Synchrotron X-ray Diffraction Study Research Articles

In situ synchrotron X-ray diffraction study of synthesis reactions in mechanically activated Ti + Al powder mixture under linear heating conditions

In the present work, we studied the features of phase formation in mechanically activated Ti + Al powder mixture at various heating rates for the first time. The study was carried out using high-resolution diffractometry method which made it possible to study the processes of phase formation in situ at any stage of heating. It was established that ignition of the activated mixture can be initiated in the solid phase with an extremely low content of reaction products formed at the preheating stage. An increase in the heating rate leads to a decrease in the average burning rate and an increase in the ignition temperature. At high heating rates, the ignition is initiated in the presence of a liquid phase when the ignition temperatures are close to the melting temperature of aluminum. In this case, the content of reaction products formed during preheating stage is relatively high. It was found that the all main compounds presented in the equilibrium diagram of Ti-Al system are synthesized in parallel. The content of phases in the reaction products depends on the heating rate.

In-situ synchrotron X-ray diffraction study of the effects of grain orientation on the martensitic phase transformations during tensile loading at different strain rates in metastable austenitic stainless steel

In this work, in-situ high-energy X-ray diffraction was used to analyze the effects of strain rate and austenite (γ) grain orientation on the strain-induced martensitic transformation in metastable austenitic stainless steel 301LN. The diffraction measurements were carried out at strain rates ranging from 10−3 s−1 to 1 s−1 continuously without interrupting the experiment and thus creating nearly adiabatic conditions at the highest studied strain rate. The results indicate that <100>γ fiber-oriented grains preferentially transform at the strain rate of 10−3 s−1 when the true strain is above 0.10, whereas the <111>γ fiber-oriented grains transform only at later stages of plastic deformation. The phase transformation rate of the <111>γ and <100>γ fiber-oriented grains decreases with increase in strain rate. A theoretical model based on stacking fault width as a function of external stress and temperature (stacking fault energy) was used to predict lower-bound estimates for the critical tensile stress needed to start ε-martensite and α’-martensite phase transformations. The model can predict the experimentally observed phase transformation behavior of the <111>γ fiber orientations at all strain rates but is unable to predict the decrease of phase transformation rate of <100> fiber-oriented γ grains with increase in strain rate, which could be related to change in dislocation structure.

Mechanistically Guided Materials Chemistry: Synthesis of Ternary Nitrides, CaZrN2 and CaHfN2.

Recent computational studies have predicted many new ternary nitrides, revealing synthetic opportunities in this underexplored phase space. However, synthesizing new ternary nitrides is difficult, in part because intermediate and product phases often have high cohesive energies that inhibit diffusion. Here, we report the synthesis of two new phases, calcium zirconium nitride (CaZrN2) and calcium hafnium nitride (CaHfN2), by solid state metathesis reactions between Ca3N2 and MCl4 (M = Zr, Hf). Although the reaction nominally proceeds to the target phases in a 1:1 ratio of the precursors via Ca3N2 + MCl4 → CaMN2 + 2 CaCl2, reactions prepared this way result in Ca-poor materials (CaxM2-xN2, x < 1). A small excess of Ca3N2 (ca. 20 mol %) is needed to yield stoichiometric CaMN2, as confirmed by high-resolution synchrotron powder X-ray diffraction. In situ synchrotron X-ray diffraction studies reveal that nominally stoichiometric reactions produce Zr3+ intermediates early in the reaction pathway, and the excess Ca3N2 is needed to reoxidize Zr3+ intermediates back to the Zr4+ oxidation state of CaZrN2. Analysis of computationally derived chemical potential diagrams rationalizes this synthetic approach and its contrast from the synthesis of MgZrN2. These findings additionally highlight the utility of in situ diffraction studies and computational thermochemistry to provide mechanistic guidance for synthesis.

