去合金化制备纳米多孔铜

 以Mn-Cu合金为前驱体合金,在0.1 mol/L HCl 溶液中自由腐蚀去合金化成功制备出纳米多孔铜,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,Mn-Cu合金在0.1 mol/L HCl 溶液中发生锰的选择性溶解,制备出的纳米多孔铜呈3维网络状均匀结构,平均系带尺寸53 nm,平均孔径尺寸为140 nm。     

Mn-Cu合金成分对去合金化法制备纳米多孔铜的影响

 采用电弧熔炼制备出前驱体Mn-Cu合金,在稀盐酸溶液中自由腐蚀去合金化,制备出具有双连续结构的纳米多孔铜。研究了前驱体合金的成分对纳米多孔铜微观结构及Mn的选择性腐蚀程度的影响。结果表明：前驱体Mn-Cu合金的Cu原子分数为43%时,其去合金化受到抑制,存在明显的未完全去合金化的岛状结构;前驱体Mn-Cu合金的Cu原子分数为32%～23%时,可完全去合金化,形成平均孔径尺寸为20～100 nm,平均系带尺寸为30～80 nm,具有双连续结构的纳米多孔铜;前驱体Mn-Cu合金的Cu原子分数低至20%时,去合金化后存在大量裂纹,形成纳米颗粒聚集体。纳米多孔铜中存在少量的残余Mn,残余Mn的原子分数随着前驱体合金Mn原子分数的增高而降低。实验表明腐蚀液浓度对纳米多孔铜形貌也存在影响。     

去合金化工艺对纳米多孔铜纯度的影响

采用腐蚀去合金化方法制备纳米多孔铜材料。研究了固溶时间、腐蚀时间及腐蚀温度对纳米多孔铜表面形貌及残余Mn含量的影响。研究表明:由于固溶时间的延长，合金成分越来越均匀化，去合金化后所得纳米多孔铜的残余Mn原子分数降低。固溶95 h的前驱体合金，随着腐蚀时间的延长，其残余Mn含量降低不明显；随着温度的升高，其残余Mn原子分数由25 ℃的3.54%降至60℃的1.14%，但是60 ℃腐蚀后的孔隙与丝径尺寸明显粗化，样品易碎。通过调整去合金化参数，实验所制备的纳米多孔铜呈现均匀的海绵状纳米多孔结构，残余Mn原子分数1.23%, 平均丝径尺寸40 nm。     

空心微球结构Au/Ag合金泡沫块体的制备

将平均晶粒尺寸为4.6 nm的金粒子通过静电作用粘附于聚苯乙烯（PS）微球表面用于化学镀,化学镀金后PS表面的金沉积层几乎达到完全包覆,厚度70~90 nm;在Au/PS表面进行化学镀银,沉积的银颗粒堆积紧密,颗粒大小较先前沉积的金颗粒大,镀覆层厚度增厚至200~400 nm;模板去除后,获得了完全自支撑的Au40Ag60空心微球结构的圆柱状泡沫材料。制备的金银合金泡沫由直径约10 m的空心球壳组成,圆柱体直径约5 mm,密度约1.2 g/cm3。     

纳米多孔SiO2薄膜的制备与红外光谱研究

以正硅酸乙酯为原料,采用溶胶-凝胶法,结合旋转涂胶、超临界干燥工艺在硅片上制备了纳米多孔SiO2薄膜。XRD表明薄膜为无定形态;SEM显示薄膜具有多孔网络结构,其SiO2粒子直径为10~20nm。利用FTIR研究了薄膜的结构,纳米多孔SiO2薄膜含有Si—O—Si与Si—OR结构,呈疏水性;该SiO2薄膜热处理后因含有Si—OH基团而呈吸水性;用三甲基氯硅烷对热处理SiO2薄膜进行修饰可使其呈疏水性,修饰后的薄膜在N2中温度不高于450℃可保持其疏水性与多孔结构。     

FePt薄膜中磁相互作用

采用磁控溅射方法在自然氧化的单晶Si(100)衬底上制备了纳米结构的Fe₅₃Pt₄₇薄膜，并研究热处理后薄膜中的磁相互作用、晶粒尺寸与热处理温度的关系.经400℃热处理后，FePt薄膜中有明显的面心四方相形成，薄膜表现出硬磁性，晶粒尺度在20 nm，薄膜内部存在软硬磁交换耦合作用；随着热处理温度升高，硬磁相含量增加.同时由于FePt薄膜的晶粒长大，部分软硬磁晶粒之间的交换耦合作用失效；600℃热处理后，FePt的面心立方相已经完全转变为面心四方相，薄膜矫顽力由硬磁相之间的静磁作用贡献. 关键词： 磁性薄膜 纳米晶 磁性能 热处理     

