纳米结构氧化铝纤维的静电纺制备及性能研究
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摘要
氧化铝纤维因其各种优异的物理化学性质而被人们广泛研究,本论文主要是利用溶胶凝胶结合静电纺丝技术制备柔性氧化铝纳米结构纤维,并探讨了氧化铝纤维的形成机制及材料微观结构和性能之间的关系。具体内容包括纳米片组成的柔韧性α-A12O3纤维的制备及其力学性质研究；掺杂CaO-SiO2的α-Al2O3纤维的制备及其隔热性质研究；柔韧性双疏γ-Al2O3纤维毡的制备及其抗腐蚀性质研究。通过调节静电纺丝过程参数(体系参数、工艺参数、环境参数)对氧化铝纤维的尺寸、形貌和微观结构进行了调控,对纤维在不同条件下的形成机理进行了探讨,分析了所合成的氧化铝纤维结构与性能之间的关系。本论文工作不仅丰富了氧化铝纳米结构纤维领域的研究,还为氧化铝纳米结构纤维的潜在应用提供了理论基础和技术支持。本论文的主要工作如下：
1.纳米片组成的柔韧性α-Al2O3纤维的制备及其力学性质
以异丙醇铝和硝酸铝为前躯体,硝酸为催化剂,无水硫酸镁为添加剂,乙醇的水溶液为溶剂制备溶胶,利用聚乙烯吡咯烷酮(PVP K90)调节溶胶的粘度。通过溶胶-凝胶结合静电纺丝技术制备了直径在300-400nm之间的α-Al2O3纳米纤维。纤维由厚度在20-50nm之间的α-AI2O3纳米片定向排列而成。MgSO4作为添加剂起初可以稳定γ-A12O3的结构,延迟纤维从γ-Al2O3向α-Al2O3的相转变。然后形成尖晶石MgAl2O4晶界相抑制晶粒的长大,有效的促进烧结。制备的纳米纤维具有较好的热稳定性,经1400℃煅烧12h后仍能保持其微观结构。直径为350nm的单根α-Al2O3纤维的弹性模量为23.8Gpa,说明其具有较好的柔韧性。当纤维在使用过程中受到热环境和机械接触引发的应力和应变时,好的热稳定性和柔韧性有利于延长纤维的使用时间,这有利于纤维在高温催化和过滤方面的应用。
2.掺杂CaO-SiO2的α-Al2O3纤维的制备及其隔热性质
以氯化铝和铝粉为原料,添加CaO-SiO2两相添加剂,水为溶剂,90℃下磁力搅拌回流5h形成透明溶液,将回流后得到的透明溶液在80℃水浴中浓缩5h后冷却至室温,加入PVP形成透明溶胶。通过溶胶-凝胶结合静电纺丝技术制备了掺杂CaO-SiO2两相添加剂的柔性α-Al2O3纳米纤维。少量的CaO-SiO2两相添加剂可以延迟γ-Al2O3的形成,抑制γ-Al2O3向α-Al2O3的相转变,并有效抑制烧结中颗粒的长大。经1300℃煅烧后,含CaO/SiO2两相添加剂纤维的组成颗粒比不含添加剂纤维的组成颗粒小,这可能是由于纤维中θ-Al2O3的存在造成的。含CaO/SiO2的摩尔比为1：10的纤维经1300℃煅烧后具有较好的柔韧性和较低的导热系数(0.07329W/m-K),这有利于纤维在隔热领域中的应用。
3.柔韧性双疏γ-Al2O3纤维毡的制备及其抗腐蚀性质
以异丙醇铝和硝酸铝为前躯体,硝酸和冰醋酸为催化剂,水为溶剂制备溶胶,利用PVP调节溶胶的粘度。通过溶胶-凝胶结合静电纺丝技术制备了氧化铝凝胶纤维,煅烧后得到γ-Al2O3纤维毡,然后利用十七氟癸基三甲氧基硅烷(FAS)对得到的γ-Al2O3纤维毡进行表面修饰得到了双疏性γ-Al2O3纤维毡。当PVP的加入量为0.3g时,纤维的直径要比加入量为0.4g和0.5g的小,研究表明,纤维毡的双疏性能随着纤维直径的减小而增强,较小的纤维直径使纤维毡具有较大的表面粗糙度,使纤维毡具有较好的双疏性能。同时,经过FAS改性的纤维毡具有-定的抗腐蚀性能,对pH值(1-14)范围的酸碱水溶液均有较好的疏水性。另外,纤维毡还具有较好的柔韧性,将其折到薄的硬纸片上弯曲时,纤维毡无裂痕,这将拓展纤维毡在很多重要的工业领域中的应用。
Alumina fibers have been widely investigated due to their unique physical and chemical properties. This dissertation is focused on the preparation of alumina nano-structured fibers by sol-gel method combined with an electrospinning process. The formation mechanism of the alumina fiber is discussed. The analysis was done on the relationship between the microstructure of electrospun alumina fibers and their properties. The contents comprise fabrication and mechanical properties of flexible a-alumina fibers composed of nanosheets, fabrication and insulation properties of α-alumina fibers with CaO-SiO2additive, and fabrication and anti-corrosion properties of flexible and amphiphobic y-alumina mats. The sizes, morphology and microstructures of alumina fibers can be well controlled by adjusting the electrospinning process parameters (system parameters, process parameters and environment parameters). The formation mechanism of the alumina fiber under different conditions is discussed. The effects of structure of alumina fibers on their properties were investigated. This work is not only enriching the alumina nano-structured fibers investigations, but also providing a theoretical foundation and technical support to alumina fibers potential application. The detailed information of the dissertation is listed as follows:
1. Fabrication and mechanical properties of flexible a-alumina fibers composed of nanosheets
a-alumina nanofibers with diameters of300-400nm were fabricated by the sol-gel method combined with an electrospinning process. The sol was prepared with aluminum isopropoxide and aluminum nitrate as the precursors, nitric acid as the catalyst, small amounts of anhydrous magnesium sulfate as additive, and ethanol aqueous solution as the solvent. Polyvinylpyrrolidone (PVP K90) was applied to tune sol viscosity. The fibers are composed of α-Al2O3nanosheets with thickness of20-50nm which stack unidirectionally along the axis. Small amounts of anhydrous magnesium sulfate as additive acted to stabilize the γ-Al2O3structure and retard its conversion to α-Al2O3firstly, and subsequently MgAl2O4was formed at the grain boundaries to inhibit grain growth and effectively promoted sintering. The nanofibers have good thermal stability, for their microstructure can be maintained even after heat treatment at1400℃for12h. For a single α-Al2O3fiber with a diameter of ca.350nm, the elastic modulus was23.8GPa, indicating the good flexibility. The good thermal stability and flexibility may extend the service life even when it is subject to stresses and strains resulting from thermal tensions and mechanical contact, which favors their application in catalysis and filtration at high temperature.
2. Fabrication and insulation properties of a-alumina fibers with CaO-SiO2additive
CaO-SiO2two-component doped flexible a-alumina fibers were successfully prepared through the sol-gel method combined with an electrospinning process. The sol was prepared with aluminum chloride hexahydrate and aluminum powder as raw materials, calcium oxide-silica (CaO-SiO2) was applied as two-component additive, and water as the solvent. The mixture was heated to90℃and refluxed for5h with magnetic stirring to form a transparent solution. The resulting transparent solution was condensed for5h using a water bath (80℃). Finally, PVP was added with continuously stirring at ambient temperature to form a transparent sol. Small amounts of CaO-SiO2additive was applied to retard the formation of γ-Al2O3and the phase transformation from γ-Al2O3to α-Al2O3, and control the size of the grains during sintering. With the addition of the CaO-SiO2in the system, the size of the particles composed the fibers calcined at1300℃significantly decreased compared to that without additive, which might due to the formation of6-alumina in the samples. The alumina fiber mat calcined at1300℃with the CaO/SiO2ratio of1:10had good flexibility and low thermal conductivity (0.07329W/m·K), which favored its application in insulation.
