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Journal Club for October 2020: Toughening Transparent Ceramics with Bio-inspired Architectures

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Toughening Transparent Ceramics with Bio-inspired Architectures

Zhen Yin (1, 2)

1 McGill University, Canada

2 Max Planck Institute for Intelligent Systems, Germany

Acknowledgement: This journal club was posted on my last day in Montreal. Thanks Prof. Francois Barthelat and all the group memebers for the wonderful six years. A special thanks goes to Prof. Francois Barthelat for his advisory in these years that makes this journal club possible. 


1. Introduction

Transparent ceramics such as glass and crystals have received sustained demands for their hardness, durability and optical properties. However, transparent ceramics are inherently brittle materials that have low deformability, toughness and impact resistance, which limits their applications. Conventionally, thermal/chemical tempering is used to increase the strength of glass, but tempered glass will have explosive catastrophic failure by even slight damage. Glass and other ceramics can also be laminated with polymeric interlayers to form laminated glass/ceramics. Lamination improves the post-fracture behaviors by holding the fragments together, but the ceramic layers remain brittle [1, 2]. 

Interestingly many hard biological materials (e.g.: mollusk shells, tooth enamel and crustacean exoskeletons) achieve high toughness (energy term) magnitudes of times higher than their mineral constituents (e.g.: calcium carbonate, hydroxyapatite) (Figure. 1) [3-6]. The amplification of toughness originates from the well-optimized hierarchical architectures of these biological materials. The hierarchical architectures are usually made of hard mineralized building blocks (e.g.: tablet, lamella, fiber) and ductile organic interfaces arranged in an ordered structure (e.g.: staggered, cross-ply, Bouligand, etc.) [7]. The synergies between hard building blocks and ductile organic interfaces in the hierarchical structures triggers various toughening mechanisms such as crack deflection, crack bridging and interfacial sliding. Many tough biological materials (e.g.: teeth of deep-sea fish) are also highly transparent despite having complex multiphase microstructures [8, 9].

Figure 1: (a) Design concepts of dense architectured materials. (b) Toughness and Young’s modulus of hard biological materials compared to pure minerals.


Hard biological materials provide interesting templates for us to overcome the brittleness of transparent ceramics. However, it has been a challenge to generate highly controlled material architectures in large volumes and duplicate the toughening mechanisms of biological materials [10]. In addition, achieving high transparency for bulk architectured materials is even more challenging due to the presence of complex microscale architectures [11-13]. Many fabrication methods have been explored including freeze casting, vacuum filtration, additive manufacturing, 3D laser engraving, etc. However, many of these fabrication methods still have limitations on structural control, cost-efficiency, and the ability to duplicate the toughening mechanisms of biological materials. Identifying the primary toughening mechanisms in biological templates should be one of the keys to simplify the design and fabrication of the bio-inspired architectured materials. 

In this post, structure and mechanics of selected hard biological materials will be discussed first, followed by discussions on our works on toughening glass with laser engraved bio-inspired architectures as well as other recent studies on developing transparent architectured ceramics. 


2. Hard Biological Materials

Structure, composition and mechanics of hard biological materials vary depending on species. Hard biological structures and materials usually combine various types of architectures to simultaneously achieve high stiffness, strength and toughness. The discussion here selects architectures that contribute to the toughness of hard biological materials. A recent study on a transparent hard biological material is also discussed. 


Figure 2: Architectures in hard biological materials. (a) Brick-and-mortar structure in nacre [14]. (b) Hierarchical cross-ply structure in conch shell [5, 15]. (c) Decussation zone in tooth enamel [16, 17]. (d) Helicoidal (Bouligand) structure in Stomatopod dactyl club [18]. The club is divided into: the impact region (blue), the medial periodic region (red), the lateral periodic region (yellow), and the striated region (green). (e) Sutured structures in various biological systems [19-22].