High-pressure structural behavior and elastic properties of Ce2In and Ce3In: A combined in situ synchrotron X-ray diffraction and density functional theory study

Across the cerium (Ce)-indium (In) binary phase diagram, there are five line compounds including Ce3In, Ce2In, Ce3In5, CeIn2 and CeIn3. So far, CeIn3 is the only compound whose high-pressure structural behavior and elastic properties have been studied in detail. In this work, we investigated the compression behavior of Ce3In and Ce2In at pressures up to 26.2 GPa using in situ high-pressure angle dispersive synchrotron powder X-ray diffraction (XRD). Our results indicate that Ce3In retains its Cu3Au-type structure in the pressure range investigated, whereas Ce2In undergoes a phase transformation from the Ni2In-type structure to an unidentified phase at ∼4.6 GPa. Unit-cell parameters as a function of pressure were obtained by Rietveld analysis of XRD data. Unit cell volumes were fitted to a second order Birch-Murnaghan equation of state (EOS). The experimentally determined bulk moduli (K0) of the two cerium indides are 50 ± 3 GPa for Ce3In and 39.2 ± 1.6 GPa for Ce2In. The zero-pressure compressibilites of the a-axis (βa,0) for Ce3In is 6.67 (±0.36) × 10–3 GPa–1 and of the a- and c-axis for Ce2In are βa,0 = 8.85 (±0.39) × 10−3 GPa−1 and βc,0 = 9.26 (±0.51) × 10−3 GPa−1, respectively. These results are in general agreement with those calculated by density functional theory (DFT + U) and open-source machine learning algorithms.

Freeze-Induced Phase Transition and Local Pressure in a Phospholipid/Water System: Novel Insights Were Obtained from a Time/Temperature Resolved Synchrotron X-ray Diffraction Study.

Water-to-ice transformation results in a 10% increase in volume, which can have a significant impact on biopharmaceuticals during freeze-thaw cycles due to the mechanical stresses imparted by the growing ice crystals. Whether these stresses would contribute to the destabilization of biopharmaceuticals depends on both the magnitude of the stress and sensitivity of a particular system to pressure and sheer stresses. To address the gap of the "magnitude" question, a phospholipid, 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC), is evaluated as a probe to detect and quantify the freeze-induced pressure. DPPC can form several phases under elevated pressure, and therefore, the detection of a high-pressure DPPC phase during freezing would be indicative of a freeze-induced pressure increase. In this study, the phase behavior of DPPC/water suspensions, which also contain the ice nucleation agent silver iodide, is monitored by synchrotron small/wide-angle X-ray scattering during the freeze-thaw transition. Cooling the suspensions leads to heterogeneous ice nucleation at approximately -7 °C, followed by a phase transition of DPPC between -11 and -40 °C. In this temperature range, the initial gel phase of DPPC, Lβ', gradually converts to a second phase, tentatively identified as a high-pressure Gel III phase. The Lβ'-to-Gel III phase transition continues during an isothermal hold at -40 °C; a second (homogeneous) ice nucleation event of water confined in the interlamellar space is detected by differential scanning calorimetry (DSC) at the same temperature. The extent of the phase transition depends on the DPPC concentration, with a lower DPPC concentration (and therefore a higher ice fraction), resulting in a higher degree of Lβ'-to-Gel III conversion. By comparing the data from this study with the literature data on the pressure/temperature Lβ'/Gel III phase boundary and the lamellar lattice constant of the Lβ' phase, the freeze-induced pressure is estimated to be approximately 0.2-2.6 kbar. The study introduces DPPC as a probe to detect a pressure increase during freezing, therefore addressing the gap between a theoretical possibility of protein destabilization by freeze-induced pressure and the current lack of methods to detect freeze-induced pressure. In addition, the observation of a freeze-induced phase transition in a phospholipid can improve the mechanistic understanding of factors that could disrupt the structure of lipid-based biopharmaceuticals, such as liposomes and mRNA vaccines, during freezing and thawing.

