Characterization of the hierarchical architecture and micromechanical properties of walnut shell (Juglans regia L.).

In the present work a comprehensive characterization of the hierarchical architecture of the walnut shell (Juglans regia L.) was carried out using scanning electron microscopy (SEM), atomic force microscopy (AFM) and confocal laser scanning microscopy (CLSM). Furthermore, micromechanical properties (hardness, HIT and elastic modulus, EIT) of plant tissues were evaluated at cell wall level by applying the instrumented indentation technique (IIT). The complex architecture of the material was described in terms of four hierarchical levels (HL): endocarp (H1), plant tissues (H2), plant cells (H3) and cell wall (H4). Our findings revealed that the walnut shell consists of a multilayer structure (sclerenchyma tissue, ST; interface tissue, IT; porous tissue, PT; and flattened parenchyma tissue, FPT), where differences in the microstructure and composition of plant tissues generate parallel gradients along the cross-section. The indentation tests showed a functional gradient with a sandwich-like configuration, i.e., a lightweight and soft layer (PT, HIT = 0.04 GPa) is located between two dense and hard layers (ST, HIT = 0.33 GPa; FPT, HIT = 0.28 GPa); where additionally there is an interface between ST and PT (IT, HIT = 0.16 GPa). This configuration is a successful strategy designed by nature to improve the protection of the kernel by increasing the strength of the shell. Therefore, the walnut shell can be considered as a functionally graded material (FGM), which can be used as bioinspiration for the design of new functional synthetic materials. In addition, we proposed some structure-property-function relationships in the whole walnut shell and in each of the plant tissues.

Morphological and micromechanical characterization of calcium oxalate (CaOx) crystals embedded in the pecan nutshell (Carya illinoinensis).

The morphology and micromechanical properties of the mineral crystals embedded in the pecan nutshell (Carya illinoinensis) were characterized. Qualitative and quantitative morphological analyses carried out revealed that the crystals were comprised of calcium oxalate (CaOx) and have a wide range of sizes, with prismatic shapes, distributed heterogeneously in the sclerenchyma tissue. From indentation tests, it was found that CaOx crystals are stiffer structures compared to stone cells (sclerenchyma tissue), showing hardness and elastic modulus values of 0.53 ±â€¯0.19 GPa and 9.4 ±â€¯1.80 GPa, respectively. Additionally, the values of fracture toughness (0.08 ±â€¯0.02 MPa m0.5) and the brittleness index (9336 m-0.5) revealed that these types of structures are extremely brittle. The results obtained suggest that the main function of the CaOx crystals is to provide structural support to tissue. The presented methodology demonstrates the potential of the instrumented indentation technique (IIT) for in situ micromechanical characterization of mineral crystals located in plant tissues.