先驱体转化法制备Si-Al-Zr-O及Ti-Si-O-C系先进复相陶瓷研究
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摘要
本论文研究了通过受控转化预制的陶瓷先驱体,合成Si-Al-Zr-O及Ti-Si-O-C先进复相陶瓷材料的工艺过程。对制得陶瓷材料微观结构以及性能做了深入探讨,揭示了先驱体转化制备的复相陶瓷材料结构与特性的相关关系,突显使用该方法制备先进结构陶瓷及功能陶瓷优势。研究工作主要包括：使用受控晶化深冷制备得到的Si-Al-Zr-O系非晶先驱体,合成了高性能的纳米复相增韧陶瓷；使用溶胶-凝胶工艺制备Ti-Si-O-C系陶瓷先驱体,在不同条件下转化制备出具有高比表面积的介孔氧化物及碳化物复合材料。针对先驱体转化获得的先进纳米复相陶瓷的微观结构性能以及相关问题做了具体研究,得到如下几点重要结论：
(1)通过受控晶化转化深冷制备得到的Si-Al-Zr-O系非晶先驱体可以制备出结构均匀,致密的氧化锆增韧莫来石微纳米复相陶瓷,且结构性能可以调整。先驱体转化中,四方氧化锆(t-ZrO2)的析出温度约为1000℃,形成尺寸比较完整的莫来石(3Al2O3·2SiO2)晶粒温度为1150℃。研究表明,经1150℃晶化处理后的的Z15样品(氧化锆含量为15wt%)机械性能最佳。
(2)对不同温度热处理后Z15非晶先驱体的微观结构进行的透射电子显微分析研究发现：短棒状的氧化锆晶粒由于生长初期没有被莫来石包裹从而尺寸较大,长度在可以长大到100nm以上；而另一类氧化锆颗粒被其周围生长的莫来石包裹,导致长大受阻,从而尺寸较小(<60nnm)。四方氧化锆晶粒在55纳米以下时能够维持球形形貌,由于其<001>晶向生长速率高于<100>晶向生长速率,会逐渐形成短棒状颗粒,热处理温度从1150℃升高到1200℃以后只有少量堇青石(2MgO·2Al2O3-5SiO2)产生,而莫来石相继续生长,直到和第一类氧化锆形成晶界,非晶大幅度减少仅部分存在于两相晶界处。
(3)研究了非晶先驱体添加到原料粉末中对普通烧结过程及其产物的结构性能的影响。使用原料粉末烧结制备Si-Al-Zr-O系复相陶瓷,到1580℃以上才能形成氧化锆-莫来石相,相比之下通过控制非晶析晶能在相对较低的温度获得。非晶的添加能够明显的促进烧结陶瓷致密化,提高断裂韧性,添加量小于10wt%范围内最为明显。
(4)通过热处理转化溶胶-凝胶法制备Ti-Si-O-C系先驱体,得到介孔-微孔组织的氧化钛-氧化硅-碳复合材料。由于聚合的糠醇(PFA)为憎水性,与水解后的金属氧化物(亲水性)不相容,导致其在混合的三元体系中分离团聚,形成球形分相。通过调整金属氧化物(TTIP和TEOS).碳源(FA)和表面活性剂(P123)的添加量,可以达到控制分相以及其微观孔结构的目的,如比表面积(23-397m2/g),孔尺寸(2.6-7nm),孔体积以及介孔和微孔的面积等。在空气中煅烧TSC凝胶先驱体除掉碳后可以制备出高表面积(95m2/g-700m2/g)的氧化钛-氧化硅复合材料,并形成具有大孔-介孔复合材料。
(5)研究了先驱体溶胶陈化时间、溶胶干燥工艺、溶胶超声分散等工艺条件,对煅烧后的氧化钛-氧化硅-碳复合材料孔隙结构,显微组织以及化学成分的变化影响。研究表明：长的陈化时间增加糠醇聚合度,更易在复合材料中形成大的富碳分相；提高干燥的速度能有效的控制分相的产生及其尺寸；超声分散促进了PFA团聚,促进了析出物长大。样品的表面积及孔结构主要受干燥条件控制,陈化时间的改变对其没有明显的影响。氧化硅-氧化钛-碳复合材料中的残余碳含量随陈化时间增加降低。通过对溶胶-凝胶处理工艺条件的控制和调整,可制备出一系列具有不同比表面积(1m2/g-288m2/g)和显微结构(富碳析出物尺寸：0μm-10μm)氧化硅-氧化钛-碳复合材料。
(6)以Ti-Si-O-C先驱体为原料,在不同温度下进行热处理制备得到了具有3-4nm孔径的介孔组织、比表面积达272m2/g、晶化程度高的纳米碳化钛-碳化硅-碳复合材料。在碳热还原反应时,高度分相的先驱体会导致基体由于缺碳而形成氧化物-碳化物-碳的介孔复合材料。在碳化物-碳中出现的多级介孔分布,小孔(3-5nnm)主要分布在基体中的残留碳网络,而大孔(10-20nm)是纳米颗粒之间不规则堆积所产生的间隙。提高氧化物-碳先驱体的均一度有利制备具有高比表面积的介孔碳化物复合材料。
(7)探讨了一种制备大块介孔C-TiC/SiC纳米复合陶瓷的材料的新工艺,即通过直接碳热还原受控溶胶-凝胶制备得到大块Ti-Si-O-C先驱体,从而获得高晶化程度的碳化物复合材料。研究发现石墨烯在TiC晶粒(111)面上生长,并通过“桥接”、“缠绕”等机制连接其他晶粒,而这个现象没有在β-SiC上观察到。残留的碳纳米晶网络支撑了碳化物晶粒,组成了一个具有一定机械强度的介孔复合材料块体,其折减弹性模量(Er)和硬度(H)的平均值分别为13.78±0.71GPa(Er)和0.85±0.072GPa(H)。材料的弹性回复能力与组织中碳含量增加而增高。
