X射线光电子能谱测定固体粉末样品的制备方法比较

样品制备方法对X射线光电子能谱测试结果具有较大影响,以导电样品锂电材料和不导电样品奶粉为测试对象,探讨了不同制样方法对两者测试效果的影响.试验结果表明,导电样品锂电材料使用导电胶铜片制样效果较好,而不导电样品奶粉使用导电胶压片或3M胶带压片效果较好.     

制样方法对固体粉末X射线光电子能谱测试结果的影响

为了得到准确且分辨率高的X射线光电子能谱(XPS)数据,采用不同制样方法对不同类型的导电、不导电和混合粉末的测试结果进行了研究. 从图谱半峰宽、是否有荷电、真实性、制样效率和数据处理等方面阐述不同制样方法对测试结果的影响. 试验结果表明,对于导电和不导电粉末,粘取制样略优于铟片制样,其中使用碳导电胶带制样效果更好. 对于混合样品,Scotch双面胶带粘样后的测试结果优于其他3种制样方式. 此外,铟片制样可作为数据处理时荷电校正的参考方法.     

银包玻珠核壳复合粒子的表面处理及环氧导电胶的电性能

以化学还原法合成的银包玻珠核壳复合粒子(Ag/GM)为原料, 乙二胺为表面处理剂, 制备了表面吸附有乙二胺的Ag/GM, 并用它作为导电填料组成了导电胶. 与化学还原法直接合成或沸水处理的Ag/GM相比, 乙二胺处理的Ag/GM能更有效地分散在环氧树脂胶黏剂中, 且能与环氧树脂基体产生化学键合, 降低Ag/GM和环氧树脂基体间的界面能, 用其制备的导电胶的导电率较高, 导电渗滤阈值较低. 同时, 结合导电网络理论和等效电路图, 阐明了用乙二胺处理的Ag/GM作填料制备的导电胶具有较低体积电阻率的原因.     

环氧树脂导电胶用铜粉抗氧化性

根据铜本身具有的性质,选用γ-氨丙基甲基二乙氧基硅烷（KH-902）对铜粉进行改性,并采用FT-IR、超景深显微镜、TG、SEM及EDS技术对改性铜粉及铜粉导电胶进行表征。 结果表明,添加硅烷偶联剂KH-902可以有效改善铜粉的易氧化的问题,当添加量为3%时,不仅可以明显改善铜粉导电胶在高温固化下抗氧化性能,而且铜粉在环氧树脂胶体体系中能够均匀分散,且铜粉与铜粉之间的搭接紧密,具有良好的导电性能,体积电阻率仅1.31×10-2 Ω·cm。     

关于Pt-Sn/γ-Al_2O_3催化剂X光电子能谱分析方法的研究

本文总结了应用XPS分析Pt-Sn/Υ-Al_2O_3类催化剂的方法。文中提出:将催化剂颗粒直接压片再用铝箔包边的制样方法,所录取的光电子峰较强,分辨率也较高。选用Al靶作为激发源,可避免在锡的价态区域内出现干扰峰。对荷电效应的校正,以内标法为主,并同时采用电中和法。另外,为获得还原类样品的真实信息,应保证它们从制备到分析的全过程都处于与空气隔绝的状态。     

芯片电泳推拉式压力进样方法

芯片电泳作为微流控分析系统的典型代表,广泛涉及材料、微加工方法、微液流控制、分离模式和检测方法等诸多方面.与传统分析系统一样,样品制备和引入也是微全分析系统实现样品到结果首先面临的问题.电进样一直是芯片电泳系统的主流进样方法.而传统毛细管电泳系统中与电进样同样经常使用的压力进样方法则很少用于芯片电泳系统.     

Gd3+掺杂对NaY(MoO4)2:Eu3+荧光粉发光性能影响的研究

采用微乳液-水热法制备了NaY(MoO4)2∶Eu3+和Na(Y,Gd)(MoO4)2∶Eu3+荧光粉.利用X射线衍射(XRD)、扫描电镜(SEM)和荧光光谱手段对样品进行了表征.所制样品的X射线衍射峰与标准卡片PDF# 82-2369基本吻合.SEM图谱显示所制备的纳米粒子直径为0.5～0.8μm.激发-发射光谱显示...     