3. Fabrication and anti-corrosion properties of flexible and amphiphobic γ-alumina mats
Alumina gel fibers were by the sol-gel method combined with an electrospinnin process. The sol was prepared using aluminum isopropoxide and aluminum nitrate as the precursors, nitric acid and acetic acid as catalysts, water as the solvent, and polyvinylpyrrolidone (PVP) was applied to tune sol viscosity. The γ-alumina mats were obtained after calcination of the gel fibers. Amphiphobic γ-alumina mats were fabricated by (fluoroalkyl)silane (FAS) modification of the obtained γ-alumina mats. When the content of PVP was0.3g, the average fiber diameters were smaller than those with0.4and0.5g PVP, and the resulting larger surface roughness endowed the modified alumina mat better amphiphobicity. At the same time, the modified alumina mat exhibited a hydrophobic property in the pH range from1to14, indicating that it had a certain anti-corrosion resistance. Additionally, the modified alumina mat was flexible and would not rapture even folding it on a paper, which may extend the application of fiber mats in many important industrial fields.
Flexible α-alumina nanofibers were fabricated by the sol-gel method combined with an electrospinning process. The sol was prepared with aluminum isopropoxide and aluminum nitrate as the precursors, nitric acid as the catalyst, and ethanol aqueous solution as the solvent. Small amounts of anhydrous magnesium sulfate as additive acted to stabilize the γ-Al2O3structure and retard its conversion to α-Al2O3firstly, and subsequently MgAl2O4was formed at the grain boundaries to inhibit grain growth. Polyvinylpyrrolidone (PVP) was applied to tune sol viscosity. The fibers with diameters of300-400nm are composed of α-Al2O3nanosheets with thickness of20-50nm which stack along [0001] at the axial direction. The fibers exhibited good flexibility and thermal stability.
Alumina fibers were fabricated by the sol-gel method combined with an electrospinning process using aluminum chloride hexahydrate (AICl3·6H2O) and aluminum powder as raw materials in water solvent. Calcium oxide-silica (CaO-SiO2) was applied as two-component additive to retard the phase transformation of alumina and control the size of the grains during sintering. With the addition of the CaO-SiO2in the system, the size of the particles that composed the fibers calcined at1300℃significantly decreased compared to that without additive, which might be due to the formation of θ-alumina in the samples. In addition, the fiber had low thermal conductivity and good flexibility, which favored its application in insulation.
1.纳米片组成的柔韧性α-Al2O3纤维的制备及其力学性质
以异丙醇铝和硝酸铝为前躯体,硝酸为催化剂,无水硫酸镁为添加剂,乙醇的水溶液为溶剂制备溶胶,利用聚乙烯吡咯烷酮(PVP K90)调节溶胶的粘度。通过溶胶-凝胶结合静电纺丝技术制备了直径在300-400nm之间的α-Al2O3纳米纤维。纤维由厚度在20-50nm之间的α-AI2O3纳米片定向排列而成。MgSO4作为添加剂起初可以稳定γ-A12O3的结构,延迟纤维从γ-Al2O3向α-Al2O3的相转变。然后形成尖晶石MgAl2O4晶界相抑制晶粒的长大,有效的促进烧结。制备的纳米纤维具有较好的热稳定性,经1400℃煅烧12h后仍能保持其微观结构。直径为350nm的单根α-Al2O3纤维的弹性模量为23.8Gpa,说明其具有较好的柔韧性。当纤维在使用过程中受到热环境和机械接触引发的应力和应变时,好的热稳定性和柔韧性有利于延长纤维的使用时间,这有利于纤维在高温催化和过滤方面的应用。
2.掺杂CaO-SiO2的α-Al2O3纤维的制备及其隔热性质
以氯化铝和铝粉为原料,添加CaO-SiO2两相添加剂,水为溶剂,90℃下磁力搅拌回流5h形成透明溶液,将回流后得到的透明溶液在80℃水浴中浓缩5h后冷却至室温,加入PVP形成透明溶胶。通过溶胶-凝胶结合静电纺丝技术制备了掺杂CaO-SiO2两相添加剂的柔性α-Al2O3纳米纤维。少量的CaO-SiO2两相添加剂可以延迟γ-Al2O3的形成,抑制γ-Al2O3向α-Al2O3的相转变,并有效抑制烧结中颗粒的长大。经1300℃煅烧后,含CaO/SiO2两相添加剂纤维的组成颗粒比不含添加剂纤维的组成颗粒小,这可能是由于纤维中θ-Al2O3的存在造成的。含CaO/SiO2的摩尔比为1：10的纤维经1300℃煅烧后具有较好的柔韧性和较低的导热系数(0.07329W/m-K),这有利于纤维在隔热领域中的应用。
