液相硝基苯加氢Ni-Zr-B非晶态合金催化剂制备及结构表征

将化学还原法制备的Ni-Zr-B非晶态合金催化剂用于硝基苯液相加氢制苯胺的反应,并通过XRD,TEM和H2-TPD技术对催化剂进行表征,研究了Zr含量对Ni-Zr-B催化剂微观结构和其催化加氢性能的影响。结果表明,Ni-B非晶态合金催化剂表现出较高硝基苯转化率和苯胺选择性,Zr助剂的引入减小了催化剂非晶态结构短程有序范围和催化剂粒径,粒径由60nm减小至10nm左右;增多了Ni活性中心数,并减弱了Ni化学吸附氢强度,使得吸附的氢物种更易于在各吸附中心间迁移并参与反应,导致Ni-B非晶态合金催化硝基苯加氢的活性和选择性进一步提高。当Zr含量为8%时,催化剂具有最优的催化加氢性能,硝基苯转化率和苯胺选择性分别高达99.6%和100%。     

KOH活化处理碳纳米管对其负载非晶态NiP催化性能的影响

经KOH活化处理和未经活化处理的碳纳米管分别用于负载非晶态NiP合金.以苯加氢为探针反应,研究了KOH活化处理温度和时间对碳纳米管的性质及其负载非晶态NiP催化剂活性的影响.研究结果表明:碳纳米管经KOH处理可以提高其负载非晶态NiP催化剂的催化活性,催化剂活性随活化温度升高和活化时间延长而增加.由于KOH处理改变了碳纳米管的微观结构,增加了其比表面积,所以非晶态NiP在碳纳米管上更易沉积分散,其负载的非晶态NiP合金催化剂的催化活性较高.     

乙酰丙酮铁为催化剂源在碳纤维表面生长碳纳米管的工艺研究

以乙酰丙酮铁为催化剂源,三甘醇为溶剂,通过溶剂热法在碳纤维表面负载催化剂前驱体,在H2与N2中一定温度下进行还原,采用化学气相沉积法在碳纤维表面生长碳纳米管。研究了催化剂的负载条件和碳纳米管的生长条件,采用XRD、FTIR、RAMAN对乙酰丙酮铁在三甘醇中反应在碳纤维表面负载催化剂前驱体产物进行分析,用SEM、TEM对催化剂前驱体粒子及碳纳米管的形貌进行表征。结果表明:催化剂前驱体为粒径30nm左右的Fe3O4颗粒,当催化剂的还原温度为415℃、还原时间为60min时,Fe3O4颗粒还原成纳米Fe颗粒;当碳纳米管的生长温度为750℃、生长时间为30min、气流体积比为V(N2)∶V(H2)∶V(C2H2)=50∶10∶10时能在碳纤维表面生长出形貌均一、管径为30~60nm的碳纳米管。     

堇青石载镍催化剂对燃烧合成碳纳米管的影响

借助于硝酸镍溶液, 利用浸渍法在堇青石表面均匀负载镍催化剂颗粒, 在甲烷扩散火焰中活化并催化生成碳纳米 管. 实验结果表明, 生成的多壁碳纳米管直径为30～50nm, 长度约为十几微米, 空腔比较小, 管壁石墨结晶结构良好.提高浸渍液浓度, 催化剂颗粒尺寸明显变大, 但对碳纳米管的形态影响比较小. 延长浸渍时间, 可使催化剂颗粒密度提高, 碳纳米管出现成束生长现象. 结合碳管成核生长过程和火焰燃烧的特点, 探讨了催化剂对于碳纳米管生长的影响机制.     

