聚苯胺纳米刺/掺氮空心碳球复合材料的制备及电容性能

以掺氮空心碳球（N-HCS）为骨架,通过化学氧化聚合法制备了聚苯胺纳米刺/掺氮空心碳球复合材料（PANI/N-HCS）,采用扫描电子显微镜、透射电子显微镜和红外光谱仪等对样品的形貌、结构等进行了表征. 采用循环伏安、计时电位和交流阻抗等方法在1 mol/L H₂SO₄水溶液中考察了材料的电化学性能. 结果表明,PANI/N-HCS具有良好的电化学性能,在0.5 A/g电流密度下,PANI/N-HCS的比电容达346 F/g;当电流密度为20 A/g时,PANI/N-HCS比电容值为228 F/g,电容保持率为66%;在5 A/g电流密度下,经1000次充放电循环后,电容保持率为76%.     

催化裂解C2H2制备空心碳球

在高岭土负载的镍催化剂上,于850 ℃催化裂解乙炔制备了直径约500 nm 的空心碳球.用XRD、TEM、SEM和显微激光Raman光谱对所得的碳球及催化剂进行了表征,并初步探讨了反应机理.     

碳空心球/硫复合材料制备和电化学性能研究

采用PMMA为模板制备碳空心球材料,并以碳空心球材料为导电骨架与硫材料复合制得碳空心球/硫复合材料. SEM和TEM照片显示,硫材料能均匀地填充在碳空心球的孔道和腔体内部. 采用恒电流充放电测试碳空心球/硫复合电极的电化学性能. 结果表明,在100 mA·g^-1、500 mA·g^-1、1 A·g^-1、2 A·g^-1 和5 A·g^-1电流密度下,碳空心球/硫复合电极可逆放电容量分别为1145 mAh·g^-1、824 mAh·g^-1、702 mAh·g^-1、586 mAh·g^-1和395 mAh·g^-1,呈现出较优异的倍率循环寿命.     

负载酞菁铁的氮掺杂中空碳球的电催化氧还原性能（英文）

开发低成本、高性能的氧还原反应（ORR）催化剂是当前的研究热点.虽然酞菁铁（FePc）在几十年前就被证明能高效地电催化氧还原反应,但由于其电子传导性和稳定性较差,无法取代商用的Pt/C催化剂.氮掺杂碳材料不仅化学性质稳定、电子传导性好,还有一定的氧还原催化活性.本文首先制备了聚苯乙烯@聚多巴胺球前驱体,经过高温碳化后制得了氮掺杂中空碳球,进而负载酞菁铁后制备了负载酞菁铁的氮掺杂中空碳球复合材料（FePc-NHCS）.通过调整煅烧温度和酞菁铁的负载量,可进一步调控FePc-NHCS的多孔结构、石墨化程度、氮掺杂的种类与含量及酞菁铁的负载状态.优化后的FePc-NHCS在碱性电解质中显示出优异的ORR催化活性,其半波电位和稳定性均高于商用Pt/C催化剂.研究结果表明,掺杂与复合是增强单项催化组分活性的有效途径.此外,通过调控催化剂的结构和组分也能有效地优化催化剂的氧化还原性能.     

海胆状硫化镍空心球的制备及电化学性能研究

以乙二醇为溶剂,硫代乙酰胺为硫源,采取简单的溶剂热法成功合成了由纳米棒组成的海胆状硫化镍空心球,扫描电镜图片清楚地揭示了海胆状空心结构,XRD测试结果表明产品中存在α和β两种相结构,但主要组分为β-NiS. 跟踪产物随时间的变化,研究了海胆状空心球的形成过程. 先形成实心的海胆状结构,进一步熟化导致空心结构的形成. 作为锂离子电池的阴极材料,测定了海胆状硫化镍空心球的电化学性能,首次放电容量超过900mAh g-1,高于文献报道的理论容量,循环五十次后,稳定在约200 mAh g-1.     

模板法制备复合中空微球

本文报道以一种商品化的聚苯乙烯中空球为模板, 采用溶胀聚合技术合成了具有IPN(Inter-Penetrating Network)结构的复合中空球; 对其中的一种高分子网络进行化学改性引入所需官能团, 制得带有羧基的聚合物凝胶中空球; 利用凝胶诱导生长特性, 成功制得聚合物复合中空球. 此方法无需去除模板就可批量制备各种复合功能中空球.     

