XPS法研究煤表面碳官能团的变化及硫迁移行为

采用XPS对六枝（Liuzhi）和遵义（Zunyi）原煤及其固定床热解半焦表面的含碳官能团和硫迁移行为进行了研究。在氮气气氛下,在400℃～700℃遵义煤焦表面O=C－O, C－H 和 C－C含量与原煤相比,呈现下降趋势,而C=O和O－C－O、C－O含量却呈现增加趋势; 六枝煤焦表面的O=C－O、C=O和O－C－O、C－O含量的变化规律与遵义煤相似,而C－H和C－C含量的变化却与遵义煤相反。在氢气气氛下, 遵义煤焦表面不仅O=C－O含量与原煤相比下降, 而且C=O和O－C－O、C－O含量也下降,但C－H和C－C含量却增加; 六枝煤除了C=O 和O－C－O含量下降外, 其他官能团的变化与其在氮气气氛下相似。两种煤焦表面S/C比在氮气气氛下随着温度的升高而升高,氢气气氛下在400℃~600℃随着温度的升高却下降,700℃又显著升高。这说明在热解过程中硫在两种气氛下都能从体相向表面迁移,但是氢气能够和含硫自由基反应,所以氢气气氛下煤焦表面的S/C比率低于其氮气气氛下的。     

氧气氛中紫外光辐照官能化HDPE的结构与性能研究

采用FT－IR，XPS，WAXD，DXC，凝胶和表面自由能力分析，研究了氧化氛中紫外辐照官能化高密度聚乙烯（HDPE）的化学结构、晶体结构和表面自由能的变化。与空气相比，在氧气氛中紫外辐照HDPE能提高C－O，C（＝O）O和C＝O等含氧基团的引入速度，同时又能降低HDPE中的凝胶含量，在空气和氧气氛中紫外辐照后，HDPE的晶型没有发生变化，仍为正交晶系；HDPE的晶胞参数a,b,c以及（110），（200），（020），（011），（111）等晶面间距基本保持不变；HDPE的熔融温度下降，但熔融热焓升高，结晶度增大，表面自由能增大，且在氧气氛中辐照HDPE的变化幅度较大。     

木粉/聚乙烯复合材料的等离子体表面处理——等离子体处理时间对复合材料表面特性的影响

为改善木粉/聚乙烯复合材料的表面粘接性,实现木粉/聚乙烯复合材料的无缝连接,利用低温等离子体处理技术,对木粉/聚乙烯复合材料进行了表面处理.采用接触角测试、傅立叶变换红外光谱分析(FTIR)以及X射线光电子能谱分析(XPS)研究了等离子体处理前后复合材料表面性能的变化.试验结果表明,经等离子体处理后,复合材料表面的接触角减小,表面润湿性得以改善;FTIR分析结果表明,经等离子体处理后,复合材料表面有—OH、—C=O和—O—C=O基团生成;XPS分析表明,经等离子体处理后,复合材料表面含氧基团的含量增加,在较短的时间内表面氧元素含量增加会达到平衡,且生成大量的—O—C=O基团。     

电晕放电引发丙烯酸表面接枝LDPE薄膜的研究

本文采用接枝量测定、ATRIR和ESCA研究了电晕放电引发丙烯酸表面接枝LDPE薄膜,实验结果表明:电晕放电能有效地引发丙烯酸在LDPE薄膜表面的接枝聚合反应,随反应时间延长、反应温度提高和丙烯酸单体浓度增大,表面接枝量增大。当丙烯酸浓度为20%、聚合温度为70℃、反应15小时时,经电晕放电处理72秒后的LDPE薄膜表面接枝量高达22055μgcm2。     

光催化作用下丙酮改性对神府煤煤岩组分表面性质影响的研究

研究了光催化作用下丙酮对不同煤岩组分表面改性的作用,分析了改性时间对神府丝炭和神府镜煤表面性质的影响,为建立增大煤岩组分表面性质差异的新方法提供理论依据。光催化作用下丙酮改性可以明显改变煤岩组分表面性质,改性时间为3min时,神府丝炭和神府镜煤润湿性差异最大。改性后煤岩组分表面C－O、C=O和COO－等含氧官能团含量发生了变化,且神府丝炭表面C=O和COO－含量的变化较神府镜煤更为明显。
     

沉淀铁催化剂在F-T合成反应过程中的物相变化

 采用元素分析、X射线衍射和穆斯堡尔谱等手段研究了喷雾干燥沉淀Fe-Cu-K/SiO2催化剂在F-T合成反应过程中的物相变化. 结果表明,新鲜催化剂样品主要由α-Fe2O3组成,且81.1%的α-Fe2O3粒径小于13.5 nm. 随着反应时间的延长,催化剂表面碳沉积物的含量逐渐增多,不饱和度逐渐增大; χ-Fe5C2的含量逐渐增多,Fe3O4的含量逐渐减少并趋于稳定. 超顺磁Fe3+的含量呈先增加后减少的变化趋势. 由于碳沉积物是由CO生成的,而χ-Fe5C2是由α-Fe2O3经Fe3O4生成的,故催化剂表面碳沉积物的生成先于χ-Fe5C2的生成.     

