直流碳弧法制备碳包覆铁纳米颗粒机理研究

采用直流碳弧等离子体法成功制备了碳包覆铁纳米颗粒,利用透射电子显微镜和高分辨透射电子显微镜、X射线衍射、X射线能谱仪对样品的形貌、物相结构、化学成分和粒度进行表征分析,并对碳包覆纳米金属颗粒的形成机理进行初步探讨。结果表明:直流碳弧等离子体技术制备的碳包覆纳米金属颗粒具有明显的铁核(bcc-Fe)/碳壳(石墨层片)包覆结构,颗粒大多呈球形和椭球形,粒径分布在20~60nm范围,平均粒径为44nm,铁粒子外碳层的厚度为5~8nm。碳包覆铁纳米铁颗粒是通过颗粒内部固态形式的碳自行扩散至颗粒表面和颗粒外部气态形式的碳沉积到颗粒表面形成的。     

直流碳弧等离子体法制备碳包覆铁纳米颗粒研究

在惰性保护气氛下,采用直流碳弧等离子体法成功制备了碳包覆铁纳米颗粒,并利用x射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、X射线能谱仪(EDS)、透射电子显微镜(TEM)和相应选区电子衍射(ED)等测试手段,对样品的化学成分、形貌、物相结构、粒度等特征进行表征分析.实验结果表明:直流碳弧等离子体技术制备的碳包覆纳米金属颗粒具有明显的核-壳结构,内核金属结晶度较高,外壳碳为类石墨层结构,颗粒大多呈球形和椭球形,粒径分布在20nm～60nm范围,平均粒径为44nm.     

高能球磨合成纳米碳包覆α-Al2O3复合粉体

以膨胀石墨和α-Al2O3微粉为原料,采用高能球磨制备了纳米碳包覆的α-Al2O3复合粉体,研究了高能球磨时间和球磨速率对复合粉体物相及形貌的影响。采用X射线衍射仪、场发射扫描电子显微镜和透射电子显微镜对复合粉体的物相、形貌和微观结构进行了表征。结果表明:按膨胀石墨与α-Al2O3质量百分比为1:2,球磨速率为600 r/min,球磨5 h可得到被粒度为20～50 nm碳颗粒包覆的α-Al2O3复合粉体;随着球磨时间延长,石墨(002)晶面特征峰逐渐消失,膨胀石墨中纳米片层会随球磨时间延长不断剥离脱落,并逐渐龟裂成纳米碳颗粒;相同球磨时间下,提高球磨速率可以促进纳米碳颗粒形成,但超过一定速率后纳米碳颗粒粒度不再减少;480 r/min速率球磨5 h未形成纳米碳颗粒包覆复合粉体,600和700 r/min速率球磨5 h后复合粉体形貌基本一致。     

甲烷气氛中激光-感应复合加热制备碳包覆纳米铝粉

在甲烷气氛中采用激光-感应复合加热法制备了碳包覆纳米铝粉。使用XRD、TEM、HRTEM对碳包覆纳米铝粉进行物相、形貌、结构分析。结果表明，制备的纳米胶囊粒径范围为8～40nm。平均粒径28nm，纳米铝粒子表面包覆了3-4层石墨碳。对碳包覆纳米铝粉的形成机理进行了讨论。     

微米空心碳球串珠结构的制备与形成机理

以还原Fe粉和活性炭为原料, 通过热CVD法制备出微米级的空心碳球串珠结构. 利用TEM、EDS和多点氮吸附仪进行形貌、成分、比表面积及孔径分布表征. 串珠结构由f(1~2)μm的空心碳球串联而成, 长度可达十几微米. 碳球的壁厚为3~5nm的石墨球壳结构. 所制备产物的比表面积 S _BET 达到306.523m²/g, 其孔径分布在中孔范围, 峰值位于3.761nm. 微米级空心碳球串珠结构的形成机理为含C的Fe微液滴在低温区凝聚并以石墨烯片层的方式析出C, 外延于Fe液滴形成石墨层, 与Fe液滴构成Fe/石墨层核壳结构, 石墨球壳的收缩趋势挤压Fe液滴沿轴向移动. 循环往复上述即形成空心串珠结构. 该结构在节能材料、药物、染料和催化剂等的载体材料、储氢、储能等方面可能具有良好的应用前景.     

