不同特性燃料条件下柴油机缸内微粒纳观结构、表面官能团及氧化活性的研究
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摘要
燃料特性、缸内压力、温度等外界条件对柴油机微粒的纳观结构及其表面官能团影响很大，而微粒的纳观结构和表面官能团又会影响微粒在氧化过程中的反应活性。因此，研究柴油机燃烧过程中不同特性燃料缸内微粒纳观结构、表面官能团及氧化活性的变化规律，对进一步了解柴油机微粒的形成历程和减少微粒的排放具有重要的意义。本文基于全气缸取样系统，应用TEM图像处理、EELS、Raman光谱、FT-IR光谱、XPS和TGA等分析检测技术，针对燃料特性不同的正庚烷、正庚烷/甲苯、柴油和F-T柴油所生成的柴油机缸内微粒，开展了燃烧过程中缸内微粒微观结构、表面官能团及氧化活性演变机制的研究，取得的主要研究成果如下：
1．四种燃料在燃烧过程中均形成了两类结构特性不同的缸内微粒，即由基本碳粒子构成的典型微粒和富含金属和非金属元素的非典型微粒。典型微粒具有分形结构特性，其中正庚烷、20%甲苯/80%正庚烷（体积比）、柴油和F-T柴油的典型微粒分形维数分别介于1.63~1.96、1.48~1.92、1.32~1.84和1.48~1.91之间，且在燃烧过程中均为先减小后增加的变化规律，分形维数的最小值出现在扩散燃烧阶段的初期。燃料中芳香烃和环烷烃组分能够促进分形维数较低的微粒形成。
2．四种燃料基本碳粒子粒径呈类似高斯分布，峰值介于15~25nm，平均粒径在燃烧过程中呈单峰变化趋势，最大值出现在预混燃烧阶段的中后期。平均层面间距和平均曲率随着燃烧进行总体呈逐渐减小的趋势，仅在预混燃烧阶段末期至扩散燃烧阶段初期出现一个突然的上升；微晶尺寸变化趋势则正相反。燃料中的芳香烃和环烷烃组分能够促进基本碳粒子的成长，使平均粒径、层面间距和曲率增大，微晶尺寸减小。此外，Raman光谱IG/ID及EELS中Iπ*/Iδ*的变化规律与微晶尺寸的变规律基本一致，验证了微粒微观结构特征参数提取结果的准确性。
3．微粒表面的脂肪族C–H官能团当量浓度随着曲轴转角的增大整体呈逐渐减小的趋势，仅在预混燃烧阶段末期至扩散燃烧阶段初期出现一个突然的上升。C–OH和C=O官能团浓度均呈“双峰”变化趋势，分别在预混燃烧阶段中期和扩散燃烧阶段末期各出现一个峰值。燃料中的芳香烃及环烷烃通过降低微粒的石墨化程度和纳观结构有序性，增大了微粒表面脂肪族C–H和含氧官能团的浓度。
4．四种燃料生成的缸内微粒氧化所需的表观活化能介于114.57~181.02kJ/mol；燃烧过程中，脂肪族C–H表面官能团是影响微粒的氧化活性主要因素，微观结构和表面含氧官能团则属于相对次要的因素。
Combustion conditions, such as initial fuel composition, in-cylinder pressure andtemperature, play an important role on the nanostructure and surface functionalgroups of diesel particulates. The variations in nanostructure and surface functionalgroups can in turn affect the particulate reactivity toward oxidation. Therefore,detailed invesigations of the diesel in-cylinder particulates generared from differentfuels is necessary for better understanding of the diesel particulates evolutionmechanism and the reduction of particulate pollutions. In this dissertation, a totalcylinder sampling system, fueled with n-heptane, n-heptane/toluene, EuroⅢ lowsulfur diesel fuel and F-T fuel respectively, was employed to obtain in-cylinder sootsamples. The evolution mechanism of nanostructure, surface functional groups andoxidation reactivity of in-cylinder soot was subsequently studied using the analyticalmethod such as digital image processing, electron energy-loss spectroscopy, Ramanspectrum, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy,and thermogravimetric analysis. The major work and achievements of this dissertationare listed as follows:
1. The in-cylinder particulates generated from the four kinds of fuels all presenttwo sorts of morphology: One is the representative particulate which formed throughagglomeration of small sphere-like primary particles, and the other is amorphousparticulate containing abundant metal and nonmetal elements. The representativeparticles are aggregated in the form of fractal-like geometry. The fractal dimensionsfor the N-heptane, N-heptane blended with20%toluene (v/v), EuroⅢ diesel fuel andF-T fuel particulates are in a range of1.63~1.96、1.48~1.92、1.32~1.84and1.48~1.91respectively. During the combustion process, the fractal dimensions of in-cylinderparticulates first decline at the premixed combustion and early diffusion combustionstages, and then increase at the middle/late diffusion combustion and late combustionstages. The minimum particulate fractal dimension lies within the early diffusioncombustion period. The aromatic and cyclanes compounds in fuels can promote thegeneration of particles with low fractal dimensions.