Au@SiO_2中空微球的制备及催化性能

以天然高分子阿拉伯树胶(AG)为还原剂和稳定剂制备了金纳米粒子;将含有金纳米粒子(Au NPs)、阿拉伯树胶和氨水的溶液滴加到乙醇中形成AG-Au NPs复合胶团;利用正硅酸乙酯水解,在AG-Au NPs表面包覆二氧化硅壳层;通过简单水洗的方法得到了金纳米粒子@二氧化硅(Au@SiO_2)中空微球.采用透射电子显微镜(TEM)、X射线衍射仪(XRD)和氮气吸附实验等对Au@SiO_2中空微球进行表征.通过设计对比实验,证实阿拉伯树胶在中空结构形成过程中起到模板剂的作用.催化性能测试结果表明,所制备的Au@SiO_2中空微球在硼氢化钠还原亚甲基蓝的反应中表现出良好的催化活性和重复使用性.     

中空介孔碳球修饰的丝网印刷碳电极用于尼古丁的电化学检测

将一步法合成的中空介孔碳球(HMCS)修饰在丝网印刷碳电极(SPCE)上,得到了用于尼古丁电化学检测的新型电极(HMCS/SPCE)。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、粉末X射线衍射(XRD)、X射线光电子能谱(XPS)以及拉曼光谱等方法对HMCS及修饰电极HMCS/SPCE进行表征。由于HMCS具有较大的电化学活性面积和良好的导电性,修饰电极HMCS/SPCE对尼古丁表现出良好的电催化活性。在优化实验条件下,电极HMCS/SPCE对尼古丁的检测线性范围为0~500μmol/L,灵敏度为0.850 m A/(cm~2·mmol·L~(-1)),检出限为0.058μmol/L。制备的传感器具有重复性好、稳定性高等特点,可用于实际烟草样品中尼古丁的检测。     

碳包覆纳米SnO2中空纤维的制备及电容性能

采用同轴静电纺丝法制备了碳包覆纳米SnO₂中空纤维超级电容器电极材料.利用X射线衍射(XRD)、拉曼光谱、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和比表面积分析仪(BET)对材料进行表征.结果表明,纤维呈现中空形貌,平均直径为1 μm; SnO₂颗粒均匀分布于碳壳结构中,平均粒径为3-15 nm.材料的比表面积为565 m²·g^-1.在三电极体系中,当电流密度为0.25 A·g^-1时,电极材料的比容量达397.5 F·g^-1;在1.0A·g^-1电流密度下,充放电循环3000次后比容量仍保持为初始值的88%.在对称型双电极体系中,电流密度为0.25 A·g^-1时,电极材料的比容量达162.0 F·g^-1,在1.0 A·g^-1电流密度下,充放电循环3000次后比容量仍保持为初始值的84%.     

用负载型Z-N催化剂制备形貌规则的空心球形聚乙烯粒子

采用一种含二酯类内给电子体的氯化镁负载Ziegler-Natta催化剂和三异丁基铝(TIBA)助催化剂,在同一反应器中经常压丙烯预聚和加压下的乙烯与少量丙烯淤浆共聚合两步反应,高效地合成了外径为0.4~3 mm的中空球形聚乙烯粒子,其球形粒子的外表面和内部空腔的内表面均较为平滑,壳层厚度均匀.聚合反应的催化剂效率最高达到7.49 kg/g Ti·h·MPa(6.5 kg PE/g Cat.).研究了助催化剂种类、助催化剂浓度(Al/Ti摩尔比)和乙烯聚合阶段的丙烯共单体添加量对聚合物粒子形貌的影响,发现采用三乙基铝(TEA)或TEA/TIBA混合物为助催化剂时,虽然聚合物粒子仍呈中空球形形态,但其内部空腔的形状极不规则.以TIBA为助催化剂时,在一定范围内提高Al/Ti比和丙烯添加量均可显著提高催化效率,聚合反应动力学曲线由衰减型变为增长型,但聚合物粒子的中空形貌得以保持.对比丙烯预聚产物的粒子形貌发现,助催化剂含TEA时所得预聚物粒子结构较松散,内部有较多孔隙和裂纹,而改为TIBA后预聚物粒子内部相对致密.     