交流电晕对高温硫化硅橡胶性能的影响

采用针-板电极交流电晕放电试验装置研究了电晕放电对高温硫化硅橡胶憎水性、不同温度下憎水恢复性、力学性能和电气性能的影响,结果表明电晕放电作用不同时间后高温硫化硅橡胶材料憎水性丧失是一个渐进的过程,严重时硅橡胶材料憎水性会暂时性丧失,硅橡胶材料在不同温度下憎水性恢复速度不同,电晕放电作用后硅橡胶材料憎水接触角不能恢复至新试样初始水平.电晕放电不同时间后硅橡胶材料表面受电晕放电影响的范围逐渐扩大,表面产生了黑色粉末状电晕环,前期发展较快,然后逐渐由表层损坏转为纵深方向发展,材料表面和内层均可能遭到不同程度电蚀损,硅橡胶主链基团Si—O—Si、侧链基团Si—CH3和甲基中C—H键相对强度均随着电晕放电作用时间的增加呈下降趋势,材料拉伸强度和硬度有所下降,介电性能明显下降.     

环境温度对紫外辐照HDPE结构与性能的影响研究

采用元素、XPS、GPC分析，凝胶和力学性能测定，研究了空气中不同环境温度下紫外辐照官能化HDPE的结构、粘着性以及紫外辐照官能化HDPE对HDPE/聚乙烯醇(PVA)体系的增容作用。实验结果表明，提高环境温度可显著提高引入C-O、C(=O)O和C=O等含氧基团的速度。在相同辐照时间下，随环境温度提高，辐照HDPE的分子量下降、分子量分布变宽以及剥离强度提高的幅度增大，并在70℃时产生凝胶。较高环境温度下辐照的HDPE对HDPE/PVA共混体系有较好增容作用，在HDPE/PVA(83/17)体系中加入10%(质量分数)的70℃环境温度下辐照24h的HDPE，共混物的拉伸屈服强度和缺口冲击强度分别从30.8MPa和110J/m提高到34.9MPa和142J/m。     

电子辐照及再结晶P(VDF-TrFE)共聚薄膜红外光谱研究

利用傅立叶变换红外光谱(FT-IR)研究聚偏氟乙烯与聚三氟乙烯共聚薄膜[P(VDF0.80-TrFE0.20)]的电子辐照和再结晶处理过程中分子链构型变化和化学变化, 为深入探讨辐照的改性机理提供依据. 研究发现, 辐照后薄膜分子链全反构型百分含量随吸收剂量增大而迅速减少, TG构型和T3G构型百分含量显著增多. 而当吸收达一定剂量时, 三种构型相对含量基本不再变化, 表明高剂量辐照时样品极性回升不依赖分子链构型中全反型的含量的增多, 而是和高交联度的边界效应有关. 再结晶过程中分子链构型变化恰好和辐照效应产生的变化相反, 并且形成了更加稳定的C=C共轭结构.     

聚酰胺硅胶吸附茶多酚的红外光谱研究

IR谱表明:聚酰胺硅胶吸附剂中,聚酰胺的N—H和硅胶表面OH以氢键结合,υC=O无位移;室温下该吸附剂中C=O和茶多酚中O—H作用后,υC=O和υO—H分别红移了11cm-1和18cm-1;而与咖啡因及氨基酸作用后υC=O无位移。     

Effect of Corona Discharge Treatment on the Dyeability of Low-Density Polyethylene Film

The effect of corona discharge on low-density polyethylene (LDPE) film was studied in terms of surface functionality and surface energetics of the film surfaces, improving the dyeability. The introduction of a polar group (O=C-O, C=O, and C-O) to a corona-treated LDPE film with acrylic acid could be confirmed by ESCA. The Owens-Wendt and Wu models using geometric means were studied to analyze the surface free energy of corona-treated film. It was found that the corona-treated LDPE film did lead to an increase in surface free energy, mainly due to the increase of its specific (or polar) component as the corona discharge power increased. Also, the K/S values were increased as the concentrations of dye increased. From the acid-base interaction point of view, it was found that the graft polymerization of acrylic acid onto the corona-treated LDPE film plays an important role in growing the acidic character which is one of the specific components of surface free energy, resulting in improving the dyeability with basic dyeing agent. A direct linear relationship is shown between the O(1s)/C(1s) ratio and the resulting K/S value or the specific component for this work. Copyright 2001 Academic Press.     