2.1 Brick-and-mortar structure

Abalone shells are tough bio-ceramics that serve as the protective armor of abalones. These shells consist of an outer prismatic calcite layer and an inner nacreous layer (Figure. 2a) [14, 23]. The stiff prismatic layer prevents external penetration, but they are prone to brittle failure. Despite of high mineral content (95 vol%), the nacreous layer (nacre) is relatively softer and much tougher (Figure. 2a) that hinders the crack propagation and keep the shell integration when the prismatic layer cracks. Nacre has a brick-and-mortar structure where polygonal aragonite tablets are bonded by biopolymer interfaces (Figure. 1c). Under tension, these mineral tablets slide on each other over large volumes (Figure. 2a), a mechanism mediated by the shearing of the ductile organic interfaces [14]. The organic interfaces are highly deformable and have low strength to ensure that deformation and cracking occur at the interfaces. The sliding mechanism dissipates large amounts of mechanical energy and leads to crack bridging and process-zone toughening [24, 25]. Local strain hardening mechanisms at the interfaces such as the viscoplastic deformation of organic interfaces, tablet waviness, mineral bridges and nano-asperities prevent excessive local tablet sliding and failure so that the deformation can spread over large volumes [26]. 


2.2 Cross-ply structure

Cross-ply structure can be found in many hard biological materials such as conch shell [15], tooth enamel [17] and fish scale [27]. Conch shell has a hierarchical cross-lamellar (ply) structure, consisting three lamellar orders (Figure. 2b). The weak interfaces channel cracks (Figure. 2b), triggering crack bridging by the uncracked lamellae [15, 28]. The uncracked lamellae also deconcentrate stresses near the crack tip, hindering crack propagation [29]. Crack bridging and stress deconcentration significantly increase the toughness despite the high mineral content of about 99 vol% aragonite. For tooth enamel (Figure. 2c), the outer region consists of prismatic hydroxyapatite rods that provides hardness and stiffness. These prismatic rods turn into decussation (a cross-ply structure) in the inner enamel [17]. The decussation deflects cracks from enamel surface into weak protein interfaces, causing stable crack growth, which is similar to the toughening mechanisms in conch shells. 


2.3 Bouligand structure

Bouligand structure can be found in many hard biological materials including fish scales [30] and arthropod exoskeletons.  One of the most famous examples would be the dactyl club of mantis shrimps (stomatopods).  The dactyl club of Stomatopods is a highly mineralized multiphase composite consisting of hydroxyapatite, calcium phosphate and carbonate, and chitin fibrils (as the organic matrix), and it can be divided into several regions depending on the local micro-/nano-architectures (Figure. 2d) [18]. The outermost layer has a high content of oriented (prismatic) crystalline hydroxyapatite that provides high surface hardness [18]. A recent study by Huang et al. [31] shows that under high-strain-rate impact, the outermost layer serves as the impact resistant coating by breakage/rotation/translation of meso-crystalline hydroxyapatite nanoparticles and by dislocation/amorphization of the nanocrystalline network. The function of the inner periodic region is to provide toughness and absorb energy by the Bouligand architecture constructed from mineralized chitin fibrils [18]. The Bouligand structure causes nested and twisted microcracks (Figure. 2D). The nucleation and growth of these microcracks without crack coalescence dissipate energy and lead to stress relaxation [32, 33]. In the Bouligand architecture, the pitch angle is one of the most important geometrical parameter. Larger pitch angle is preferred so that higher degree of crack twisting can be achieved to provide higher fracture resistance. However, the pitch angle being too large will result in fiber breakage and delamination that reduce the mechanical performances [33, 34].


2.4 Sutured structure

As mentioned previously in the discussion of nacre, tablet waviness provides progressive locking and hardening that delays strain localization and spread inelastic deformation over large volumes. Using similar concepts, in many biological materials, sutured interfaces with complex geometries and re-entrant features can be found to channel large deformation and dissipate energy. The morphologies of sutured interfaces vary depending on species (Figure. 2e). In general, sutured interfaces toughen the material through friction, interlocking, and channeling crack propagation. The interlocking geometry can particularly increase strength in addition to energy dissipation and provide hardening for spreading toughening mechanisms through large volumes [35, 36].


