中间相沥青基泡沫炭的制备及性能研究
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摘要
中间相沥青基泡沫炭是以中间相沥青为原料,经过发泡、固化、炭化、石墨化等制备过程所得到的一种新型炭泡沫材料。它所特有的泡孔结构以及其原料结构性质决定了中间相沥青基泡沫炭作为高尖端工程材料的优越性,中间相沥青基泡沫炭的优越性能源于其理想的泡孔结构。发泡工艺和前驱体性质是决定孔径分布、开孔情况的重要因素。本文以热缩聚方法制备中间相沥青,再以自制中间相沥青和日本三菱中间相沥青为前驱体采用自挥发方法制备泡沫炭,经焦化、炭化、石墨化获得最终产品。本文在研究中间相沥青及其泡沫炭制备工艺的基础上,重点考察了原料前躯体和制备方法对中间相沥青基泡沫炭结构和性能的影响,并对泡沫炭微裂纹的控制进行了讨论,力图建立起制备高性能中间相沥青基泡沫炭的方法体系。
利用不同热缩聚时间在420℃时分别制备了一系列中间相沥青,并以自制的沥青为原料发泡制备了一系列泡沫炭,对中间相沥青基泡沫炭的制备进行了初步研究。研究发现较长时间制备的中间相沥青呈现纤维状结构。以由4小时和5.5小时制备的中间相沥青为原料制备的泡沫炭泡孔结构不均匀,而以6.5小时以上制备中间相沥青为原料制备的泡沫炭孔结构较均匀,结构良好。
利用较长时间热缩聚可以制备高软化点的中间相沥青,本文提出了一种较简单的低压制备中间相沥青基泡沫炭的方法。通过对所制备的泡沫炭物理特点、表面形貌和微晶参数的研究,发现可以在0.5-2MPa的压力范围内制备的泡沫炭体积密度范围为0.514-0.624 g/cm3。SEM照片显示由高软化点沥青制备的泡沫炭,炭化和石墨化后显示较小的热收缩。OM照片显示由高软化点沥青制备的泡沫炭无论在节点还是在韧带处都具有较少的微裂纹。XRD数据显示由较高软化点沥青制备的泡沫炭石墨化后具有较小的石墨层间距和较大的微晶尺寸。本文提出的方法可以显示降低制备泡沫炭的压力并降低制备成本。
利用不同的热缩聚时间制备了两种具有不同中间相含量的沥青,并以此沥青为原料发泡制备泡沫炭,研究发现由100%中间相含量的沥青制备泡沫时可以在较宽的温度范围内成功制备样品。而由非100%中间相含量的沥青制备泡沫炭时,只能在沥青的最大热失重处停留较长时间才可以成功制备泡沫炭。由100%中间相含量的沥青制备的泡沫炭石墨化后具有较好的炭层取向和较大的微晶尺寸。利用具有不同天然石墨含量的中间相沥青成功制备了天然石墨/中间相沥青基泡沫炭复合材料,并对泡沫炭结构和天然石墨的添加量之间的关系进行了研究。研究表明天然石墨的添加可以明显减少泡沫炭的微裂纹,当天然石墨的添加量为30%的时候泡沫炭的比压缩强度从2.0MPa/g.cm3提高到5.84MPa/g.cm3,而且随着天然石墨的添加量的增加石墨微晶的层间距先减小后增大。光学照片显示天然石墨的添加明显减小了泡沫炭光学区域的尺寸。
从固化方式的角度考察了氧化固化和焦化固化方式对泡沫炭结构及性能的影响并以三菱AR中间相沥青为原料对发泡机理进行了初步研究。利用SEM、XRD、偏光显微镜等测试手段对泡沫炭微观形貌、孔隙分布等结构参数进行了表征分析。研究表明长时间焦化固化方式比氧化固化方式制备的泡沫炭具有更好的分子取向和较少的微裂纹,石墨化后具有较小的层间距(0.3376nm和0.3381nm);泡沫炭的泡孔形状受体积密度的影响,当体积密度较小时在平行重力方向是椭圆形而在垂直重力方向是圆形,并且气泡首先在沥青上表面形成。
Mesophase-pitch was foamed, stabilized, carbonized and graphitized resulting in a novel foam material Mesophase-pitch-based carbon foam. It is an excellent engineering material due to its unique porous structure and carbon material properties. Porosity, foaming process and properties of the pitch precursor are important factors that affect the final properties of the carbon foam. In this work, mesophase-pitch was prepared by traditional pyrocondensation method and then used the as-received pitch and AR mesophase pitch as precursor to prepare carbon foams, the obtained foam was stabilized, carbonized and graphitized. On the base of researching the preparation processes of mesophase pitches and carbon foams, the text studied the effects of the properties of precursors and preparation methods on the properties of the mesophase pitch derived carbon foams. In addition, the controlling of the microcraks of the foams was discussed in detail and tried to give a principle for preparing mesophase pitch derived carbon foams.