Boosting Supercapacitor Performance of Graphene by Coupling with Nitrogen-Doped Hollow Carbon Frameworks

Graphene as a suitable electrode has been extensively used for electrochemical double-layer capacitors based on its excellent properties, including high electrical conductivity and large specific surface area. However, one of the drawbacks is the unavoidable stacking tendency between the graphene nanosheets, resulting in limited electrochemically specific surface area. Herein, novel graphene nanosheets supported by hollow nitrogen-doped carbon frameworks derived from ZIF-8 (GPNC) were fabricated through a simple polyethyleneimine (PEI)-assisted pyrolysis strategy, to boost capacitance performance. Benefiting from the unique scaffold/support role of hollow nitrogen-doped carbon frameworks within the graphene interlayer, the GPNC with a large specific surface area, along with ample micropore/mesopore channels and high nitrogen content, is capable of facilitating electron and electrolyte ion migration kinetics and enhancing intrinsic electrochemical activity. Thus, the GPNC exhibits the highest charge storage of 218 F g⁻¹ and superior rate capability of 74 % when the current density increased from 0.5 to 20 Ag⁻¹ in comparison to pristine graphene and common ZIF-derived carbon/graphene electrodes. The assembled GPNC//GPNC two-electrode system further delivers a maximum power of 9080 Wkg⁻¹ with outstanding electrochemical retention of 84 % over 10 000 cycles.     

掺磷酚醛树脂炭嵌锂性能研究

以添加不同含量五氧化二磷的热塑性酚醛树脂为前驱体 ,经热固化后升温至 70 0℃裂解制备掺磷树脂裂解炭 .X射线衍射考察了裂解炭的微晶结构变化 ;恒电流技术研究了裂解炭的充放电性能 .实验表明 ,五氧化二磷的加入使树脂裂解炭微晶结构发生了很大改变 ,随着磷含量的增加微晶层间距减小 ,而且更加无序 ;其放电可逆容量随五氧化二磷掺杂量的增加先增而后减 ,当P2 O5含量为 9wt%时 ,可逆容量达到最大值 (5 2 8mA·h·g- 1) ,是未掺杂 (2 30mA·h·g- 1)的 2倍多     

三维有序SiC空心球的制备及表征

以三维有序多孔碳为模板, 以聚甲基硅烷(PMS)为前驱体, 经过前驱体的渗入、交联和陶瓷转化以及多孔碳模板的烧除, 制备了长程三维有序SiC空心球. 所制备的SiC空心球的外径(135-896 nm)、 球壳厚度(14-79 nm)、 BET比表面积(50.8～5.0 m2/g)及微孔体积(0.265～0.038 cm3/g)受不同孔径的多孔碳模板(150-1 000 nm)或不同前驱体浓度的控制. 所制备的SiC空心球以hcp结构排列成长程三维有序的序列.     

新型氧化铝空心球的制备及表征

以胶体碳球为模板, 廉价的硝酸铝为铝源, 成功制备出了新型的大小可控的氧化铝空心球. 通过透射电子显微镜(TEM)、扫描电子显微镜(SEM)、能量扩散X射线(EDX)、X射线粉末衍射(XRD)等手段对合成产品进行了表征, 并考察了不同合成条件对空心球形貌的影响. 实验结果表明, 合成的氧化铝空心球大小均一, 粒径及壁厚均可调节. 在该实验条件下, 硝酸铝浓度及吸附时间的改变对产品结果没有明显的影响, 而吸附温度的改变引起了产品表面光滑度及壁厚的改变.     