3.柔韧性双疏γ-Al2O3纤维毡的制备及其抗腐蚀性质
以异丙醇铝和硝酸铝为前躯体,硝酸和冰醋酸为催化剂,水为溶剂制备溶胶,利用PVP调节溶胶的粘度。通过溶胶-凝胶结合静电纺丝技术制备了氧化铝凝胶纤维,煅烧后得到γ-Al2O3纤维毡,然后利用十七氟癸基三甲氧基硅烷(FAS)对得到的γ-Al2O3纤维毡进行表面修饰得到了双疏性γ-Al2O3纤维毡。当PVP的加入量为0.3g时,纤维的直径要比加入量为0.4g和0.5g的小,研究表明,纤维毡的双疏性能随着纤维直径的减小而增强,较小的纤维直径使纤维毡具有较大的表面粗糙度,使纤维毡具有较好的双疏性能。同时,经过FAS改性的纤维毡具有-定的抗腐蚀性能,对pH值(1-14)范围的酸碱水溶液均有较好的疏水性。另外,纤维毡还具有较好的柔韧性,将其折到薄的硬纸片上弯曲时,纤维毡无裂痕,这将拓展纤维毡在很多重要的工业领域中的应用。
Alumina fibers have been widely investigated due to their unique physical and chemical properties. This dissertation is focused on the preparation of alumina nano-structured fibers by sol-gel method combined with an electrospinning process. The formation mechanism of the alumina fiber is discussed. The analysis was done on the relationship between the microstructure of electrospun alumina fibers and their properties. The contents comprise fabrication and mechanical properties of flexible a-alumina fibers composed of nanosheets, fabrication and insulation properties of α-alumina fibers with CaO-SiO2additive, and fabrication and anti-corrosion properties of flexible and amphiphobic y-alumina mats. The sizes, morphology and microstructures of alumina fibers can be well controlled by adjusting the electrospinning process parameters (system parameters, process parameters and environment parameters). The formation mechanism of the alumina fiber under different conditions is discussed. The effects of structure of alumina fibers on their properties were investigated. This work is not only enriching the alumina nano-structured fibers investigations, but also providing a theoretical foundation and technical support to alumina fibers potential application. The detailed information of the dissertation is listed as follows:
1. Fabrication and mechanical properties of flexible a-alumina fibers composed of nanosheets
a-alumina nanofibers with diameters of300-400nm were fabricated by the sol-gel method combined with an electrospinning process. The sol was prepared with aluminum isopropoxide and aluminum nitrate as the precursors, nitric acid as the catalyst, small amounts of anhydrous magnesium sulfate as additive, and ethanol aqueous solution as the solvent. Polyvinylpyrrolidone (PVP K90) was applied to tune sol viscosity. The fibers are composed of α-Al2O3nanosheets with thickness of20-50nm which stack unidirectionally along the axis. Small amounts of anhydrous magnesium sulfate as additive acted to stabilize the γ-Al2O3structure and retard its conversion to α-Al2O3firstly, and subsequently MgAl2O4was formed at the grain boundaries to inhibit grain growth and effectively promoted sintering. The nanofibers have good thermal stability, for their microstructure can be maintained even after heat treatment at1400℃for12h. For a single α-Al2O3fiber with a diameter of ca.350nm, the elastic modulus was23.8GPa, indicating the good flexibility. The good thermal stability and flexibility may extend the service life even when it is subject to stresses and strains resulting from thermal tensions and mechanical contact, which favors their application in catalysis and filtration at high temperature.
