金属相1T´ MoS2增强类石墨相C3N4的可见光催化性能

通过煅烧和静电自组装的方法制备了1T′ MoS₂超薄纳米片和类石墨烯相氮化碳(g-C₃N₄)纳米片的复合材料. 该材料在光催化实验中展现出6.24 μmol?g^?1?h^?1的产氢速率, 优于贵金属铂修饰的g-C₃N₄纳米片的性能(4.64 μmol?g^?1?h^?1). 此外, 该复合材料在光催化降解有机染料甲基橙的实验中表现出0.19 min^?1的催化速率, 而纯g-C₃N₄纳米片只有0.053 min^?1的催化速率. 材料光催化性能的提升可归结于1T′MoS₂ 和g-C₃N₄之间的协同效应, 包括光吸收的增强以及因1T′MoS₂优异电子导电性而得到的高效电荷分离.     

锗酸锌纳米棒@石墨烯复合负极材料的制备及储锂性质

以二氧化锗和二水合醋酸锌为原料,采用水热法制备了锗酸锌纳米棒,并将其与氧化石墨烯复合,制备了石墨烯包覆的锗酸锌纳米棒三维复合材料. SEM等测试表明,锗酸锌纳米棒均匀地穿插在石墨烯片中,阻止了石墨烯片之间相互堆垛,而石墨烯片层之间相互连接,形成三维的空间导电网络,提高了材料的电子导电性.电化学测试表明,石墨烯片作为稳定的框架,能够有效缓冲活性物质在脱嵌锂过程中产生的体积变化,在500 mA·g^-1电流密度下循环190次后, Zn₂GeO₄@RGO复合材料的嵌锂容量仍有1189.5 mAh·g^-1;在3.2 A·g^-1的大电流密度下,嵌锂容量达到449.5mAh·g^-1,表明该复合材料具有优异的长循环稳定性和良好的倍率性能.     

石墨烯氧化过程中的热分析-质谱以及脉冲热分析方法研究

本文由氧化石墨烯通过水热法制备直接获得石墨烯。采用热重-差热分析方法检测了石墨烯受热过程中的质量变化和氧化温度。利用热分析-质谱联用技术在400-650 ℃温度区间得到了水和二氧化碳正离子质谱峰,这说明石墨烯氧化过程中的质量损失是由羟基水和二氧化碳脱除造成的。同时,还采用非等温热分析动力学方法,利用5、10、15 ℃·min^-1三种不同升温速率获得了石墨烯材料在空气气氛下的热分析动力学参数。通过Kissinger方法计算出石墨烯氧化过程中的活化能（E_a）和指前因子的对数（lg（A/s^-1））分别为155.11 kJ·mol^-1和6.90。利用Ozawa-Flynn-Wall （FWO）方法还建立了活化能和指前因子与反应转化率之间的关系。基于以上研究结果,本工作将对石墨烯在热界面、导热和先进复合材料等领域的应用提供参考价值。     

微波诱导等离子体技术制备rGO@S复合正极及其在高倍率锂硫电池中的应用

锂硫电池具有高能量密度、低成本和环境友好等优势,有望满足市场日益增长的需求。然而,其正极材料中的活性物质硫存在溶解穿梭等问题,限制了锂硫电池的大规模应用。本文利用氧化石墨(GO)作为碳源、升华硫作为硫源,通过微波诱导等离子体技术(MIP)快速高效(30-40 s)地制备得到了还原氧化石墨烯负载硫纳米颗粒锂硫电池复合正极材料(rGO@S),其中,rGO褶皱卷曲、相互连接的层片状结构,有利于电解液中的锂离子向电极材料中扩散和迁移,同时有利于提高电极材料的导电性,且rGO上的含氧官能团也能够起到对硫纳米颗粒的固定作用,有利于电极材料循环稳定性的提升。得益于其独特的形貌结构,rGO@S在电池测试中表现出优异的倍率性能和良好的循环稳定性。在0.1 A·g^-1的电流密度下,rGO@S的可逆比容量为1036 mAh·g^-1,当电流密度增大到8 A·g^-1其可逆比容量仍高达832 mAh·g^-1,且经过8 A·g^-1的超大电流密度充放循环,当电流密度回到0.1 A·g^-1...     