2.5 Tough transparent biological composites

Despite having complex multiphase micro-/nano-architectures, many hard biological materials such as animal lens [8] and teeth of deep-sea fish are transparent [9]. A recent study by Velasco-Hogan et al. [9] investigated the nature of the transparent teeth of deep-sea dragonfish (Figure. 3). The transparency and reduced scattering are caused by the absence of microscale features such as dentin tubules. The nanoscale structure of high content of hydroxyapatite and reduced amount of collagen (compared to other animal teeth) is much smaller than the interacting light wavelength, allowing light to pass through and leading to reduced Rayleigh scattering. In addition, the Rayleigh scattering is further reduced by the sufficiently thin teeth (~60 µm). These features indicate that to develop highly transparent architectured materials, structural features at microscale should be reduced or even completely removed, and higher content of hard mineral ingredients (glass and ceramics) is preferred. 

Figure 3: Transparent teeth of deep-sea dragonfish. (a) Visual appearance. (b) Light transmittance.


3. Transparent architectured ceramics

One of the most important aspects of developing transparent architectured materials or any architectured materials in general is the fabrication method. Without suitable fabrication methods, all the designs and concepts only look beautiful on paper. There have been decades of research efforts to fabricate highly controlled bio-inspired material architectures in large volumes but it still remains a challenge. Making transparent dense architectured ceramics is even more challenging. Most of these transparent ceramics are either thin-film materials or have relatively low structural control.

In general, the fabrication methods can be classified into bottom-up methods, where disordered ingredients are assembled into ordered structure, top-down methods, where ordered structures are generated within bulk, and hybrid methods combining the two [10]. This section discusses several recently developed methods to make transparent dense architectured materials, from bottom-up methods to top-down methods. 


3.1 Vacuum filtration, sintering and polymer infiltration

Margrini et al. [12] recently developed a nacre-inspired glass composite through vacuum-aided filtration of glass flakes, compaction, sintering and then infiltration by a refractive-index matching polymer (PHN:PMMA) (Figure. 4a). The nacre-inspired glass composite achieves high strength (Figure. 4b) and improved fracture toughness with a rising R-curve (Figure. 4c). The primary toughening mechanism is crack deflection by the glass/polymer interfaces (Figure. 4d), which leads to stable crack growth. One of the advantages of this nacre-inspired composite is that the fabrication protocol is relatively simple and straightforward. However, its relatively limited structural control and the presence of microarchitectures cause reduced light transmittance and increased scattering (Figure. 4e, f). In addition, the relatively stiff polymer matrix favors high strength but does not favor the sliding of glass flakes, so that only crack deflection is triggered, and the toughening mechanism is localized (Figure. 4d). Vacuum filtration is also used in making transparent nano-clay films [37, 38] and cellulose paper [39, 40], but these materials are usually in the form of thin films.

Figure 4: The nacre-inspired glass made of glass flakes and PMMA. (a) Fabrication protocol using vacuum-aided filtration and sintering. (b) Force-displacement curves under three-point bending. (c) Crack growth resistance curve. (d) Crack deflection. (e) Light transmittance. (f) Photographs of the glass composite under light from above and from below. 


3.2 Biosynthesis

Guan et al.  [41] recently reported a biosynthesis method to fabricate nacre-inspired nano-clay/cellulose composite films (Figure. 5a). Nano-clay aerosol is sprayed uniformly to a thin layer of bacteria cellulose (BC) formed by Gluconacetobacter xylinus during fermentation, which gradually result in a nano-clay/BC hybrid hydrogel. The hybrid hydrogel is then hot pressed into thin nanocomposite films that have a “brick-and-fiber” structure (Figure. 5b).  The nanocomposite films exhibit very high strength and decent deformability (Figure. 5c), which indicates very high work of fracture. Nano-clay platelets separate the bundles of BC fibers that leads to increased strength by deconcentrating stresses and reducing defect size of BC fiber networks, and increased work of fracture by allowing more slippage between fibers and nano-clay platelets. Being very thin, the nanocomposite film shows relatively high light transmittance. 

