加SiO2纳米壳层的厚度，羰基铁／SiO2核壳复合粒子的抗热氧化能力提高，比饱和磁化强度出现最大值，矫顽力和剩余磁化强度出现最小值，微波介电常数单调降低；用其制备的吸波涂层材料在壳层厚度为15nm时，反射损耗≤-8dB的带宽达到最大值，超过10GHz，     

在硫基功能化碳纳米管上组装壳层厚度可控的Au@Pt核壳纳米粒子以获得高的甲醇电催化氧化活性

本工作致力于研究核壳结构Au@Pt 纳米粒子(Au@Pt NPs)在多壁碳纳米管(MWCNTs)上的组装,试图获得高的甲醇电催化氧化活性。利用光化学晶种生长法合成了Au@Pt NPs,并通过改变Au与Pt的原子比来控制壳层(Pt层)的厚度,然后将不同壳层厚度的Au@Pt NPs组装到巯基(-SH)功能化的MWCNTs上,获得了一系列Au@Pt/MWCNTs复合物。应用透射电子显微镜(TEM)和X射线光电子能谱(XPS)研究了Au@Pt NPs和Au@Pt/MWCNTs复合物的形貌结构、表面化学组成和化学价态,并结合电化学方法研究了Au@Pt NPs的Pt壳层厚度对其组装效果的影响,以及测试了Au@Pt/MWCNTs催化剂对甲醇的电催化氧化的活性。结果表明,Au@Pt NPs通过其表面的Au或Pt与MWCNTs上的-SH形成共价键,从而实现Au@Pt NPs在MWCNTs上的组装。Pt壳层厚度对Au@Pt NPs在MWCNTs上组装的影响较大:当Pt壳层没有完全包裹Au核时,Au@Pt NPs表面暴露的Au促进了Au@Pt NPs在MWCNTs上的组装;而当Pt壳层完全包裹Au核时,Au@Pt NPs表面呈氧化态的Pt(Ⅱ)则对核壳纳米粒子的组装不利。Au、Pt原子比例为1∶1时,Au@Pt NPs能均匀地组装在MWCNTs上,且Au@Pt/MWCNTs(1∶1)催化剂对甲醇的电催化氧化具有较高的活性和稳定性。     

羰基铁/Al2O3核壳复合粒子的制备和性能

制备壳层形貌不同的羰基铁/Al2O3核壳复合粒子,研究了Al2O3纳米壳层形貌对羰基铁/Al2O3核壳复合粒子的抗氧化性能、微波电磁性能和吸波涂层力学性能的影响.结果表明,羰基铁/Al2O3核壳复合粒子的壳层形貌强烈依赖制备过程中酸的种类和pH值.与羰基铁相比,羰基铁/Al2O3核壳复合粒子的抗氧化性能、电磁参数及其与基体的界面相容性明显改善.均匀致密的颗粒状Al2O3纳米壳层有利于在保持磁导率基本不变的前提下改善热稳定性,并降低微波介电常数;纤维状的Al2O3壳层更有利于改善其与基体的界面相容性,提高涂层力学性能.     

堇青石-氧化锆红外辐射复合粉体的制备

为获得具有高红外辐射性能的粉体,以堇青石颗粒为基体,采用液相共沉淀法,用氧化锆前驱体包覆堇青石基体,煅烧后得到堇青石-氧化锆红外辐射复合粉体;对制备的复合粉体进行热分析、物相分析及形貌分析,并测试其红外辐射性能。结果表明,利用非均匀形核可将氧化锆前驱体包覆于堇青石颗粒表面,氧化锆结晶温度在800～900℃之间,900℃煅烧后得到的氧化锆晶粒尺寸约为8 nm;当在一定初始溶液浓度范围内改变反应物的用量时,可以控制氧化锆的包覆量并且避免其自发团聚;通过氧化锆纳米颗粒包覆的工艺可以提高堇青石粉体在3～5μm波段的红外辐射性能,当氧化锆包覆质量分数为21.11%时,复合粉体具有最佳的红外辐射性能。     

Conformal nanocoating of zirconia nanoparticles by atomic layer deposition in a fluidized bed reactor

Primary zirconia nanoparticles were conformally coated with alumina ultrathin films using atomic layer deposition (ALD) in a fluidized bed reactor. Alternating doses of trimethylaluminium and water vapour were performed to deposit Al(2)O(3) nanolayers on the surface of 26?nm zirconia nanoparticles. Transmission Fourier transform infrared spectroscopy was performed ex situ. Bulk Al(2)O(3) vibrational modes were observed for coated particles after 50 and 70?cycles. Coated nanoparticles were also examined with transmission electron microscopy, high-resolution field emission scanning electron microscopy and energy dispersive spectroscopy. Analysis revealed highly conformal and uniform alumina nanofilms throughout the surface of zirconia nanoparticles. The particle size distribution and surface area of the nanoparticles are not affected by the coating process. Primary nanoparticles are coated individually despite their high aggregation tendency during fluidization. The dynamic aggregation behaviour of zirconia nanoparticles in the fluidized bed plays a key role in the individual coating of nanoparticles.     