CdS纳米颗粒填充的自支撑多孔硅光致发光特性

为了研究CdS纳米颗粒填充的自支撑多孔硅的光致发光特性,选用电阻率为0.01~0.02Ω·cm的P型硅片,先采用二步阳极氧化法制备自支撑多孔硅,再利用电泳法将CdS纳米颗粒填充入该自支撑多孔硅中.采用扫描电子显微镜、X射线能谱分析、X射线衍射分析、光致发光谱分析对所制备样品的形貌、相结构、组份及发光性能进行研究.实验结果表明:自支撑多孔硅内部成功填充了CdS纳米颗粒,该CdS纳米颗粒衍射峰为(210);CdS纳米颗粒填充的自支撑多孔硅光致发光峰峰位发生红移,且从570nm转移到740nm;电泳时间直接影响CdS纳米颗粒的填充量,导致相关的发光峰强度及发光峰位明显不同.     

纳米多孔金薄膜显微结构分析

 采用亚硫酸金钠为主盐,在阳极氧化铝模板上进行了化学镀和电镀金实验研究。通过扫描电子显微镜和X射线衍射分析测试表明:采用以上两种方法均能制备出纳米多孔金薄膜。两种方法制备的多孔金薄膜微观结构存在较大的差异。化学镀制备的多孔金薄膜微观上是枝晶状的,电镀制备的多孔金薄膜微观上由纳米线构成。     

水热腐蚀时间对铁钝化多孔硅表面形貌和光致发光的影响

采用水热腐蚀法制备了4个腐蚀时间不同的铁钝化多孔硅样品,铁钝化多孔硅样品表面呈海绵结构,随着腐蚀时间增加,样品表面的平整度下降,腐蚀孔尺寸差别有增大的趋势。在250nm光激发下,样品发光峰位于620nm附近,半峰全宽约130nm。腐蚀时间从10min增加到40min,4个样品的发光峰并未出现定向的红移或蓝移。结合样品傅里叶变换红外吸收光谱的结果,铁钝化多孔硅的光致发光行为可归因于量子限制-发光中心作用,相应的辐射复合发光中心为非桥氧空穴。     

一种新的制备ZnO纳米粒子的方法--阴极电沉积法

用阴极电沉积法制备高质量ZnO纳米薄膜，电沉积采用含有不同浓度的ZnCl2的非水二甲基亚砜溶液做电解液，室温下恒流沉积，得到纳米ZnO薄膜。研究了ZnCl2浓度对薄膜结构和光学性质的影响。沉积薄膜的ZnO粒径尺寸分别为9．8，10．4，14．5nm。随着ZnCl2浓度的增加而增大。薄膜的可见光致发光谱以紫外的自由激子发射为主。研究表明：以浓度为0.03mol/L的ZnCl2电解液制备的ZnO薄膜光学性质最好。     

The effect of laser remelting in the formation of tunable nanoporous Mn structures on mild steel substrates

Nanoporous manganese was fabricated by a three-step process involving high power laser cladding of a homogeneous Cu₄₀Mn₆₀ alloy coatings onto a mild steel substrate, laser remelting for tuning the grain size and the composition homogeneity followed by selectively electrochemical de-alloying for removal of Cu element and formation of nanoporous Mn. The microstructure and homogeneity of the precursor Cu₄₀Mn₆₀ alloys have a significant influence on the evolution of nanopores during selectively electrochemical de-alloying. Laser remelting can significantly refine the microstructure. The second dendrite arm spacing decreases with increasing of laser remelting scanning speed. A SDAS of 1.17 μm was obtained at the laser scanning speed of 133 mm/s. When the remelting scanning speed reaches 100 mm/s, a nanoporous structure with average pore size less than 100 nm was achieved under optimized dealloying electrode current density about 2 mA/cm². Nanoporous Mn with nanopore sizes ranging from 80 to 130 nm was fabricated by this method. Surface-enhanced Raman scattering characteristics of the nanoporous materials have been investigated. It is found that smaller nanoporosity leads to significant improvements in surface-enhanced Raman scattering.     

Fabrication of nanoporous AuPt nanoparticles modified indium tin oxide electrode and their electrocatalytic effect

This paper describes the synthesis of nanoporous AuPt nanoparticles (np-AuPt NPs) by galvanic replacement reactions that involve large-sized silver nanoparticles (Ag NPs) electrodeposited upon an indium tin oxide (ITO) film glass as a sacrificial template. Compared to a previous synthetic route based on the formation and dealloying of Ag/Au alloy nanoparticles, this method can easily fabricate nanoporous Au nanoparticles (np-Au NPs), as well as nanoporous AuPt nanoparticles. Structural characterization indicated that the products had a particle size of ～170 nm with a ligament size of tens of nanometers. The fabricated np-Au NPs/ITO and np-AuPt NPs/ITO electrode were also tested and compared for the oxidation of hydrogen peroxide in a phosphate buffer solution (pH 7.0). The np-AuPt NPs/ITO electrode showed a much higher electrocatalytic efficiency and detection sensitivity to hydrogen peroxide than the np-Au NPs/ITO electrode.     