空气氧化法提纯碳纳米管的研究

以乙炔为原料气，采用铁-镍复合催化剂，在700℃下，由化学气相沉积法(CVD)制得了直径为10nm～30nm的多壁碳纳米管(MWNT)。然后通过空气氧化法对所获碳纳米管进行提纯，去除了碳纳米管中的无定形炭、炭纳米颗粒及炭纤维等非晶碳成分，提高了碳纳米管的纯度；并研究了提纯温度和时间的关系。结果表明：碳纳米管在空气中440℃加热3h后，烧损率趋于平稳，基本上稳定在2％左右。使用透射电镜(TEM)考察提纯前后碳纳米管的形貌，发现碳纳米管在空气中440℃加热3h后，非晶碳成分基本去除，纯度得到提高。     

功能化多壁碳纳米管的抗菌行为研究

分别以十二烷基苯磺酸钠、十八烷基三甲基溴化铵及两者的复配体系为分散剂对多壁碳纳米管进行非共价功能化处理,并考察了它们对多壁碳纳米管的分散能力。TG、FT-IR、UV-Vis吸收光谱和TEM分析结果表明,表面活性剂分子已成功吸附在多壁碳纳米管表面且复配体系对多壁碳纳米管的分散能力高于单一表面活性剂。另外,以金黄色葡萄球菌为实验菌种,通过考察功能化多壁碳纳米管悬浮液处理该菌2h后的光密度生长曲线和平板计数结果可知,复配体系功能化的多壁碳纳米管具有良好的抗菌活性。     

碳纤维表面生长碳纳米管及其增强复合材料性能的研究

通过电化学阳极氧化法改性碳纤维表面,利用浸渍法在连续的碳纤维表面加载了均匀的催化剂前驱体涂层,并通过化学气相沉积法(CVD)在碳纤维表面催化生长了均匀、规整的碳纳米管。利用场发射扫描电镜(FESEM)研究了电化学氧化电流强度对碳纤维表面加载催化剂颗粒的形貌与碳纤维表面催化生长碳纳米管形貌的影响,发现最佳的电化学氧化电流强度为0.4 A;Co作为催化剂时,500℃气相沉积10min后制备的复合材料层间剪切强度与未做任何处理的碳纤维及脱浆后的碳纤维作为增强体时相比,分别提高了11.0%与26.5%。     

用气相流动催化热解法合成单壁碳纳米管

以正硅酸乙酯(TEOS)为前驱体，二茂铁为催化剂前驱体，利用气相流动催化热解法在850～1160℃连续合成了单壁碳纳米管(SWNTs)．在此过程中，以由TEOS分解得到的二氧化硅颗粒和二茂铁分解得到的铁颗粒在气流中直接形成的复合粒于作为催化剂，二氧化硅作为铁颗粒的载体．电于显微镜和激光拉曼光谱的观测和分析表明，在所得到的产物中SWNTs的含量约为10％，其直径为1～2nm。     

水热法合成氧化镍-二氧化硅催化剂及其用于碳纳米管的制备

以硝酸镍和正硅酸乙酯为原料，制得Ni(OH)2／SiO2二元胶体，经水热晶化法和常压干燥法分别合成了纳米级氧化镍-二氧化硅复合粉体催化剂}用这两种催化剂在相同催化裂解条件下分别制得了多壁碳纳米管；采用XRD和TEM等测试手段对两种催化剂物相、形貌及由两种催化剂制得的碳纳米管形态、收率及纯度作了比较，结果表明：水热晶化法比常压干燥法合成的催化剂粉体颗粒粒径小(为10～20nm），分散性好，催化活性高，使得所制得的碳纳米管管径小(为10～16nm)、分布窄、纯度和收率都相对较高；同时对用不同水热反应温度合成的催化剂(物相不同)制备碳纳米管进行了研究。     

碳纳米管／PMMA／PVAc复合膜的制备及其导电性能研究

用竖式炉流动法，以二茂铁为催化剂，硫为助催化剂，苯为碳源制备碳纳米管（CNT），反应温度为1100-1200℃，碳纳米管的外径为20-40nm，内径10-30nm，长度5-20μm，并在2800℃对碳纳米管进行石墨化处理。用超声分散和溶液浇铸工艺制备碳纳米管，聚甲基丙烯酸甲酯（PMMA）／聚醋酸乙烯酯（PVAc）复合膜和石墨化碳纳米管／PMMA／PVAc复合膜，石墨化碳纳米管复合膜的导电性能明显优于碳纳米管复合膜，石墨化碳纳米管／PMMA／PVAc复合膜和碳纳米管／PMMA／PVAc复合膜的渗流阈值分别为2．5％和5％（质量分数），碳纳米管／PMMA／PVAc复合膜是很好的气敏候选材料。     

