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.     

以天然沥青岩为原料制备高压缩强度的泡沫炭(英文)

以安纳托利亚东南部的天然沥青岩为原料制备泡沫炭。所制泡沫炭的平均孔径和密度分别为150μm和800 kg/m3。主要研究了压力、温度、泄压时间及在最高温度时的停留时间对泡沫形成的影响,同时还评价了炭化过程对泡沫结构的影响。主要研究了压力、温度、泄压时间及在最高温度时的停留时间对泡沫炭进行了表征,并进行了密度及抗压强度分析。结果表明,1 323 K炭化后,泡沫炭压缩强度由10 MPa增加到18.7 MPa。沥青的灰分含量(41.76%)对泡沫炭的密度和压缩强度起重要作用。     

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.     

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。     

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。     

制备条件对炭泡沫结构的影响

利用沥青在热解过程中产生挥发性气体自发泡和高压渗氮的原理，以石油中间相沥青为原料，采用高压反应釜制备炭泡沫材料。用SEM和偏光显微镜观察了材料的孔结构，分析了制备条件对炭泡沫结构的影响。结果表明，温度和压力是影响炭泡沫材料结构的重要因素，在实验条件范围内，较高的反应温度和压力有利于制备出较高性能的炭泡沫，其气孔率较高，韧带炭层排布规则。     

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。     

热解炭过渡层-中间相沥青基炭/炭复合材料的微观结构

借助偏光显微镜、扫描电镜、透射电镜对具有热解炭过渡层的中间相沥青基炭/炭复合材料的微观结构进行了研究。结果表明:材料的基体由热解炭和中间相沥青炭组成,在偏光显微镜下均呈现出光学各向异性。材料内部形成了多层次的界面结构,热解炭与纤维的界面连续,界面层内的石墨微晶择优取向度较高,晶格条纹排列规整;中间相沥青炭与热解炭界面不连续,为"裂纹型"界面,界面层内主要为非晶态碳。材料中炭纤维、热解炭、中间相沥青炭的石墨微晶大小逐渐增大,择优取向度逐渐增高,晶格条纹的排列逐渐规整。片层条带状结构的中间相沥青炭以及材料内的微裂纹平行于炭纤维轴向。     

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.     

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)。     

Template synthesis of nanophase mesocarbon

Templating techniques are used increasingly to create carbon materials with precisely engineered pore systems. This article presents a new templating technique that achieves simultaneous control of pore structure and molecular (crystal) structure in a single synthesis step. With the use of discotic liquid crystalline precursors, unique carbon structures can be engineered by selecting the size and geometry of the confining spaces and selecting the template material to induce edge-on or face-on orientation of the discotic precursor. Here mesophase pitch is infiltrated by capillary forces into a nanoporous glass followed by slow carbonization and NaOH etching. The resulting porous carbon material exhibits interconnected solid grains about 100 nm in size, a monodisperse pore size of 60 nm, 42% total porosity, and an abundance of edge-plane inner surfaces that reflect the favored edge-on anchoring of the mesophase precursor on glass. This new carbon form is potentially interesting for a number of important applications in which uniform large pores, active-site-rich surfaces, and easy access to interlayer spaces in nanometric grains are advantageous.     

The influence of processing temperature on the structure and properties of mesophase-based polygranular graphites

Two polygranular graphites were prepared by sintering a coal-tar pitch based mesophase and a naphthalene-based mesophase. The influence of temperature on the structural (density, porosity and light texture), mechanical (flexural strength) and electrical (electrical resistivity) properties of the carbons was studied at different stages of carbonization/graphitization (400–2600°C). The results show that the density of the materials increases continuously with temperature, pores mainly appearing below 800°C, during the low-sintering phase and at the initial stages of the solid-sintering process. Above this temperature, porosity decreases due to the densification of the materials. Densification is clearly evidenced by a reduction in interlayer spacing and an increase in crystallite size. Flexural strength and electrical resistivity follow a different trend depending on the temperature range. Thus, flexural strength reaches its maximum value at 1000°C, while electrical resistivity decreases continuously with temperature. Any variation in these properties is mainly related with porosity and crystallographic order. The different composition of the raw materials causes structural, mechanical and electrical changes to occur to different extent in both materials.     

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.     

Fe3O4纳米粒子作为催化剂和致孔剂制备高比表面积块体石墨化炭

报道了一种以Fe3O4纳米晶粒为催化剂和致孔剂制备具有高比表面积块体石墨化炭的方法.首先采用共沉淀法合成粒径＜10nm的Fe3O4纳米颗粒,然后将其均匀分散到以2,4-二羟基苯甲酸(D)、甲醛(F)为原料,无水Na2 CO3为催化剂形成的聚合物(DF)中,通过溶胶-凝胶过程和炭化过程得到掺杂Fe的石墨化炭.最后经过酸洗,得到纯的高比表面积块体石墨化炭.随炭化温度的升高(700℃～900℃),样品的石墨化程度增加.在800℃炭化,样品已具有明显的石墨化结构,且比表面积较大.     

HKT800碳纤维微观结构与性能

为深入剖析国产HKT800碳纤维的微观结构和性能,用扫描电子显微镜、原子力显微镜、拉曼光谱、X射线衍射仪、压汞仪等对HKT800碳纤维进行了表征,并与东丽T800碳纤维进行了对比分析,结果表明:HKT800碳纤维的表面带有沟槽,少量碳纤维截面呈腰果形,不同于T800碳纤维,且表面粗糙度较大;HKT800碳纤维拉曼测试ID/IG比值为1.07,表面微晶尺寸较小;2种碳纤维层间距均为0.347 nm,孔隙率均为17.4%,比较一致,但HKT800碳纤维堆叠尺寸、取向度略高于T800碳纤维,而微孔偏离碳纤维轴取向程度、微孔长度、微孔横截面平均切割线长度均略低于T800碳纤维,HKT800碳纤维中微孔尺寸、数量的分布也不同于T800碳纤维.     

