苯胺-对苯二胺共聚物纳米材料的合成和结构表征

采用化学氧化无模板法,以苯胺和对苯二胺为单体,盐酸为掺杂剂,过硫酸铵为氧化剂,经氨水脱掺杂合成出聚苯胺(PANI)、聚对苯二胺(PPDA)、苯胺-对苯二胺共聚物P(ANI-PDA)纳米材料。用红外光谱(FTIR)、紫外可见分光光谱(UV)、X-衍射光谱仪(XRD)、热重分析仪(TGA)和扫描电镜(SEM)对3种聚合物的结构、结晶度、热稳定性和微观形貌进行表征分析,并测试了3种聚合物在水中的分散性。结果表明,与PANI相比,PPDA和P(ANI-PDA)中醌式结构较少,PANI的热稳定性最好;PANI的形貌为无规则的多孔颗粒团聚结构,PPDA和P(ANI-PDA)的微观形貌中出现了大量的纳米片状和棒状结构,通过XRD分析和聚合物在水中分散性测试得出P(ANI-PDA)的结晶度最高,在水中的分散性最好,说明纳米片状结构有利于提高聚合物的结晶度和在水中的分散性。     

聚苯胺/石墨烯/金复合材料的制备及超电容性能研究

以对苯二胺( p-PDA)为单体,氯金酸(HAuCl4)为氧化剂和Au源,氧化石墨烯(GO)为基底,通过原位聚合伴随Au纳米粒子生成的方法获得了聚苯胺/石墨烯/金(PpPD/GO/Au)的纳米复合材料.FESEM、FT-IR、XRD等测试表明,聚苯胺类衍生物、氧化石墨烯以及金纳米粒子三相在整个纳米复合材料中共存.材料的...     

聚吡咯网状纳米结构的合成及表征

采用原位聚合法,以聚乙二醇-6000(PEG-6000)为表面活性剂合成网状纳米聚吡咯(PPy),并考察了反应物的物质的量比对产品的形貌和吸波性能影响。利用扫描电子显微镜(SEM)、傅里叶变换红外光谱仪(FT-IR)、矢量网络分析仪对其进行表征,结果表明,Py∶HCl∶FeCl3物质的量比为1∶0.5∶2时,聚吡咯的吸波性能最佳,在3430MHz处达到了-38.9dB。     

水相沉淀法制备纳米片状钼铜矿（Cu3（MoO4）2（OH）2）（英文）

以硝酸铜、钼酸钠及氢氧化钠为原料,采用简单的水相沉淀法,在60℃下合成出钼铜矿(Cu3(MoO4)2(OH)2).通过X射线衍射、扫描电镜、透射电镜、热重与差热分析、红外光谱及荧光光谱等测试手段对材料的微观结构、形貌、热稳定性及谱学特性进行表征分析.结果显示,制备的产物为结晶性良好的、至少一维是纳米的片状结构材料,属于单斜型(晶胞参数a=0.53863 nm,b=1.40006 nm,c=0.56003 nm),其元素摩尔含量比约为3:2:10,与推测的分子式完全吻合.热重与差热分析数据表明Cu3(MoO4)2(OH)2纳米晶具有很好的热稳定性且起始分解温度为320℃.通过软件测得的d(021)面与d(ī21)面的晶间面距分别为0.435 nm与0.358 nm,与理论值基本相符.经测量,Cu3(MoO4)2(OH)2纳米晶具有强的荧光性质,在激发波长369 nm的作用下在530 nm表现为强发射峰.此外,还探讨了Cu3(MoO4)2(OH)2纳米晶的形成机理.     