XPS分析中使用样品磁透镜引起的谱峰位移和峰形畸变

发现当使用Mg/Al双阳极和样品磁透镜进行非导电样品（或与样品托绝缘的导电样品）的X射线光电子能谱分析时，谱峰出现异常大的位移和谱形出现畸变；在同时使用电子中和枪时谱峰位移变小，当导电样品与样品托有良好的电接触时谱峰位移消失；作者提出这种异常大的位移来自样品荷电效应，后者是由于样品磁透镜的磁场与来自X射线枪A1窗的低能杂散电子发生了相互作用并使这些杂散电子不能到达样品表面起中和作用所致。     

荷电膜的研究进展

荷电膜以其特殊的分离机理,使之与电中性膜相比在分离性能、通量及膜的使用寿命等方面具有不可比拟的优势.大多数的荷电膜是经过一系列物理化学改性制得的,荷电膜材料的研究为新型膜材料的开发拓宽了领域,随着对膜性能要求的日益提高,荷电膜的研究具有重要的意义.本文首先介绍了荷电膜所用到的材料及其用途,并对所用到的材料进行分类,然后重点论述了荷电膜的制备及其表征方法(膜电位的测试方法),最后指出荷电膜需要进一步深入研究的内容.     

用FTIR定量研究环氧树脂固化反应动力学制样方法的确定

利用FTIR进行环氧树脂固化反应的动力学研究需要精确的样品制备方法,摸索到一套合适的样品制备方法。将KBr研成细粉,通过孔径为0.074mm筛子使粒子均匀,在120~150℃下加热24h后,取0.25g,放入红外压片模具,在压力为800MPa条件下加压时间5~10min,压制成厚度为0.08mm的透明均匀KBr盐片。将环氧树脂均匀涂在这种KBr盐片上,放入微型反应器中反应,之后一同放入FTIR仪中进行扫描,实验证明这种制样方法可以保证红外定量分析的可靠性。     

Electrically conductive epoxy‐based nanocomposite adhesives loaded with silver‐coated copper and silver‐coated reduced graphene oxide nanoparticles

In this research, a conductive adhesive based on epoxy resin as the polymer matrix and silver‐coated copper powder and silver‐coated reduced graphene oxide as conductive fillers was synthesized. Graphene oxide was synthesized by modified Hummer's method. It was reduced and modified by silver powder. Copper particles were coated with silver using the electroless plating method. Finally, conductive nanocomposite adhesives were prepared using conductive fillers with different weight fractions. The structural properties of fillers were identified by Fourier‐transform infrared (FTIR) and induced coupled plasma (ICP) analysis and the morphology of the samples by scanning electron microscopy (SEM). Finally, conductive properties, lap shear strength, and thermal stability of adhesive were evaluated. The conductive adhesive prepared with optimized properties have 70% weight percentage silver‐coated copper powder and 1% weight percentage silver‐coated reduced graphene oxide. The bulk resistivity of the optimum sample was 1.6 × 10^‐2 Ω.cm, and the lap shear strength was 7.10 MPa. Also, thermogravimetric analysis showed that the weight loss of adhesive decreased from 88.72% to 30.55% during heating, which showed the addition of fillers improves the thermal stability of adhesive.     

