Processing and Properties of Al2O3 Microstructure Composites

Open Access
Author:
Pavlacka, Robert Joseph
Graduate Program:
Materials Science and Engineering
Degree:
Doctor of Philosophy
Document Type:
Dissertation
Date of Defense:
May 01, 2009
Committee Members:
  • Gary Lynn Messing, Dissertation Advisor
  • Gary Lynn Messing, Committee Chair
  • David John Green, Committee Member
  • John Richard Hellmann Jr., Committee Member
  • Albert Eliot Segall, Committee Member
Keywords:
  • texture
  • templated grain growth
  • non-catastrophic failure
  • fracture
  • alumina
  • microstructure composite
  • composite
Abstract:
We have proposed a new class of composites that accesses different component properties not through the use of distinct materials, but through the exploitation of the microstructure-property relationship within a single material. That is, we seek to adapt composite concepts to take advantage of the considerable variance in properties associated with different microstructures. This new class of composites is called microstructure composites. Microstructure composites are predominately single phase ceramics that utilize multiple distinct microstructure features in the same composite to obtain unique property combinations. Spatial control and composite connectivity of the individual microstructure components of a microstructure composite are ultimately the key to developing and controlling useful and unique properties. Microstructural features can be controlled via the starting location and transport of the dopants, minority second phases, and liquid phases that are used to manipulate microstructure development. This work focuses on textured-equiaxed microstructure in the Al2O3 system. Texture is obtained in situ using templated grain growth (TGG). To control microstructure development locally during microstructure composite fabrication, it is important to use relatively low levels of dopant to mitigate the effects of dopant interdiffusion. Therefore, the development of texture in α-Al2O3 using TGG was explored under low liquid-phase dopant concentration conditions. High temperature dilatometry was performed to quantify the effect of template constraint on x-y plane shirinkage and the extent to which this constraint could be mitigated as a function of the dopant concentration. x-y plane shrinkage was observed to be increasingly constrained with increasing template loadng and decreasing dopant concentration. Final x-y plane shrinkage was greater for samples with 0.14 wt% dopant than for those without dopant, despite have a much lower peak strain rate. It was concluded that densification was impeded by the dopant at lower temperatures but enhanced significantly above 1450°C. Texture is highly developed in samples with no dopant and 0.14 wt% dopant by 1550°C and in samples with 2 wt% dopant by 1350°C. We proposed a new class of composites (called microstructure composites) that accesses different component properties not through the use of distinct materials, but rather through the exploitation of the microstructure-property relationship within a single material. Microstructure composites, therefore, are single phase ceramics that combine components with distinct microstructures within a single composite to obtain unique property combinations. Spatial control and composite connectivity of the individual microstructural ‘components’ of a microstructure composite are ultimately the key to developing and controlling useful and unique properties. Microstructural components are developed by controlling the starting location and transport of dopants during processing and sintering. This work focuses on α-Al2O3 microstructure composites that combine textured components, developed in situ using templated grain growth (TGG), and fine-grained equiaxed components. To control microstructure development locally during composite fabrication, it is important to use relatively low levels of dopant to mitigate the effects of dopant interdiffusion. Therefore, the development of texture in α-Al2O3 using low liquid-phase dopant concentrations was explored, with a focus on the effect of template constraint on texture plane shrinkage. High quality texture was obtained with just 0.14 wt% (SiO2 + CaO) dopant. Textured Al2O3 exhibited transgranular fracture, as well as lower strength and fracture toughness than the fine-grained equiaxed Al2O3. A processing strategy using tape casting was developed for the fabrication of textured-equiaxed Al2O3 microstructure composites with 2-2 connectivity. Dopants used to promote TGG (SiO2 + CaO) were included in the templated tapes and dopants used to prevent abnormal grain growth (MgO) were included in the non templated tapes, which are subsequently stacked, laminated, and co-sintered. Appropriate dopant concentrations and sintering conditions that enable the production of well-textured layers and fine-grained equiaxed layers seperated by a sharp interface were identified. It was found that densification and microstructure development within textured and equiaxed layers is affected by changes in both differential sintering stress and dopant diffusion distance associated with layer thickess and the volume percent of textured layers within the composite. Significant crack deflection was observed during bend testing of composites with porous textured layers (2-5 vol% porosity), resulting in highly non-catastrophic failure (with W.O.F. up to 1 kJ/m2). Crack deflection, often millimeters in length, occurred along the basal faces of templated grains within the textured. Textured layers that deflect cracks (i.e. those with porosity) had significantly lower interfacial fracture energies than textured layers that do not deflect cracks (i.e. those without porosity). It was determined that crack deflection is a composite effect and the result of the combination of the anisotropic fracture energy of textured Al2O3 and the residual compressive stresses developed from thermal expansion mismatch. Other observed fracture phenomena include multiple cracking / crack arrest and preliminary evidence of flaw tolerance. Textured-equiaxed Al2O3 microstructure composites of additional connectivities, (including 1-3, 0-3, and 3-3) were produced by screen printing and co-casting processes. Template alignment during the screen printing process was demonstrated, allowing the capability to print complex textured features. Co-casting was used to produce single tapes with templated and non-templated segments. A variety of stacking strategies were employed to generate various 1-3 and 3-3 composites (including cross-ply composites). Observations during fracture testing of complex composites included non-catastrophic failure without crack deflection and improved delamination resistance.