碳纳米管强韧化氧化铝陶瓷基复合材料研究
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摘要
碳纳米管以其优秀的力学性能在增韧陶瓷基复合材料方面具有独特优势，但是碳纳米管的纠缠团聚状态严重影响了其应用，碳纳米管的分散一直是碳纳米管复合材料领域的难点。本文在总结前人对碳纳米管分散方法的研究基础上，重点探索了碳纳米管直接在氧化铝陶瓷粉体中的分散方法，并分别采用氢气气氛常压烧结、热压烧结、放电等离子烧结制备了碳纳米管-氧化铝复合材料。
首先，采用剪切挤出法将碳纳米管均匀分散在氧化铝粉中，制备了均匀分散的碳纳米管-氧化铝复合粉体。通过碳纳米管分散方法的研究，发现碳纳米管分散具有3个过程：碳纳米管团聚体的散开，长碳纳米管的剪断，短碳纳米管的分散。粘度、断口缺陷率、SEM结果都显示出剪切挤出法具有三个阶段。
通过对剪切挤出过程的分析，建立了剪切挤出法分散碳纳米管的分散模型；分散过程的主要驱动力为挤出过程聚合物熔体流动的层流剪切力，陶瓷刚性粉体的相对位移运动是促进碳纳米管分散的关键因素，聚合物熔体的位阻效应可以有效的保持碳纳米管的分散状态；给出了剪切挤出法分散碳纳米管的热力学特征，动力学方程及其边界条件。
以剪切挤出法制备得到的碳纳米管-氧化铝复合粉体为基础，分别采用氢气气氛常压烧结、热压烧结、放电等离子烧结等烧结工艺制备了碳纳米管-氧化铝复合材料。发现对于常压烧结，当碳纳米管含量为1wt%时碳纳米管-氧化铝复合材料断裂韧性达到6.11MPa﹒m~(1/2)，相对不添加碳纳米管提高了93.2%。对于热压烧结，碳纳米管-氧化铝复合材料的致密度达到98.8%以上，当碳纳米管含量为2wt%时复合材料断裂韧性达到6.32MPam~(1/2),相对不添加碳纳米管提高了99.2%。对于放电等离子烧结，在更低的烧结温度更短的烧结时间下，碳纳米管-氧化铝复合材料致密度达98.5%以上的，当碳纳米管含量为2wt%时，复合材料的断裂韧性达到大约6.55MPam~(1/2)，相对不添加碳纳米管提高了105%。
研究发现，在本实验条件下，碳纳米管的含量存在一个最佳值，常压烧结为1wt%，压力烧结为2wt%，继续增加碳纳米管含量，对碳纳米管-氧化铝复合材料的断裂韧性有害。在常压烧结中，由于增加碳纳米管含量，降低了碳纳米管-氧化铝复合材料的致密度，引起断裂韧性的下降。在压力烧结中，增加碳纳米管含量，碳纳米管-氧化铝复合材料致密度保持稳定，断裂韧性依然降低，可能是由于碳纳米管含量的增加使分散的碳纳米管搭接、附着在一起的几率增大，复合材料的缺陷率提高引起的。
通过对不同烧结方法制得的碳纳米管-氧化铝复合材料进行XRD分析，发现碳纳米管的添加使复合材料中氧化铝基体的峰位漂移，常压烧结的峰位向低角度漂移，压力烧结的峰位向高角度漂移，这可能是残余应力引起的。常压烧结时，碳纳米管与氧化铝基体热失配，引起残余拉应力；压力烧结时，外部压力引起碳纳米管与氧化铝基体间残余压应力。
通过对不同烧结方法制得的碳纳米管-氧化铝复合材料进行SEM分析，表明碳纳米管均匀弥散于氧化铝基体材料中，增韧机理以拔断增韧和拔出增韧为主。
The agglomerated state of carbon nanotubes seriously damaged to its applications, whichhad excellent mechanical properties with unique advantages in toughened ceramic matrixcomposites. It was a key issue that how to dispersing carbon nanotubes uniformly in thefield of carbon nanotubes composites. In this thesis, with the aim of reinforced ceramic, thestudy of carbon nanotubes reinforced alumina composite was raised, which had greatresearch significance and application value. Dispersing carbon nanotubes uniformly intoalumina powder was studied. Carbon nanotubes reinforced alumina composites werefabricated by hydrogen atmosphere normal pressure sintering, hot pressing sintering andspark plasma sintering.