The effect of mixing methods on the dispersion of carbon nanotubes during the solvent-free processing of multiwalled carbon nanotube/epoxy composites

Several solvent-free processing methods to disperse multiwalled carbon nanotubes (MWCNTs) in bisphenol F-based epoxy resin were investigated, including the use of a microfluidizer (MF), planetary shear mixer (PSM), ultrasonication (US) and combinations. The processed mixture was cured with diethyl toluene diamine. Three complimentary techniques were used to characterize the dispersion of the MWCNTs in cured composite samples: optical microscopy, micro Raman spectroscopy, and scanning electron microscopy (SEM). For sample MF + PSM, optical micrographs and Raman images showed reduced agglomeration and a homogeneous distribution of MWCNTs in the epoxy matrix. SEM analysis of fractured specimen after tensile testing revealed breakage of nanotubes along the fracture surface of the composite. A comparison of the MWCNT dispersion in the epoxy samples processed using different methods showed that a combination of MF and PSM processing yields a more homogeneous sample than the PSM or US + PSM processed samples. Mechanical testing of the composites showed about 15% improvement in the tensile strength of samples processed by the MF + PSM method over other methods. Thermogravimetric analysis (TGA) results showed a small decrease in the onset degradation temperature for poorly dispersed samples produced by PSM compared with the well-mixed samples (MF + PSM). These results strongly suggest that the MF + PSM processing method yield better-dispersed and stronger MWCNT/epoxy composites. © 2012 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2013     

Preparation and Characterization of DGEBA/EPN Epoxy Blends with Improved Fracture Toughness

The physical and mechanical properties of blends composed of two kinds of epoxy resins of different numbers of functional groups and chemical structure were studied.One of the resins was a bifunctional epoxy resin based on diglycidyl ether ofbisphenol A and the other resin was a multifunctional epoxy novolac resin.Attempt was made to establish a correlation between the structure and the final properties of cured epoxy samples.The blend samples containing high fraction of multifunctional epoxy resin showed higher solvent resistance and lower flexural modulus compared with the blends containing high fraction of bifunctional epoxy resin.The epoxy blends showed significantly higher ductility under bending test than the neat epoxy samples.The compressive modulus and strength increased with increasing of multifunctional epoxy in the samples,probably due to enhanced cross-link density and molecular weight.Morphological analysis revealed the presence of inhomogeneous sub-micrometer structures in all samples.The epoxy blends exhibited significantly higher fracture toughness (by 23％ at most) compared with the neat samples.The improvement of the fracture toughness was attributed to the stick-slip mechanism for crack growth and activation of shear yielding and plastic deformation around the crack growth trajectories for samples with higher content of bifunctional epoxy resin as evidenced by fractography study.     

Statistical Analysis of Polymer Nanocomposites for Mechanical Properties

Epoxy resins, due to their high stiffness, ease of processing, good heat, and chemical resistance obtained from cross-linked structures, have found applications in electronics, adhesives coatings, industrial tooling, and aeronautic and automotive industries. These resins are inherently brittle, which has limited their further application. The emphasis of this study is to improve the properties of the epoxy resin with a low-concentration (up to 0.4% by weight) addition of Multi-Walled Carbon Nanotubes (MWCNTs). Mechanical characterization of the modified composites was conducted to study the effect of MWCNTs infusion in the epoxy resin. Nanocomposites samples showed significantly higher tensile strength and fracture toughness compared to pure epoxy samples. The morphological studies of the modified composites were studied using Scanning Electron Microscopy (SEM).     

含导电炭黑环氧树脂固化过程电测法

用电阻法测定了添加导电炭黑的环氧树脂固化过程。由于载流子是导电炭黑提供的电子,因而体系电阻率大大降低,测量方法得以简化,并使固化过程的测量可以一直进行,从而发现了环氧树脂固化过程存在着两个阶段:第一阶段,反映树脂粘度增加的电阻值上升;第二阶段,反映树脂密度增加的电阻值下降。     

三元脂肪酸/膨胀石墨复合相变材料的制备、包覆定形及热性能

采用癸酸、 月桂酸和棕榈酸的三元共晶混合物作为相变材料, 以膨胀石墨为基体, 通过膨胀石墨多孔结构的毛细吸附和复合涂饰剂的包覆定形, 将多元相变材料固定在膨胀石墨的孔道结构中, 制备出结构稳定、 密封性能优异、 热稳定性好和高导热的新型三元脂肪酸/膨胀石墨复合定形相变材料. 膨胀石墨具有膨胀疏松的多孔结构和良好的吸附性能; 其熔融潜热为95.6 J/g, 结晶焓为82.8 J/g, 说明其具有很好的相变蓄热特性和热循环稳定性; 材料的导热性能可增加至0.738 W/(m·K), 与脂肪酸相比得到大幅度提高.     

