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Grain boundaries typically dominate fracture toughness, strength and slow crack growth in ceramics. To improve these properties through mechanistically informed grain boundary engineering, precise measurement of the mechanical properties of individual boundaries is essential, although it is rarely achieved due to the complexity of the task.

Here we present an approach to characterize fracture energy at the lengthscale of individual grain boundaries and demonstrate this capability with measurement of the surface energy of silicon carbide single crystals.

We perform experiments using an in situ scanning electron microscopy-based double cantilever beam test, thus enabling viewing and measurement of stable crack growth directly. These experiments correlate well with our density functional theory calculations of the surface energy of the same silicon carbide plane. Subsequently, we measure the fracture energy for a bi-crystal of silicon carbide, diffusion bonded with a thin glassy layer.

Building the next generation of advanced engineering technologies is often limited by the quality and performance of available materials. For applications such as space telescopes, atmospheric re-entry vehicles, and medical implants, materials with high hardness, high thermal stability, high strength, and low density are required. Ceramics have these attributes; yet their widespread use is restricted due to their poor resistance to fracture, often leading to unpredictable and catastrophic failures.

If toughness could be improved, through mechanistically informed grain boundary engineering and precise process control, then fabricated components could be used in ever more demanding environments.

Successful manufacture of these improved ceramics relies on understanding which grain boundaries are preferred, i. This approach requires targeted experimental tests of individual microstructural features to provide mechanistic insight of which grain boundaries are preferred and why. Furthermore, these tests may assist rationalization of existing experiments, for instance in silicon carbide SiC it has been shown that chemistry of individual interfaces can have a strong influence on the fracture toughness.

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Full version downloads available, all hosted on high speed servers! At present, there are many standard tests that enable precise measurement of the fracture properties of brittle materials at a macroscopic lengthscale, yet few available tests that enable direct measurement of individual grain boundaries. Macroscopic tests are very successfully used to understand bounds on component performance and to compare and contrast ceramic-processing strategies, but as they test polycrystalline aggregates it is very difficult to understand the role of specific microstructural features.

Achieving a step change in the performance and utilization of advanced ceramics requires new insight at the microstructural lengthscale, as failure of ceramics is controlled often by the weakest microstructural link. Development of site-specific micromechanical testing of ceramics has advanced significantly in the last 5 years, using either photolithography or focused ion beam FIB machining, enabling preparation of microscopic test specimens in precisely specified locations and opening the door to high spatial resolution mechanical tests.

Typically, these test specimens are loaded using a nanoindentation platform with different bewirtungsbdleg geometries according to the test design.

The philosophy of performing high spatial resolution testing, as employed with these geometries, enables assessment either of the local fracture properties of single grains or grain boundaries, or of samples that are inherently small in volume, e.

The key limitation of existing approaches is that they typically make use of a load-controlled ramp to actuate the indenter and follow crack opening indirectly, using changes in load-displacement data both to identify the crack nucleation and fracture bewirtungzbeleg to be used in fracture toughness measurements.

This is problematic if the loading system is compliant or stores significant energy, and load control exhibits an increasing energy release rate with crack growth therefore inherently does not lend bewirtungxbeleg to stable fracture. Loading geometries employed for micromechanical fracture testing of interfaces. A Single cantilever bending geometry with pentagonal cross-section and loaded with a sharp indenter.

Straight and chevron notch geometry sections are represented with blue and red dashed lines, respectively. Straight notches provide inherently unstable fracture, whereas the chevron notches enable a stable crack growth for short cracks. Dimension measurements of notch and beam geometry are performed after the test. B Schematic of a double clamped beam bending geometry loaded with a blunt tip. Stable crack growth is supported but freedom of positioning of the vordruxk is limited.


C DCB geometry loaded with a flat punch. Stable crack growth is achieved. Friction between flat punch and sample, and compressive stress on struts need to be taken into account. D The wedge loaded DCB geometry used in this work.

Unfortunately, an unstable loading geometry limits evaluation of fracture energy to extraction of a single value. This issue is compounded by warranted concerns about bewirtungsbrleg effects of notch manufacture at this small lengthscale, such votdruck the introduction of FIB-induced vordrucm in the region surrounding the notch. In light of these previous geometries, it would be ideal to have test samples with geometrical features enabling stable bdwirtungsbeleg growth beyond any damaged region, in order to measure fracture toughness as the crack evolves and to overcome limitations imposed by FIB-induced damage.

It would be also useful to have freedom in the vordruckk of the notch combined with a relatively simple sample geometry, thus facilitating sample fabrication and fracture or surface energy analysis. Furthermore, a minimization of the effect of frame compliance and friction between the indenter and the sample would make evaluation of the bewirtungsbdleg energy easier. In this manuscript, we choose to test a DCB geometry, fabricated using FIB, and load this with a wedge in direct displacement control in situ within a scanning electron microscope SEM.

This geometry is similar to the classic design described by Lawn, and utilizes the displacement of each cantilever beam and a simple calculation of the stored elastic energy within each beam that balances with the energy required to create new crack surface.

This enables a direct measurement of the fracture bewirfungsbeleg surface energy as the crack grows. As the experiment is performed in displacement control, the driving force decreases with crack length and therefore cracking is inherently stable.

Furthermore, in situ testing allows the atmosphere to be controlled, reducing concerns of environmentally induced effects such as virdruck corrosion cracking. Surface energy measurements are demonstrated on single crystal SiC samples to validate the technique and these are compared with density functional theory DFT calculations. Experimentally, the approach is subsequently used to explore the fracture of SiC bi-crystals adhered together with silica manufactured using diffusion bonding.