Effect of reactive oxygen species generated with ultraviolet lamp and plasma on polyimide surface modification

Understanding the effect of reactive oxygen species (ROS), such as singlet oxygen molecule and atomic oxygen, on polyimide (PI) film properties, such as wettability, morphology, and chemical bonding state, is essential for further development of PI‐based surfaces. We investigated the effect of different ROS generated during ultraviolet (UV) and plasma treatment in oxygen gas on surface modification of Kapton PI. Different surface modification techniques, UV and plasma treatment, are known to generate different ROS. In this work, we demonstrate the effect of different ROS on PI surface modification. From the diagnostics of ROS by means of electron spin resonance and optical emission spectroscopy, we confirmed that during UV treatment, excited singlet oxygen molecules are the main ROS, while plasma treatment mainly generated atomic oxygen. The wettability of PI surface treated by UV and plasma resulted in hydrophilic PI surfaces. XPS results show that the wettability of PI samples is mainly determined by their surface O/C ratio. However, chemical bonding states were different: while UV treatment tended to generate C=O bonds, while plasma treatment tended to generate both C―O and C=O bonds. Singlet oxygen molecules are concluded to be the main oxidant during UV treatment, and their main reaction with PI was concluded to be of the addition type, leading to an increase of C=O groups on the surface of PI film. Meanwhile, atomic oxygen species were the main oxidant during plasma treatment, reacting with the PI surface through both etching and addition reaction, resulting in a wider variety of bonds, including both C―O and C=O groups.     

Influence of the Particle Size of CaCO3 on the Adhesion of Filled EVA Materials

A surface treatment with corona discharge was used to improve the adhesion properties of ethylene vinyl acetate copolymer (EVA) containing small amounts of four CaCO₃ with different particle size. The nature of the surface modifications produced by the corona discharge treatment and the adhesion to a polychloroprene adhesive were assessed. Treatment of CaCO₃ filled EVA with corona discharge produced a decrease in water contact angle value, irrelevant to the different particle size of the calcium carbonates. The corona discharge treatment created C-O and C=O moieties on the EVA surface and also increased the peel strength, more markedly as the CaCO₃ particle size increased. In general, a mixed (adhesion + cohesive in the EVA) failure in the filled EVA material was produced (assessed by IR-ATR spectroscopy and SEM micrographs of the failed surfaces), but the failure was more cohesive in the EVA containing higher particle size CaCO₃. The durability of the joints was also studied.     

电火花引发丙烯酰胺接枝BOPP薄膜的研究

采用FT-IR,ESCA,试样与水接触角和接枝率的测定探索了电火花用于引发丙烯酰胺(AAM)在BOPP薄膜表面接枝聚合反应的方法,研究了接枝BOPP薄膜的表面结构和亲水性能。结果表明,电火花能有效地引发AAM在BOPP薄膜表面的接枝聚合反应,随着电火花处理时间和接枝反应时间的延长,AAM在BOPP薄膜表面的接枝率增大。电火花处理10min,BOPP薄膜在70℃,20%(质量分数)的AAM水溶液中反应1h,接枝率高达2.06%。接枝后BOPP薄膜与水的接触角显著下降,亲水性能得到明显改善。     

氮化铝薄膜的组成分析

Al N是一种无机非铁性压电材料 ,具有宽的带隙、高的电阻率、高的抗击穿电压、高的声传播速率和低的传输损耗 ,在微电子器件中有着广泛的应用前景 [1] .由于 Al N薄膜的声速在整个无机非铁性材料中最高 ,因而成为 GHz级声表面波器件的首选材料 [2 ] .要实现 Al N薄膜的表面声波器件应用 ,不但结构重要 [1] ,组成也很重要 [3] ,因为薄膜的组成对其性质影响很大 .Al N压电薄膜要求整个膜层的 Al/N比一致 .富 Al会使薄膜介电性能变差 ,富 N会使薄膜结构致密度变差 .因而对其组成研究是非常重要的 .Penza等 [3] 采用X射线光电子能谱 ( X…     

Effect of the corona treatment and of the 1,4-cyclohexanedimethanol on the surface characteristics of the poly(ethylene terephthalate) film