A series of mesophase pitches were prepared by the pyrocondensation under different pyrocondensation time and the as-obtained mesophase pitches were used as precursor to prepare carbon foams. The foaming process was given preliminary study, and experimental results show that the mesphase pitch prepared by long holding time exhibits fibre-like structure. Carbon foams from the mesophase pitches prepared by 4.5h and 5.5h exhibit non-uniform foam structure, and carbon foams prepared from mesophase pitches prepared above 6.5 have good foam structure.
A simple method for preparing the meosphase-pitch-based carbon foams at low pressures through prolonging the soaking time in the preparation process of the mesophase pitch was disclosed. The physical properties, morphologies and the crystal structure of the as-obtained foams were investigated. Bulk density of the resultant carbon foams cover a range 0.514-0.624 g/cm3, under the preparation pressure range 0.5-2 MPa. The SEM micrographs revealed that the thermal shrinkage of the graphitized foams derived from the higher softening point mesophase pitch was less than that of the foam from the lower softening point; Optical micrographs showed that higher softening point mesophase pitch derived carbon foams exhibited better orientation and less microcracks in both junctions and ligaments; The XRD results revealed that higher softening point pitch derived graphitized foams exhibited smaller interlayer spacing and larger crystallite size. The properties of the carbon foam can be severely affected by the properties of the precursor, so it is critical to tailor the properties of the pitch precursor so as to obtain high performance and low cost products.
Two kinds of mesophase pitches were prepared and used as precursor to prepare carbon foams in order to study the effects of mesophase content on the properties of the final products. The experimental results show that carbon foams with cell size uniformity can be prepared from the non-100% mesophase content pitch only under the temperature around the maximum rate of weight loss. The non-100% mesophase content pitch derived foams exhibit more microcracks and worse mesophase domain orientation in the cell walls than that of 100% mesophase content pitch derived foams. After graphitization, the foams from non-100% mesophase content pitch show lower graphitization degree and smaller crystallite sizes. The properties of the carbon foams can be severely affected by the mesophase content, and carbon foams prepared from the non-100% mesophase content pitch give a potential process to prepare foams with properties between insulating and high-thermal-conductivity carbon foams and thus maximizing the potential use of carbon foams. Graphite foams were prepared from the mesophase pitch with addition of natural graphite and the relationship between properties and structure of these foams was investigated in detail. These graphite foams possessed high specific compressive strength and experimental results show that reduced microcracks appeared on the cell walls of foam by adding of natural graphite. The specific compressive strength increased from 2.0 to 5.84 MPa/g.cm3 with the addition of 30 wt% natural graphite, and the inter layer spacing of graphite foams decreased with the increase of the natural graphite content in the pitch. In addition, the optical micrograph shows that the anisotropic domain size of the foam decreased with the addition of natural graphite and it also affects the compressive strength of the foams.