Amorphous Fe Nanoclusters Embedded inside Balloon-Like N-Doped Hollow Carbon for Efficient Electrocatalytic Oxygen Reduction

Rational designs of electrocatalytic active sites and architectures are of great importance to develop cost-efficient non-noble metal electrocatalysts towards efficient oxygen reduction reaction (ORR) for high-performance energy conversion and storage devices. In this work, active amorphous Fe-based nanoclusters (Fe NC) are elaborately embedded at the inner surface of balloon-like N-doped hollow carbon (Fe NC/C_h sphere) as an efficient ORR electrocatalyst with an ultrathin wall of about 10 nm. When evaluated for electrochemical performance, Fe NC/C_h sphere exhibits decent ORR activity with a diffusion-limited current density of ~5.0 mA/cm² and a half-wave potential of ~0.81 V in alkaline solution, which is comparable with commercial Pt/C and superior to Fe nanoparticles supported on carbon sheet (Fe NP/C sheet) counterpart. The electrochemical analyses combined with electronic structure characterizations reveal that robust Fe-N interactions in amorphous Fe nanoclusters are helpful for the adsorption of surface oxygen-relative species, and the strong support effect of N-doped hollow carbon is benefitial for accelerating the interfacial electron transfer, which jointly contributes to improve ORR kinetics for Fe NC/C_h sphere.     

Nickel/Cobalt Molybdate Hollow Rods Induced by Structure and Defect Engineering as Exceptional Electrode Materials for Hybrid Supercapacitor

Oxygen defects and hollow structures positively impact pseudocapacitive properties of diffusion/surface-controlled processes, a component of critical importance when building high-performance supercapacitors. Hence, we fabricated hollow nickel/cobalt molybdate rods with O-defects (D−H−NiMoO₄@CoMoO₄) through a soft-template and partial reduction method, enhancing D−H−NiMoO₄@CoMoO₄’s electrochemical performance, yielding a specific capacitance of 1329 F g⁻¹, and demonstrating excellent durability with 95.8 % capacity retention after 3000 cycles. D−H−NiMoO₄@CoMoO₄ was used as the positive electrode to construct an asymmetric supercapacitor, displaying an energy density of up to 34.13 Wh kg⁻¹ and demonstrating good predisposition towards practical applications. This work presents an effective approach to fabricate and use hollow nickel/cobalt molybdate rods with O-defects as pseudocapacitor material for high-performance capacitive energy storage devices.     

Hydrothermal Synthesis of NiCo-layered Double Hydroxide Nanosheets Decorated on Biomass Carbon Skeleton for High Performance Supercapacitor

Afacile hydrothermal strategy is adopted to synthesize the composite of NiCo-layered double hydroxide(NiCo-LDH) with biomass carbon as substrate for supercapacitor electrodes. The prepared NiCo@BC was characterized by means of X-ray diffraction(XRD), scanning electronic microscopy(SEM), Fourier transform infrared spectroscopy(FTIR) and Raman spectroscopy, and electrochemical tests. The SEM images demonstrated that numerous NiCo-LDH nanosheets directly grew on the surface of biomass carbon uniformly. Electrochemical tests indicated that the NiCo@BC electrode exhibited good capacitive behavior with a specific capacitance of 606.4 F/g at the current density of 0.5 A/g. In addition, the composite electrode showed excellent cyclic stability of 87.1% even after 1000 cycles. These results manifest that NiCo@BC nanocomposite is a promising candidate for the electrode material for future supercapacitor practical applications.     

聚氨酯醇酸的裂解气相色谱-质谱研究

人工合成聚氨酯醇酸,用裂解气相色谱－质谱（ＰＧＣ－ＭＳ）法详细研究其热裂解产物的化学组成,探索其热裂解机理。裂解的主要产物为合成所用的单体甲苯二异氰酸酯（ＴＤＩ）、邻苯二甲酸酐及油脂相应的脂肪酸。     

胶质碳球为模板制备NiO空心球

以胶质碳球为模板、六亚甲基四胺为沉淀剂,在乙醇中溶剂热反应,再经500℃煅烧6 h制备了NiO空心球。通过X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FTIR)和低温氮吸附-脱附,对NiO的结构和形貌进行了表征。结果表明溶剂热反应时间是制备完整NiO空心球的关键因素,溶剂热反应12 h,再经空气中煅烧,可制得形貌均一的NiO空心球。所得产物是由NiO纳米粒子组装而成的具有多孔结构的空心球。同时,本文对NiO空心球结构的形成过程和可能机理进行了分析和讨论。