Several techniques have been applied for the characterization of three PET films surfaces: homopolymer PET film, corona treated PET film and a poly(ethylene terephthalate-co-1,4-cyclohexanedimethanol) film. The objective of this work is to investigate and to apply precise and mutually complementary techniques which give detailled information about theses surfaces, as there are few papers with global and conclusive results. The film surfaces were investigated to support the development of new products and envisage new apllications to the existent films. Scanning electron micrographs, attenuated total reflection Fourier transform infrared spectroscopy (FTIR-ATR) and multiple internal reflection Fourier transform infrared spectroscopy (FTIR-MIR) spectra show that the chemical composition, topography and surface roughness of the films are different. The corona-treated PET film shows high surface tension value due to the major contribution on the polar groups and oxidation level acquired. The copolyester film is much less crystalline than the other films analyzed, as demonstrated by refractive index measurements and X-ray photoelectron spectroscopy (XPS). The amorphous structures obtained and the high tension level of the corona-treated films provide a better understanding of the adhesion phenomena. In view of results obtained, one can assume that corona treated films owing to its higher surface tension and films with CHDM owing to its surface amorphization should provide manufacturing industries better processing conditions than films without surface treatment and also higher levels of adhesion to paints and coatings.     

Surface modification of clay-coated paper by atmospheric-pressure plasma in air

The aim of this work was the wettability improvement of clay-coated paper by ambient air plasma exposure. Industrial corona with a volume dielectric barrier discharge in cylindrical configuration was used as a plasma source; the exposure times varied from 0.25 up to 5 s. Water contact angle (WCA) measurement and surface free energy (SFE) evaluation were carried out for the estimation of wettability changes. Plasma treatment in the duration of 0.25 s was sufficient to decrease the WCA almost to the half of the original value, which was 76°. SFE of paper has increased by 40%–50% after plasma treatment. Long-term ageing effect study of treated samples was carried out up to 3 months after the treatment. WCA did not reach the original value even after 3 months, and it was still 20%–30% lower. O/C ratio increased from 0.7 to 1.8 in case of 5-s plasma treatment, and the new chemical bonds (C=O, O–C=O) were created on the surface.     

Surface changes brought about by corona discharge treatment of polyethylene film and the effect on subsequent microbial colonisation

Microbial colonisation of synthetic plastic films is normally slow, which affects the total period of biodegradation. Correlation between the modified surface condition and the ability for microorganisms to colonise low-density polyethylene (LDPE) film was studied. Corona discharge treatment was applied to obtain enriched and activated surface condition of LDPE film. It was found from water contact angle and FTIR spectrum evaluations that surface energy was significantly increased due to production of free radicals. Stabilised oxidised LDPE surface was also obtained by further exposure to the corona which gave more suitable condition for subsequent colonisation. Results were compared with UV irradiated (photo-oxidised) LDPE films. Colonisation of corona discharged and UV treated LDPE films were tested in the laboratory environment using known fungal isolates and in a natural compost environment. More active microbial colonisation was observed in all cases for corona discharged and UV treated LDPE films. Far longer UV exposure was required to have the same physicochemical and biological effect as the corona discharge treatment.     

SYNTHESIS AND ELECTRICAL PROPERTIES OF POLYIMIDE-Al2O3 COMPOSITES

Polyimide-alumina hybrid films were synthesized via in situ polymerization and thermal imidation process from a solution of polyimide precursor and nanosized alumina in N,N-dimethylacetamide, and the microstructure of the hybrid films was characterized by transmission electron microscope （TEM） and infra-red （IR） spectrometry. The dependence of thermal stability, tensile properties, dielectric properties and degradation endurance under corona on the nano-Al2O3 content of polyimide-alumina hybrid films was studied. The results show that with the increase of Al2O3 content, the thermal stability and the dielectric properties of the hybrids increase, while the tensile properties decrease. Better corona resistance can be achieved if the PI film is filled with α-Al2O3 nanometric particle.     

TiO2纳米膜表面结构形态特征

采用反胶束法制备TiO2纳米溶胶,用浸渍提拉法在不同的条件下制备了三种TiO2多孔纳米薄膜,并利用AFM、SEM、XRD等方法对膜表面结构物理化学特性进行表征.结果表明三种膜基本上由粒径约为59 nm的纳米粒子以不同的方式堆积而成,溶胶刚生成时浸提一次,干燥、焙烧得到膜上纳米粒子分布均匀,所生成的二次粒子粒径最小,二次粒子形成的二次表面粗糙度最小,浸提10次得到膜上纳米粒子间存在较丰富缝隙结构,二次粒子粒径及其形成的表面粗糙度较大,而溶胶制备好陈化6 h后浸提得到的膜上二次粒子粒径最大,表面粗糙度最高.由分形理论估算得到三种膜的分形维数分别是2.22、2.20和2.27. XRD测试表明,膜上TiO2为锐钛矿晶相.这些结果表明,采用不同制备步骤得到的膜,其表面结构形态存在较大的差异.