2. Fabrication and insulation properties of a-alumina fibers with CaO-SiO2additive
CaO-SiO2two-component doped flexible a-alumina fibers were successfully prepared through the sol-gel method combined with an electrospinning process. The sol was prepared with aluminum chloride hexahydrate and aluminum powder as raw materials, calcium oxide-silica (CaO-SiO2) was applied as two-component additive, and water as the solvent. The mixture was heated to90℃and refluxed for5h with magnetic stirring to form a transparent solution. The resulting transparent solution was condensed for5h using a water bath (80℃). Finally, PVP was added with continuously stirring at ambient temperature to form a transparent sol. Small amounts of CaO-SiO2additive was applied to retard the formation of γ-Al2O3and the phase transformation from γ-Al2O3to α-Al2O3, and control the size of the grains during sintering. With the addition of the CaO-SiO2in the system, the size of the particles composed the fibers calcined at1300℃significantly decreased compared to that without additive, which might due to the formation of6-alumina in the samples. The alumina fiber mat calcined at1300℃with the CaO/SiO2ratio of1:10had good flexibility and low thermal conductivity (0.07329W/m·K), which favored its application in insulation.
3. Fabrication and anti-corrosion properties of flexible and amphiphobic γ-alumina mats
Alumina gel fibers were by the sol-gel method combined with an electrospinnin process. The sol was prepared using aluminum isopropoxide and aluminum nitrate as the precursors, nitric acid and acetic acid as catalysts, water as the solvent, and polyvinylpyrrolidone (PVP) was applied to tune sol viscosity. The γ-alumina mats were obtained after calcination of the gel fibers. Amphiphobic γ-alumina mats were fabricated by (fluoroalkyl)silane (FAS) modification of the obtained γ-alumina mats. When the content of PVP was0.3g, the average fiber diameters were smaller than those with0.4and0.5g PVP, and the resulting larger surface roughness endowed the modified alumina mat better amphiphobicity. At the same time, the modified alumina mat exhibited a hydrophobic property in the pH range from1to14, indicating that it had a certain anti-corrosion resistance. Additionally, the modified alumina mat was flexible and would not rapture even folding it on a paper, which may extend the application of fiber mats in many important industrial fields.
Flexible α-alumina nanofibers were fabricated by the sol-gel method combined with an electrospinning process. The sol was prepared with aluminum isopropoxide and aluminum nitrate as the precursors, nitric acid as the catalyst, and ethanol aqueous solution as the solvent. Small amounts of anhydrous magnesium sulfate as additive acted to stabilize the γ-Al2O3structure and retard its conversion to α-Al2O3firstly, and subsequently MgAl2O4was formed at the grain boundaries to inhibit grain growth. Polyvinylpyrrolidone (PVP) was applied to tune sol viscosity. The fibers with diameters of300-400nm are composed of α-Al2O3nanosheets with thickness of20-50nm which stack along [0001] at the axial direction. The fibers exhibited good flexibility and thermal stability.
Alumina fibers were fabricated by the sol-gel method combined with an electrospinning process using aluminum chloride hexahydrate (AICl3·6H2O) and aluminum powder as raw materials in water solvent. Calcium oxide-silica (CaO-SiO2) was applied as two-component additive to retard the phase transformation of alumina and control the size of the grains during sintering. With the addition of the CaO-SiO2in the system, the size of the particles that composed the fibers calcined at1300℃significantly decreased compared to that without additive, which might be due to the formation of θ-alumina in the samples. In addition, the fiber had low thermal conductivity and good flexibility, which favored its application in insulation.
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