羊毛角蛋白原纤增强同质复合膜的制备与表征
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摘要
本论文通过复合材料仿生设计,将羊毛中分离出的微-亚微尺度原纤作为增强体,制备基质为角蛋白的同质复合材料,并对其分布排列结构特征及其对力学性质的影响进行表征,成功地解决了纯角蛋白低强、低模的问题。同时,对原纤头端作分叉处理以模仿树根结构,达到了同质复合膜的增强与增韧。
本文首次实现角蛋白同质与异质复合膜性能的对比,即羊毛原纤增强角蛋白膜与无机晶须(K2Ti6O13)增强角蛋白膜的对比。紫外-可见-近红外光谱分析表明,同质复合膜的透光性好于异质复合膜,即羊毛原纤与角蛋白基体的界面良好。红外光谱与x衍射图谱分析表明,原纤基本保持羊毛中晶区的特征,即含较多的α螺旋结构；复合膜的特征吸收峰和结晶度主要取决于基质,因增强体的混入比小于5%。再生角蛋白复合膜的力学测量表明,原纤添加质量百分数为5%、晶须为3%,且分散均匀、沿载荷方向取向排列时,得到的复合膜力学性能最佳,而同质膜较异质膜的断裂应力仍高出42%。
制备了平直原纤和分叉原纤,对其增强效能和原纤形态对强伸性贡献作了分析。平直原纤增强角蛋白膜的模量和断裂应力相对未增强膜分别提高70.2%和48.8%,仅断裂应变减少了7.8%。一级和二级分叉原纤增强复合膜的断裂应力和应变均改善,断裂应力较纯角蛋白膜分别提高了92.4%和94.9%,断裂应变则提高了7.4%和7.7%。
由修正的复合材料强度与模量的计算法则和复合膜的力学试验结果,推得平直原纤的断裂应力为206.12Mpa,弹性模量为278.28Mpa,断裂应变为0.74,剪切强度为6.87MPa。而一级与二级分叉原纤的断裂应力分别为平直原纤的1.81倍和1.86倍,弹性模量为1.28倍和0.95倍,断裂应变为1.42倍和1.96倍,平均剪切强度为1.81倍和1.86倍,说明头端分叉原纤同时具备增强及增韧效能。但原纤的头端分叉数对复合膜性能的影响不大,是由于长时间超声波处理损伤以及分叉不完整所致。
之后又从断裂力学和细观力学出发,对异质与同质复合膜,以及分叉原纤增强复合膜的损伤特征进行分析。首先对比了同/异质复合膜断裂面的显微镜照片,发现同质膜的破坏特征可以归纳为断裂短纤维破坏模型,而异质复合膜则为桥式短纤维破坏模型。而原纤的分叉头端之所以能同时起到增强与增韧,其原因是头端的分叉结构不仅有可变形性,使其在基体中能够有效减小头端应力集中,而且分叉端存在附加的摩擦力和变形力,提供了主要界面作用力在形式上的转换。还基于修正的剪滞模型,分析了并建立了单根和多根原纤存在的情况下中间一根原纤的轴向载荷传递模型方程,发现当原纤模量Ef/基质模量Em为2～50、原纤头头间距/原纤长度为0.053～0.667、原纤直径df/原纤间距d越大(即d越小,V%越大)时,原纤上的轴向载荷传递效率较高。而试验中,第一项都已达到理论范围,若要继续提高同质复合膜的力学性能,须通过改进原纤头头间距/原纤长度和提df/d值来实现。
最后,利用有限元方法对原纤与晶须增强复合膜的应力场等进行了分析,探索了复合膜的破坏机理,以及依据结构仿生理论设计的平直、一级与二级分叉原纤增强同质复合膜中,原纤形态对其力学性能的影响。揭示了同质复合膜的损伤过程为：原纤断裂后的断裂端附近产生大变形及界面剪切力,可直接促成基体裂纹和界面脱粘,但由于同质界面作用良好,使得脱粘难以继续,将使已有基体裂纹扩展或产生新的基体裂纹。
论文对无机晶须和羊毛原纤增强角蛋白膜的结构、性质和制备的研究,为同质复合角蛋白膜,甚至仿生同质复合材料的研究提供了科学依据。
This paper carried out a series of exploratory research work about bio-inspired designing composites, in which the wool fibrils at micro to sub-micro scales used as reinforcement to blend with keratin matrix, and then characterized the distribution and arrangement structure, as well as the effects of composites mechanical properties. It can successfully resolved the low strength and low modulus of neat keratin membranes. Additional, the branched fibrils, like plant roots, were also used to strengthen and toughening the composite membranes.
