Crystal Phases and Thermal Stability of Co-evaporated CsPbX3 (X = I, Br) Thin Films.

We present the growth, phase transitions, and thermal decomposition of CsPbX3 (X = I, Br) thin films monitored by in situ X-ray diffraction (XRD). The perovskite films are prepared in vacuum via co-evaporation of PbX2 and CsX (X = I, Br) onto glass substrates. In situ X-ray diffraction allows the observation of phase transitions and decomposition while the samples are heated with a linear temperature ramp. Our experiments reveal the decomposition route for the CsPbX3 perovskites in high vacuum, with a much higher stability than their hybrid organic-inorganic MAPbX3 counterparts. We also observe the response of a black CsPbI3 thin film to exposure to ambient air at room temperature using the same XRD system. Exposing the black CsPbI3 to ambient air leads to the formation of yellow orthorhombic δ-CsPbI3, whose crystal structure could be identified by its X-ray diffraction pattern. Additionally, the linear coefficients of expansion are determined for δ-CsPbI3 and the (020)-orientation of CsPbBr3.

Monitoring the Phase Formation of Coevaporated Lead Halide Perovskite Thin Films by in Situ X-ray Diffraction.

Perovskite solar cells based on (CH3NH3)Pb(I,Cl)3 have recently demonstrated rapidly increasing cell efficiencies. Here, we show progress identifying phases present during the growth of (CH3NH3)Pb(I,Cl)3 perovskite thin films with the vacuum-based coevaporation approach using two sources under varying deposition conditions. With in situ X-ray diffraction, crystalline phases can be identified and monitored in real time. For different (CH3NH3)I-to-PbCl2 flux ratios, two distinct (CH3NH3)Pb(IxCl(1-x))3 phases with high (x > 0.95) and with lower (x < 0.5) iodine content as well as a broad miscibility gap in-between were found. During post deposition annealing we observe recrystallization and preferential orientation effects and finally the decomposition of the perovskite film to PbI2 at temperatures above 200 °C.

The irradiation action on human dental tissue by X-rays and electrons--a nanoindenter study.

It is known that ionizing radiation is used in medicine for Roentgen diagnostics and for radiation therapy. The radiation interacts with matter, in particular with biological one, essentially by scattering, photoelectric effect, Compton effect and pair production. To what extent the biological material is changed thereby, depends on the type and the amount of radiation energy, on the dose and on the tissue constitution. In modern radiation therapy two different kinds of radiation are used: high energy X-rays and electron radiation. In the case of head-neck tumors the general practice is an irradiation with high energy X-rays with absorbed dose to water up to 70 Gy. Teeth destruction has been identified as a side effect during irradiation. In addition, damage to the salivary glands is often observed which leads to a decrease or even the complete loss of the salivary secretion (xerostomia). This study shows how the different energy and radiation types damage the tooth tissue. The effects of both, high X-ray energy and high energy electrons, on the mechanical properties hardness and elasticity of the human dental tissue are measured by the nanoindentation technique. We compare these results with the effect of the irradiation of low X-ray energy on the dental tissue.

Effect of tumor therapeutic irradiation on the mechanical properties of teeth tissue.

Tumor irradiation of the head-neck area is accompanied by the development of a so-called radiation caries in the treated patients. In spite of conservative therapeutic measures, the process results in tooth destruction. The present study investigated the effects of irradiation on the demineralization and remineralization of the dental tissue. For this purpose, retained third molars were prepared and assigned either to a test group, which was exposed to fractional irradiation up to 60 Gy, or to a non-irradiated control group. Irradiated and non-irradiated teeth were then demineralized using acidic hydroxyl-cellulose gel; afterwards the teeth were remineralized using either Bifluorid12 or elmex gelee. The nanoindentation technique was used to measure the mechanical properties, hardness and elasticity, of the teeth in each of the conditions. The values were compared to the non-irradiated control group. Irradiation decreased dramatically the mechanical parameters of enamel and dentine. In nonirradiated teeth, demineralization had nearly the same effects of irradiation on the mechanical properties. In irradiated teeth, the effects of demineralization were negligible in comparison to non-irradiated teeth. Remineralization with Bifluorid12 or elmex gelee led to a partial improvement of the mechanical properties of the teeth. The enamel was more positively affected by remineralization than the dentine.

Assessment of composition and anisotropic elastic properties of secondary osteon lamellae.

Measurement of the elastic properties of single osteon lamellae is still one of the most demanding tasks in bone mechanics to be solved. By means of site-matched Raman microspectroscopy, acoustic microscopy and nanoindentation the structure, chemical composition and anisotropic elasticity of individual lamellae in secondary osteons were investigated. Acoustic impedance images (911-MHz) and two-dimensional Raman spectra were acquired in sections of human femoral bone. The samples were prepared with orientations at various observation angles theta relative to the femoral long axis. Nanoindentations provided local estimations of the elastic modulus and landmarks necessary for spatial fusion of the acoustic and spectral Raman images. Phosphate nu(1) (961 cm(-1)) and amide I (1665 cm(-1)) band images representing spatial distributions of mineral and collagen were fused with the acoustic images. Acoustic impedance was correlated with the indentation elastic modulus E(IT) (R(2)=0.61). Both parameters are sensitive to elastic tissue anisotropy. The lowest values were obtained in the direction perpendicular to the femoral long axis. Acoustic images exhibit a characteristic bimodal lamellar pattern of alternating high and low impedance values. Since this undulation was not associated with a variation of the phosphate nu(1)-band intensity in the Raman images, it was attributed to variations of the lamellar orientation. After threshold segmentation and conversion to elastic modulus the orientation and transverse isotropic elastic constants were derived for individual ensembles of apparent thin and thick lamellae. Our results suggest that this model represents the effective anisotropic properties of an asymmetric twisted plywood structure made of transverse isotropic fibrils. This is the first report that proves experimentally the ability of acoustic microscopy to map tissue elasticity in two dimensions with micrometer resolution. The combination with Raman microspectroscopy provides a unique way to study bone and mineral metabolism and the relation with mechanical function at the ultrastructural tissue level.