中间相沥青基泡沫炭的气泡生长过程

以AR合成中间相沥青为原料,在不同的温度下发泡制得了泡沫炭.采用扫描电镜和光学显微镜等分析手段对中间相沥青基泡沫炭的气泡生长机理进行了初步研究,讨论了温度对泡孔结构的影响.结果表明,当温度从480℃升至540℃时,平均泡孔直径从500μm升到800μm.最初形成的泡沫在熔融沥青中分布不均匀,汇集在沥青的上表面;气泡在Z轴方向的形状是椭球形,在Z轴垂直方向为球形.中间相沥青基泡沫炭气孔的形状和泡沫的体积密度密切相关.形成的泡沫体在z轴方向存在明显的体积密度梯度.     

磷酸法活化煤焦油渣制备活性炭研究

研究了以陕西煤焦油渣作为原料,用磷酸作为活化剂,在400～1000℃的条件下经一步炭活化法制备活性炭。研究了炭活化温度、时间、料剂比对煤焦油渣制备活性炭吸附性能及孔结构的影响。实验结果表明炭活化温度、炭活化时间主要影响活性炭产品的得率,高温和长时间会导致更多的碳损失;活性炭的吸附性能及孔结构主要受炭活化温度和料剂比影响。最佳活化工艺条件为850℃、3h、1∶3。通过其活性炭表面孔径分布及表面官能团含量变化表征,用磷酸浸泡煤焦油渣制备活性炭有利于大、中孔结构的产生,其最佳活化条件下孔径分布约在20～100nm。     

A porous carbon foam prepared from liquefied birch sawdust

Carbon foam was prepared by submitting birch sawdust to liquefaction, resinification, foaming, carbonization, and activation steps. The foam was characterized by TG and DTG, XRD, SEM, and nitrogen adsorption at 77 K. A mechanism for the formation of the porous carbon foam was proposed. Solid non-graphitized lightweight carbon foams with specific surface areas of 534–555 m²/g and cell sizes of 100–200 μm were obtained, depending on the carbonization or activation temperature used. The intermediate liquefied birch-based resin foam exhibits thermal stability superior to liquefied wood and inferior to phenolic resin, and decomposes rapidly in two stages, at 285.7 and 412.9 °C, respectively. Further activation of the carbon foam in a stream of nitrogen above 800 °C improves the pore structure and homogeneity of the cell size significantly. The matrix of the foams contains a large number of micropores, and the microstructure becomes more ordered as the activation temperature is increased.     

电耦合CVI制备穿刺C/C喉衬材料的微结构及性能

采用电耦合化学气相渗透（CVI）联合树脂浸渍碳化工艺制备了穿刺碳纤维预制体增强C/C喉衬材料,利用μ-CT表征了穿刺C/C材料增密不同阶段孔隙尺寸,研究了该材料2 800℃拉伸性能和缩比固体发动机烧蚀性能。结果表明,电耦合CVI增密后穿刺C/C喉衬材料孔隙主要存在于纤维束间,呈现空间联通的网状结构,树脂碳循环致密后材料内部仍残存少量体积0~0.08 mm³的微小孔隙,孔隙呈现孤立的点分布状态。穿刺C/C材料2 800℃拉伸强度略高于室温,断裂应变比室温提高118%,表现出优异的非线性断裂行为。穿刺C/C喉衬缩比固体发动机点火试验后线烧蚀率0.077 mm/s,喉衬不同区域的烧蚀机制有一定差异,喉衬收敛段穿刺纤维束承受驻点烧蚀,产生蜂窝状烧蚀凹坑,烧蚀较严重,喉部和扩散段烧蚀较为平滑。     

Graphitic Carbon Nitride (g‐C3N4)‐Derived N‐Rich Graphene with Tuneable Interlayer Distance as a High‐Rate Anode for Sodium‐Ion Batteries

Heteroatom‐doped carbon materials with expanded interlayer distance have been widely studied as anodes for sodium‐ion batteries (SIBs). However, it remains unexplored to further enlarge the interlayer spacing and reveal the influence of heteroatom doping on carbon nanostructures for developing more efficient SIB anode materials. Here, a series of N‐rich few‐layer graphene (N‐FLG) with tuneable interlayer distance ranging from 0.45 to 0.51 nm is successfully synthesized by annealing graphitic carbon nitride (g‐C₃N₄) under zinc catalysis and selected temperature (T = 700, 800, and 900 °C). More significantly, the correlation between N dopants and interlayer distance of resultant N‐FLG‐T highlights the effect of pyrrolic N on the enlargement of graphene interlayer spacing, due to its stronger electrostatic repulsion. As a consequence, N‐FLG‐800 achieves the optimal properties in terms of interlayer spacing, nitrogen configuration and electronic conductivity. When used as an anode for SIBs, N‐FLG‐800 shows remarkable Na⁺ storage performance with ultrahigh rate capability (56.6 mAh g^?1 at 40 A g^?1) and excellent long‐term stability (211.3 mAh g^?1 at 0.5 A g^?1 after 2000 cycles), demonstrating the effectiveness of material design.