石墨烯负载Ni2P纳米片作为锂硫电池的硫基复合正极材料

将磷化镍纳米片均匀负载到石墨烯(G)上制备出Ni₂P/G复合材料,并将其作为硫载体构筑了硫基复合材料(S/Ni₂P/G)。研究表明,磷化镍纳米片对可溶性多硫化物具有强的化学作用和较高的电催化活性,使S/Ni₂P/G硫基复合材料表现出良好的电化学性能。特别是,在高硫含量(80.3%)和低电解液用量(15μL·mg^-1)条件下,S/Ni₂P/G硫基复合材料展现出1 164.7 m Ah·g^-1的质量比容量和良好的循环稳定性。此外,S/Ni₂P/G复合材料具有高的振实密度(1.02 g·cm^-3),其体积比容量高达954.0 m Ah·cm^-3,约为S/G复合材料体积比容量的1.6倍。     

3D石墨烯/镍铝层状双金属氢氧化物的制备及超级电容性能

超声分散氧化石墨和聚苯乙烯微球于去离子水形成稳定分散液, 加入氨水和水合肼还原氧化石墨得到包覆石墨烯纳米片的聚苯乙烯微球, 经6 mol·L^-1 KOH碱蚀和甲苯洗脱聚苯乙烯制备3D石墨烯. 将3D石墨烯超声分散于去离子水, 然后分别以硝酸镍、硝酸铝和尿素为镍源、铝源和碱源化合物水热合成3D石墨烯/镍铝层状双金属氢氧化物复合材料. 采用红外、拉曼、X射线衍射、扫描电镜、透射电镜和恒电流充-放电测试对材料的结构、形貌及电化学性质进行研究. 结果表明, 氧化石墨被还原形成有微孔结构的3D石墨烯. 镍铝双金属氢氧化物纳米片均匀分散在3D石墨烯孔壁. 在1 A·g^-1的电流密度下, 复合材料电极的比电容为1054.8 F·g^-1. 当电流密度增加到8 A·g^-1时, 比电容为628.1 F·g^-1. 循环充-放电1000次后, 比电容仍保持在97%以上, 呈示该复合材料具有优异的电化学性能.     

高性能锂离子电池用N掺杂C-Sn交联纳米纤维自支撑电极的理性设计（英文）

为了提高碳材料作为锂离子电池负极材料的比容量,将氮掺杂的碳纤维与高容量的Sn进行复合。通过静电纺丝及低温碳化制备了均匀镶嵌Sn纳米颗粒的氮掺杂碳纳米纤维(C-Sn)复合膜。该复合膜直接用作自支撑锂离子电池负极时表现出较好的电化学性能,Sn的引入显著提高了碳纳米纤维膜的电化学性能。碳均匀包覆Sn后形成的纤维结构可以促进离子电子的传导,并能有效缓冲Sn纳米粒子在循环过程中的体积变化,从而有效抑制粉化与团聚。Sn含量约为25.6%的CSn-2电极具有最高的比容量和更优异的倍率性能。电化学测试结果表明,在2A·g^-1的电流密度下,充放电循环1000圈后充电(放电)比容量为412.7(413.5)mAh·g^-1。密度泛函理论(DFT)计算结果表明,N掺杂非晶碳与锂具有良好的亲和性,有利于将合金化反应之后形成的Sn_xLi_y合金锚定在碳表面,进而缓解了充放电过程中的Sn的体积变化。本文为高性能储锂材料的设计提供了一种切实可行的策略。     

影响热还原氧化石墨烯超级电容器性能的因素比较

通过改进的Hummer法制得氧化石墨烯,并在不同温度的氩气气氛中还原得到一系列热还原氧化石墨烯（T-RGO）. 电化学测试表明,T-RGO作为超级电容器电极材料时,良好的导电性是必需的,但石墨烯表面含氧官能团对其电容性能的影响要远大于导电性和比表面积的影响,900 °C还原的T-RGO比表面积为314 m²·g^-1电导率为2421 S·m^-1,但其容量只有56 F·g^-1,然而300 °C还原的T-RGO比表面积为18.8 m²·g^-1电导率为574 S·m^-1,其容量却达到281 F·g^-1. 材料表征分析表明,300 °C 还原的石墨烯之所以有更高的电容,是因为除双电层电容外,更多的是由其表面含氧官能团提供的赝电容,这使作者以后在设计制备超级电容器等储能设备用石墨烯基电极材料时更加有针对性.     

热剥离法制备石墨烯纳米片对Pb2+和Cd2+的吸附

石墨粉氧化后,在氮气气氛下,快速高温剥离制得石墨烯纳米片。采用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(HRTEM)、拉曼(Raman)光谱、傅里叶变换红外(FT-IR)光谱和氮气吸附-脱附等分析手段对石墨烯样品进行了表征。这些分析测试结果显示:石墨烯样品主要由很薄的1-4层石墨组成,呈褶皱状态,比表面积为628.5 m²·g^-1。研究了石墨烯吸附水溶液中的Pb²⁺和Cd²⁺的pH值、吸附时间、吸附温度和金属离子初始浓度等影响因素, Pb²⁺和Cd²⁺的最大吸附量分别为460.20和72.39 mg·g^-1。结果表明,热剥离法制得的高质量石墨烯纳米片可以作为一种高效的从水中去除Pb²⁺和Cd²⁺的吸附材料。     