(8)使用受控喷雾干燥以及先驱体转化法制备得到的TiC微球,种具体有介孔组织的纳米晶微球。微球尺寸均一度可以通过调整先驱体溶胶陈化时间以及喷雾干燥气流温度来控制。在陈化3.5天,干燥温度为150℃条件下获得较佳形貌的先驱体凝胶微球。通过两步热处理凝胶微球先驱体成功转化成介孔碳化钛陶瓷微球,直径约为45μm。介孔碳化钛微球具有很高的比表面积,达到267m2/g。材料的介孔组织是碳热还原反应中自发形成。介孔碳化钛微球的平均纳米晶粒尺寸在50nm左右,通过石墨烯包裹以后,在残余碳网络的支撑下形成完整的碳化钛微球。
Advanced ceramic materials were synthesized through a controlled transformation of pre-ceramic precursors. Two major parts of work were included:I, Synthesizing Si-Al-Zr-O amorphous pre-ceramic bulk by deep cooling the melted oxides, then heat-treat as-made precursor to ob-tain crystalline ceramics; Ⅱ, Fabricating Ti-Si-O-C monolithic gel pre-cursor through controlled sol-gel routes and transform it into mesoporous TiO2/SiO2/C and C-TiC/SiC nanocomoposites. The unique nano struc-tures and outstanding properties were achieved for both ceramic systems. And the detail research results are shown as following.
(1) Dense zirconia-mullite ceramics with uniform dispersed nano grains can be synthesized by a controlled crystallization of Si-Al-Zr-O amorphous bulk. Teragonal ZrO2was first crystallized at～1000℃and mullite was formed at relatively higher temperature,1150℃. The me-chanical properties were adjustable by chemical composition and heat treatment temperatures. The sample with15wt%zirconia (Z15) and heat treated at1150℃showed the highest flexural strength and fracture toughness,520MPa and5.13MPa-m1/2, respectively.
(2) Z15sample heated at1150℃showed two kinds of zirconia grains, rod like and spherical nano grains. The size of rod like zirconia grains reached over100nm, the other type of zirconia grains which were embedded in mullite grains showed the size within60nnm. The ZrO2grains maintain as spherical shapes when it is smaller then55nm. The growth rate of ZrO2grains along<001> direction is higher than that along <100> direction, which result in rod-like ZrO2with time. Cordierite crystallized after1200℃, and higher temperature promoted the grain growth of ZrO2and mullite, and the amount of amorphous phase reduced drmatically and only existed between grains boundary.