Preparation and electrochemical performances of nanoporous/cracked cobalt oxide layer for supercapacitors

Nanoporous/cracked structures of cobalt oxide (Co₃O₄) electrodes were successfully fabricated by electroplating of zinc–cobalt onto previously formed TiO₂ nanotubes by anodizing of titanium, leaching of zinc in a concentrated alkaline solution and followed by drying and annealing at 400 °C. The structure and morphology of the obtained Co₃O₄ electrodes were characterized by X-ray diffraction, EDX analysis and scanning electron microscopy. The results showed that the obtained Co₃O₄ electrodes were composed of the nanoporous/cracked structures with an average pore size of about 100 nm. The electrochemical capacitive behaviors of the nanoporous Co₃O₄ electrodes were investigated by cyclic voltammetry, galvanostatic charge–discharge studies and electrochemical impedance spectroscopy in 1 M NaOH solution. The electrochemical data demonstrated that the electrodes display good capacitive behavior with a specific capacitance of 430 F g^?1 at a current density of 1.0 A g^?1 and specific capacitance retention of ca. 80 % after 10 days of being used in electrochemical experiments, indicating to be promising electroactive materials for supercapacitors. Furthermore, in comparison with electrodes prepared by simple cathodic deposition of cobalt onto TiO₂ nanotubes(without dealloying procedure), the impedance studies showed improved performances likely due to nanoporous/cracked structures of electrodes fabricated by dealloying of zinc, which provide fast ion and electron transfer routes and large reaction surface area with the ensued fast reaction kinetics.     

激光烧蚀制备分布反馈式有机激光器件

采用激光烧蚀的方法结合激光全息技术,直接在高分子聚合物MEH-PPV薄膜表面烧蚀光栅结构,制备了分布反馈式有机激光器。这一方法具有工艺简单、光栅参数的可控性和重复性好等优点。器件MEH-PPV的膜厚是400 nm。利用波长为355 nm的Nd-YAG纳秒激光器进行单脉冲烧蚀,获得的光栅周期和光栅高度分别为370 nm和 100 nm。利用飞秒激光放大器作为泵浦源激射DFB激光器件,得到激射阈值约为182 μJ·cm^-2·pulse^-1,光谱的波峰约在609 nm处,半高宽为4.2 nm。通过改变两光束的夹角获得了周期为360, 370, 380, 390 nm的光栅,它们对应的激光波峰分别为602.91, 609.24, 613.26, 619.01 nm。     

Uniaxial compression testing of bulk nanoporous gold

Abstract

The mechanical properties of bulk nanoporous gold (np–Au) with a relative density of 0.35 were investigated by compression testing of millimetre-scale specimens. Young’s modulus, Poisson’s ratio and yield strength values were determined from uniaxial, quasi-static experiments using a custom-built mechanical testing system. The cuboid-shaped specimens were fabricated following a specific, controlled process (including cutting and grinding) that guaranteed a precise and repeatable geometry. The np–Au structure was created from a silver–gold alloy by electrochemical dealloying in nitric acid. Mechanical properties obtained from compression testing are compared to values reported in the literature and to scaling relations. Values are found to agree with a recently proposed scaling relation for the yield strength of np–Au that incorporates a ligament size effect and a modified scaling exponent.     

Surface effects on saturation magnetization in nanoporous Ni

Nanoporous Ni specimens with ligament lengths of 10–210 nm and specific surface areas of 0.03–0.58 nm^?1 were fabricated by the dealloying of Ni_0.25Mn_0.75 alloy and annealing at 473–873 K, and saturation magnetization investigated in terms of their size dependence. Saturation magnetization decreased with decreasing ligament length or increasing specific surface area. This trend is the same as that for nanoparticle Ni. However, the saturation magnetization of nanoporous Ni tends to be lower than that of the nanoparticle Ni when their specific surface areas are the same. It is suggested, therefore, that the surface effect due to a noncollinear arrangement is enhanced by the surface defects in the nanoporous Ni.     

激光熔覆铜锰合金选择性脱合金制备纳米多孔涂层的研究

本文通过激光加工结合电化学腐蚀脱合金法, 成功实现了纳米多孔涂层的制备. 采用激光熔覆首先在45钢表面制备了成形良好、稀释率低的铜锰合金熔覆层, 并通过快速重熔工艺实现了初始材料组织细化. 研究表明, 在不同的电解液下,铜锰合金的临界腐蚀电位出现了明显的偏移; 在不同的腐蚀电流下,铜锰合金腐蚀后的形貌迥异. 最终,通过选择性腐蚀成功实现了纳米多孔铜和纳米多孔锰涂层的制备, 并利用电位-pH图对脱合金的选择性腐蚀进行了详细的理论解释.