中间相沥青基泡沫炭的制备、结构及性能

以萘系中间相沥青为原料,考察了发泡条件、炭化和石墨化工艺对所制泡沫炭结构和性能的影响.结合粘温曲线、TG-DTG热重曲线以及不同发泡条件下泡沫炭的表面形貌分析,其最佳发泡条件为:发泡温度600℃,升温速率5℃/min,发泡压力5MPa.石墨化升温速率越低越有利于泡沫炭石墨微晶的生长及压缩强度的提高,其中以5℃/min升温至2800℃并恒温30min所制泡沫炭的压缩强度达1.38MPa.     

发泡温度对炭泡沫结构及性能的影响

以AR中间相沥青为原料,采用中间相沥青自发泡法在初始发泡压力为3MPa、发泡温度在390～450℃范围内制备了4种炭泡沫。利用SEM观察了炭泡沫的孔隙结构,并测定了其体积密度、抗压强度和导热系数,考察了发泡温度对炭泡沫结构及性能的影响。结果表明,采用较低的发泡温度(430℃)可以消除大的孔隙缺陷;当发泡温度为410℃时,炭泡沫导热系数最高,为0.256W/(m·K)。     

CVD PyC对炭泡沫结构及性能的影响

以AR中间相沥青为原料,采用中间相沥青自发泡法在发泡压力为0.1、3.0MPa,发泡温度为450℃的条件下制备了两种不同体积密度的炭泡沫CF-1和CF-2.将CF-1经过10h和70h化学气相沉积热解炭(CVDPyC)处理后得到炭泡沫CF-1-PC1和CF-1-PC2.测定了炭泡沫的抗压强度和导热系数,利用SEM和光学显微镜观察了炭泡沫的孔结构,考察了CVD PyC对炭泡沫结构及性能的影响.研究结果表明,CVD PyC处理可以增加炭泡沫韧带宽度,封填孔壁微裂纹;沥青炭和热解炭之间无明显界面,结合良好;经过CVD PyC处理后得到的CF-1-PC1和CF-1-PC2的体积密度、抗压强度、导热系数分别为, 0.196g·cm-3、1.89MPa、0.314W·m-1·K-1和0.461g·cm-3、11.93MPa、1.581W·m-1·K-1.     

炭泡沫的制备、性能及应用

炭泡沫是具有广阔应用前景的新型炭材料,自出现起就成为炭材料研究中的热点.以中间相沥青基炭泡沫为重点,介绍了炭泡沫的发展历史和研究进展,总结了现有炭泡沫制备技术,包括发泡剂发泡法、模板法、中间相沥青自发泡法和限空间法等,概述了炭泡沫的性能和应用前景,并展望了其发展方向.     

中间相沥青基泡沫炭的制备与结构表征

将石油系中间相沥青利用限定尺寸法发泡后获得了泡沫炭,泡沫炭再经氧化、炭化和石墨化处理获得了具有良好孔结构的泡沫炭.利用SEM和XRD分析了泡沫炭的形态和结构.发现调整发泡模具中的自由空间可以控制泡沫炭的孔径;炭化和石墨化后泡沫炭的孔径减小,孔壁片层取向接近石墨;泡沫炭的孔壁由平直孔壁和“Y”形孔壁结构成,前者内部片层取向优于后者.大孔径泡沫炭的孔壁具有更紧密的内部分子排列,但其微晶尺寸较小.     

预氧化对中间相沥青泡沫炭结构和性能的影响机制研究

研究了预氧化对萘系中间相沥青的表面化学性质、族组成分布以及对泡沫炭的发泡条件、泡孔形成、孔结构及微结构的影响机制.当中间相沥青经210℃预氧化2h后,其喹啉不溶物含量增加32.3%,族组成分布变窄.在600℃/3MPa发泡条件下,所制石墨化泡沫炭的平均孔径、压缩强度分别为200μm、2.8MPa.     