碳包覆NiO纳米颗粒的制备与性能

采用直流电弧放电等离子体技术成功制备了碳包覆NiO(NiO@C)纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜、X射线衍射、X射线能量色散分析谱仪、拉曼散射光谱和N_2吸-脱附等测试手段进行了分析。实验结果表明:直流电弧等离子体技术制备的NiO@C纳米颗粒具有典型的核壳结构,内核为面心立方结构的NiO纳米颗粒,外壳为碳层。颗粒形貌主要为立方体结构,粒度均匀,分散性良好,粒径分布在30~70nm范围,平均粒径为50nm,外壳碳层的厚度为5nm。NiO@C纳米颗粒BET比表面积为28m~2/g,等效直径为46nm,与TEM和XRD测得的结果基本一致。Raman光谱说明样品中碳包覆层的石墨化程度较低,发生了红移现象。     

碳包覆氧化亚钴纳米颗粒的制备与性能研究

采用直流电弧放电等离子体技术成功制备了碳包覆氧化亚钴纳米颗粒,并对样品的形貌、晶体结构、粒度、比表面积和孔结构采用高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)、X射线能量色散光谱(XEDS)、拉曼散射光谱(Raman)和N_2吸-脱附等测试手段进行了分析。HRTEM表明该方法制备的碳包覆氧化亚钴纳米颗粒具有典型的核壳结构,颗粒形貌主要为球形或椭球结构,粒度均匀,分散性良好,粒径分布在20~60nm,平均粒径为40nm,外壳碳层的厚度为5nm。XRD证明样品的内核为面心立方结构的氧化亚钴纳米颗粒,外壳为碳层。XEDS图谱表明样品中主要存在Co、O和C元素的特征峰。Raman光谱说明样品中碳外包覆层的石墨化程度较低,发生了红移现象。样品的N_2吸附-脱附等温曲线属Ⅳ型,BET比表面积为33m~2/g,BJH脱附累积总孔孔容和脱附平均孔径分别为0.078cm~3/g和11nm。当量粒径为43nm,与TEM和XRD测得的结果基本一致。     

金属对炭黑转化为洋葱状中空结构纳米碳的影响

研究了炭黑分别在 Fe、Co、Ni 三种金属化合物作用下的催化转化行为, 以期使炭黑质点中不连续的无规则小石墨片层重新组装、构筑成洋葱状中空结构纳米碳. 采用透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)和Raman光谱分析表征了炭黑及其催化炭化产物的微观形貌和结构. 结果表明: 尽管三种金属催化剂均可通过溶碳-析出机制形成过渡态碳包覆纳米金属颗粒, 继而构筑成由准球形同心石墨壳层组合的洋葱状中空结构纳米碳, 但三种金属催化剂显示不同的催化效果, 终碳产物的形态和纯度差异较大, 其中以Fe 的催化效果最好.     

石墨微粒的表面化学沉积包覆

通过中温沥青在人造石墨表面发生热缩聚反应制备单颗粒"核-壳"型复合炭。扫描电子显微镜(SEM)和粒度测试结果表明:随着反应时间的延长,石墨片层的微观表面明显改变,包覆物首先在较为尖锐的棱角处形成,继而由石墨碎片的边缘向石墨片层表面延伸,直至覆盖石墨片层。X-射线衍射(X-ray)、红外光谱(FT-IR)、示差扫描量热(DSC)等分析结果表明:表面包覆物由中间相沥青组成。石墨微粒的表面化学沉积包覆机理为:中温沥青首先经过热分解和热缩聚反应形成平面稠环分子,继而在石墨微粒表面吸附并不断层积和继续生长,直至实现单颗粒石墨表面化学沉积包覆。     

H_2O_2处理碳包覆铁纳米颗粒的表面特性及分散行为

采用体积分数30%的H2O2处理碳包覆铁纳米粒子外层的非晶态类石墨碳层,并将其超声分散于水介质中,通过改变pH值分析测定碳包覆铁纳米粒子表面zeta电位和粒径。结果表明:碳包覆铁纳米粒子非晶碳层的特殊结构可通过双氧水化学处理使其表面产生羧基和羟基;在强碱性介质下,羟基和羧基可强化颗粒间的静电斥力,提高碳包覆铁纳米粒子在水介质中的分散性能。当pH值约为11.5时,碳包覆铁纳米粒子表面zeta电位为48 mV,水合粒子粒径可达到110 nm。     

8-羟基喹啉锌/碳微球复合材料的合成表征及发光性能

利用流变相反应法制备了碳微球(CMSs)负载8-羟基喹啉锌(Znq2)的复合材料.通过场发射扫描电子显微镜、X射线衍射仪、热重分析仪、X射线光电子能谱仪、傅里叶红外光谱仪和荧光分光光度计等对Znq2/CMSs复合材料结构和发光性能进行了表征和分析.结果表明:Znq2以非共价键形式负载于直径均匀的CMSs(300～400...     