具有三维导电网络结构的锡纳米颗粒/石墨烯纳米片复合电极材料的储镁性能研究

镁二次电池具有安全性高、价格低廉等优点,是一种具有潜在应用前景的高能量密度电池体系.目前,镁二次电池的研究重点之一是寻找合适的电极材料.最近,我们通过水热和热处理相结合的方法成功制备了具有三维导电网络结构的锡纳米颗粒/石墨烯纳米片复合电极材料.研究发现,在石墨烯的三维导电网络片层上,均匀分布了粒径小于100 nm的锡纳米颗粒.将锡纳米颗粒/石墨烯纳米片复合材料作为镁二次电池电极材料,当电流密度为15 mA·g^-1和300 mA·g^-1时,首次放电容量分别达到了545.4 mAh·g^-1和238.8 mAh·g^-1,经过150圈后,容量保持率达到了93%,库伦效率为99%,表现出了较高的电化学活性.研究还发现,镁离子嵌入复合材料中形成镁锡合金,当镁离子脱出后,再次形成锡纳米颗粒/石墨烯纳米片复合电极材料,镁离子的脱出和嵌入具有很高的可逆性.这对未来研究设计高性能镁离子电极材料具有十分重要的意义.     

Efficient Use of Carbon Fibers as Heating Elements for Curing of Epoxy Matrix Composites

The aim of this study is to achieve a fully cured thermoset matrix that is heated by a direct electric current passing through the reinforcement fibers i.e., the Joule heating effect. Two types of fibers were used as heating elements for curing the epoxy resins. Kanthal resistance fibers were used as reference heating elements and subsequently, they were replaced by a Torayca Carbon Tow of the same radius. The specimens were cured by the heat produced by a direct electric current passing through the fibers and achieving temperatures of 50 °C and 70 °C. Specimens cured in a conventional oven were also manufactured, to compare the resistance heating method to the conventional one. Next, all specimens were mechanically characterized in a quasi-static three-point bending mode of loading and experimental results were compared to derive useful conclusions concerning the applicability of the technique to polymer/composite materials mass production. Finally, a preliminary economical study concerning power consumption needed for the application of both the traditional oven curing and the carbon fibers heating elements use for the manufacturing of the same amounts of materials is presented, showing a maximum financial benefit that can be achieved, on the order of 68%.     

Degradation of β-Carbolines Harman and Norharman in Edible Oils during Heating

The β-carbolines, mainly including harman and norharman, are a group of naturally occurring, plant-derived alkaloids, and are also considered as nonpolar heterocyclic aromatic amines. Sesame seed oils contain a high level of β-carbolines (harman and norharman). In China, sesame seed oil blends are one of the most popular types of vegetable oils blends, which can be used as cooking oils or frying oils. Thus, it is meaningful to investigate the degradation of β-carbolines (harman and norharman) in sesame seed oil blends as frying oils during heating. In this work, the loss of harman and norharman in different types of sesame seed oil blends have been investigated. The results showed that the degradation of harman and norharman were dependent both on the type of oil blends, heating temperature and time. Harman and norharman were more degraded during heating (150 °C, 180 °C) in oleic acid-rich oil blends compared to polyunsaturated acid-rich oil blends. Mechanistic investigation suggested that the reduction in harman and norharman in oil blends during heating was mainly due to the oxidative degradation reaction between β-carbolines and lipid oxidation products. Therefore, the contents of β-carbolines (harman and norharman) in sesame seed oil blends when used as frying oils and heated can be decreased with prolonged cooking time.     

Human genomic DNA analysis using a semi-automated sample preparation, amplification, and electrophoresis separation platform

The growing importance of analyzing the human genome to detect hereditary and infectious diseases associated with specific DNA sequences has motivated us to develop automated devices to integrate sample preparation, real-time PCR, and microchannel electrophoresis (MCE). In this report, we present results from an optimized compact system capable of processing a raw sample of blood, extracting the DNA, and performing a multiplexed PCR reaction. Finally, an innovative electrophoretic separation was performed on the post-PCR products using a unique MCE system. The sample preparation system extracted and lysed white blood cells (WBC) from whole blood, producing DNA of sufficient quantity and quality for a polymerase chain reaction (PCR). Separation of multiple amplicons was achieved in a microfabricated channel 30 microm x 100 microm in cross section and 85 mm in length filled with a replaceable methyl cellulose matrix operated under denaturing conditions at 50 degrees C. By incorporating fluorescent-labeled primers in the PCR, the amplicons were identified by a two-color (multiplexed) fluorescence detection system. Two base-pair resolution of single-stranded DNA (PCR products) was achieved. We believe that this integrated system provides a unique solution for DNA analysis.     