聚二联噻吩和聚三联噻吩的固相法合成与性能

以二噻吩(BT)和三联噻吩(TT)为单体,FeCl3为氧化剂,在不同n(FeCl3)/n(单体)比例下,通过固相反应法合成出了聚(二噻吩)(poly(BT))和聚(三噻吩)(poly(TT))。并以傅立叶变换红外光谱、紫外可见吸收光谱、X射线衍射、热重分析和透射电镜等测试方法对聚合物进行了表征,研究了不同n(FeCl3)/n(单体)比例对聚合物结构与性能的影响。结果表明,n(FeCl3)/n(BT)为4∶1和n(FeCl3)/n(TT)为8∶1时,所得聚合物相对于其它比例下的聚合物表现出了较高的分子量、共轭程度和热稳定。其中,poly(TT)的分子量、共轭程度、热稳定、结晶性等特性随单体与FeCl3比例发生明显变化,但在微观形貌上无明显变化,而poly(BT)则随单体与FeCl3比例变化结果与poly(TT)相反,只是在微观形貌上产生了一定的差异。     

以阳极氧化铝模板为基底水热法合成纳米氧化铜

本文将阳极氧化铝(AAO)模板与水热法相结合,在150℃的条件下,以AAO模板为衬底制备了CuO纳米片及片状CuO晶体网络结构。反应过程中不需要添加任何辅助试剂,硫酸铜氨分解成氧化铜,并在阳极氧化铝模板上生成氧化铜纳米片及氧化铜纳米片网状结构。用SEM、XRD对制备的纳米CuO进行了形貌表征和结构分析,初步探讨了CuO纳米片网状结构的形成机理。     

超声辐照条件下HCl掺杂聚苯胺纳米棒的结构和性能

在超声辐照条件下,以HCl为掺杂剂、(NH4)2S2O8为氧化剂,通过溶液聚合得到了HCl掺杂聚苯胺(PA-NI)纳米棒.采用傅里叶变换红外光谱(FTIR)、透射电子显微镜(TEM)、X-射线衍射(XRD)、四电极电导率仪、热重分析(TGA)和电化学工作站对材料的结构与性能进行研究.研究结果表明,超声辐照条件下HCl掺杂PANI具有较高的掺杂程度和结构规整度,形成直径为50～65 nm左右的纳米棒状结构.与传统方法相比,超声辐照法所得材料的热稳定性在270～500℃有明显上升,室温电导率升至0.25 s/cm,并具有较好的电容行为和较高的电化学活性.     

不同酸对界面聚合法合成聚联苯胺性能的影响

采用界面聚合法合成了本征态和樟脑磺酸、b-萘磺酸、盐酸掺及硫酸掺杂聚联苯胺.利用红外光谱(FT-IR)、电子扫描显微镜(SEM)、X射线衍射(XRD)、循环伏安(cyclic voltamogram)等测试方法,对聚合物进行了表征.研究了掺杂酸种类对聚合结构、颗粒形貌、结晶性及电化学性能的影响.结果表明,本征态聚联苯胺呈现微米级棒状分布,具有一定的结晶性和电化学活性,质子酸掺入后其形貌虽无明显变化但尺寸有减少趋势;结晶性有所提高,其中硫酸掺杂聚联苯胺的结晶性最佳;循环伏安行为也有所改善,其中盐酸掺杂聚联苯胺的电化学活性相对较好且其电导率为1.41×10-3S/cm.     

碳包覆纳米SnO2锂离子电池负极材料合成及其性能研究

采用热解Sn(OH)4和淀粉混合物制备碳包覆纳米SnO2的方法合成了无定形碳包覆纳米SnO2.采用XRD、SEM、TEM、STEM-EDX以及充放电测试等手段对其结构、形貌和性能进行表征.结果表明,样品材料中无定形碳呈薄片状,被包覆的纳米SnO2(20～50nm)均匀分布在片状无定形碳中.产物中SnO2与碳的不同比例影响了产物的性能,样品(SnO2∶ C＝1∶ 1)首次循环的可逆比容量达到404mAh·g-1,20次循环内无明显衰减.     

