Experimental Soft Condensed Matter Group
Harvard University, Prof. D. A. Weitz

Investigation of Grain Boundaries in Colloidal Crystals

studied with confocal microscopy

Contact: Claudia Friedsam

Research objective

Almost all engineering applications of metals involve their use in polycrystalline form. Recently the emphasis in the study of mechanical properties has moved away from the processes which occur inside the individual grains to those which are governed by the boundaries between the grains. Diverse phenomena such as high temperature creep, superplasticity, recrystallization, yielding and embrittlement all depend strongly on effects at grain boundaries. Grain boundaries are also important for diffusion phenomena as they provide pathways for diffusions into or within a material that are orders of magnitude faster than through crystalline regions. Interactions of grain boundaries and defects are also a topic of current research. Recent studies emphasize the role of grain boundaries for premelting of a crystal. Despite the important role of grain boundaries in material properties our knowledge at the microscopic level is limited. The direct observation of grain boundary structure is limited by the lack of spacial resolution as well as the time resolution of experimental techniques such as high resolution transmission electron microscopy. Thus colloidal crystals can serve as a model system to study grain boundary properties and monitor dynamic processes that occur in the grain boundary region as they are much larger and show a much slower dynamics which makes them accesible to experimental techniques like confocal microscopy.



Template based crystal growth

In our experiments we use a template that contains the particular grain boundary of interest to grow the desired crystal structure. A crystal of Silica colloids with radius of 1.5 µm is allowed to grow on this template in an index matched solution at a very slow sedimentation speed. The process is is sketched in figure 1.The structure and the general properties of these grain boundaries can be studied by confocal based video microscopy or laser diffraction microscopy.

 


Figure 1: Template based crystal growth.



Static properties of different grain boundaries in colloidal bicrystals


So far we have investigated three different types of grain boundaries whose templates are shown in the upper row in the figure below: a &Sigma 5 grain boundary (a), a &Sigma 17 grain boundary(b) and a &Sigma 3 grain boundary (c) which differ in orientation and excess volume.

Figure 2: Templates for the different types of grain boundaries (upper row) and 3D-structure of the corresponding bicrystals (lower row).

The lower row shows the structure of the different crystals grown on these templates for the 25th layer. The only grain boundary that shows a regular 3D-structure is the Σ 3 grain boundary (c). The other bicrystals show a concentration of stacking faults around the grain boundaries that are typically accompanied by different features: for the Σ 5 grain boundary additional grains can be found frequently in the grain boundary section whereas the bicrystal with the Σ 17 boundary tends to show a curved grain boundary in the upper regions.


Dynamic measurements

Colloidal crystals provide an excellent model system to study the nucleation and propagation of defects in colloidal crystals which has been show before. Thus it is straightforward to study the nucleation and propagation of defects close to a certain grain boundary. As the Σ 3 grain boundary shows a stable 3D-structure it was chosen as a starting point for the dynamic measurements. If a sewing needle is pushed on the crystal on one side of the grain boundary as shown in figure 3, defects are induced and their propagation in the bicrystal and their diffusion through the grain boundary can be monitored in confocal video-microscopy

 


Figure 3:
External forces exerted in indentation experiments allow the investigation of defect propagation close to a grain boundary.



The sequence below shows the defect structure in the 3D-reconstruction of the confocal movies at different points in time during a typical indentation experiment. The needle is moved at a slow indentation speed of about 3.33 µm/h for about 3 h, resulting in a total indentation of approximately 10 µm.

Figure 3: Evolution of defects in a typical indentation experiment.


The four different colors mark the 4 hexagonal planes on which the stacking faults can propagate. In the beginning the crystal is almost defect free. After about 70 min a couple of defects have grown at the right half of the bicrystal, where the indentation takes place. After 166min the right side is filled with stacking faults and some of them broke through the grain boundary and induced defect structures on the left side. The diffussion of a defect through the grain boundary can be monitored in detail as is shown below:




Figure 3: Breakthrough of a defect through the grain boundary (indicated by the arrow).



Smaller defects just induce an elastic reaction of the grain boundary or result in smaller breakups of the grain boundary which typically recover within a short time period. Processes like this can be observed in the beginning of the experiment. Later on, when a big ensemble of defects has formed like in the sequence above the grain boundary cannot resist the exerted strain any longer and breaks up, allowing the difffusion of a defect through the grain boundary.


Future investigations

The experiments presented above allow to study the static properties of different types of grain boundaries in colloidal bicrystals as well as the characterization of dynamic phenomena in a grain boundary region. The indentation experiments provide a detailed picture of the processes that occur when a defect is pushed through a grain boundary. Future experiments will focus on the variation of experimental parameters like indentation speed, indentation distance as well as alteration of the grain boundaries. The spectrum of experiments can be enlarged by including indentation in small grains with multiple grain boundaries or shear experiments to study grain boundary migration.


Website maintained by Claudia Friedsam.