In this paper, it realized the properties comparison between homogeneous and heterogeneous composites, namely wool fibrils reinforced composites compared to inorganic K2Ti6O13whisker reinforced composites. The result of UV-Vis-NIR absorption spectrum analysis showed that the light transmission in homogeneous composites is superior to in heterogeneous composites, which indicating that the wool fibrils and keratin matrix has good interface. FT-IR spectrum and X-ray diffraction were employed to investigate the molecular structural changes of fibrils and membranes, and the results showed the fibrils almost maintained the characteristics of wool, both many disulphide bonds and a-helix molecules. Characteristic absorption peaks and crystallinity of composite membranes mainly depended on the keratin matrix, and almost have no influence of the reinforcements. The mechanical testing results of keratin composites showed that when fibrils quality percentage is5%, whiskers quality percentage is3%, and also uniformly dispersed and highly oriented, the composite membranes have optimal mechanical properties. However, the strength of homogeneous composites is higher than heterogeneous ones by42%.
Then, branched fibrils were prepared, and the strengthen efficiency of different types fibrils were analyzed. The modulus and strength of plain fibrils reinforced membranes increased70.2%and48.8%respectively than those of neat keratin membranes, only strain at break decreased7.8%. Compared with the neat keratin membranes, ultrasonic processed one-step and two-step branched fibrils reinforced membranes have better mechanical properties, the stress increased92.4%and94.9%respectively, and strain at break increased7.4%and7.7%respectively.
With the aid of corrected law of mixtures and the mechanics experimental results of composite membranes, here calculated the stress of plain fibrils is206.12Mpa, modules is278.28Mpa, strain at break is0.74, and shear stress is6.87Mpa. However, the stress of one-and two-step branched fibrils are1.81and1.86times as many as plain fibrils respectively, and modules are1.28and0.95times, and strain at break are1.42and1.96times, and shear strengths are1.81and1.86times. It confirmed that the branched structure has a better effect on strengthen and toughen, but the number of branched ends has little impact on the properties of composites, not only because the long time ultrasonic processing easily decrease the properties of fibrils, as well as the incomplete branching.
In addition, this paper also took fracture mechanics and micromechanics to analysis the damage characteristics of heterogeneous and homogeneous composite membranes, as well as the branched fibrils reinforced membranes. Firstly, the micrographs of cross-sections shown that whiskers performed bridging fibre fracture model and fibrils performed breaking fibres fracture model. The analysis results revealed that the branched fibrils could achieve both reinforcement and toughness simultaneously, not only because fibrils ends deformation, which can effectively reduce the stress concentration, but also because the additional friction and deforming force of fibrils ends. On the basis of modified shear lag model, the axial load transfer model equations of single fibril among multi-fibrils were established, in which found that when fibril modulus Ef/matrix modulus Em is2～50, the value of longitudinal spacing/the length of fibrils equal to0.053～0.667, and the ratio (df/d) of fibril diameter (df) to the space (d) of between the fibrils is larger (namely d smaller, or V%larger), the axial load transfer efficiency higher. In experiment, the first item have reached the theory range, to enhance the mechanical properties of homogeneous composite membrane just can by improving the value of longitudinal spacing/the length of fibrils and df/d value.
Through the establishment of finite element model, it defined that the stress distribution of fibrils and whiskers reinforced composite membranes. The researches include the fracture pattens of heterogeneous composites, and based on the structural bionics, the plain, one-and two-step branched fibrils were prepared to reinforce homogeneous membranes, the influence of fibrils ends shapes on the mechanical properties were also discussed. Finally, it revealed the fracture process of homogeneous composite membranes, large matrix deformation and interfacial shear stress around fibrils fracture easy to product matrix crack and interfacial debonding, however, due to the good interfacial interaction, made the interfacial debonding too difficult to continue, instead by the existing or new matrix crack.