Sol–gel synthesis and characterization of mesoporous yttria-stabilized zirconia membranes with graded pore structure

Mesoporous yttria-stabilized zirconia (YSZ) membranes can be used for liquid phase applications in harsh environments and as supports for ultra-thin dense ceramic, carbonate, or metallic membranes. This article reports on the synthesis and characterization of three-layer mesoporous ceramic membranes consisting of a mesoporous YSZ layer, a macroporous YSZ intermediate layer, and macroporous α-alumina support. The macroporous YSZ intermediate layer was coated on the alumina support using a suspension of submicron-sized YSZ powders, and the mesoporous YSZ layer was obtained by dip-coating with diluted zirconia sol doped with yttrium nitrate. The mesoporous YSZ layer has desired cubic phase structure. Crack-free mesoporous YSZ membranes could be obtained by multiple dip-coating, drying, and calcination using a dilute YSZ sol at a concentration of 0.014 M with the help of using a drying control chemical additive. The 5 times dip-coated mesoporous YSZ membranes were about 1 μm in thickness with an average pore diameter of 3 nm. The mesoporous YSZ membranes exhibited Knudsen separation factor. The characteristics of the dip-coating process for the mesoporous YSZ membranes on the macroporous YSZ support are similar to those on the macroporous alumina support.     

Effect of barrier layer thickness and composition on fracture toughness of layered zirconia/alumina composites

Composites of yttria or ceria-partially-stabilized zirconia with layers of either alumina or a mixture of 50% by volume of alumina and zirconia were fabricated by sequential centrifuging of powder suspensions. This method allowed formation of layers with thickness of 10 to 70 m. In both cases (Y-ZrO₂ and Ce-ZrO₂ matrices), a significant increase in fracture toughness, work of fracture and bending strength was observed only for composites with barrier layers made of a pure alumina. A crack deflection in alumina layer was found to be the main mechanism responsible for an increase in mechanical properties. For confirmation this thesis, no increase in the transformation zone width was observed. As it was shown, crack deflection angle was dependent on alumina layer thickness. Higher deflection angles for a thicker alumina layers were found. Explanation of this phenomenon was given by determination of residual stress distribution in barrier layers made by piezospectroscopy. A correlation between the crack deflection angle and the difference of stress between the layer boundary and the centre of the layer was noticed. The residual stresses observed are a result of thermal expansion mismatch between alumina and zirconia and thermal anisotropy of alumina. Shrinkage mismatch, especially in the case of Ce-ZrO₂ and Al₂O₃, as a third source of stress is suggested.     

Synthesis and Enhanced Superplasticity of the Zirconia-dispersed Alumina Nanocomposite

A series of alumina-zirconia composites with various grain sizes were prepared from the nano-sized powders with different agglomerations. Microstructural analysis of the sintered compacts indicates that the as-sintered material is a typical intra/inter granular nanocomposite with uniform distribution of the zirconia grains in the alumina matrix. Superplastic deep drawing test under different conditions demonstrates that dense Al2O3/ZrO2 samples with average grain size of 230 nm can be elongated to a dome height of at least 12 mm at the punch rate of 0.6 mm·min-1 at 1400℃. Further drawing tests show that for the composites with larger grain size, such elongation cannot be achieved at such a strain rate.     

Estimation of Pore Charge on Zirconia Membrane Prepared by Sol-gel Route Using Zeta Potential Measurement

Zirconia membrane was prepared in the sol-gel process by filtering viscous colloidal zirconia sol through microporous alumina support and gelling followed by sintering at 743 K. The scanning electron micrograph show that mean pore size was 543 nm and pore density was 1.47×107/cm2.The filtration characteristics during membrane layer formation showed that the membrane layer formation started after 40 min. The membrane layer thickness and the porosity of the membrane were determined gravimetrically by finding out the amount of water present in the pores. The membrane layer thickness was found to be 3 micron and the porosity was found out to be 0.38. The pore charge density was estimated from the particle charge density, pore density, pore diameter and the thickness of the membrane layer.     