Pressure-driven structural transformation and lattice deformation in TiB reinforced titanium matrix composites: An in-situ synchrotron x-ray diffraction study

Understanding the mechanical responses of structural materials to extreme pressures has particular implication for not only their intrinsic solid properties, e.g., phase transformation, equation of state, lattice deformation, but also the mechanical engineering for extreme environments. In this work, the structural transformation of TiB reinforced Ti (Ti-TiBw) composite particles under hydrostatic, uniaxial and dynamic pressures has been comparatively investigated by diamond anvil cells combined with in-situ synchrotron x-ray diffraction. According to the variation of critical pressure of α → ω martensitic transformation, it is found that, under uniaxial pressure, the presence of nano-TiBw network could largely enhance structural resistance to deviatoric stress for the composites. A fit to the equation of state of Ti-TiBw composites under hydrostatic and uniaxial pressure yields the bulk modulus of ∼120 and ∼ 133 GPa, respectively, which increases 2.56% and 11.76% relative to pure Ti. Furthermore, the lattice deformation behaviors in Ti-TiBw composites and pure Ti during martensitic and its reversible transformation vary with pressure, deviatoric stress and compression rate. Due to the constraints by rigid TiBw network rather than “soft” grain boundary, the lattice deformation along the basal, prismatic, and pyramidal planes in Ti-TiBw system suggests an isotropic behavior, though the deviatoric strain of basal plane displays obvious dependence upon uniaxial pressure.

In situ synchrotron x-ray imaging and diffraction study of additively manufactured AlSi10Mg alloy under uniaxial tension

In situ synchrotron x-ray imaging and diffraction are used to investigate deformation dynamics in two kinds of additively manufactured AlSi10Mg with different pore configurations. The pre-existing pore configurations are characterized with synchrotron x-ray computed tomography. The specimens are subjected to tensile loading along the build direction and the longitudinal direction. Bulk stress–strain curves (macroscale), strain fields (mesoscale) and x-ray diffraction patterns (microscale) are obtained simultaneously. Scanning electron microscopy characterization is performed as a complement. For the small-pored AlSi10Mg, preferred orientations of pores lead to anisotropic ductility, and only ductile dimples are observed. For the large-pored AlSi10Mg, ductility loss is significant due to its higher porosity, and no remarkable anisotropy is found; both ductile and brittle fracture features are identified. For both types of AlSi10Mg, strain localization occurs around the pores. At the lattice scale, the Al matrix deforms plastically but the Si phase is still strained elastically, and thus, significant stress concentration occurs in the Si phase for the small-pored AlSi10Mg, while stress is more evenly partitioned between the Al matrix and the Si phase for the large-pored AlSi10Mg.

In situ Raman spectroscopy and synchrotron X-ray diffraction studies on maleic acid under high pressure conditions

Maleic acid was studied by Raman spectroscopy and powder synchrotron X-ray diffraction (XRD) under high pressure conditions by using a diamond anvil cell. The Raman spectroscopy measurements were performed from ambient pressure up to 9.2 GPa in the 100–3200 cm−1 spectral range. While the XRD measurements were performed up to 10.1 GPa. Here we present the pressure-dependence behavior from both the Raman modes and cell parameters. Maleic acid lattice parameters decrease anisotropically as a function of pressure and a reduction of 27% in the volume of the unit cell was observed. Modifications in the material’s compressibility were observed at around 2 and 6 GPa.

High-pressure structural phase transition on Bi14MoO24

In situ high-pressure powder synchrotron X-ray diffraction studies on tetragonal Bi14MoO24 have been carried out up to 11.5 GPa at room temperature. A tetragonal (I4/m) to monoclinic (C2/m) structural phase transition has been identified around 5 GPa and possible evidence for a second phase transition is observed at the highest pressure of this study. Both phase transitions are reversible upon decompression. The evolution of the lattice parameters, axial ratio, and volume under pressure have been determined for both the low pressure tetragonal and high-pressure monoclinic phases. A volume collapse of 2.7% observed at the tetragonal to monoclinic phase transition indicates it to be of first-order character. The phase transition involves a shear deformation perpendicular to the b-axis and a displacement of the Mo atoms along the b-axis. The details of the mechanism of the tetragonal-monoclinic transition are discussed. The bulk modulus of the low-pressure tetragonal and high-pressure monoclinic phases have been estimated to be 67(7) GPa and 64(3) GPa, respectively. The linear compressibilities of both phases show an anisotropic response to pressure. The obtained results are compared with the high-pressure behavior of its isomorph counterpart Bi14CrO24 and with high-temperature behavior on Bi14MoO24.