组成对类水滑石生长调控机制的影响研究

采用均匀共沉淀法,制备了纳米片状Zn2Al-LDHs、花状结构ZnMgxAl-LDHs(x=1,2)以及微纳米结构Mg2Al-LDHs。利用XRD、SEM-EDX分析手段分别对产物的尺寸、结构和形貌进行了表征,并研究了组成变化对类水滑石结构形貌等生长调控作用。结果表明,所得含锌LDHs均具有较高的结晶度,其中Zn2Al-LDHs为多层板片状颗粒,晶体生长复合face-face片层团聚机理;ZnMgAl-LDHs为单层板片状颗粒,所得ZnMg2AlLDHs为双层板片状颗粒。镁离子含量是含锌水滑石结晶度及晶面生长方向的关键调控因素,随着镁离子含量的提高,含锌LDHs由face-face片层团聚为主向face-edge片层团聚现象过渡。Mg2Al-LDHs为花瓣状纳米片包覆颗粒晶,晶体生长复合face-edge片层团聚机理。     

Core-shell magnesium hydroxide/polystyrene hybrid nanoparticles prepared by ultrasonic wave-assisted in-situ copolymerization

In this paper, vinylated magnesium hydroxide (MH) nanosheets were prepared with 3-(trimethoxysilyl) propyl methacrylate (γ-MPS) and pristine MH nanosheets, then the MH/polystyrene (PS) hybrid nanoparticles were prepared by ultrasonic wave-assisted in-situ copolymerization of vinylated MH nanosheets and styrene (St). The morphology, thermal stability and chemical structure of the final products were investigated in detail with transmission electron microscopy (TEM), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier-transform infrared spectra (FTIR). The TEM and FTIR results showed that the uniformly-dispersed core-shell structure of MH/PS nanocomposites with MH-cores and PS-shell was formed. TGA indicated that the covalent interaction between PS and MH improved the thermal stability of PS. A possible formation mechanism of the MH/PS core-shell nanocomposites was also proposed.     

One-step and cost-effective synthesis of micrometer-sized saw-like silver nanosheets by oil/water interfacial method

One-step synthesis of silver saw-like nanosheets was introduced by using aqueous AgNO₃ and benzene-soluble p-phenylenediamine (pPD). Based on the X-ray diffraction pattern and selected-area electron diffraction pattern, the silver was single crystal. As indicated by Scanning Electron Microscopy, Transmission Electron Microscopy and the auxiliary characterization by Fourier transform infrared and Raman Spectroscopy, the nanosheets are ~ 20 μm in edge length and are coated by poly(p-phenylenediamine) (PpPD) thin films. The role of oil/water interface and PpPD on the formation of sheet-like morphology was analyzed. This method is facile and cost-effective.     

聚乳酸/石墨/多壁碳纳米管复合材料的制备及性能

通过共溶剂法制备了由石墨(GN)和多壁碳纳米管(MWCNTs)掺杂的聚乳酸(PLA)纳米复合材料,借助扫描电镜等手段,研究了MWCNTs用量对复合材料微观结构、热稳定性、导热和导热性能及介电性能的影响。结果显示,MWC-NTs和GN在PLA基体中形成了稳定的导电和导热网络结构,从而导致复合材料具有较低的导电和导热逾渗阈值,其值约为MWCNTs/GN=0.5/1。MWCNTs和GN均匀分散和协同增强效应促使复合材料热稳定性、导热和导电性能明显提高。与纯PLA相比,填料在逾渗阈值附近的复合材料的初始分解温度提高了近16℃,导热系数提高了1倍,体积电阻降低了109数量级。     