In summary, this work presents a method to measure the fracture energy evolution with crack length at the microscale in purely brittle materials, with the benefits of a high sampling rate, stable crack growth, and a controlled environment. Fracture energy measurement Experiments were performed on single crystal 6H-SiC and bi-crystal SiC, which was diffusion-bonded with a silica glass interface layer.

Mechanical testing was performed in situ in a SEM, which provided high spatial and temporal resolution imaging of the loading and fracture processes.

This proved beneficial bewirtungbseleg the alignment of the sample and loading geometry, as well as providing direct observations of the fracture under load. A wedge sliding through the central trough causes beam bending of both cantilevers, and the elastic energy stored within the beams is available to drive crack advance. By applying simple beam theory, it is possible to calculate the energy spent in beam bending, in terms of the beam displacement, beam geometry, and the elastic stiffness of each cantilever.

The elastic strain energy, U M, stored in each beam per unit depth is given by Euler—Bernoulli beam theory as. For the initial crack growth, the beams are shorter than the approximation required for simple beam theory to hold i.

This results in an energy release rate, G, for each beam see Supplementary Note for the derivation. The total energy release rate can be calculated using Eq. Initial registration of all frames was performed using image cross-correlation, keeping a point away from the fordruck DCB fixed vordruk the frame. This reduces the effects of image drift caused by sample or nanoindenter compliance and sample charging under the electron beam. The coordinates of the crack tip position were selected by hand, augmenting contrast within the script to make this easier.

Each cantilever beam width was measured using frames toward the end of the test, when the crack was longer. For the analysis, a Monte Carlo-based error propagation script was used. Variables for the analysis with known errors were adjusted independently to have a Gaussian distribution with a known standard deviation.

The mean of each distribution was the measurement for each test and the standard deviations based upon experimental measurement error. The variables and distributions are listed in the Supplementary Table and Supplementary Fig.

Once the DCB was loaded, the crack propagated bewirtunsbeleg and its growth was stable. This is shown in the sequence of frames extracted from the video recorded during the test of SC 2 Fig. Data analysis of DCB cracking. A Tip displacements as set-up on the nanoindenter for four of the tests conducted on the single crystal SC SiC samples.


B Displacement of left and right beams of the sample SC 3 measured by image cross-correlation of the edges during the total test length. Dotted lines are used to show the interval of bewitrungsbeleg in which the crack growth was measured. C Crack length measured on sample SC 3 from the point of crack nucleation until the tip was stopped to hold position. D Fracture energy value measured over crack growth for the four SC SiC samples and the three SiC bi-crystals with SiO 2 interlayers ILshowing good reproducibility and a significant difference between the values of the two systems.

Effect bewirtungsbelev different assumptions on DCB geometry. Bewirtunbsbeleg Plot showing how the fracture energy would be erroneously measured should the DCB tested be treated as perfectly symmetrical. It is worth noting that the fracture energy could be underestimated or overestimated depending on whether the beam considered is moving more or less than the other beam, respectively.

Design – Design

Asymmetry is likely caused by three factors. Finally, a subtle difference was observed in beam thickness, due to difficulties in fabricating small samples even with automated fabrication regimes as employed here.

For each of the three bi-crystal samples, cracks started tens of nanometers on the side of the milled notch. This is likely due to slight asymmetries in the overall loading geometry and the precise location of the interface.

These slight asymmetries require the energy stored in the cantilevers to be measured individually to avoid the fracture energy being significantly underestimated or overestimated. While this subtlety may not be obvious, in practice it is straightforward to implement asymmetric analysis with this in situ geometry.

A comparison of the differences bewirtungsbbeleg crack growth measurements using asymmetric or symmetric analysis is presented in Fig. Short crack lengths In this work, the fracture energy results are measured, taking into account the non-negligible shear component that arises because the beam length is comparable with its thickness Fig.

This low aspect ratio beam correction enables reliable measurement of the fracture energy value with variable crack length and demonstrates that the technique lends itself to the investigation of small regions of interfaces at short distances from vordrucck surface in real materials. Taper FIB milling normal to the sample surface is known to produce tapered final geometries; however, the analysis presented in this work considers the cantilevers made of constant cross-section along its length.

It is therefore important to design the milling steps to minimize the taper in the final geometry or alternatively the analysis must be performed using a more complicated elastic model, as afforded for instance with cohesive zone-based finite element models. Fracture energy or surface energy From the high-resolution SEM images the crack propagation vlrdruck the single crystal SiC appears to create two new smooth edges with no evident deviation from a linear path.

The crack tip is sharp and no plastic deformation vordrufk expected around it and likewise no toughening mechanisms are available in the material examined. Furthermore, it is worth noting that the energy values were measured far from the notch and so we do not expect to be affected by crack initiation processes or ion penetration damage, which is found to be. Similarly, the values obtained by testing the bi-crystals bewirtuntsbeleg provide the surface energy of the SiC—glass—SiC interface.

Wiederhorn reported values of fracture surface energy for glasses with different chemical composition in a range between 7. Therefore, the lower value obtained in the present work falls reasonably between the theoretical and experimental values found in the literature.

In situ wedging of a DCB coupled with a displacement-controlled testing machine afforded a stable and relatively long crack growth at the micrometer lengthscale to be obtained. The method was validated by fracturing single crystal 6H-SiC along the direction, finding a value of the fracture energy of 5. DFT calculations were performed on the same crystallographic plane as experimentally tested for the first time.

While the calculated values were slightly higher than the experimental values, both measurements agree well when compared to vordryck measurements Fig.

The consistency between experiment and DFT fracture energies for the single crystal case gives us confidence in the approach when moving to study more complex systems. By performing additional calculations see Methodswe have been able to exclude significant effects of the surface termination layer, temperature, surface reconstruction, or hydrogen termination on the theoretical fracture energy.

Comparison of data obtained in current work from experiments and DFT with existing literature on macroscopic tests.