溶胶-凝胶法制备多孔纳米金属铜膜

为了制备多孔纳米金属膜材料,以醋酸铜为前躯体、聚乙二醇为模板剂、二乙醇胺为络合剂,通过溶胶-凝胶法在玻璃基片上制备了多孔纳米金属铜膜.利用XRD、IR、TG-DTG和SEM对所制备的纳米金属铜膜材料进行了分析及表征,并研究了溶胶浓度、PEG添加量、退火温度对多孔铜膜结构的影响.结果表明,当溶胶浓度为0.6 mol/L时,铜离子与PEG1000的毫克分子比值是42.86∶1,退火温度为500℃时,可以得到较好的多孔结构纳米Cu薄膜.不同的PEG加入量、溶胶浓度以及热处理温度都会对薄膜的形貌有较大的影响.     

蝌蚪型POSS丙烯酸酯嵌段共聚物及其蜂窝状多孔膜的制备和性能

采用一锅逐步加料的原子转移自由基聚合方法(ATRP)制备了一种蝌蚪型多面体低聚倍半硅氧烷(POSS)丙烯酸酯嵌段共聚物, 并用静态呼吸图法制备该共聚物蜂窝状结构的多孔膜, 研究成膜条件如溶剂种类、聚合物浓度、相对湿度等对聚合物多孔膜形貌的影响, 以及空气/硅片、空气/水和空气/冰3种成膜界面对膜形貌的影响。结果表明, 在空气/硅片界面上, 以三氯甲烷为溶剂, 环境相对湿度为80%, 浓度为20 mg·mL^-1时, 可形成圆形孔的多孔膜, 孔排列成六方形; 在相同的条件下在空气/水和空气/冰界面上均可制备出类似规整形貌的多孔结构, 但多孔膜的孔径、孔间距有很大的不同, 在空气/冰界面上的孔径更小、孔间距更窄。这种多孔膜具有良好的疏水性, 且其接触角随着孔径的减小而增大; 该多孔膜还具有良好的耐强酸强碱性和耐热性能。     

NH4HCO3用量对Ni/La10Si5.8Mg0.2O26.8阳极微观结构的影响

磷灰石型硅酸镧是新型的氧离子导体。本研究采用柠檬酸-硝酸盐溶胶-凝胶法制备磷灰石型硅酸镧(La₁₀Si_5.8Mg_0.2O_26.8)纳米粉末, 将其与NiO纳米粉末按4:6的质量比、并添加不同量的NH₄HCO₃造孔剂进行混合, 通过在1400℃温度下烧结及在600℃氢气中还原制备Ni/La₁₀Si_5.8Mg_0.2O_26.8多孔复合阳极。采用XRD和SEM对样品进行了物相和表面微观形貌表征。采用阿基米德排水法和交流阻抗谱测定了样品的孔隙率和阳极片的室温电阻。实验结果表明, 多孔复合阳极片不含微观裂纹, 未还原陶瓷样品的平均热膨胀系数为10.7×10^-6 K^-1。随着NH₄HCO₃造孔剂加入量的增加, Ni、磷灰石型硅酸镧的晶粒尺寸及气孔尺寸减小, 孔隙率增加, 孔隙率为30%~45%; 阳极电阻先降低后增加。综合考虑阳极片的物相、表面微观形貌、孔隙率和电阻, 以加入30wt% NH₄HCO₃造孔剂所制得的阳极片最佳。     

微量Y2O3对多孔Mg-Al合金组织和性能的影响

镁基多孔材料在生物医用领域具有广阔的应用前景，为提高多孔Mg-Al合金在人体体液中的耐腐蚀性，采用粉末冶金法制备多孔Mg-Al合金，添加不同含量(0,0.2%,0.4%,0.6%)的Y₂O₃对Mg-Al合金进行改性。采用金相显微镜、XRD、SEM、万能试验机和电化学工作站探究了Y₂O₃含量对多孔Mg-Al合金的孔隙率和孔隙形貌、显微组织、抗压强度及其在Hank’s仿生溶液中耐蚀性的影响。结果表明：采用粉末冶金法制备的多孔Mg-Al合金的孔隙率为39%左右，粉末冶金法可较为准确地控制多孔Mg-Al合金的孔隙形貌和大小。多孔Mg-Al合金主要由Mg和第二相Al₁₂Mg₁₇组成，Y₂O₃的添加可使多孔Mg-Al合金晶粒得到细化、晶粒尺寸均匀化，第二相分布更加均匀，并提高多孔Mg-Al合金的抗压强度及其在Hank’s仿生溶液中的耐蚀性。当Y₂O₃含量为0.4%时，多孔Mg-Al...     

