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In biomineralized tissues such as bone, the recurring structural motif at the supramolecular level is an anisotropic stiff inorganic component reinforcing the soft organic matrix. The high toughness and defect tolerance of natural biomineralized composites is believed to arise from these nanometer scale structural motifs. Specifically, load transfer in bone has been proposed to occur by a transfer of tensile strains between the stiff inorganic (mineral apatite) particles via shearing in the intervening soft organic (collagen) layers. This raises the question as to how and to what extent do the mineral particles and fibrils deform concurrently in response to tissue deformation. Here we show that both mineral nanoparticles and the enclosing mineralized fibril deform initially elastically, but to different degrees. Using in situ tensile testing with combined high brilliance synchrotron X-ray diffraction and scattering on the same sample, we show that tissue, fibrils, and mineral particles take up successively lower levels of strain, in a ratio of 12:5:2. The maximum strain seen in mineral nanoparticles (∼0.15-0.20%) can reach up to twice the fracture strain calculated for bulk apatite. The results are consistent with a staggered model of load transfer in bone matrix, exemplifying the hierarchical nature of bone deformation. We believe this process results in a mechanism of fibril-matrix decoupling for protecting the brittle mineral phase in bone, while effectively redistributing the strain energy within the bone tissue.

Understanding the assembly of nanoparticles into superlattices with well-defined morphology and structure is technologically important but challenging as it requires novel combinations of in-situ methods with suitable spatial and temporal resolution. In this study, we have followed evaporation-induced assembly during drop casting of superparamagnetic, oleate-capped γ -Fe 2 O 3 nanospheres dispersed in toluene in real time with Grazing Incidence Small Angle X-ray Scattering (GISAXS) in combination with droplet height measurements and direct observation of the dispersion. The scattering data was evaluated with a novel method that yielded time-dependent information of the relative ratio of ordered (coherent) and disordered particles (incoherent scattering intensities), superlattice tilt angles, lattice constants, and lattice constant distributions. We find that the onset of superlattice growth in the drying drop is associated with the movement of a drying front across the surface of the droplet. We couple the rapid formation of large, highly ordered superlattices to the capillary-induced fluid flow. Further evaporation of interstitital solvent results in a slow contraction of the superlattice. The distribution of lattice parameters and tilt angles was significantly larger for superlattices prepared by fast evaporation compared to slow evaporation of the solvent.

The plasma protein fetuin-A/alpha2-HS-glycoprotein (genetic symbol Ahsg) is a systemic inhibitor of extraskeletal mineralization, which is best underscored by the excessive mineral deposition found in various tissues of fetuin-A deficient mice on the calcification-prone genetic background DBA/2. Fetuin-A is known to accumulate in the bone matrix thus an effect of fetuin-A on skeletal mineralization is expected. We examined the bones of fetuin-A deficient mice maintained on a C57BL/6 genetic background to avoid bone disease secondary to renal calcification. Here, we show that fetuin-A deficient mice display normal trabecular bone mass in the spine, but increased cortical thickness in the femur. Bone material properties, as well as mineral and collagen characteristics of cortical bone were unaffected by the absence of fetuin-A. In contrast, the long bones especially proximal limb bones were severely stunted in fetuin-A deficient mice compared to wildtype littermates, resulting in increased biomechanical stability of fetuin-A deficient femora in three-point-bending tests. Elevated backscattered electron signal intensities reflected an increased mineral content in the growth plates of fetuin-A deficient long bones, corroborating its physiological role as an inhibitor of excessive mineralization in the growth plate cartilage matrix--a site of vigorous physiological mineralization. We show that in the case of fetuin-A deficiency, active mineralization inhibition is a necessity for proper long bone growth.

Muscle contraction is driven by the motor protein myosin II, which binds transiently to an actin filament, generates a unitary filament displacement or ‘working stroke’, then detaches and repeats the cycle. The stroke size has been measured previously using isolated myosin II molecules at low load, with rather variable results 1 , 2 , 3 , 4 , but not at the higher loads that the motor works against during muscle contraction. Here we used a novel X-ray-interference technique 5 , 6 to measure the working stroke of myosin II at constant load 7 in an intact muscle cell, preserving the native structure and function of the motor. We show that the stroke is smaller and slower at higher load. The stroke size at low load is likely to be set by a structural limit 8 , 9 ; at higher loads, the motor detaches from actin before reaching this limit. The load dependence of the myosin II stroke is the primary molecular determinant of the mechanical performance and efficiency of skeletal muscle.

Muscles generate force and shortening in a cyclical interaction between the myosin head domains projecting from the myosin filaments and the adjacent actin filaments. Although many features of the dynamic performance of muscle are determined by the rates of attachment and detachment of myosin and actin 1 , the primary event in force generation is thought to be a conformational change or ‘working stroke’ in the actin-bound myosin head 2 , 3 , 4 , 5 , 6 , 7 , 8 . According to this hypothesis, the working stroke is much faster than attachment or detachment, but can be observed directly in the rapid force transients that follow step displacement of the filaments 3 . Although many studies of the mechanism of muscle contraction 9 , 10 , 11 , 12 , 13 have been based on this hypothesis, the alternative view—that the fast force transients are caused by fast components of attachment and detachment 14 , 15 , 16 , 17 —has not been excluded definitively. Here we show that measurements of the axial motions of the myosin heads at ångström resolution by a new X-ray interference technique 18 rule out the rapid attachment/detachment hypothesis, and provide compelling support for the working stroke model of force generation.