Thermomagnetic surgery for cancer

Thermomagnetic Surgery is a unique technique that takes advantage of the phenomenon of hysteresis heating of a ferromagnetic material to produce intense but controlled temperatures within solid organs or tumors to cause coagulation necrosis. By controlling the power of the electromagnetic coil system, the degree of heating of the tumor can be controlled through temperature monitoring that allows limitation of the area of destruction to the disease process and avoids damage to surrounding structures. If the ferromagnetic material is delivered by the arterial route to the tumor or organ, there is an additional beneficial effect of ischemic necrosis of the tissue and in time more concentration of the ferromagnetic particles. This new technique is applicable to selected cases of human cancer because no ill effect has been shown to exposure of the electromagnetic field or the ferromagnetic material in experimental animals.     

The effect of heating on polyaniline powders studied by real-time synchrotron radiation diffraction,mass spectrometry and thermal analysis

The effect of heating on four chemically synthesized polyanilines, three of which were doped by HCI, H₂SO₄, HCIO₄, and one sample which was dedoped, was investigated. The structural variations during thermal decomposition were studied by real-time synchrotron radiation diffractometry and correlated with mass spectrometry (MS), thermal gravimetry (TG), and differential thermal analysis (DTA). These macroscopic and microscopic techniques were combined in order to shed more light on the role played by the water and the counteranion molecules on the structure of doped polyaniline. Evidence for two H₂O fractions was found for HCI-doped polyaniline. Chain degradation was observed for HCIO₄ and H₂SO₄-doped polyaniline. The results indicate that intermediate sulphonation of polymer chains occurs in the latter case.     

微波加热法快速合成T型分子筛

由于具有高的水热稳定性和优良的孔道结构．T型分子筛已成为一种高选择性的催化剂．在低碳化合物的催化和重整等方面有较多的应用。近年来．报道采用晶种法在无机多孔陶瓷支撑体上制备的T型分子筛膜．在脱除有机物／水混合物中的水时．表现出优异的渗透汽化分离性能。然而，提高T型分子筛膜的致密性和生长速率仍是亟待解决的问题。T型分子筛的合成研究较少．制备过程均采用普通加热（Conventional Heating．CH）法。在无模板剂的条件下．T型分子筛的结晶区间较窄，结晶速率慢．合成时间通常需要6d以上。     

Gas chromatography using a resistively heated column with mass spectrometric detection for rapid analysis of pyridine released from Bacillus spores

Gas chromatography using a resistively heated analytical column with full scan electron impact mass spectrometry (EI-MS) was used to detect pyridine generated from heating Bacillus spores in a custom designed furnace inlet, along with gasoline range aromatic (GRA) hydrocarbons representing an environmental contaminant that could interfere with detection of the biologically-derived compound. Gas phase materials from the furnace inlet were collected onto a section of cooled open tubular column, and carrier gas flow was then routed through the trapping column onto the analytical column. Both sections of column were contained within low thermal mass tubular metal sheaths, with each independently and resistively heated allowing rapid temperature ramps and cooling. An analysis time of 2 min resolved spore-derived pyridine from the other organics, and allowed identification by mass spectrum match. Throughput of 20 analyses per hour was shown to be possible with a 1-min column cool-down time between analyses.     

微波场中T型分子筛的合成及晶化研究

研究了微波场中T型分子筛的结晶过程。考察了微波加热体系中合成参数如合成时间、溶胶组成、反应压力和模板剂用量对分子筛晶化的影响。微波加热的主要优点是减少合成时间,无模板剂的溶胶在普通加热条件下的晶化时间需要120 h,而在微波场中则仅需要20～25 h。另一方面,由于微波的快速加热特性促进了稳定相钙十字沸石的生成,从而减小了次稳定相T型分子筛的结晶区间。在未添加模板剂条件时,100 ℃下微波水热合成T型分子筛的结晶区间为：20≤n_SiO2/n_Al2O3≤22和0.31≤ n_M2O/n_SiO2≤0.33(其中M₂O=Na₂O+K₂O, n_Na/n_K=3和n_M2O/n_SiO2=11.70)。在普通加热和微波加热合成体系中,添加模板剂均能扩大结晶区间,同时还可以进一步减少合成时间。     

Application of Microwave Heating Technique to Esterification

Introduction Although the application of microwave technique has been reported as a new type of energy source chemically, it is only in recent years that this technique has been used as the energy source for organic synthesis. In 1986, R. Gedye, et al., published the report of the benzoate synthesis from the respective reactions between benzene carboxylic acid and methanol, propanol or butanol under microwave heating and the catalysis of H_2SO_4.