Absence of magnetostriction and transition from rapid positive thermal expansion to negative thermal expansion at high temperatures in Sm0.5Y0.5Fe0.58Mn0.42O3 – A synchrotron X-ray diffraction study

X-ray photoemission spectroscopic (XPS) studies and temperature dependent synchrotron X-ray diffraction (SXRD) investigation have been conducted on polycrystalline samples of Sm0.5Y0.5Fe0.58Mn0.42O3 [SYFM (58-42)]. Room temperature XPS measurements revealed the mixed valance of the Fe and Mn ions along with the traces of oxygen vacancies in the material. The room temperature synchrotron X-ray diffraction (SXRD) of specimen shows the monophasic nature of the prepared composition, without the presence of any magnetic or non-magnetic impurity phases. SXRD measurements at variable temperatures between 298 and 873 K, indicates the absence of magnetostriction in the specimen at the magnetic transition temperatures TSR1 ≈ 348 K, TSR2 ≈ 300 K and TN ≈ 361 K. At much higher temperatures above TN, an anisotropic rapid positive thermal expansion (RPTE) to negative thermal expansion (NTE) of the a lattice parameter of the unit cell is further revealed for T > 573 K. The anomalous variation of phonons, are suggested to give rise to anomalous thermal variation in a lattice parameter of the specimen.

Structural modulation and spin glassiness upon oxidation in oxygen storage material LnFeMnO4+x for Ln = Y, Lu, and Yb

The mixed valence multiferroic LnFe2+Fe3+O4 (where Ln = Y, Lu, and Yb) can reversibly uptake oxygen into its lattice, which is evidenced by a crystallographic phase transition along with the appearance of structural modulations. In this study, we show that the Mn-substituted version of this multiferroic can also be readily oxidized to LnFe3+Mn3+O4.5 revealing similar oxygen storage behavior. Through neutron, electron, and synchrotron x-ray diffraction studies, we observe a structural modulation that we attribute to a displacement wave in the fully oxidized compound. This wave exhibits commensurability with a wavevector q = (−2/7, 1/7, 0). Bond valence summation analysis of plausible interstitial oxygen positions suggests that oxygen insertion likely occurs at the middle of the Fe/Mn–O bipyramid layers. The structural modulation of LnFeMnO4.5 is two-dimensional, propagates along the ab-plane, and is highly symmetric as 12 identical modulation vectors are observed in the diffraction patterns. The nature of the lanthanide, Ln3+, does not seem to influence such modulations since we observe identical satellite reflections for all three samples of Ln = Y, Lu, and Yb. Both LnFeMnO4 and LnFeMnO4.5 display spin glassy behavior with 2D short-range magnetic ordering being observed in LnFeMnO4. Analysis of the neutron diffraction data reveals a correlation length of ∼10 nm. Upon oxidation to LnFeMnO4.5, the short-range magnetic order is significantly suppressed.

Role of solute in stress development of nanocrystalline films during heating: An in situ synchrotron X-ray diffraction study

The effect of the solute (Mo) on the stress development of nanocrystalline Ni and Ni–Mo films upon heating has been investigated in real time using in situ synchrotron X-ray diffraction. The complex and distinct relationship between the film stress and grain boundaries (GBs) has been examined by the evolution of real-time intrinsic stress in combination with the in situ grain growth and thermal characterizations. The different intrinsic stress evolutions in the Ni and Ni–Mo films during the heating process result from the modification of GBs by Mo alloying, including GB amorphization, GB relaxation, and GB segregation. It has been found that GBs play a vital role in the stress development of nanocrystalline films. The addition of a solute can not only inhibit grain growth but also influence the stress evolution in the film by changing the atomic diffusivity at the GBs. This work provides valuable and unique insights into the effect of solutes on stress development in nanocrystalline films during annealing, permitting control of the film stress through solute addition and heat treatment, which is critical for improving the design, processing, and lifetime of advanced nanocrystalline film devices at high temperatures.