Figure 5: Nacre-inspired nanocomposite films of nano-clay platelets and bacteria cellulose (BC). (a) The fabrication protocol. (b) Top-down (left) and cross-section (right) of the nano-clay/BC nanocomposite film. (c) Tensile stress-strain curves of the film. (d) BC nanofiber bundles are separated by nano-clay platelets during biological fermentation. (e) Light transmittance and haze. (f) Visual appearance of the nanocomposite film. 


3.3 Additive manufacturing

Glass and other transparent ceramics are known to be difficult to be 3D printed [13]. Early approaches such as fused deposition modeling (FDM) of molten soda-lime glass [42] and selective laser melting (SLM) of glass filaments [43] require high temperature (around 1000 ℃) to melt glass and generate rough surface. The resulted 3D printed glasses are not transparent. Nguyen et al. [44] reported a direct ink writing method using silica-filled ink (Figure. 6a). The content of silica loading and the thermal processing (drying and sintering) are carefully tuned to generate transparent 3D printed glass without crack formation and organic contamination (Figure. 6b). Stereolithography printing using a mixture of ultraviolet curable monomer and amorphous silica nanoparticles were proposed by Kotz et al. [13]. The printed polymerized composite are sintered at high temperature to have a transparent 3D printed fused silica glass (Figure. 6c). This method shows high feature resolution (Figure. 6d) and the ability to achieve high transparency (Figure. 6e). Another stereolithography printing method using bi-continuous phase separating resins (organic polymer and pre-ceramic polymer) was also recently reported [45]. This method also is capable of generating complex architectures with high resolution and high transparency. In general, additive manufacturing of glass has high structural control that can produce highly controlled complex architectures. However, state-of-the-art 3D printed glasses are still brittle materials.

Figure 6: (a) The fabrication protocol of 3D printed glass using direct ink writing. (b) Thermal processing of the 3D printed glass (direct ink writing) to achieve crack-free, transparent glass. (c) Fabrication of fuse silica glass using stereolithography. (d) Demonstration of feature resolution and structure quality of stereolithography. (e) Light transmittance of the 3D printed fused silica glass using stereolithography.


3.4 Laser engraving

Our group proposed a method to generate highly controlled 3D architectures in glass using high precision 3D laser engraving (Figure. 7a) [16]. An ultraviolet laser beam is focused within glass to generate microdefects at predefined locations. Arrays of these microdefects form weak interfaces, defining 2D or 3D architectures. Resolution and toughness of the laser engraved weak interfaces can be tuned by laser power and defect spacing (Figure. 7b, c). The weak interfaces can guide crack propagation into toughening configurations through tuning the interfacial toughness (Figure. 7d). The laser engraving method can generate highly controlled complex architectures in high resolution without any high temperature thermal processing that is time consuming and requires large amounts of energy.

Figure 7: Top-down fabrication with laser engraving. (a) Generating controlled weak interfaces using 3D laser engraving. (b) Effects of laser power on the size of the microdefects. (c) Effects of defect spacing on the interfacial toughness. (d) Crack deflection with the laser engraved weak interfaces. 