中间相沥青基炭泡沫体的制备、结构及性能

以合成中间相萘沥青为原料，采用加压发泡法制备孔径均匀的初生炭泡沫体，经700℃～1000℃和2300℃～2800℃热处理制备出炭化和石墨化炭泡沫体；以700℃炭化处理所得的炭泡沫体作为芯材制成夹芯复合材料。研究了原料性能、发泡以及热处理工艺参数对炭泡沫微观结构和力学性能的影响，考察了炭泡沫体夹芯复合材料的微波吸收性能。结果表明：发泡过程中保持均匀的温度场是制备孔径均匀的炭泡沫体的关键因素，压力是影响孔结构的主要因素。炭泡沫体的微晶结构、力学性能以及微波吸收性能沿xy和XZ面方向（分别表示垂直和平行于重力方向）具有各向异性。     

分级结构沸石/泡沫炭整体复合材料的制备

用T型沸石/聚酰胺酸悬浊液浸渍聚氨酯泡沫,然后在900℃下热处理制备原位担载的T型沸石/泡沫炭复合材料。用SEM,XRD和物理吸附仪等设备对所得样品进行表征。结果表明:所得复合材料为分级结构整体块状材料,泡沫炭基体的大孔平均尺寸约为500μm;泡沫炭孔壁表面均匀镶嵌了大量沸石分子筛。所得复合材料的微孔孔径分布集中于0.45nm左右,比表面积达到328m2/g。复合材料中沸石分子筛自身的结构特性和化学组成保持不变。     

泡沫炭的制备和性能

泡沫炭是一种开孔相连的轻质炭材料,其最大的特点是多样性和可设计性,具有成为新一代功能材料、结构材料的潜力.以美国橡树岭实验室所制备的泡沫炭为主线,综述了制备泡沫炭的主要方法及其性能,并展望了泡沫炭的应用.     

中间相沥青基炭泡沫

1993年，在第21届国际炭双年度会议上。Hager等结合自己的一些前期研究工作通过模型分析预测了不同于以往的炭泡沫材料的韧带式网架结构的石墨化炭泡沫的存在。1998年，美国橡树岭国家实验室(ORNL)的炭材料研究人员James W．Klett在从沥青制备炭材料时偶然发现了一种石墨化多孔炭材     

加热条件对炭泡沫材料孔结构和性能的影响

以AR沥青为原料,利用高压釜在不同恒温条件下制备了炭泡沫,并测定了其孔结构、体积密度、显气孔率、压缩强度、常温热导率以及微晶参数.结果表明:相对于短恒温时间,长恒温时间制得的炭泡沫孔径大(412nm)、显气孔率高(83.82%)、体积密度小(0.34g/cm~3)、压缩强度高(4.92MPa),多孔连通结构更丰富.经过石墨化处理后,石墨泡沫呈现出较高的常温热导率(71.34W/(m·K))和较小的层片间距d_(002)(0.33556nm).石墨泡沫的常温比导热率能达到210(W·(m·K)~(-1)) /(g·cm~(-3)),是铜的5倍,铝的4倍.     

前驱体对炭泡沫孔结构的影响

分别以煤沥青、石油中间相沥青和AR沥青为前驱体制备炭泡沫材料。采用GPC测定前驱体分子量,SEM观察所制炭泡沫的孔结构,光学显微镜测量所制炭泡沫的孔径及其分布。结果发现,由于煤焦油沥青不含中间相,且QI含量较高,导致在实验条件下不能直接制备出合格的炭泡沫。以石油中间相沥青和AR沥青为原料均能制备出具有分布均匀开孔结构,且微观各向异性的炭泡沫。由AR沥青制备的炭泡沫呈现平均孔径较小(212μm)、孔壁较薄、孔径分布较窄(180μm~300μm)、开孔率较高、以及韧带排列较规整等特点,表明低QI含量、低分子量且分布较窄的前驱体有利于发泡。     

Preparation of polybenzoxazine foam and its transformation to carbon foam

An organic foam derived from a new type of phenolic resin, namely polybenzoxazine, was successfully prepared with a noncomplex and economical foaming method by using azodicarbonamide (AZD) as a foaming agent. The influence of foam density on the physical and mechanical properties of the foams was studied. All resulting polybenzoxazine foams and carbon foams exhibit a tailorable uniform microstructure. Polybenzoxazine foams showed a density in the range of 273–407 kg/m³, and a compressive strength and a compressive modulus in the range of 5.2–12.4 MPa and 268–681 MPa, respectively. The foam density not only affects the physical and mechanical properties, but also affects the deformation response of the foam. In addition, the polybenzoxazine foam was further transformed into carbon foam by carbonization at 800 °C under an inert atmosphere, and its properties were examined.     