Time and space resolved operando synchrotron X-ray and Neutron diffraction study of NMC811/Si–Gr 5 Ah pouch cells

Silicon–Graphite blended electrodes in Li-ion batteries have been proposed as a way to harness the high capacity of Si as an anode material, while minimising the negative effects of their large volume expansion. NMC 811 is the current state-of-the-art layered oxide cathode material, where the cobalt content of the cathode has been minimised. These are the two of the most promising materials for achieving electric vehicle targets in terms of performance, cyclability and price, however their degradation mechanism is not fully understood. Here these two materials have been used to manufacture 5 Ah prototype multi-layer pouch cells, which are aged and then studied using two complimentary diffraction techniques. Neutron diffraction has enabled a quantitative analysis of phase transitions in Si–Gr anodes in a pristine and degraded cell, and the alloying behaviour of Si and Li has been inferred by comparison of identical cells with either graphite or Si–Gr anodes. Synchrotron X-ray Diffraction has been used to make an operando 2D map of the cathode and anode lithiation in the pouch cell, as well as to map the volume expansion across the cell. This approach has revealed that degradation entails significant inhomogeneities across both electrodes, linked to the inhomogeneous volume expansion of the Si–Gr anodes.

Nanolamellar phase transition in an additively manufactured eutectic high-entropy alloy under high pressures

Much is unknown about how phase transitions link to micro-/nano-structures in high-entropy systems, especially under extreme pressure and temperature conditions. This work studies the evolution of dual-phase nanolamellar eutectic high-entropy alloy phases of AlCoCrFeNi2.1 generated by laser powder-bed fusion (L-PBF) for pressures up to 42 GPa. We compare quasi-hydrostatic high pressure synchrotron x-ray diffraction studies on L-PBF printed cylindrical samples up to 5.5 GPa (large-volume Paris–Edinburgh cell) to those carried out on an L-PBF printed foil in a diamond anvil cell where the pressure reached 42 GPa. Our results show that the initially alternating face-centered cubic (FCC) and body-centered cubic (BCC) nanolamellar structure of AlCoCrFeNi2.1 transformed into single-phase FCC nanolamellae under high pressure with BCC–FCC phase transformation completion at 21 ± 3 GPa. Our results indicate a diffusionless BCC–FCC transformation in this additively manufactured far-from-equilibrium microstructure and demonstrate that the FCC phase is stable up to very high pressures. The measured equation of state for the FCC phase of AlCoCrFeNi2.1 is presented up to 42 GPa and shows excellent agreement between the data obtained in large-volume press and diamond anvil cell experiments.

Insertion of CO2 in metal ion-doped two-dimensional covalent organic frameworks

Carbon capture is one of the essential low-carbon technologies required to achieve societal climate goals at the lowest cost. Covalent organic frameworks (COFs) are promising adsorbents for CO2 capture because of their well-defined porosity, large surface area, and high stability. Current COF-based CO2 capture is mainly based on a physisorption mechanism, exhibiting smooth and reversible sorption isotherms. In the present study, we report unusual CO2 sorption isotherms featuring one or more tunable hysteresis steps with metal ion (Fe3+, Cr3+, or In3+)-doped Schiff-base two-dimensional (2D) COFs (Py-1P, Py-TT, and Py-Py) as adsorbents. Synchrotron X-ray diffraction, spectroscopic and computational studies indicate that the sharp adsorption steps in the isotherm originate from the insertion of CO2 between the metal ion and the N atom of the imine bond on the inner pore surface of the COFs as the CO2 pressure reaches threshold values. As a result, the CO2 adsorption capacity of the ion-doped Py-1P COF is increased by 89.5% compared with that of the undoped Py-1P COF. This CO2 sorption mechanism provides an efficient and straightforward approach to enhancing the CO2 capture capacity of COF-based adsorbents, yielding insights into developing chemistry for CO2 capture and conversion.