氧化石墨烯纳米片/环氧树脂复合材料的制备与性能

氧化石墨烯(GO)是石墨烯重要的衍生物之一,通过氧化和超声波分散制备了GO纳米片/环氧树脂复合材料。采用XRD、拉曼光谱、FTIR和TEM表征了GO纳米片的结构与形貌,研究了GO纳米片用量对GO纳米片/环氧树脂复合材料热稳定性、力学性能及介电性能的影响。结果表明:GO纳米片的加入提高了GO纳米片/环氧树脂复合材料失热稳定性;随着GO纳米片填充量的增加,GO纳米片/环氧树脂复合材料的冲击强度和抗弯性能先提高后降低,其介电常数和介电损耗则先减小后增加。GO纳米片填充量为0.3wt%的GO纳米片/环氧树脂复合材料的失重5%时的热分解温度由纯环氧树脂的400.2℃提高到424.5℃,而冲击强度和弯曲强度分别在GO纳米片填充量为0.2wt%和0.3wt%时达到最大,冲击强度由纯环氧树脂的10.5kJ/m2提高到19.7kJ/m2,弯曲强度由80.5 MPa提高到104.0 MPa。     

In-Situ Chemosynthesis of ZnO Nanoparticles to Endow Wood with Antibacterial and UV-Resistance Properties

Hybrid wood materials have attracted considerable attention because they have combined advantages of both wood and inorganic compounds. This work investigated the microstructural morphology, thermal stability, ultraviolet(UV) stability, and antibacterial property of composites made from wood/ZnO hybrid materials through a facile in-situ chemosynthesis methods. The X-ray diffraction(XRD) and thermogravimetric analysis(TGA) results indicated that the synthesized ZnO particles had an average grain size of about 10.8 nm. The scanning electron microscopy(SEM) observations showed that ZnO nanoflowers self-assembled with nanosheets were presented in wood cell lumens and increased with increasing Zn~(2+)concentrations. ZnO nanoparticles were also generated in the wood cell wall, which was confirmed by the results of energy-dispersive spectroscopy(EDS). The TGA tests also indicated that the thermal stability of wood/ZnO hybrid materials was improved after the formation of ZnO inorganic particles. Finally, the results of antibacterial efficacy tests and UV resistance tests revealed that ZnO nanoparticles showed a promising future as antimicrobial agents against Escherichia coli(E.coli) and UV resistance agents for wood protection.     

新型二维TiSe2纳米片的可控合成及其生长机理

溶液法是一种反应温和、易控制且常用的合成方法。目前已报道的溶液法制备TiSe₂时通常采用三辛基膦(TOP)为溶剂, 但这种试剂有毒, 对人体和环境都有潜在的危害。本研究通过简单的、无TOP的溶液法成功地制备了单分散的六边形TiSe₂纳米片, 并通过调整反应时间研究TiSe₂纳米片的形貌演变规律。利用XRD、SEM、EDS和紫外-可见漫反射对其物相、形貌、元素以及光学性能进行了系统的表征; 根据SEM结果对其生长过程及形貌演变规律进行了研究, 并提出一种螺旋状逐层生长的机理; 分析考察了TiSe₂纳米片对罗丹明B(RhB)的光催化活性, 发现其具有高于P25的降解能力, 这表明TiSe₂纳米片作为光催化材料具有广阔的应用前景。     

2D-titanium carbide (MXene) based selective electrochemical sensor for simultaneous detection of ascorbic acid,dopamine and uric acid