Carbon nanotubes was dispersed into alumina matrix, and alumina composite powderof carbon nanotubes was prepared by shear extrusion method.8times shearing was betterin the results of viscosity, fracture defect rate and SEM. To dispersing carbon nanotubesuniformly, three processes were essential, including breaking agglomeration of carbonnanotubes up, breaking long carbon nanotubes off and dispersing short carbon nanotubes.The model of dispersing carbon nanotubes by shear extrusion method was build. Drivingforces included laminar shear stress of melt flow of organic binder and relativedisplacement of rigid ceramic particles. Steric effect of organic binder kept dispersion stateof carbon nanotubes. Thermodynamic characteristics, kinetic equation and boundaryconditions were shown.
Carbon nanotubes reinforced alumina composites were fabricated by hydrogenatmosphere normal pressure sintering, hot pressing sintering and spark plasma sintering. Byhydrogen atmosphere normal pressure sintering, fracture toughness of composite up to6.11MPa﹒m~(1/2)with1wt%carbon nanotubes contents, relatively increased93.2%. By hotpressing sintering, fracture toughness of composite up to6.32MPa﹒m~(1/2)with2wt%carbon nanotubes contents, relatively increased99.2%. By spark plasma sintering, fracture toughness of composite up to6.55MPa﹒m~(1/2)with2wt%carbon nanotubes contents,relatively increased105%.
Carbon nanotubes had a better value with1wt%of normal pressure sintering and2wt%of pressing sintering. Increasing contents of carbon nanotubes to continue, fracturetoughness of composites were damaged. In normal pressure sintering, the reason wasreduced density with increased carbon nanotubes contents. In pressing sintering, the reasonwas increased rate of attachment and bonding of carbon nanotubes with increased carbonnanotubes contents.
results of XRD of carbon nanotubes reinforced alumina composites prepared bydifferent sintering processes show that alumina matrix peaks of carbon nanotubesreinforced alumina composites drift, compared with alumina material, which may be causedby residual stress. In normal pressure sintering, the peaks drift to low angle by residualtensile stress. In pressing sintering, the peaks drift to high angle by residual compressivestress.
Results of SEM show that carbon nanotubes bonded alumina matrix as a dispersedpart. The main toughness mechanisms of carbon nanotubes were broken drawingtoughening and pulling out toughening.
首先，采用剪切挤出法将碳纳米管均匀分散在氧化铝粉中，制备了均匀分散的碳纳米管-氧化铝复合粉体。通过碳纳米管分散方法的研究，发现碳纳米管分散具有3个过程：碳纳米管团聚体的散开，长碳纳米管的剪断，短碳纳米管的分散。粘度、断口缺陷率、SEM结果都显示出剪切挤出法具有三个阶段。
通过对剪切挤出过程的分析，建立了剪切挤出法分散碳纳米管的分散模型；分散过程的主要驱动力为挤出过程聚合物熔体流动的层流剪切力，陶瓷刚性粉体的相对位移运动是促进碳纳米管分散的关键因素，聚合物熔体的位阻效应可以有效的保持碳纳米管的分散状态；给出了剪切挤出法分散碳纳米管的热力学特征，动力学方程及其边界条件。
以剪切挤出法制备得到的碳纳米管-氧化铝复合粉体为基础，分别采用氢气气氛常压烧结、热压烧结、放电等离子烧结等烧结工艺制备了碳纳米管-氧化铝复合材料。发现对于常压烧结，当碳纳米管含量为1wt%时碳纳米管-氧化铝复合材料断裂韧性达到6.11MPa﹒m~(1/2)，相对不添加碳纳米管提高了93.2%。对于热压烧结，碳纳米管-氧化铝复合材料的致密度达到98.8%以上，当碳纳米管含量为2wt%时复合材料断裂韧性达到6.32MPam~(1/2),相对不添加碳纳米管提高了99.2%。对于放电等离子烧结，在更低的烧结温度更短的烧结时间下，碳纳米管-氧化铝复合材料致密度达98.5%以上的，当碳纳米管含量为2wt%时，复合材料的断裂韧性达到大约6.55MPam~(1/2)，相对不添加碳纳米管提高了105%。
研究发现，在本实验条件下，碳纳米管的含量存在一个最佳值，常压烧结为1wt%，压力烧结为2wt%，继续增加碳纳米管含量，对碳纳米管-氧化铝复合材料的断裂韧性有害。在常压烧结中，由于增加碳纳米管含量，降低了碳纳米管-氧化铝复合材料的致密度，引起断裂韧性的下降。在压力烧结中，增加碳纳米管含量，碳纳米管-氧化铝复合材料致密度保持稳定，断裂韧性依然降低，可能是由于碳纳米管含量的增加使分散的碳纳米管搭接、附着在一起的几率增大，复合材料的缺陷率提高引起的。