(3) Comparing to amorphous bulk precursor, the sintering of starting oxides powder requires higher heating temperature to form zirco-nia-mullite phase. Adding amorphous Si-Al-Zr-O precursor powder to starting oxides can promote the mechanical properties and the density of sintered ceramics. The most effective amount of amorphous precursor added for sintering is10w%.
(4) The extent of the ploy(furfuryl alcohol) PFA phase separation can be controlled by adjusting the ratio of silica and titania precursors (TEOS and TTIP), the amounts of FA and surfactant P123. The BET surface area (23-397m2/g), pore size (2.6-7nm), pore volume and the me-so/micropore ratio of the composites are all tunable in varied degrees by changing the chemical composition. Increase of silica to titania ratio gives higher porosity of the composite but results in an intense separation of carbon rich domains from the matrix and a high microporosity. Calci-nation of the as-synthesized monolithic gel at550℃in air could produce mesoporous titania/silica composites containing different amounts of ma-cropores. The demonstrated research here shows a facile approach to synthesize macro/meso/microporous titania/silica/carbon and titania/silica composites. Moreover, it also provides a feasible route to control the phase separation of PFA through composition changes, which can be widely used as hybrid precursors for synthesis of porous carbon, oxides, oxide/carbon and carbide/carbon nanocomposites.
(5) The BET surface area (1m2/g-288m2/g) and separated carbon size (sphere size0μm-10μm) on silica/titania/carbon nanocomposite can be tunled through controlment of the ageing time, drying process and ultrasonic treatment in the sol-gel process. Increasing the ageing time will promote polymerization of furfuryl alcohol, causing more carbon phase separation. High drying rate will decrease the agglomerate rate of PFA which also control the phase separation. The pore structure is determined by the dry process, and ageing time has no obvious effect on it. But the residual carbon content in the silica/titania/carbon nanocomposite de-crease with ageing time.
(6) We have demonstrated the synthesis of nanostructured (pore size3-4nm) bulk mesoporous C-TiC/SiC ceramics with high crystallinity by direct carbothermal reduction of pre-fabricated Ti-Si-O-C precursors. Benefiting from the homogenously dispersed components and intercon-nected channels, the carbothermal reduction takes place very efficiently at a relatively low temperature (starting at1100℃and completing at1450℃). The high mesoporosity (272m2/g) is obtained by in situ reaction of metal oxide with the surrounding carbon. The small pores (～3nm) were generated by removing of the surfactant (P123) during gel calcination, and they partially remained in the residual carbon for TSC-1450. Large pores (～10nm) were formed by the packing of nanoparticles. The high homogeneity is benefitial to the synthesis of highly mesoporous carbide ceramics.
(7) The nano sized carbide grains are bonded into bulk materials by ploy(furfuryl alcohol)(PFA) derived nanocrystalline carbon framework because of its "bridge","entanglement" and "adhesive" effects. The gra-phenes are found to bond on the (111) plane of TiC grains, while no simi-lar coating is found for SiC grains. The bonding of graphitic carbon lay-ers on carbide grains support the nanostructure and also result in the de-sired combination of functional and mechanical properties. The average values of reduced elastic modulus, Er, and hardness, H, of the mesopor-ous carbides sample (TSC-1450) obtained from the nanoindentation tests were13.78±0.71GPa (Er) and0.85±0.072GPa (H), respectively. The coating and bridging of graphene sheets on TiC grains maintained the nanostructure and also resulted in a desired bulk material. Moreover, the process described here also provides an alternative concept for fabrication of bulk carbide composites through bonding of a carbon framework, avoiding granular sintering.