Two-dimensional (2D) titanium carbide (MXene) nanosheets exhibited excellent conductivity,flexibility,high volumetric capacity,hydrophilic surface,thermal stability,etc.So,it has been exploited in various applications.Herein,we report synthesis of mixed phase 2D MXene as a catalytic material for simultaneous detection of important biomolecules such as ascorbic acid (AA),dopamine (DA) and uric acid (UA),Crystalline structure,surface morphology and elemental composition of mixed phase titanium carbide (Ti-C-Tx) MXene (Tx =-F,-OH,or-O) nanosheets were confirmed by X-ray diffraction (XRD),Raman spectroscopy,high-resolution transmission electron microscopy (HR-TEM),high-resolution scanning electron microscopy (HR-SEM) and Energy-dispersive X-ray spectroscopy (EDS) mapping analysis.Furthermore,Ti-C-Tx modified glassy carbon electrode (GCE) was prepared and its electrochemical properties are studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV).It was found that Ti-C-Tx modified GCE (Ti-C-Tx/GCE) showed excellent electrocatalytic activity and separated oxidation peaks of important biomolecules such as AA (at 0.01 V),DA (at 0.21 V) and UA (at 0.33 V).Also,Ti-C-Tx/GCE sensor is enabled their simultaneous detection in physiological pH from 100 to 1000 μM for AA,0.5-50 μM for DA and 0.5-4 μM & 100-1500 μM for UA.The limit ofdetection's (LOD) was estimated as 4.6 μM,0.06 μM and 0.075 μM for AA,DA and UA,respectively.Moreover,real sample analysis indicated that spiked AA,DA and UA can be determined accurately by Ti-C-Tx/GCE with the recovery ratio in the range between 100.5％-103％ in human urine samples.The proposed Ti-C-Tx modified electrode exhibited good stability,selectivity and reproducibility as an electrochemical sensor for the detection ofAA,DA and UA molecules.     

Coassembly of exfoliated Ni–In LDHs nanosheets with DNA and infrared emissivity study

The biomolecule–inorganic hybrid materials are potential candidates for low infrared emissivity materials due to the combined functionalities of the biomolecules and the inorganic components. In this study, we describe a facile approach to fabricate DNA/layered double hydroxides (LDHs) nanohybrid by coassembly of exfoliated Ni–In LDHs nanosheets with DNA. In the assembly progress, exfoliated LDHs nanosheets and DNA with different initial DNA/LDHs mass ratio were mixed together, and the DNA intercalated LDHs nanohybrid was obtained only when the input DNA/LDHs mass ratio is ≤0.3 mg/mg. The structure and morphology of as-fabricated hybrid materials were characterized by X-ray diffraction (XRD), UV–Vis absorption spectra, Fourier transform infrared (FT-IR) spectra, thermogravimetry (TG), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results indicate that the reassembled product has layered structures incorporated with DNA biomolecule. The nanohybrid with expanding LDHs structure of d ₀₀₃ = 2.6 nm confirms the intercalation of DNA molecules into the LDHs interlayer. The helix chain oriented parallel to the basal plane of host layer forming ordered sandwich structure. The infrared emissivity value of the DNA/LDHs nanohybrid was then investigated. It was found that the infrared emissivity values were significantly reduced by coassembly of exfoliated LDHs nanosheets with DNA, which may be attributed to the synergistic effect and interfacial interaction between the DNA biomolecule and inorganic LDHs layers reinforced by the construction of ordered sandwich structure.     

聚丙撑碳酸酯/聚苯乙烯复合材料的制备与性能

利用熔融共混的方法制备了聚丙撑碳酸酯/聚苯乙烯(PPC/PS)复合材料,并通过万能试验机、差示扫描量热分析仪(DSC)、热重分析仪(TG)以及扫描电子显微镜(SEM)分别研究了复合材料的力学性能、热性能及微观形态.结果表明,PS的引入提高了复合材料的拉伸强度和拉伸模量及热稳定性,对体系中两相的玻璃化转变温度也有一定的影响.因此,通过简单的熔融共混的方法制备PPC/PS复合材料,可达到对PPC增强改性的目的,且大大降低了PPC的应用成本,对PPC的工业化应用提供了一条新的途径.     

Iodine-Assisted Solid-State Synthesis and Characterization of Nanocrystalline Zirconium Diboride Nanosheets

A solid-state route was developed to prepare zirconium diboride nanosheets with the dimension of about 500 nm and thickness of about 20 nm from zirconium dioxide, iodine and sodium borohydride at 700°C in an autoclave reactor. The obtained ZrB₂ product was investigated by X-ray diffraction, scanning electron microscope and transmission electron microscopy. The obtained product was also studied by thermogravimetric analysis. It had good thermal stability and oxidation resistance below 400°C in air. Furthermore, the possible formation mechanism of ZrB₂ was also discussed.