电纺制备多孔Ni1-xZnxFe2O4超细纤维的结构与磁性能

采用静电纺丝技术结合后期的热处理制备了具有多孔结构的Ni_1-xZn_xFe₂O₄(x=0~0.8)超细纤维. 利用X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、场发射扫描电镜(FESEM)、低温N₂吸附-脱附和振动样品磁强计(VSM)对纤维样品的晶体结构、微观形貌、孔特征和室温磁性能进行了研究. 结果表明, 550℃焙烧2?h得到的多孔Ni_1-xZn_xFe₂O₄超细纤维均为单相尖晶石结构, 平均粒径约为25~30?nm, 纤维直径主要分布在200~500?nm之间, 且具有较大的长径比; 所制备的Ni_0.5Zn_0.5Fe₂O₄多孔纤维的孔结构主要以狭缝状介孔为主, 其平均孔径约为11?nm; 随着Zn含量x由0增加0.8, Ni_1-xZn_xFe₂O₄纤维的晶格常数a线性增大, A位的红外特征振动频率单调递减, 矫顽力由13.8?kA/m逐步减小到2.3?kA/m, 比饱和磁化强度先增大后减小, 在x=0.4时达到最大值66.8?A·m²/kg. 与相近尺寸的Ni-Zn铁氧体纳米粒子相比, Ni-Zn铁氧体超细纤维由于其形状各向异性而表现出更高的矫顽力.     

直流电化学腐蚀法制备多孔硅的表面形貌研究

采用正交实验，直流电化学腐蚀法制备多孔硅。用原子力显微镜对表面进行观察，研究电化学腐蚀参数对其表面形貌的影响。氢氟酸浓度（CHF）升高，使临界电流密度（JPS）增大，有利于多孔硅的形成。电流密度（J）增大，多孔硅的孔隙率和孔径随之变大，而其纳米粒径将变小。腐蚀时间（t）越长，孔径越大，孔越深。     

Cu-Au-Ag三元去合金化制备纳米多孔金材料

采用磁控溅射镀铜金银多层膜,经过长时间高温热处理合金化制备前驱体三元合金,以不同的酸溶液自由腐蚀去合金化去除合金中的铜元素和银元素,成功制备出纳米多孔金薄膜。采用扫描电镜和X射线能谱仪对去合金腐蚀前后样品的形貌和成分进行了分析。结果表明,400℃,36h热处理后铜金银多层膜完全合金化,获得了Au_3Ag_(28.5)Cu_(68.5)合金材料;FeCl_3+HCl溶液自由腐蚀去除铜可获得连续均匀的纳米尺寸孔隙结构,获得了几乎不含铜的样品;采用渐进浓度的硝酸自由腐蚀去合金化后去除银后获得了孔隙率约84%的纳米多孔金薄膜,其微观结构为连续的三维多孔结构,其系带尺寸10~35nm,并且20~25nm的系带分布达77%。     

介孔TiO2/WO3空心球的制备及其可见光光催化性能

以硫酸氧钛和偏钨酸铵为前驱体, 以柠檬酸作为络合剂, 采用喷雾干燥-高温煅烧两步法制备了介孔TiO₂/WO₃空心球复合材料。利用SEM、TEM、BET、XRD、UV-Vis DRS等手段对样品的形貌、微结构、比表面积、晶相组成和光学性能进行了表征和分析, 以亚甲基蓝为模拟降解物考察其光催化性能。结果表明: 复合材料为介孔空心球状结构, 球体分散好, 直径主要分布在1 μm左右; 球壁由纳米颗粒和空隙构成, 随着煅烧温度的升高, 颗粒粒径不断增大, 空隙孔径不断增大。性能研究结果表明, TiO₂与WO₃复合后, 样品对光的吸收范围扩展到了可见光区域, 这有利于提高太阳光的利用率; 当前驱体中WO₃含量为3mol%, 样品的煅烧温度为500℃时, 复合材料具有最好的光催化性能: 对亚甲基蓝降解率可达99.1%, 而P25的降解率仅为29.5%。     

MEMS中多孔硅绝热技术

主要介绍了多孔硅的制备方法(化学法、电化学法及原电池法等)、多孔硅导热系数测试的几种常用手段(温度传感器法、显微拉曼散射法及光声法等)、导热系数的理论模型及影响因素．此外,采用不同方法制备了多孔硅样品,分析了其表面形貌并用显微拉曼光谱法测定了导热系数．结果发现,化学法制备的多孔硅孔径尺寸大于微米量级,而利用大孔硅电化学和原电池法得到的样品孔径尺寸小(约20nm),属于介孔硅．由于腐蚀条件的不同,多孔硅的孔隙率和厚度也不同,多孔硅的导热系数随孔隙率和厚度的增大而迅速减小．     