The effects of different stabilization methods on the structural properties of the carbon foams were also studied; the foaming mechanism of carbon foam prepared using AR mesophase-pitch as precursor was also studied. SEM, XRD, OM, et al were used to detect the bubble shape and the morphology of the as-obtained foams. The results show that the bubble structure and structural properties of carbon foam can be controlled by the softening point of the pitch precursor. Carbon foam prepared by long-time-coking method exhibit better molecular orientation, larger mesophase domain, less microcracks and less interlayer spacing (0.3376nm and 0.3381nm) when the carbon foam were graphitized. The initial foam bubble are not uniformly dispersed in the molten pitch but start to grow at the upper section of the pitch; the cross section bubble shape at gravitational direction is spherical but at the direction perpendicular to gravitational direction is elliptical. Research show that the bulk density is the key factor to determine the bubble shape of the final mesophase-pitch-based carbon foams and the bulk density gradient exist in the as-received carbon foams.
利用不同热缩聚时间在420℃时分别制备了一系列中间相沥青,并以自制的沥青为原料发泡制备了一系列泡沫炭,对中间相沥青基泡沫炭的制备进行了初步研究。研究发现较长时间制备的中间相沥青呈现纤维状结构。以由4小时和5.5小时制备的中间相沥青为原料制备的泡沫炭泡孔结构不均匀,而以6.5小时以上制备中间相沥青为原料制备的泡沫炭孔结构较均匀,结构良好。
利用较长时间热缩聚可以制备高软化点的中间相沥青,本文提出了一种较简单的低压制备中间相沥青基泡沫炭的方法。通过对所制备的泡沫炭物理特点、表面形貌和微晶参数的研究,发现可以在0.5-2MPa的压力范围内制备的泡沫炭体积密度范围为0.514-0.624 g/cm3。SEM照片显示由高软化点沥青制备的泡沫炭,炭化和石墨化后显示较小的热收缩。OM照片显示由高软化点沥青制备的泡沫炭无论在节点还是在韧带处都具有较少的微裂纹。XRD数据显示由较高软化点沥青制备的泡沫炭石墨化后具有较小的石墨层间距和较大的微晶尺寸。本文提出的方法可以显示降低制备泡沫炭的压力并降低制备成本。
利用不同的热缩聚时间制备了两种具有不同中间相含量的沥青,并以此沥青为原料发泡制备泡沫炭,研究发现由100%中间相含量的沥青制备泡沫时可以在较宽的温度范围内成功制备样品。而由非100%中间相含量的沥青制备泡沫炭时,只能在沥青的最大热失重处停留较长时间才可以成功制备泡沫炭。由100%中间相含量的沥青制备的泡沫炭石墨化后具有较好的炭层取向和较大的微晶尺寸。利用具有不同天然石墨含量的中间相沥青成功制备了天然石墨/中间相沥青基泡沫炭复合材料,并对泡沫炭结构和天然石墨的添加量之间的关系进行了研究。研究表明天然石墨的添加可以明显减少泡沫炭的微裂纹,当天然石墨的添加量为30%的时候泡沫炭的比压缩强度从2.0MPa/g.cm3提高到5.84MPa/g.cm3,而且随着天然石墨的添加量的增加石墨微晶的层间距先减小后增大。光学照片显示天然石墨的添加明显减小了泡沫炭光学区域的尺寸。
从固化方式的角度考察了氧化固化和焦化固化方式对泡沫炭结构及性能的影响并以三菱AR中间相沥青为原料对发泡机理进行了初步研究。利用SEM、XRD、偏光显微镜等测试手段对泡沫炭微观形貌、孔隙分布等结构参数进行了表征分析。研究表明长时间焦化固化方式比氧化固化方式制备的泡沫炭具有更好的分子取向和较少的微裂纹,石墨化后具有较小的层间距(0.3376nm和0.3381nm);泡沫炭的泡孔形状受体积密度的影响,当体积密度较小时在平行重力方向是椭圆形而在垂直重力方向是圆形,并且气泡首先在沥青上表面形成。
Mesophase-pitch was foamed, stabilized, carbonized and graphitized resulting in a novel foam material Mesophase-pitch-based carbon foam. It is an excellent engineering material due to its unique porous structure and carbon material properties. Porosity, foaming process and properties of the pitch precursor are important factors that affect the final properties of the carbon foam. In this work, mesophase-pitch was prepared by traditional pyrocondensation method and then used the as-received pitch and AR mesophase pitch as precursor to prepare carbon foams, the obtained foam was stabilized, carbonized and graphitized. On the base of researching the preparation processes of mesophase pitches and carbon foams, the text studied the effects of the properties of precursors and preparation methods on the properties of the mesophase pitch derived carbon foams. In addition, the controlling of the microcraks of the foams was discussed in detail and tried to give a principle for preparing mesophase pitch derived carbon foams.