膨胀石墨基镍/炭复合物(英文)

NiO粒子修饰的压缩膨胀石墨(EGNiO)浸以煤焦油沥青,经550℃裂解,继而800℃水蒸气活化,制得Ni/C复合物块体。应用TEM考察了复合物中含Ni纳米粒的微结构排列方式。以N2吸附测定分析了复合物的比表面积和孔隙度。以2,2,3—三甲基戊烷脱氢裂解模型反应评估了复合物的催化活性并与EGNiO常规H2处理获得的参照物的活性做了比较。     

镀镍碳纳米管的微波吸收性能研究

用竖式炉流动法制备了碳纳米管,碳纳米管的外径40nm～70nm,内径7nm～10nm,长度50μm～1000μm,呈直线型,用化学镀法在碳纳米管表面镀上了一层均匀的金属镍。碳纳米管吸波涂层在厚度为0.97mm时,在8GHz～18GHz,最大吸收峰在11.4GHz(R=-22.89dB),R<-10dB的频宽为3.0Hz,R<-5dB的频宽为4.7GHz。镀镍碳纳米管吸波涂层在相同厚度下,最大吸收峰在14GHz(R=-11.85dB),R<-10dB的频宽为2.23Hz,R<-5dB的频宽为4.6GHz。碳纳米管表面镀镍后虽然吸收峰值变小,但吸收峰有宽化的趋势,这种趋势对提高材料的吸波性能是有利的。碳纳米管作为偶极子在电磁场的作用下,会产生耗散电流,在周围基体作用下,耗散电流被衰减,从而雷达波能量被转换为其它形式的能量。     

Synthesis and magnetic properties of shuriken-like nickel nanoparticles

Shuriken-like nickel nanoparticles were successfully synthesized by a thermal decomposition method at 200 °C with Nickel(II) acetylacetonate (Ni(acac)₂) as the precursor and oleylamine (OAm) as the solvent and reductant, respectively. The phase structures, morphologies and sizes, and magnetic properties of the as-synthesized nickel products were characterized in detail by using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). Some key reaction parameters, such as the reaction time, reaction temperature and surfactants, have important influence on the morphology of the final products. XRD pattern indicated that the products are well-crystallized face-centered cubic (fcc) nickel phase. SEM images demonstrated that the nickel nanoparticles are shuriken-like morphology with average size around 150 nm. The mechanism of shuriken-like Ni nanoparticles (NPs) is proposed. The magnetic hysteresis loops of shuriken-like and spherical nickel products illustrated the ferromagnetic nature at 300 K, indicating its potential applications in magnetic storage.     

高锰酸钾对炭微球表面的改性

首先采用化学气相沉积法,在氩气气氛下,以脱油沥青为原料制备了炭微球(CMSs);然后用不同浓度的KMnO4溶液对CMSs进行处理,使得CMSs表面被氧化并包覆一层MnO2;最后用草酸洗涤产物,除去MnO2。通过场发射扫描电镜对CMSs氧化前后的形貌进行观察,用X-射线衍射对产物进行结构表征,并考察了氧化前后的CMSs在水和乙醇中的分散性。结果表明:当用0.1mol/L的KMnO4氧化改性CMSs后,CMSs表面包覆了一层MnO2,形成MnO2/CMSs复合材料。经过量的草酸进行洗涤,得到的产物在水中分散效果很好,且在乙醇中也有一定分散性。氧化后CMSs的表面存在亲水活性位点,为CMSs的进一步功能修饰奠定了基础。     

单分散镍碳复合纳米球和碳微球的制备

以脱油沥青(deoiled asphalt)为碳源,采用化学气相沉积法(CVD)制备碳微球,其裂解后的残渣经真空热处理制得单分散镍碳复合纳米球.用场发射扫描电镜(FESEM)、高分辨透射电镜(HRTEM)和X射线衍射仪(XRD)对产物进行表征.结果表明,碳微球高纯,属无定型碳结构,大小分布在1～2μm范围内;镍碳复合纳米球为准球形核壳结构,核为镍,壳为碳,尺寸在10～30nm范围,晶化程度较高,结构较完善.     