通过对不同烧结方法制得的碳纳米管-氧化铝复合材料进行XRD分析，发现碳纳米管的添加使复合材料中氧化铝基体的峰位漂移，常压烧结的峰位向低角度漂移，压力烧结的峰位向高角度漂移，这可能是残余应力引起的。常压烧结时，碳纳米管与氧化铝基体热失配，引起残余拉应力；压力烧结时，外部压力引起碳纳米管与氧化铝基体间残余压应力。
通过对不同烧结方法制得的碳纳米管-氧化铝复合材料进行SEM分析，表明碳纳米管均匀弥散于氧化铝基体材料中，增韧机理以拔断增韧和拔出增韧为主。
The agglomerated state of carbon nanotubes seriously damaged to its applications, whichhad excellent mechanical properties with unique advantages in toughened ceramic matrixcomposites. It was a key issue that how to dispersing carbon nanotubes uniformly in thefield of carbon nanotubes composites. In this thesis, with the aim of reinforced ceramic, thestudy of carbon nanotubes reinforced alumina composite was raised, which had greatresearch significance and application value. Dispersing carbon nanotubes uniformly intoalumina powder was studied. Carbon nanotubes reinforced alumina composites werefabricated by hydrogen atmosphere normal pressure sintering, hot pressing sintering andspark plasma sintering.
Carbon nanotubes was dispersed into alumina matrix, and alumina composite powderof carbon nanotubes was prepared by shear extrusion method.8times shearing was betterin the results of viscosity, fracture defect rate and SEM. To dispersing carbon nanotubesuniformly, three processes were essential, including breaking agglomeration of carbonnanotubes up, breaking long carbon nanotubes off and dispersing short carbon nanotubes.The model of dispersing carbon nanotubes by shear extrusion method was build. Drivingforces included laminar shear stress of melt flow of organic binder and relativedisplacement of rigid ceramic particles. Steric effect of organic binder kept dispersion stateof carbon nanotubes. Thermodynamic characteristics, kinetic equation and boundaryconditions were shown.
Carbon nanotubes reinforced alumina composites were fabricated by hydrogenatmosphere normal pressure sintering, hot pressing sintering and spark plasma sintering. Byhydrogen atmosphere normal pressure sintering, fracture toughness of composite up to6.11MPa﹒m~(1/2)with1wt%carbon nanotubes contents, relatively increased93.2%. By hotpressing sintering, fracture toughness of composite up to6.32MPa﹒m~(1/2)with2wt%carbon nanotubes contents, relatively increased99.2%. By spark plasma sintering, fracture toughness of composite up to6.55MPa﹒m~(1/2)with2wt%carbon nanotubes contents,relatively increased105%.
Carbon nanotubes had a better value with1wt%of normal pressure sintering and2wt%of pressing sintering. Increasing contents of carbon nanotubes to continue, fracturetoughness of composites were damaged. In normal pressure sintering, the reason wasreduced density with increased carbon nanotubes contents. In pressing sintering, the reasonwas increased rate of attachment and bonding of carbon nanotubes with increased carbonnanotubes contents.
results of XRD of carbon nanotubes reinforced alumina composites prepared bydifferent sintering processes show that alumina matrix peaks of carbon nanotubesreinforced alumina composites drift, compared with alumina material, which may be causedby residual stress. In normal pressure sintering, the peaks drift to low angle by residualtensile stress. In pressing sintering, the peaks drift to high angle by residual compressivestress.
Results of SEM show that carbon nanotubes bonded alumina matrix as a dispersedpart. The main toughness mechanisms of carbon nanotubes were broken drawingtoughening and pulling out toughening.
引文
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