A series of mesophase pitches were prepared by the pyrocondensation under different pyrocondensation time and the as-obtained mesophase pitches were used as precursor to prepare carbon foams. The foaming process was given preliminary study, and experimental results show that the mesphase pitch prepared by long holding time exhibits fibre-like structure. Carbon foams from the mesophase pitches prepared by 4.5h and 5.5h exhibit non-uniform foam structure, and carbon foams prepared from mesophase pitches prepared above 6.5 have good foam structure.
A simple method for preparing the meosphase-pitch-based carbon foams at low pressures through prolonging the soaking time in the preparation process of the mesophase pitch was disclosed. The physical properties, morphologies and the crystal structure of the as-obtained foams were investigated. Bulk density of the resultant carbon foams cover a range 0.514-0.624 g/cm3, under the preparation pressure range 0.5-2 MPa. The SEM micrographs revealed that the thermal shrinkage of the graphitized foams derived from the higher softening point mesophase pitch was less than that of the foam from the lower softening point; Optical micrographs showed that higher softening point mesophase pitch derived carbon foams exhibited better orientation and less microcracks in both junctions and ligaments; The XRD results revealed that higher softening point pitch derived graphitized foams exhibited smaller interlayer spacing and larger crystallite size. The properties of the carbon foam can be severely affected by the properties of the precursor, so it is critical to tailor the properties of the pitch precursor so as to obtain high performance and low cost products.
Two kinds of mesophase pitches were prepared and used as precursor to prepare carbon foams in order to study the effects of mesophase content on the properties of the final products. The experimental results show that carbon foams with cell size uniformity can be prepared from the non-100% mesophase content pitch only under the temperature around the maximum rate of weight loss. The non-100% mesophase content pitch derived foams exhibit more microcracks and worse mesophase domain orientation in the cell walls than that of 100% mesophase content pitch derived foams. After graphitization, the foams from non-100% mesophase content pitch show lower graphitization degree and smaller crystallite sizes. The properties of the carbon foams can be severely affected by the mesophase content, and carbon foams prepared from the non-100% mesophase content pitch give a potential process to prepare foams with properties between insulating and high-thermal-conductivity carbon foams and thus maximizing the potential use of carbon foams. Graphite foams were prepared from the mesophase pitch with addition of natural graphite and the relationship between properties and structure of these foams was investigated in detail. These graphite foams possessed high specific compressive strength and experimental results show that reduced microcracks appeared on the cell walls of foam by adding of natural graphite. The specific compressive strength increased from 2.0 to 5.84 MPa/g.cm3 with the addition of 30 wt% natural graphite, and the inter layer spacing of graphite foams decreased with the increase of the natural graphite content in the pitch. In addition, the optical micrograph shows that the anisotropic domain size of the foam decreased with the addition of natural graphite and it also affects the compressive strength of the foams.
The effects of different stabilization methods on the structural properties of the carbon foams were also studied; the foaming mechanism of carbon foam prepared using AR mesophase-pitch as precursor was also studied. SEM, XRD, OM, et al were used to detect the bubble shape and the morphology of the as-obtained foams. The results show that the bubble structure and structural properties of carbon foam can be controlled by the softening point of the pitch precursor. Carbon foam prepared by long-time-coking method exhibit better molecular orientation, larger mesophase domain, less microcracks and less interlayer spacing (0.3376nm and 0.3381nm) when the carbon foam were graphitized. The initial foam bubble are not uniformly dispersed in the molten pitch but start to grow at the upper section of the pitch; the cross section bubble shape at gravitational direction is spherical but at the direction perpendicular to gravitational direction is elliptical. Research show that the bulk density is the key factor to determine the bubble shape of the final mesophase-pitch-based carbon foams and the bulk density gradient exist in the as-received carbon foams.
引文
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