A variety of architectures to toughen glass have been explored with the help of the laser engraving method. Early works focused on 2D architectures such as sutured (Figure. 8a) and nacre-inspired bowtie structure (Figure. 8d), engraved on single glass sheet. The jigsaw-like sutured structure toughens the glass by suture pull-out that triggers interlocking and dissipate energy through friction (Figure. 8b) [16]. Models and experiments [35, 36] further reveals that to maximize stiffness, strength and energy absorption, low coefficients of friction and high interlocking angles are preferred to respectively minimize stresses near frictional contact and increase mechanical resistance to pull-out. Infiltrating the sutured interface with polymer adhesives also improve the strength of the sutured structured glass (Figure. 8c). The bowtie structure inspired by tablet waviness in nacre can also improve energy absorption and deformability of glass under tension. The interlocking between bowtie tablets trigger hardening at the interfaces that spread tablet sliding over large volumes (Figure. 8e). Weak interfaces combined with interlocking mechanisms improves fracture toughness through crack deflection and crack branching. In general, the limitations of laser engraved 2D architectured glass are their low strength and weak resistance to transverse loadings.   

Figure 8: 2D architectured glass by laser engraving. (a) Sutured design. (b) Sutured structures under mode-I fracture. (c) Sutured structures under tension. (c) 2D nacre-inspired design with bowtie tablets. (d) Delocalized deformation and tablet pull-out failure mode of 2D nacre-inspired structures (bowtie tablets) under tension. (e) Crack deflection and crack branching in 2D nacre-inspired structures.


Generating highly controlled 3D architectures with laser engraving can be challenging because in fabrication, it is difficult to have weak enough interfaces while keeping the integrity of engraved glass and fixing the positions of building blocks in 3D space. The topologically interlocked structure (Figure. 9a) adds geometrical variations of the building blocks in the transverse direction, triggering interlocking mechanisms when the structure is confined by in-plane compressions [46-49]. The topologically interlocked designs of building blocks include truncated tetrahedra, octahedra, rhombohedron and many others [47, 48]. In general, the topologically interlocked structures have non-linear deformation, progressive and confined damage that completely change the way glass deforms and fails (Figure. 9b). The energy is dissipated through friction at the interfaces between building blocks and catastrophic failure is prevented by segmented building blocks that deconcentrates stresses [47-49]. Without the need to add a second polymer phase at the interfaces, the topologically interlock structures are suitable for high temperature applications. However, the limitation is that in-plane confinements are required to keep the integrity of the structure.

Another type of 3D architectures for transparent ceramics we have explored is the architectured laminated glass (Figure. 9c) where ductile thermoplastic polymers (Surlyn and EVA) are used to bind building blocks and provide energy dissipation through viscoplastic deformation [11, 29]. To keep the integrity of engraved glass sheets and fix the predefined positions of building blocks, a temporary polyimide film is attached to the engraved sheet before lamination and rigid confinement frames are applied during the lamination . This method can generate highly controlled 3D architectures at meso-scale (Figure. 9d, h). The “trick” we use for obtaining high transparency for architectured laminated glass is to optimize the architectures at meso-scale (10^2-10^3 µm) instead of micro-scale. In this way, light only gets scattered at the thin interfaces (10^0-10^1 µm) between adjacent building blocks within each layer, which only accounts for a small fraction of the total volumes of the glass panel.

Using this fabrication protocol for architectured laminated glass, two-layer cross-ply glass that has high transparency (Figure. 9e) were developed [29]. The cross-ply glass can have significantly improved deformability and energy absorption (up to 100 times) compared to plain laminated glass (Figure. 9f). The high deformability and energy absorption are achieved by delocalized sliding and large rotation of glass plies, which can be controlled by the ply orientation angle (the dominant parameter) and ply width. Under mode-I fracture (Figure. 9g), the cross-ply glass shows stable crack growth and achieve significantly improved resistance to both crack initiation (stress intensity, up to 4 times) and crack propagation (fracture energy, up to 50 times). The amplified fracture resistance is resulted by a variety of toughening mechanisms similar to the ones in conch shells, including stress deconcentration and crack bridging by uncracked plies near the crack tip, crack deflection, crack branching and viscoplastic shear deformation of the EVA interlayer. To achieve high puncture resistance, Multi-layer nacre-like laminated glass has also been developed (Figure. 9h) (Video 1). In contrast to the brittle behavior of monolithic glass and plain laminated glass, the nacre-like glass panels show delocalized inelastic deformation by tablet sliding and progressive failure (Figure. 9i). To prevent penetration and to improve stiffness and strength, we combined outer plain layers and inner nacre-like layers into hybrid structures, similar to the prismatic and nacreous layer in abalone shells and in many other biological materials. The hybrid structures achieve a combination of high stiffness, strength and energy absorption (Figure. 9i). Under high-strain-rate impact, the nacre-like glass panels have similar deformation and failure mechanisms as in quasi-static puncture, outperforming other transparent materials including plain laminated glass and tempered glass by two-fold [11].  The limitation of architectured laminated glass is that it can not be used in high temperature where the thermoplastic polymer will be softened or even melted.