The present thesis researched the inorganic whisker and wool fibrils reinforced keratin composite membranes systemically, especially including structure, properties and preparation technology. The achievements with research play a beneficial role in the development and application of keratin regeneration composites and provide a theoretical basis for related field.
本文首次实现角蛋白同质与异质复合膜性能的对比,即羊毛原纤增强角蛋白膜与无机晶须(K2Ti6O13)增强角蛋白膜的对比。紫外-可见-近红外光谱分析表明,同质复合膜的透光性好于异质复合膜,即羊毛原纤与角蛋白基体的界面良好。红外光谱与x衍射图谱分析表明,原纤基本保持羊毛中晶区的特征,即含较多的α螺旋结构；复合膜的特征吸收峰和结晶度主要取决于基质,因增强体的混入比小于5%。再生角蛋白复合膜的力学测量表明,原纤添加质量百分数为5%、晶须为3%,且分散均匀、沿载荷方向取向排列时,得到的复合膜力学性能最佳,而同质膜较异质膜的断裂应力仍高出42%。
制备了平直原纤和分叉原纤,对其增强效能和原纤形态对强伸性贡献作了分析。平直原纤增强角蛋白膜的模量和断裂应力相对未增强膜分别提高70.2%和48.8%,仅断裂应变减少了7.8%。一级和二级分叉原纤增强复合膜的断裂应力和应变均改善,断裂应力较纯角蛋白膜分别提高了92.4%和94.9%,断裂应变则提高了7.4%和7.7%。
由修正的复合材料强度与模量的计算法则和复合膜的力学试验结果,推得平直原纤的断裂应力为206.12Mpa,弹性模量为278.28Mpa,断裂应变为0.74,剪切强度为6.87MPa。而一级与二级分叉原纤的断裂应力分别为平直原纤的1.81倍和1.86倍,弹性模量为1.28倍和0.95倍,断裂应变为1.42倍和1.96倍,平均剪切强度为1.81倍和1.86倍,说明头端分叉原纤同时具备增强及增韧效能。但原纤的头端分叉数对复合膜性能的影响不大,是由于长时间超声波处理损伤以及分叉不完整所致。
之后又从断裂力学和细观力学出发,对异质与同质复合膜,以及分叉原纤增强复合膜的损伤特征进行分析。首先对比了同/异质复合膜断裂面的显微镜照片,发现同质膜的破坏特征可以归纳为断裂短纤维破坏模型,而异质复合膜则为桥式短纤维破坏模型。而原纤的分叉头端之所以能同时起到增强与增韧,其原因是头端的分叉结构不仅有可变形性,使其在基体中能够有效减小头端应力集中,而且分叉端存在附加的摩擦力和变形力,提供了主要界面作用力在形式上的转换。还基于修正的剪滞模型,分析了并建立了单根和多根原纤存在的情况下中间一根原纤的轴向载荷传递模型方程,发现当原纤模量Ef/基质模量Em为2～50、原纤头头间距/原纤长度为0.053～0.667、原纤直径df/原纤间距d越大(即d越小,V%越大)时,原纤上的轴向载荷传递效率较高。而试验中,第一项都已达到理论范围,若要继续提高同质复合膜的力学性能,须通过改进原纤头头间距/原纤长度和提df/d值来实现。
最后,利用有限元方法对原纤与晶须增强复合膜的应力场等进行了分析,探索了复合膜的破坏机理,以及依据结构仿生理论设计的平直、一级与二级分叉原纤增强同质复合膜中,原纤形态对其力学性能的影响。揭示了同质复合膜的损伤过程为：原纤断裂后的断裂端附近产生大变形及界面剪切力,可直接促成基体裂纹和界面脱粘,但由于同质界面作用良好,使得脱粘难以继续,将使已有基体裂纹扩展或产生新的基体裂纹。
论文对无机晶须和羊毛原纤增强角蛋白膜的结构、性质和制备的研究,为同质复合角蛋白膜,甚至仿生同质复合材料的研究提供了科学依据。
This paper carried out a series of exploratory research work about bio-inspired designing composites, in which the wool fibrils at micro to sub-micro scales used as reinforcement to blend with keratin matrix, and then characterized the distribution and arrangement structure, as well as the effects of composites mechanical properties. It can successfully resolved the low strength and low modulus of neat keratin membranes. Additional, the branched fibrils, like plant roots, were also used to strengthen and toughening the composite membranes.