SiC/PyC复合涂层碳纤维微观结构及氧化行为研究

采用两步法在碳纤维表面制备了碳化硅/热解碳(SiC/PyC)复合涂层,PyC内涂层的制备采用等温化学气相渗透法,SiC外涂层的制备采用碳热还原法.借助X射线衍射、场发射扫描电镜、透射电镜分析了SiC/PyC复合涂层碳纤维的物相组成以及微观结构,利用热重分析研究了SiC/PyC复合涂层、PyC涂层以及无涂层碳纤维的氧化行为.结果表明,在碳纤维表面制备的SiC/PyC复合涂层连续致密、厚度均匀,PyC内涂层厚度约为200nm,SiC外涂层厚度约为160nm,SiC层中存在大量孪晶面高度有序的SiC孪晶.SiC/PyC复合涂层能够有效地改善碳纤维的抗氧化性能,较无涂层碳纤维起始氧化温度提高了近250℃.     

Nanocoating of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> additive on ZrO<Subscript>2</Subscript> powder and its effect on the sintering behaviour in ZrO<Subscript>2</Subscript> ceramic

ZrO₂ powder was coated with Al₂O₃ precursor generated by a polymeric precursor method in aqueous solution. The system of nanocoated particles formed a core shell-like structure in which the particle is the core and the nanocoating (additive) is the shell. A new approach is reported in order to control the superficial mass transport and the exaggerated grain growth during the sintering of zirconia powder. Transmission electron microscopy (TEM) observations clearly showed the formation of an alumina layer on the surface of the zirconia particles. This layer modifies the sintering process and retards the maximum shrinkage temperature of the pure zirconia.     

Determination of residual stresses in three-layer alumina composites using an indentation technique

The distribution of residual stresses in three-layer reaction bonded alumina (RBAO) composites with 17.5 vol % zirconia in the inner layer and 40 vol % mullite in the outer layers was determined by an indentation technique. It could be shown that the outer layers are subject to a residual compressive stress while the inner layer is under a tensile stress. With increasing outer layer thickness, the residual compressive stress decreases, and the residual tensile stress increases. Compressive stresses up to 550 MPa were measured in this study. It was found that the residual stresses are not uniform throughout the layers. The magnitude of the stresses decreases with increasing distance from the interfaces. This is attributed to creep during cooling from the sintering temperature. This revised version was published online in September 2006 with corrections to the Cover Date.     

原子层沉积技术合成氧化铝薄膜包覆二硝酰胺铵

通过原子层沉积(ALD)技术以三甲基铝和水作为前驱体在二硝酰胺铵(ADN)表面沉积氧化铝包覆膜。分别采用扫描电子显微镜(SEM), X射线光电子能谱(XPS)对包覆后ADN的表面形貌、化学成分进行了分析, 通过蒸汽吸附分析仪(VSA)对包覆氧化铝薄膜的ADN样品进行了吸湿性测试, 并且对ADN表面氧化铝薄膜生成机理进行了探讨。结果表明: ALD氧化铝薄膜对ADN表面形成了完整的包覆, 薄膜厚度最高可达数百纳米。包覆有ALD氧化铝薄膜的ADN样品暴露在潮湿空气中48 h形貌不发生明显变化。在25℃, 湿度70%的环境条件下, VSA测得包覆200和400周期氧化铝薄膜的ADN吸湿率分别为40.99%和40.75%。以上研究结果表明, 尽管ALD氧化铝对ADN表面实现了完整包覆并在潮湿空气中维持了样品形貌, 被包覆的ADN样品吸湿性尚未获得明显改善。     

Nanocomposite Al2O3–ZrO2 thin films grown by reactive dual radio-frequency magnetron sputtering

Crystalline alumina–zirconia nanocomposites have been synthesized at 450 °C and 750 °C with reactive magnetron sputtering using radio-frequency power supplies. The composition of the films ranged from pure alumina to pure zirconia as measured by ion beam techniques. Microstructural characterization showed the presence of monoclinic zirconia in the pure zirconia films and γ-alumina in the pure alumina films while the nanocomposites contained either an amorphous compound, γ-alumina, cubic zirconia or a mixture of these. The grain size was  5 nm for the nanocomposite compared to larger grains in the pure oxide films. Electron energy loss spectroscopy showed a clear progression from the pure alumina to the pure zirconia.