3D laser engraving provides an effective and relatively fast method to generate highly controlled 2D and 3D architectures for transparent ceramics. However, one of the present challenges is that time consumption of the fabrication process is directly influenced by the moving speed of the laser, and scale cubically with ceramic volumes. Another challenge is that the weak interface by laser engraving is at micro-scale that still scatters light and reduce transparency if the building blocks get smaller. 

Figure 9: 3D architectured glass by laser engraving. (a) Design and (b) impact performances of topologically interlocked glass panels. (c) The fabrication protocol of architectured laminated glass using laser engraving and pressed lamination. (d) The engraved glass sheet is attached to a polyimide film to fix the positions of glass building blocks during lamination. (e) Light transmittance of two-layer cross-ply glass. (f) Tensile behaviors of two-layer cross-ply glass. (g) Mode-I fracture of plain laminated glass and cross-ply glass. (h) Light transmittance of ten-layer nacre-like (hexagonal tablet) glass panels, and the design of tablet geometry and arrangement. (i) Quasi-static puncture of nacre-like glass panels.


4. Challenges and outlook

One of the challenges of developing tough transparent ceramics is to find a fabrication method that can balance transparency, structural control, energy and time consumption. One of the keys may lie on identifying the deciding toughening mechanisms so that the architectures can be simplified. It requires joint research efforts and interdisciplinary collaborations from the fields of solid mechanics, material science, chemistry, optics and many others.

Another interesting point is that utilizing the synergies between mechanically dissimilar components to achieve high toughness is not only used in ceramics but also in polymers (e.g.: semi-crystalline polymers, double network hydrogels) and metals (e.g.: Damascus steel). Some of the findings in tough bio-inspired ceramics may inspire other fields as well. 


Thansk for reading! Have fun and please leave your comments if you want to join the discussion! 


Related journal clubs:

June 2017, 3D-printing biomimetic structures to reveal the mechanics of natural systems, Michael M Porter


Bonus pictures:

Two cross-ply glass panels (natural light), photo credit: Zhen Yin


A nacre-like glass panel and flowers (natural light), photo credit: Zhen Yin


A nacre-like glass panel resting on a wood chair (natural light), photo credit: Zhen Yin


Gathering at the sea floor, Abalone shell, striped bass, and mantis shrimp. Painting by Zhen Yin



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Great work! 

I cannot resist to suggest you to watch this talk by Prof. Krishnamurthy, where he talks about technique to generate various interlocking topologies (Video link). I think it might be helpful, not sure. I am not familiar with either of the research areas, however, this appears to me as a connecting link. 


Zhen Yin's picture

Thank you Nitesh! I just got time to go through the video. The video your suggested is very helpful especially on the generation of 3D interlocked topologies. Although I did not invovle too much on this research topic, Prof. Francois Barthelat's group is working quite a lot on the fabrication and mechanics of topologically interlocked structures (by Aram Bahmani, Ahmed Dalaq and Mohammad Mirkhalaf Valashani). I think Prof. Krishnamurthy is exploring more types of toplogies than we are but we are exploring different techniques to fabricate toplogically interlocked materials. There might be some collaboration opportunites.

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