The assembly of tiny magnetic particles in external magnetic fields is important for many applications ranging from data storage to medical technologies. The development of ever smaller magnetic structures is restricted by a size limit, where the particles are just barely magnetic. For such particles we report the discovery of a kind of solution assembly hitherto unobserved, to our knowledge. The fact that the assembly occurs in solution is very relevant for applications, where magnetic nanoparticles are either solutionprocessed or are used in liquid biological environments. Induced by an external magnetic field, nanocubes spontaneously assemble into 1D chains, 2D monolayer sheets, and large 3D cuboids with almost perfect internal ordering. The self-assembly of the nanocubes can be elucidated considering the dipole–dipole interaction of small superparamagnetic particles. Complex 3D geometrical arrangements of the nanodipoles are obtained under the assumption that the orientation of magnetization is freely adjustable within the superlattice and tends to minimize the binding energy. On that basis the magnetic moment of the cuboids can be explained.

The molecular mechanism of muscle contraction was investigated in intact muscle fibres by X-ray diffraction. Changes in the intensities of the axial X-ray reflections produced by imposing rapid changes in fibre length establish the average conformation of the myosin heads during active isometric contraction, and show that the heads tilt during the elastic response to a change in fibre length and during the elementary force generating process: the working stroke. X-ray interference between the two arrays of myosin heads in each filament allows the axial motions of the heads following a sudden drop in force from the isometric level to be measured in situ with unprecedented precision. At low load, the average working stroke is 12 nm, which is consistent with crystallographic studies. The working stroke is smaller and slower at a higher load. The compliance of the actin and myosin filaments was also determined from the change in the axial spacings of the X-ray reflections following a force step, and shown to be responsible for most of the sarcomere compliance. The mechanical properties of the sarcomere depend on both the motor actions of the myosin heads and the compliance of the myosin and actin filaments.

Structural ordering in the concentrated magnetic colloids containing 50 × 5 nm hard magnetic disc-like SrFe 12 O 19 nanoparticles was investigated by cryogenic scanning electron microscopy, optical microscopy, magnetic measurements, and small-angle X-ray scattering. It was revealed that macroscopically homogeneous magnetic liquid consists of dynamic threads of stacked nanoparticles. The threads align into quasiperiodic arrays with the distances between individual threads of a few micrometers. They also can form pseudodomain structures with ~ 90° domain boundaries realized through T-type thread interconnects. The effects of magnetic attraction and electrostatic repulsion on the equilibrium interplatelet distance in the threads were studied. It was demonstrated that this distance can be tuned by the control of the particles charge and electric double layer screening from Stern layer thickness (~ 1 nm) to tens of nanometers. It was shown that the permanent magnetic field is not able to cause any structural changes in the ordered magnetic liquid phase, while alternating field draws particles apart by their vibrations. External variation of interparticle distance up to 6% was achieved using an alternating magnetic field of low intensity. Experimental data were complemented by the theoretical models of screened electrostatic interactions between spherical and platelike magnetic particles. The last model provides good predictive power and correlates with the experimental data. The stabilization energy of the condensed phase in the order of 1–10 k B T was derived from the model. An approach allows controlling of an equilibrium interparticle distance and interparticle distance distribution by adjusting the magnetization and surface charge of the particles as well as the ionic strength of the solvent.

Dry coir fibers are characterized by wide-angle X-ray scattering coupled with tensile tests. The fibers exhibit elastic and plastic behavior with the yield point at a strain of about 2%. In-situ experiments document that the cyclic loading and unloading beyond the yield point does not reduce the stiffness of the fibres, since they recover their initial stiffness by every increase of the strain. The diffraction data show that the microfibril angle (MFA) of cellulose fibrils in the coir fibre cells is inversely proportional to the magnitude of the applied strain. In average, the relatively high MFA of about 45° in the unstrained state decreases linearly upon straining until the fibers break at about 35% strain. When the strain is released during the tensile experiment the MFA tends to recover its original magnitude. No significant differences in the dependence of MFA on strain are detected in elastic and plastic regions, respectively. The results demonstrate that the tissue with helical architecture does not have to be saturated with water in order to exhibit the effect of the recovery of the mechanical function when cyclically loaded. This indicates differences in the architecture of the coir cell wall in comparison with that of compression wood with high MFA whereby similar phenomena were observed in the wet state.

Samples of lyocell fibres were taken in the form of filaments from fibre tow of potentially infinite length and in their final condition of staple fibres. Mechanical testing showed comparable tensile strength, but a 50% lower modulus of elasticity for staple fibres and a higher elongation at break compared to filaments from fibre tow. Structural investigation by means of synchrotron wide angle X-ray scattering and birefringence measurement revealed a significantly lower degree of preferred orientation together with less fibre straightness for staple fibres than for filaments. It is concluded that plastic deformation during the processing of staple fibres from filaments induces permanent changes in the orientation of cellulose chains in the fibres, which in turn is responsible for the observed differences in mechanical performance.