In this paper, it realized the properties comparison between homogeneous and heterogeneous composites, namely wool fibrils reinforced composites compared to inorganic K2Ti6O13whisker reinforced composites. The result of UV-Vis-NIR absorption spectrum analysis showed that the light transmission in homogeneous composites is superior to in heterogeneous composites, which indicating that the wool fibrils and keratin matrix has good interface. FT-IR spectrum and X-ray diffraction were employed to investigate the molecular structural changes of fibrils and membranes, and the results showed the fibrils almost maintained the characteristics of wool, both many disulphide bonds and a-helix molecules. Characteristic absorption peaks and crystallinity of composite membranes mainly depended on the keratin matrix, and almost have no influence of the reinforcements. The mechanical testing results of keratin composites showed that when fibrils quality percentage is5%, whiskers quality percentage is3%, and also uniformly dispersed and highly oriented, the composite membranes have optimal mechanical properties. However, the strength of homogeneous composites is higher than heterogeneous ones by42%.
Then, branched fibrils were prepared, and the strengthen efficiency of different types fibrils were analyzed. The modulus and strength of plain fibrils reinforced membranes increased70.2%and48.8%respectively than those of neat keratin membranes, only strain at break decreased7.8%. Compared with the neat keratin membranes, ultrasonic processed one-step and two-step branched fibrils reinforced membranes have better mechanical properties, the stress increased92.4%and94.9%respectively, and strain at break increased7.4%and7.7%respectively.
With the aid of corrected law of mixtures and the mechanics experimental results of composite membranes, here calculated the stress of plain fibrils is206.12Mpa, modules is278.28Mpa, strain at break is0.74, and shear stress is6.87Mpa. However, the stress of one-and two-step branched fibrils are1.81and1.86times as many as plain fibrils respectively, and modules are1.28and0.95times, and strain at break are1.42and1.96times, and shear strengths are1.81and1.86times. It confirmed that the branched structure has a better effect on strengthen and toughen, but the number of branched ends has little impact on the properties of composites, not only because the long time ultrasonic processing easily decrease the properties of fibrils, as well as the incomplete branching.
In addition, this paper also took fracture mechanics and micromechanics to analysis the damage characteristics of heterogeneous and homogeneous composite membranes, as well as the branched fibrils reinforced membranes. Firstly, the micrographs of cross-sections shown that whiskers performed bridging fibre fracture model and fibrils performed breaking fibres fracture model. The analysis results revealed that the branched fibrils could achieve both reinforcement and toughness simultaneously, not only because fibrils ends deformation, which can effectively reduce the stress concentration, but also because the additional friction and deforming force of fibrils ends. On the basis of modified shear lag model, the axial load transfer model equations of single fibril among multi-fibrils were established, in which found that when fibril modulus Ef/matrix modulus Em is2～50, the value of longitudinal spacing/the length of fibrils equal to0.053～0.667, and the ratio (df/d) of fibril diameter (df) to the space (d) of between the fibrils is larger (namely d smaller, or V%larger), the axial load transfer efficiency higher. In experiment, the first item have reached the theory range, to enhance the mechanical properties of homogeneous composite membrane just can by improving the value of longitudinal spacing/the length of fibrils and df/d value.
Through the establishment of finite element model, it defined that the stress distribution of fibrils and whiskers reinforced composite membranes. The researches include the fracture pattens of heterogeneous composites, and based on the structural bionics, the plain, one-and two-step branched fibrils were prepared to reinforce homogeneous membranes, the influence of fibrils ends shapes on the mechanical properties were also discussed. Finally, it revealed the fracture process of homogeneous composite membranes, large matrix deformation and interfacial shear stress around fibrils fracture easy to product matrix crack and interfacial debonding, however, due to the good interfacial interaction, made the interfacial debonding too difficult to continue, instead by the existing or new matrix crack.
The present thesis researched the inorganic whisker and wool fibrils reinforced keratin composite membranes systemically, especially including structure, properties and preparation technology. The achievements with research play a beneficial role in the development and application of keratin regeneration composites and provide a theoretical basis for related field.
引文
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