Synthesis of nano-carbon (nanotubes,nanofibres, graphene) materials

In the present study, we report the synthesis of carbon nanotubes (CNTs) using a new natural precursor: castor oil. The CNTs were synthesized by spray pyrolysis of castor oil-ferrocene solution at 850°C under an Ar atmosphere. We also report the synthesis of carbon nitrogen (C-N) nanotubes using castor oil-ferrocene-ammonia precursor. The as-grown CNTs and C-N nanotubes were characterized through scanning and transmission electron microscopic techniques. Graphitic nanofibres (GNFs) were synthesized by thermal decomposition of acetylene (C₂H₂) gas using Ni catalyst at 600°C. As-grown GNFs reveal both planar and helical morphology. We have investigated the structural and electrical properties of multi-walled CNTs (MWNTs)-polymer (polyacrylamide (PAM)) composites. The MWNTs-PAM composites were prepared using as purified, with ball milling and functionalized MWNTs by solution cast technique and characterized through SEM. A comparative study has been made on the electrical property of these MWNTs-PAM composites with different MWNTs loadings. It is shown that the ball milling and functionalization of MWNTs improves the dispersion of MWNTs into the polymer matrix. Enhanced electrical conductivity was observed for the MWNTs-PAM composites. Graphene samples were prepared by thermal exfoliation of graphite oxide. XRD analysis confirms the formation of graphene.     

碳纳米管对Fe-P非晶的力学性能和晶化行为影响的研究

采用快速凝固技术制备了碳纳米管／铁碳非晶复合材料,并对其组织、力学性能和热稳定性进行了研究检测结果表明,碳纳米管在非晶基体中的弥散存在,使得非晶抗拉强度提高,晶化激活能增加,晶化特征温度明显提高,加入２Ｗ／％碳纳米管,使铁磷非晶的室温抗拉强度提高了１２０％,晶化激活能增加了约４０％,晶化开始温度提高了约１００Ｋ,此外,在温度高于其晶化温度约２００Ｋ时,碳纳米管和非晶基体界面间发生了固相反应。     

Characterization of an interaction between functionalized carbon nanotubes and an enzyme

Carbon nanotubes (CNTs) did not exhibit strong interactions with Biliverdin IX beta reductase enzyme (BVRB) in water. With the use of noncovalent functionalization by the surfactant Triton X-100, the surfaces of the CNTs were changed from hydrophobic to hydrophilic. The hydrophilic surface of the CNT-Triton conjugate interacts with the hydrophilic surface of BVRB, thus creating a water-soluble complex. Results from ultracentrifugation through a sucrose gradient and gel electrophoresis show the presence of the enzyme. Raman spectroscopy confirmed that the enzyme indeed interacts with CNT-Triton conjugates.     

调变Ni／Mo／MgO催化剂中Ni／Mo比例可控合成薄壁碳纳米管

采用摩尔分数1%Ni及负载少量Mo的Ni/MO/MgO催化剂裂解甲烷合成薄壁碳纳米管.通过SEM、TEM、XRD和Raman光谱表征方法研究了碳纳米管直径和催化剂中Ni/Mo比例关系.实验发现:通过控制Ni/Mo比例可以调变催化剂颗粒大小以及活性相.TEM及XRD表征发现,随着Ni/Mo比例的降低,金属Mo相逐渐从NiMo合金相中析出.NiMo合金相对应的活性组分颗粒很小,容易催化裂解甲烷形成薄壁碳纳米管;而后析出的Mo相则主要形成了大管径厚壁的碳纳米管.当Ni/Mo比例为6时可以高选择性地获得窄分布,内径为1.3nm,外径为3.0nm的溥壁碳纳米管.Raman光谱进一步验证了碳纳米管含有较少的缺陷.薄壁碳纳米管形成的关键因素主要体现为碳在其表而的快速扩散以及小颗粒的碳纳米管催化剂活性相控制.     