由中间相沥青制备泡沫炭:Fe(NO3)3的影响

以中间相沥青为前驱体制备高性能泡沫炭，在考察中间相沥青、Fe（NO3）3及其混合物热分解行为的基础上，着重研究了Fe（NO3）3对制备中间相沥青基泡沫炭的影响，揭示了Fe（NO3）3对泡沫炭孔泡结构的影响规律及其作用机制，初步研究了在泡沫炭炭化过程中形成的Fe／C之物相结构及其石墨化行为。结果表明，在不同的炭化温度下，Fe在泡沫炭中的存在形态各异；Fe物种的存在有利于提高泡沫炭的石墨化程度。     

管式炭膜制备工艺对膜孔结构的影响

研究了以中间相炭微球为原料,羧甲基纤维素为添加剂制备管式炭膜过程中膜孔的形成及控制.扫描电子显微镜(SEM)分析表明,炭膜中的孔隙主要是由微球堆积的间隙和粘结剂高温分解形成的.热重分析(TG)和气泡法孔径测试结果表明,随着添加剂用量的减少和升温速率的提高,炭膜孔径减小;同时低于800℃炭化处理能够显著增加炭膜孔径.浸渍液浓度的增加和浸渍次数的增加均能减小炭膜平均孔径,说明制备工艺条件的控制是调整膜孔结构的有效手段.     

On the use of mesophase pitch for the preparation of hierarchical porous carbon monoliths by nanocasting

Abstract

A detailed study is given on the synthesis of a hierarchical porous carbon, possessing both meso- and macropores, using a mesophase pitch (MP) as the carbon precursor. This carbon material is prepared by the nanocasting approach involving the replication of a porous silica monolith (hard templating). While this carbon material has already been tested in energy storage applications, various detailed aspects of its formation and structure are addressed in this study. Scanning electron microscopy (SEM), Hg porosimetry and N₂ physisorption are used to characterize the morphology and porosity of the carbon replica. A novel approach for the detailed analysis of wide-angle x-ray scattering (WAXS) from non-graphitic carbons is applied to quantitatively compare the graphene microstructures of carbons prepared using MP and furfuryl alcohol (FA). This WAXS analysis underlines the importance of the carbon precursor in the synthesis of templated porous carbon materials via the nanocasting route. Our study demonstrates that a mesophase pitch is a superior precursor whenever a high-purity, low-micropore-content and well-developed graphene structure is desired.     

Application of microcapsulation technology to the preparation of carbon foam

Abstract

Microcapsules were prepared by in situ polymerization and microcapsulation. Tetraethyl orthosilicate was used as the core material and phenolic resin was used as the wall material in an emulsion system of polyacrylic and tetraethyl orthosilicate. The obtained microcapsules were slowly heated such that the core material was released by evaporation, leaving hollow-core spheres. The spheres were mixed with a phenolic resin-derived binder and molded to obtain a carbon foam precursor, which was carbonized at 1100 °C under the protection of N₂ gas and graphitized at 2300 °C under the protection of Ar gas. Thus, the carbon foam of hollow closed-shelled microspheres with a graphitic structure was prepared. The properties and structure of this foam were discussed.     

Application of microcapsulation technology to the preparation of carbon foam

Microcapsules were prepared by in situ polymerization and microcapsulation. Tetraethyl orthosilicate was used as the core material and phenolic resin was used as the wall material in an emulsion system of polyacrylic and tetraethyl orthosilicate. The obtained microcapsules were slowly heated such that the core material was released by evaporation, leaving hollow-core spheres. The spheres were mixed with a phenolic resin-derived binder and molded to obtain a carbon foam precursor, which was carbonized at 1100 °C under the protection of N₂ gas and graphitized at 2300 °C under the protection of Ar gas. Thus, the carbon foam of hollow closed-shelled microspheres with a graphitic structure was prepared. The properties and structure of this foam were discussed.