(8) We demnostrate a feasible route to bulk synthesis mesoporous TiC microspheres (BET267m2/g) through in situ carbothermal reduction of precursor beads derived from a modified spray drying process. The uniform beads can be obtained from the sol aged for3.5days and spray dried at150℃. The average diameter of the as-made precursor and car-bide microsphere are75μm and45μm, respectively. No template is ap-plied to build the pore structure of the microspheres and the diameter and uniformity of spheres can be tuned by changing the ageing time and dry-ing temperature. The nano sized TiC crystal (～50nm) are connected by nanocrytalline carbon network by the mechanism discussed above and reasonable strength is obtained to maintain the spherical morphology, which could provide potential application in energy related areas.
(1)通过受控晶化转化深冷制备得到的Si-Al-Zr-O系非晶先驱体可以制备出结构均匀,致密的氧化锆增韧莫来石微纳米复相陶瓷,且结构性能可以调整。先驱体转化中,四方氧化锆(t-ZrO2)的析出温度约为1000℃,形成尺寸比较完整的莫来石(3Al2O3·2SiO2)晶粒温度为1150℃。研究表明,经1150℃晶化处理后的的Z15样品(氧化锆含量为15wt%)机械性能最佳。
(2)对不同温度热处理后Z15非晶先驱体的微观结构进行的透射电子显微分析研究发现：短棒状的氧化锆晶粒由于生长初期没有被莫来石包裹从而尺寸较大,长度在可以长大到100nm以上；而另一类氧化锆颗粒被其周围生长的莫来石包裹,导致长大受阻,从而尺寸较小(<60nnm)。四方氧化锆晶粒在55纳米以下时能够维持球形形貌,由于其<001>晶向生长速率高于<100>晶向生长速率,会逐渐形成短棒状颗粒,热处理温度从1150℃升高到1200℃以后只有少量堇青石(2MgO·2Al2O3-5SiO2)产生,而莫来石相继续生长,直到和第一类氧化锆形成晶界,非晶大幅度减少仅部分存在于两相晶界处。
(3)研究了非晶先驱体添加到原料粉末中对普通烧结过程及其产物的结构性能的影响。使用原料粉末烧结制备Si-Al-Zr-O系复相陶瓷,到1580℃以上才能形成氧化锆-莫来石相,相比之下通过控制非晶析晶能在相对较低的温度获得。非晶的添加能够明显的促进烧结陶瓷致密化,提高断裂韧性,添加量小于10wt%范围内最为明显。
(4)通过热处理转化溶胶-凝胶法制备Ti-Si-O-C系先驱体,得到介孔-微孔组织的氧化钛-氧化硅-碳复合材料。由于聚合的糠醇(PFA)为憎水性,与水解后的金属氧化物(亲水性)不相容,导致其在混合的三元体系中分离团聚,形成球形分相。通过调整金属氧化物(TTIP和TEOS).碳源(FA)和表面活性剂(P123)的添加量,可以达到控制分相以及其微观孔结构的目的,如比表面积(23-397m2/g),孔尺寸(2.6-7nm),孔体积以及介孔和微孔的面积等。在空气中煅烧TSC凝胶先驱体除掉碳后可以制备出高表面积(95m2/g-700m2/g)的氧化钛-氧化硅复合材料,并形成具有大孔-介孔复合材料。
(5)研究了先驱体溶胶陈化时间、溶胶干燥工艺、溶胶超声分散等工艺条件,对煅烧后的氧化钛-氧化硅-碳复合材料孔隙结构,显微组织以及化学成分的变化影响。研究表明：长的陈化时间增加糠醇聚合度,更易在复合材料中形成大的富碳分相；提高干燥的速度能有效的控制分相的产生及其尺寸；超声分散促进了PFA团聚,促进了析出物长大。样品的表面积及孔结构主要受干燥条件控制,陈化时间的改变对其没有明显的影响。氧化硅-氧化钛-碳复合材料中的残余碳含量随陈化时间增加降低。通过对溶胶-凝胶处理工艺条件的控制和调整,可制备出一系列具有不同比表面积(1m2/g-288m2/g)和显微结构(富碳析出物尺寸：0μm-10μm)氧化硅-氧化钛-碳复合材料。
(6)以Ti-Si-O-C先驱体为原料,在不同温度下进行热处理制备得到了具有3-4nm孔径的介孔组织、比表面积达272m2/g、晶化程度高的纳米碳化钛-碳化硅-碳复合材料。在碳热还原反应时,高度分相的先驱体会导致基体由于缺碳而形成氧化物-碳化物-碳的介孔复合材料。在碳化物-碳中出现的多级介孔分布,小孔(3-5nnm)主要分布在基体中的残留碳网络,而大孔(10-20nm)是纳米颗粒之间不规则堆积所产生的间隙。提高氧化物-碳先驱体的均一度有利制备具有高比表面积的介孔碳化物复合材料。
(7)探讨了一种制备大块介孔C-TiC/SiC纳米复合陶瓷的材料的新工艺,即通过直接碳热还原受控溶胶-凝胶制备得到大块Ti-Si-O-C先驱体,从而获得高晶化程度的碳化物复合材料。研究发现石墨烯在TiC晶粒(111)面上生长,并通过“桥接”、“缠绕”等机制连接其他晶粒,而这个现象没有在β-SiC上观察到。残留的碳纳米晶网络支撑了碳化物晶粒,组成了一个具有一定机械强度的介孔复合材料块体,其折减弹性模量(Er)和硬度(H)的平均值分别为13.78±0.71GPa(Er)和0.85±0.072GPa(H)。材料的弹性回复能力与组织中碳含量增加而增高。