An efficient nanocomposite based on carbon nanotubes functionalized with a fluorescent ink for ultrafast optical limiting

Functionalization of CNTs with different kinds of molecules is known to alter the optical properties of CNTs, leading to the development of new nanocomposites of interest to optoelctronics. This paper presents the design of a new and efficient optical limiting material based on carbon nanotubes (CNTs) functionalized with a commercial fluorescent ink. High resolution transmission electron microscopy (HRTEM) and optical spectroscopy indicate that the ink molecules get noncovalently attached to the surface of the CNTs. The mechanism of optical nonlinearity of the CNTs gets modified after functionalization. Z-scan studies on functionalized CNTs performed using mode-locked Ti:Sapphire femtosecond pulses at 780 nm reveal the predominance of two photon absorption (TPA). Efficient and low threshold ultrafast optical limiting is demonstrated in the new nanocomposite.     

浮动催化CVD法CNTs膜及CNTs膜/环氧复合材料拉伸特性

针对浮动催化化学气相沉积(CVD)法制备的碳纳米管(CNTs)膜,首先采用红外光谱表征分析了包覆在CNTs表面的无定形物质的组成,然后分别采用热处理和酸洗处理方法,考察了CNTs膜中无定形物和残留Fe催化剂对CNTs膜拉伸取向行为的影响。结果表明:采用CVD法制备的CNTs膜中CNTs表面无定形物为含氧或烷烃、烯烃类低聚物,可通过350℃有氧热处理基本去除。该CNTs膜的牵伸取向重排行为受组成影响显著,CNTs表面的低聚物可增强CNTs的管间黏结作用,Fe催化剂颗粒成为CNTs网络结构的交联结点,两者均有利于提高CNTs的取向程度和聚并成束的尺寸,进而提高CNTs膜的拉伸稳定性和断裂韧性。牵伸取向后CNTs膜与环氧树脂溶液的浸润性提高,其CNTs膜/环氧复合材料的拉伸强度和模量达到1228MPa和94.5GPa,相比初始无规CNTs膜/环氧复合材料的分别提高了337%和729%。      

High performance PA6/CNTs nanohybrid fibers prepared in the melt

Commercial and home-made carbon nanotubes (CNTs) were plasma treated under oxygen atmosphere and then added to polyamide 6 (PA6) in order to prepare fibres by melt spinning. For comparison, pristine nanofillers were used too. The effect of functionalization and of filler characteristics on the morphological, rheological, mechanical and electrical properties of the fibres was studied by TEM and SEM, rheological measurements, tensile and electrical conductivity tests. The results demonstrated that the functionalization led to a better mechanical performance and the morphological analysis confirmed that the adhesion, the dispersion and the alignment of the nanotubes within the polymer matrix were improved when using functionalized CNTs. Electrical tests marked that functionalization slightly reduced the conductivity of the materials.     

氯化聚乙烯/碳纳米管复合材料的制备及其性能研究

以三氯化铝(AlCl3)作催化剂,将多壁碳纳米管(MWNTS)悬浮在氯仿(CHCl3)溶液中,通过亲电加成反应,对MWNTS进行了侧壁化学修饰,并对化学修饰后的MWNTS作了红外光谱的分析.分别采用机械共混法和溶液共沉淀法制备了CPE/CNTs复合材料,对CPE/CNTs复合材料进行了拉伸性能及流变性能的测试,并利用扫描电子显微镜(SEM)观察了CPE/CNTs复合材料拉伸断面的形貌特征.结果表明:CPE/CNTs复合材料的拉伸强度随碳纳米管加入量的增加而增大,当碳纳米管的加入量为5份时,其拉伸强度最大,与纯氯化聚乙烯的拉伸强度相比,提高了75%;化学修饰后的碳纳米管在氯化聚乙烯基体中有了较好的分散性和相容性;CPE/CNTs复合材料的表观粘度随碳纳米管加入量的增加而逐渐增大.