Characterization of the metal particles fraction in ceramic matrix composites fabricated under high pressure

This paper presents preliminary results concerning Al₂O₃–Ni composites fabricated by sintering under a high pressure of 7.7 GPa, at a temperature below the melting temperature of nickel. The microstructure of composites was characterized by scanning and transmission electron microscopy. Quantitative measurements of size, shape and distribution of metal particles were based on image analysis.

A correlation between the size of the Ni particles and their location has been found. Small Ni particles, with a grain size in the range of 50–500 nm, are mostly located inside the ceramic grains. Some Ni particles are also situated at the grain boundaries, and large particles are surrounded by ceramic grains. The shape of the ceramic grains suggests that the ceramic powder particles underwent deformation during the process of consolidation under high pressure.     

Synthesis of multi-walled carbon nanotube supported nickel catalysts by hydrazine reduction and their electrocatalytic activity on ethanol electro-oxidation

Multi-walled carbon nanotube (MWCNT) supported nickel (Ni) catalysts were chemically synthesized via a hydrazine reduction process with addition of cetyltrimethylammonium bromide (CTAB) as a special additive. As evidenced by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and high-revolution transmission electron microscope (HR-TEM), the Ni nanoparticles (NPs) deposited on the sidewalls of MWCNTs were found to be face-centric cubic (fcc) crystal structure, and dispersed homogenously with a sharp particle size distribution centered at around 20 nm of diameter. Electro-oxidation of ethanol on MWCNT/Ni catalysts was investigated by cyclic voltammetry (CV) measurement. The MWCNT/Ni catalysts showed excellent electro-catalytic activity for the oxidation of ethanol in alkaline solution.     

Solution-processed Ni–CNTs filled ferroelectric P(VDF–TrFE) composites with improved dielectric properties and thermal conductivity

Dielectric composites made using two kinds of poly(vinylidene fluoride–trifluoroethylene) [P(VDF–TrFE)] (70/30 and 80/20 mol%) as polymer matrices and nickel particles coated carbon nanotubes (Ni–CNTs) as filler were developed via solution-processed method. The scanning electron microscopy (SEM) indicated good compatibility and dispersion of Ni–CNTs in the P(VDF–TrFE) matrix. Ni–CNTs/P(VDF–TrFE) composites exhibited high dielectric constants with low dielectric losses. The maximum dielectric constants of Ni–CNTs/P(VDF–TrFE) composites of 198 and 185 at 100 Hz were obtained at 18.0 wt% Ni–CNTs loading, respectively. The incorporation of Ni–CNTs in the P(VDF–TrFE) matrix resulted in enhanced thermal conductivity. The highest values, obtained at 18.0 wt% Ni–CNTs loading, were 1.05 and 1.03 W/m K, respectively. Although there were no very obvious difference, the dielectric properties and thermal conductivity of Ni–CNTs/P(VDF–TrFE) 70/30 mol% composites were slightly better to those of Ni–CNTs/P(VDF–TrFE) 80/20 mol% composites in many cases. The aforementioned results suggest that these high-performance composites hold great promise for application in electrical and electronic field.     

纳米镍颗粒填充碳纳米管的制备与磁性能

采用自制的实验装置, 通过阳极弧放电等离子体技术成功制备了Ni纳米颗粒填充的碳纳米管, 利用高分辨透射电子显微镜(HRTEM)、 XRD、 TEM、 X射线能量色散分析谱仪(XEDS)和振动样品磁强计(VSM)等测试手段对样品的化学成分、 形态、 微观结构和磁性能进行了表征。实验结果表明, 采用本文中实验方法能获得大量被纳米金属颗粒填充的碳纳米管, 其内部填充物为面心立方(FCC)结构的纳米Ni颗粒, 外围薄层为石墨碳层。碳纳米管的外径为30~40 nm, 壁厚5~8 nm, 内部填充的纳米颗粒呈球形和椭球形, 粒径均匀, 在管腔内不连续分布。产物具有顺磁特性, 矫顽力是78 Oe, 饱和磁化强度是33 enu/g。