多孔结构Bi2WO6光催化剂的制备及其模拟燃油催化氧化脱硫活性

采用水热法合成了多孔结构Bi₂WO₆光催化剂, 借助X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、X射线能量色散谱(EDS)、紫外-可见漫反射(UV-Vis-DRS)、N2吸附/脱附等测试手段对样品的物相组成、形貌、比表面-孔径分布和光吸收特性等进行了表征。考察了水热温度、水热反应时间对Bi₂WO₆的形貌、比表面-孔径分布和光吸收特性影响, 并探讨了Bi₂WO₆光催化剂对模拟燃油的脱硫活性。结果表明, 在强酸性条件下水热温度和水热时间对Bi₂WO₆的形貌、比表面积和催化活性影响显著, 190℃水热反应2 h所得Bi₂WO₆为新颖的鸟巢状微晶, 且鸟巢状Bi₂WO₆由片层状二级结构组装而成。XRD和EDS表明, 鸟巢状结构的Bi₂WO₆为正交晶系, 纯度较高。N₂吸附-脱附测试结果表明, 鸟巢状Bi₂WO₆具有多孔结构, 孔主要分布在10 nm, 比表面积大约为17.49 m²/g。催化活性测试结果表明, 三维介孔结构Bi₂WO₆具有较好的模拟燃油脱硫效果, 在空气流量为100 mL/min, 催化剂加入量为1.2 g/L, 可见光照射180 min, 模拟汽油脱硫率高达91.2%, 且催化剂的稳定性能较好。     

Nanoporous copper sonocatalysts prepared by dealloying Cu–Al–Ti amorphous ribbons

ABSTRACT

Nanoporous copper (NPC) with a controllable ligament width was prepared by chemically dealloying Cu₄₅Al₄₅Ti₁₀ amorphous ribbons in dilute HCl solution. X-ray diffraction and scanning electron microscopy analysis confirmed the 3D, bicontinuous, nanoporous structure constituting fcc-Cu ligaments of 39–79?nm thickness. The coarsening of NPC ligaments increased significantly with an increase of HCl concentration, reaction temperature or time. The surface diffusivity and activation energy of NPC were also calculated. Finally, the catalytic activity of NPC was validated with the ultrasound and H₂O₂-assisted degradation of methyl orange (MO), where 99% MO was degraded within 15?min.     

Synthesis and characterization of novel nanorod superstructures and twin octahedral morphologies of WO3 by hydrothermal treatment

Controlled WO₃ morphologies, such as nanorods and octahedral structures, were synthesized by the hydrothermal technique using sulfate salts based structure directing agents (SDAs). The role of the sulfate salts’ cation in controlling the shape, size and phase of WO₃ nanomaterials was investigated by choosing sulfate salts whose cations are from d-bloc elements (FeSO₄, (NH₄)₂Fe(SO₄)₂, CoSO₄, CuSO₄, ZnSO₄), an alkaline earth metal (MgSO₄) and a non-metal ((NH₄)₂SO₄). In addition chloride (MnCl₂) and acetate (Zn(CH₃CO₂)₂) anion based SDAs were also used in order to clarify the role of sulfate ions in the growth of WO₃ nanostructures. We controlled the pH of the reaction medium with oxalic acid. The obtained WO₃ samples were investigated by SEM, micro-Raman, and XRD. At pH = 1, the WO₃ samples exhibit novel superstructures consisting of aligned hexagonal nanorods, whereas at pH = 5.25, novel twin octahedral morphology with a cubic structure is obtained. The results demonstrate that the phase and morphology change is influenced by the pH and both the anion and the cation of the SDA. A growth mechanism for the obtained novel WO₃ morphologies is presented.     

Ag60．7Al39．3合金的阳极极化行为和去合金化研究

研究了Ag60．7Al39．3合金在H2SO4中的阳极极化行为。线性扫描时，当电压大于临界电位后，随着H2SO4浓度增大，电流密度增长相应加快，而其自腐蚀电位相差不大。在0．1mol／L H2SO4中，0．5V的电压能腐蚀出海绵状的双连续多孔结构，孔径在微米级。0．8V的电压下所得到的银表面形貌呈平行的片状结构。1．0V和1．4V的电压下分别呈块状堆积形貌和波浪形形貌。在0．01mol／L H2SO4中得到的小孔径宽度〈200nm，在0．05mol／LH2SO4中腐蚀后得到的孔径宽度在300nm之间。表明降低H2SO4浓度减小腐蚀电压可得到纳米级的小孔。     

Effects of pores on shear bands in metallic glasses: A molecular dynamics study

The effects of nanoscale pores on the strength and ductility of porous Cu₄₆Zr₅₄ metallic glasses during nanoindentation and uniaxial compression tests are modelled and investigated using molecular dynamics (MD) simulations. In the MD simulations, atomistic amorphous samples were digitally prepared through fast quenching from the liquid states of copper and zirconium alloy. In both of the nanoindentation and uniaxial compression simulations, shear transformation zones and shear bands are observed through the local deviatoric shear strains in the samples. The results show that the existence of pores causes strain concentrations and greatly promotes the initialization and propagation of shear bands. Importantly, only pores reaching critical size can effectively facilitate the formation of multiple shear bands. It is also observed that hardening occurs through pore annihilation and the shear band stops in porous metallic glasses.     