(8)使用受控喷雾干燥以及先驱体转化法制备得到的TiC微球,种具体有介孔组织的纳米晶微球。微球尺寸均一度可以通过调整先驱体溶胶陈化时间以及喷雾干燥气流温度来控制。在陈化3.5天,干燥温度为150℃条件下获得较佳形貌的先驱体凝胶微球。通过两步热处理凝胶微球先驱体成功转化成介孔碳化钛陶瓷微球,直径约为45μm。介孔碳化钛微球具有很高的比表面积,达到267m2/g。材料的介孔组织是碳热还原反应中自发形成。介孔碳化钛微球的平均纳米晶粒尺寸在50nm左右,通过石墨烯包裹以后,在残余碳网络的支撑下形成完整的碳化钛微球。
Advanced ceramic materials were synthesized through a controlled transformation of pre-ceramic precursors. Two major parts of work were included:I, Synthesizing Si-Al-Zr-O amorphous pre-ceramic bulk by deep cooling the melted oxides, then heat-treat as-made precursor to ob-tain crystalline ceramics; Ⅱ, Fabricating Ti-Si-O-C monolithic gel pre-cursor through controlled sol-gel routes and transform it into mesoporous TiO2/SiO2/C and C-TiC/SiC nanocomoposites. The unique nano struc-tures and outstanding properties were achieved for both ceramic systems. And the detail research results are shown as following.
(1) Dense zirconia-mullite ceramics with uniform dispersed nano grains can be synthesized by a controlled crystallization of Si-Al-Zr-O amorphous bulk. Teragonal ZrO2was first crystallized at～1000℃and mullite was formed at relatively higher temperature,1150℃. The me-chanical properties were adjustable by chemical composition and heat treatment temperatures. The sample with15wt%zirconia (Z15) and heat treated at1150℃showed the highest flexural strength and fracture toughness,520MPa and5.13MPa-m1/2, respectively.
(2) Z15sample heated at1150℃showed two kinds of zirconia grains, rod like and spherical nano grains. The size of rod like zirconia grains reached over100nm, the other type of zirconia grains which were embedded in mullite grains showed the size within60nnm. The ZrO2grains maintain as spherical shapes when it is smaller then55nm. The growth rate of ZrO2grains along<001> direction is higher than that along <100> direction, which result in rod-like ZrO2with time. Cordierite crystallized after1200℃, and higher temperature promoted the grain growth of ZrO2and mullite, and the amount of amorphous phase reduced drmatically and only existed between grains boundary.
(3) Comparing to amorphous bulk precursor, the sintering of starting oxides powder requires higher heating temperature to form zirco-nia-mullite phase. Adding amorphous Si-Al-Zr-O precursor powder to starting oxides can promote the mechanical properties and the density of sintered ceramics. The most effective amount of amorphous precursor added for sintering is10w%.