2. The size distributions of primary particles generated from these four fuels aresimilar to Gauss distribution with the peak value of particle diameter in the range of15~25nm. During the combustion process, the mean diameter of primary particlesshows a unimodal distribution with the maximum value locating at the middle/late premixed combustion stage. Meanwhile, the mean fringe separation distance andtortuosity of in-cylinder soot generally decrease, except for a sudden rise between thelate premixed combustion stage and early diffusive combustion stage. In contrast, themean fringe length shows an increasing trend. The aromatic and cyclanes compoundsin fuels can promote the growth of primary particles and bring about an increase inmean particle diameter, fringe separation distance and tortuosity, and a derease inmean fringe length of soot partitulats. Additionally, the ratio of IG/IDin Ramanexperiment and Iπ*/Iδ*in EELS experiment follows a similar trend to that of thefringe length through the combustion history, verifying that the results of the imageprocessing are reasonable.
3. The relative content of the aliphatic C–H groups on the in-cylinder soot surface,which was evaluated by the normalized peak height ratio (IC-H/IC=C), generallydecreases during the combustion process, except for a sudden rise between the latepremixed and early diffusive combustion stages. Meanwhile, the concentrations ofboth C–OH and C=O groups present bimodal distributions over the combustionhistory, with the two peaks locating at the middle premixed and late diffusioncombustion stages respectively. Both aromatic and cycloparaffinic hydrocarbons infuels affect the soot nanostructure and degree of graphitization, which has asignificant impact on the relative content of surface aliphatic C–H groups.
4. Under the applied engine operating conditions where these four fuels wereused, the apparent activation energies for soot oxidation are in a range of114.57～181.02kJ/mol at various crank angles. Aliphatic C–H groups on the soot surfaceserve as a more important factor governing the soot oxidation reactivity whencompared to the soot nanostructure and oxygenated SFGs.
1．四种燃料在燃烧过程中均形成了两类结构特性不同的缸内微粒，即由基本碳粒子构成的典型微粒和富含金属和非金属元素的非典型微粒。典型微粒具有分形结构特性，其中正庚烷、20%甲苯/80%正庚烷（体积比）、柴油和F-T柴油的典型微粒分形维数分别介于1.63~1.96、1.48~1.92、1.32~1.84和1.48~1.91之间，且在燃烧过程中均为先减小后增加的变化规律，分形维数的最小值出现在扩散燃烧阶段的初期。燃料中芳香烃和环烷烃组分能够促进分形维数较低的微粒形成。
2．四种燃料基本碳粒子粒径呈类似高斯分布，峰值介于15~25nm，平均粒径在燃烧过程中呈单峰变化趋势，最大值出现在预混燃烧阶段的中后期。平均层面间距和平均曲率随着燃烧进行总体呈逐渐减小的趋势，仅在预混燃烧阶段末期至扩散燃烧阶段初期出现一个突然的上升；微晶尺寸变化趋势则正相反。燃料中的芳香烃和环烷烃组分能够促进基本碳粒子的成长，使平均粒径、层面间距和曲率增大，微晶尺寸减小。此外，Raman光谱IG/ID及EELS中Iπ*/Iδ*的变化规律与微晶尺寸的变规律基本一致，验证了微粒微观结构特征参数提取结果的准确性。
3．微粒表面的脂肪族C–H官能团当量浓度随着曲轴转角的增大整体呈逐渐减小的趋势，仅在预混燃烧阶段末期至扩散燃烧阶段初期出现一个突然的上升。C–OH和C=O官能团浓度均呈“双峰”变化趋势，分别在预混燃烧阶段中期和扩散燃烧阶段末期各出现一个峰值。燃料中的芳香烃及环烷烃通过降低微粒的石墨化程度和纳观结构有序性，增大了微粒表面脂肪族C–H和含氧官能团的浓度。
4．四种燃料生成的缸内微粒氧化所需的表观活化能介于114.57~181.02kJ/mol；燃烧过程中，脂肪族C–H表面官能团是影响微粒的氧化活性主要因素，微观结构和表面含氧官能团则属于相对次要的因素。
Combustion conditions, such as initial fuel composition, in-cylinder pressure andtemperature, play an important role on the nanostructure and surface functionalgroups of diesel particulates. The variations in nanostructure and surface functionalgroups can in turn affect the particulate reactivity toward oxidation. Therefore,detailed invesigations of the diesel in-cylinder particulates generared from differentfuels is necessary for better understanding of the diesel particulates evolutionmechanism and the reduction of particulate pollutions. In this dissertation, a totalcylinder sampling system, fueled with n-heptane, n-heptane/toluene, EuroⅢ lowsulfur diesel fuel and F-T fuel respectively, was employed to obtain in-cylinder sootsamples. The evolution mechanism of nanostructure, surface functional groups andoxidation reactivity of in-cylinder soot was subsequently studied using the analyticalmethod such as digital image processing, electron energy-loss spectroscopy, Ramanspectrum, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy,and thermogravimetric analysis. The major work and achievements of this dissertationare listed as follows:
1. The in-cylinder particulates generated from the four kinds of fuels all presenttwo sorts of morphology: One is the representative particulate which formed throughagglomeration of small sphere-like primary particles, and the other is amorphousparticulate containing abundant metal and nonmetal elements. The representativeparticles are aggregated in the form of fractal-like geometry. The fractal dimensionsfor the N-heptane, N-heptane blended with20%toluene (v/v), EuroⅢ diesel fuel andF-T fuel particulates are in a range of1.63~1.96、1.48~1.92、1.32~1.84and1.48~1.91respectively. During the combustion process, the fractal dimensions of in-cylinderparticulates first decline at the premixed combustion and early diffusion combustionstages, and then increase at the middle/late diffusion combustion and late combustionstages. The minimum particulate fractal dimension lies within the early diffusioncombustion period. The aromatic and cyclanes compounds in fuels can promote thegeneration of particles with low fractal dimensions.
2. The size distributions of primary particles generated from these four fuels aresimilar to Gauss distribution with the peak value of particle diameter in the range of15~25nm. During the combustion process, the mean diameter of primary particlesshows a unimodal distribution with the maximum value locating at the middle/late premixed combustion stage. Meanwhile, the mean fringe separation distance andtortuosity of in-cylinder soot generally decrease, except for a sudden rise between thelate premixed combustion stage and early diffusive combustion stage. In contrast, themean fringe length shows an increasing trend. The aromatic and cyclanes compoundsin fuels can promote the growth of primary particles and bring about an increase inmean particle diameter, fringe separation distance and tortuosity, and a derease inmean fringe length of soot partitulats. Additionally, the ratio of IG/IDin Ramanexperiment and Iπ*/Iδ*in EELS experiment follows a similar trend to that of thefringe length through the combustion history, verifying that the results of the imageprocessing are reasonable.
3. The relative content of the aliphatic C–H groups on the in-cylinder soot surface,which was evaluated by the normalized peak height ratio (IC-H/IC=C), generallydecreases during the combustion process, except for a sudden rise between the latepremixed and early diffusive combustion stages. Meanwhile, the concentrations ofboth C–OH and C=O groups present bimodal distributions over the combustionhistory, with the two peaks locating at the middle premixed and late diffusioncombustion stages respectively. Both aromatic and cycloparaffinic hydrocarbons infuels affect the soot nanostructure and degree of graphitization, which has asignificant impact on the relative content of surface aliphatic C–H groups.
4. Under the applied engine operating conditions where these four fuels wereused, the apparent activation energies for soot oxidation are in a range of114.57～181.02kJ/mol at various crank angles. Aliphatic C–H groups on the soot surfaceserve as a more important factor governing the soot oxidation reactivity whencompared to the soot nanostructure and oxygenated SFGs.
引文
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