Effect of solid content on pore structure and mechanical properties of porous silicon nitride ceramics produced by freeze casting

Porous Si₃N₄ ceramics were prepared by freeze casting using liquid N₂ as refrigerant. The pore structure, porosity, α → β-Si₃N₄ transformation and mechanical properties of the obtained materials were strongly affected by the solid contents of the slurries. Increasing the solid content would reduce the porosity, decrease the pore size and change the pore structure from the aligned channels with dendrites to the round pores with decreased pore size. The formation of this round pores impeded the α → β-Si₃N₄ phase transformation, but was beneficial to the mechanical properties of the obtained porous Si₃N₄ due to its unique pore structure.     

Synthesis of mixed-phase uniformly infiltrated SBA-3-like in SBA-15 bimodal mesoporous silica from rice husk ash

The mixed-phase bimodal mesoporous silicas (BMS) were simply synthesized via sol-gel technique using rice husk ash-derived sodium silicate as a silica source, and Pluronic P123 and cetyltrimethyl ammonium bromide (CTAB) as the pore structure-directing agents. The gel solution composition in the synthesis process was based on SiO₂:Pluronic P123:CTAB:HCl:H₂O molar ratio of 1:0.088:0.088:4:200. The effect of mixing sequences of starting materials on BMS structures was investigated. The phase separation among SBA-15, SBA-3-like porous silica and xerogel was found when the gel solutions of SBA-15 and SBA-3-like were prepared separately in the primary stage, whereas the mixed-phase uniformly infiltrated SBA-3-like in SBA-15 bimodal porous silica was successfully synthesized when CTAB was added into the SBA-15 gel solution and the secondary micelle structure was formed inside the primary SBA-15 framework.     

Preparation of ZnO bulk porous nanosolids of different pore diameters by a novel solvothermal hot press (STHP) method

ZnO bulk porous nanosolids were prepared by a novel solvothermal hot press (STHP) method with different pore-forming agents using ZnO nanoparticles. The samples were characterized with SEM, XRD, FTIR, a mercury intrusion porosimeter and N₂ adsorption–desorption method. Experimental results showed that pore size of the nanosolids was between 20–32 and 20–100 nm when de-ionized water and CTAB solution were used as pore-forming agents, respectively. There was no obvious morphological change in the samples when all pore-forming agents were removed from the autoclave.     

对GASARITE脱合金制备微-纳复合多孔金属的研究

Gasar工艺是一种制备规则排列微米多孔金属的定向凝固工艺,脱合金工艺是一种通过选择性溶解固溶体合金而制备无序纳米多孔金属的工艺方法,将Gasar和脱合金工艺相结合可以制备一种有序-无序结合、微米-纳米复合的特殊结构多孔金属.选择Cu-Mn二元合金为研究对象,研究了Gasar工艺参数及合金成分对定向凝固多孔Cu-Mn合金结构的影响.脱合金工艺在Gasar工艺制备的定向凝固多孔Cu-Mn合金基础上进行,分析了腐蚀温度等脱合金工艺参数对纳米多孔结构的影响.在优化的Gasar和脱合金工艺参数下,制备得到了一种特殊结构的微-纳复合多孔金属.     

Control of morphological properties of porous biodegradable scaffolds processed by supercritical CO2 foaming

A low cost supercritical CO₂ foaming rig with a novel design has been used to prepare fully interconnected and highly porous biodegradable scaffolds with controllable pore size and structure that can promote cancellous bone regeneration. Porous polymer scaffolds have been produced by plasticising the polymer with high pressure CO₂ and by the formation of a porous structure following the escape of CO₂ from the polymer. Although, control over pore size and structure has been previously reported as difficult with this process, the current study shows that control is possible. The effects of processing parameters such as CO₂ saturation pressure, time and temperature and depressurisation rate on the morphological properties, namely porosity, pore interconnectivity, pore size and wall thickness- of the scaffolds have been investigated. Poly(d,l)lactic acid was used as the biodegradable polymer. The surfaces and internal morphologies of the poly(d,l)lactic acid scaffolds were examined using optical microscope and micro computed tomography. Preosteoblast human bone cells were seeded on the porous scaffolds in vitro to assess cell attachment and viability. The scaffolds showed a good support for cell attachment, and maintained cell viability throughout 7 days in culture. This study demonstrated that the morphology of the porous structure can be controlled by varying the foaming conditions, allowing the porous scaffolds to be used in various tissue engineering applications.