(4) The extent of the ploy(furfuryl alcohol) PFA phase separation can be controlled by adjusting the ratio of silica and titania precursors (TEOS and TTIP), the amounts of FA and surfactant P123. The BET surface area (23-397m2/g), pore size (2.6-7nm), pore volume and the me-so/micropore ratio of the composites are all tunable in varied degrees by changing the chemical composition. Increase of silica to titania ratio gives higher porosity of the composite but results in an intense separation of carbon rich domains from the matrix and a high microporosity. Calci-nation of the as-synthesized monolithic gel at550℃in air could produce mesoporous titania/silica composites containing different amounts of ma-cropores. The demonstrated research here shows a facile approach to synthesize macro/meso/microporous titania/silica/carbon and titania/silica composites. Moreover, it also provides a feasible route to control the phase separation of PFA through composition changes, which can be widely used as hybrid precursors for synthesis of porous carbon, oxides, oxide/carbon and carbide/carbon nanocomposites.
(5) The BET surface area (1m2/g-288m2/g) and separated carbon size (sphere size0μm-10μm) on silica/titania/carbon nanocomposite can be tunled through controlment of the ageing time, drying process and ultrasonic treatment in the sol-gel process. Increasing the ageing time will promote polymerization of furfuryl alcohol, causing more carbon phase separation. High drying rate will decrease the agglomerate rate of PFA which also control the phase separation. The pore structure is determined by the dry process, and ageing time has no obvious effect on it. But the residual carbon content in the silica/titania/carbon nanocomposite de-crease with ageing time.
(6) We have demonstrated the synthesis of nanostructured (pore size3-4nm) bulk mesoporous C-TiC/SiC ceramics with high crystallinity by direct carbothermal reduction of pre-fabricated Ti-Si-O-C precursors. Benefiting from the homogenously dispersed components and intercon-nected channels, the carbothermal reduction takes place very efficiently at a relatively low temperature (starting at1100℃and completing at1450℃). The high mesoporosity (272m2/g) is obtained by in situ reaction of metal oxide with the surrounding carbon. The small pores (～3nm) were generated by removing of the surfactant (P123) during gel calcination, and they partially remained in the residual carbon for TSC-1450. Large pores (～10nm) were formed by the packing of nanoparticles. The high homogeneity is benefitial to the synthesis of highly mesoporous carbide ceramics.
(7) The nano sized carbide grains are bonded into bulk materials by ploy(furfuryl alcohol)(PFA) derived nanocrystalline carbon framework because of its "bridge","entanglement" and "adhesive" effects. The gra-phenes are found to bond on the (111) plane of TiC grains, while no simi-lar coating is found for SiC grains. The bonding of graphitic carbon lay-ers on carbide grains support the nanostructure and also result in the de-sired combination of functional and mechanical properties. The average values of reduced elastic modulus, Er, and hardness, H, of the mesopor-ous carbides sample (TSC-1450) obtained from the nanoindentation tests were13.78±0.71GPa (Er) and0.85±0.072GPa (H), respectively. The coating and bridging of graphene sheets on TiC grains maintained the nanostructure and also resulted in a desired bulk material. Moreover, the process described here also provides an alternative concept for fabrication of bulk carbide composites through bonding of a carbon framework, avoiding granular sintering.
(8) We demnostrate a feasible route to bulk synthesis mesoporous TiC microspheres (BET267m2/g) through in situ carbothermal reduction of precursor beads derived from a modified spray drying process. The uniform beads can be obtained from the sol aged for3.5days and spray dried at150℃. The average diameter of the as-made precursor and car-bide microsphere are75μm and45μm, respectively. No template is ap-plied to build the pore structure of the microspheres and the diameter and uniformity of spheres can be tuned by changing the ageing time and dry-ing temperature. The nano sized TiC crystal (～50nm) are connected by nanocrytalline carbon network by the mechanism discussed above and reasonable strength is obtained to maintain the spherical morphology, which could provide potential application in energy related areas.
引文
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