Thermal and mechanical properties of polysulfide/epoxy copolymer system: the effect of anhydride content

Polymerization of a ternary system containing polysulfide (PS), as a liquid elastomer, diglycidylether of bisphenol A resin, and phthalic anhydride was conducted using “design of experiment” technique. The polymerization progress with respect to concentration variations of components were studied by Fourier transform infrared spectroscopy. Fourier transform infrared spectroscopy studies showed that the anhydride plays a decisive role in curing reaction so that, in its absence, the epoxy/PS mixture becomes gel in about 2 hr, whereas, by addition of the anhydride, the pot life of the system can be extended to 48 hr. The cured samples were investigated by thermal gravimetry analysis and differential scanning calorimetry to evaluate thermal properties. Thermal gravimetry analysis and differential scanning calorimetry results indicated that two different soft and hard segments are formed, which have different thermal decompositions. The soft segment consists of loose etheric bonds, which are attributed to PS, and the hard segment is formed during the etherification and esterification reactions of the epoxy resin. Tensile strength test was performed to investigate the mechanical properties of PS/epoxy/anhydride‐cured systems. The results showed that the tensile strength, elongation‐at‐break, and the fracture energy of specimens are essentially dependent on PS/anhydride ratios. Two different segments impart high strength and ductility simultaneously. Copyright © 2013 John Wiley & Sons, Ltd.     

环氧树脂掺量对发光树脂透水混凝土性能的影响

选择环氧树脂E51作为改性填料,制备出一系列不同树脂质量分数（0%、2%、4%和6%）的发光树脂透水混凝土。环氧树脂的引入使发光树脂透水混凝土的抗压强度和抗折强度均得到了提高,且随着树脂掺量的增加呈现出先升高后降低的趋势,在树脂质量分数为4%时,抗压强度和抗折强度均达到最大值21.7和6.11 MPa,发光树脂透水混凝土的透水系数随着环氧树脂质量分数的增加呈现出先降低后升高的趋势,在4%时透水系数最低为5.1 mm/s。微观形貌分析发现未经改性的环氧树脂透水混凝土的断面处有明显的裂痕和气孔,整体结构较为疏松,在引入环氧树脂后,裂痕和气孔的数量明显减少,整体结合较为紧密,发光树脂透水混凝土的发光时间与树脂质量分数关系不大,且发光透水混凝土在光照1 h下可以保持超过5 h的较为高效的发光时间。     

Enhanced conductivity composites for aircraft applications: carbon nanotube inclusion both in epoxy matrix and in carbonized electrospun nanofibers

The potential of carbonized electrospun nanofiber mats to render epoxy resin composites for aircraft applications electrically and thermally more conductive was investigated. The effect of carbon nanotube inclusion both inside the carbon nanofiber and in the epoxy resin matrix material was studied, in order to reveal any synergistic effects of multilevel presence of nanosized reinforcements on the conductivity and mechanical properties. The carbon nanotube inclusion into the carbonized nanofibers increased the electrical conductivity of the samples by 20–50% and the thermal conductivity by approximately three times leading to a higher value than that of the conventional composites. The preparation of layered composites with a conductive upper layer containing nonwoven carbon nanofabric and a load bearing lower layer with conventional unidirectional carbon fiber reinforcement can offer a cost‐effective and weight‐saving solution for the replacement of metal meshes in structural aircraft composites. Copyright © 2014 John Wiley & Sons, Ltd.     

Porous epoxy thermosets obtained by a reaction-induced process and their characterizations

A novel reaction-induced method with the aid of solvent for porous thermosetting epoxy was first carried out. Investigations of pore structure using scanning electron microscope （SEM） showed that porous epoxy networks with average pore size ranging from 3 to 20 μm were obtained. The pore structure generated by this method can be tailored by changing the solvent content.