Insights into thermodynamic destabilization in Mg-In-D hydrogen storage system: A combined synchrotron X-ray and neutron diffraction study

In this study, ultrafine Mg(In) solid-solution particles were successfully prepared through an arc plasma method and their deuterium uptake/release performances were systematically estimated with respect to the identically processed pure Mg particles. Thermodynamic destabilization and kinetic enhancement of Mg-In-D system were achieved simultaneously with lower deuterium ab/desorption enthalpies and decreased desorption temperatures. For the first time, an in-situ synchrotron X-ray diffraction (ISXRD) coupled with neutron powder diffraction (NPD) technique and density functional theory (DFT) calculations clearly substantiated that an indium diffusion-dominated phase transition is the driving force for the evolution from mixture of MgD2 and Mg-In intermetallic to Mg-based solid solution during the deuterium release (DR). The ISXRD results clarified the real-time phase transition from MgIn to Mg3In at 515 K and the interreaction of MgD2 and Mg3In at 640 K, by which the matrix could be destabilized to trigger an indium-diffusion governed DR reaction in deuteride. Moreover, with the aid of NPD experiment, the microstructure evolution of Mg-In-D system demonstrated the continuous diffusion of indium into Mg/MgD2 upon desorption. The solubilized indium in MgD2 effectively reduced the D-migration energy barrier and stabilized the lattice structure to restrain the constriction of Mg-D bonds, through which the noticeable improvement on both thermodynamic and kinetic performances of the Mg-In system was achieved. The combination of synchrotron X-ray and neutron diffraction offers a high-efficiency strategy to fathom the hydrogen discharging mechanism from the viewpoint of real-time phase transitions and crystalline structure evolutions.

Unveiling the strain and structural ferroelectric phase transition induced by temperature in lead titanate perovskite modified with 40% of calcium

Structurally correlated ferroelectric phase transitions induced by temperature are reported for the solid solution Pb0.6Ca0.4TiO3 compound. Such phase transitions were analyzed by considering different parameters, such as lattice parameters, microstrain, dielectric properties, and thermal analysis. Synchrotron x-ray diffraction and Rietveld refinement studies revealed a tetragonal symmetry from room temperature up to ∼550 K and uniaxial microstrain from room temperature to ∼400 K. The first thermally driven phase transition observed was from displacive ferroelectric tetragonal symmetry to another non-displacive tetragonal symmetry. The next phase transition was from the tetragonal to cubic. The electric permittivity as a function of temperature for frequency from 1 kHz to 1 MHz and the differential scanning calorimetry report features typical of ferroelectric–paraelectric phase transition only around 400 K, and no other abrupt change in properties is observed at 550 K, indicating the sequence of first- and then second-order phase transition.

Effect of cobalt content on point defects and local structure in activated Ca3(VO4)2 single-crystal solid solutions

Doping-induced structural changes of Co-activated calcium orthovanadate Ca3(VO4)2 (CVO) single crystals and specific local behavior of cobalt ions depending on the dopant content are presented in this paper. CVO is activated with over-stoichiometric Co3O4 of different concentration (CVO:xCo; x ​= ​0.1, 0.5, 1.0, 1.5, 2.0 ​wt %) during the Czochralski growth. Single-crystal synchrotron X-ray diffraction study shows gradual increase in the number of Ca crystallographic sites occupied by cobalt ions with increasing dopant concentration: from Ca3 site for CVO:0.1Co to additionally Ca2 and Ca4 sites for CVO:0.5–1.5Co, and also to Ca1 site for CVO:2.0Co. Vacancies in the tetrahedral vanadium V2 site are detected for all samples, and those in the tetrahedral V1 site are additionally found for CVO:2.0Co. Disordering of O1, O4, O7 oxygen sites is observed in all structures. Combined results of X-ray diffraction analysis and X-ray absorption spectroscopy showed that the formal charge of Co ions is mixed between 2+ and 3+ with the prevalence of 2+. A trend towards a decrease in formal charge with an increase in Co concentration is observed. The coordination number of Co(2+δ)+ ions is found to be 4.6 and polyhedron is intermediate between tetrahedral and octahedral.

A wide range room temperature antiferroelectric liquid crystal mixture with moderate spontaneous polarization and sub-millisecond switching time

A room-temperature antiferroelectric liquid crystal (AFLC) mixture has been prepared by doping two chiral fluorinated compounds into a four-component achiral phenyl pyrimidine-based host matrix. The suitability of the mixture for practical applications has been tested by optical polarizing microscopy, synchrotron X-ray diffraction, frequency-dependent dielectric, and electro-optic studies. The mixture possesses an antiferroelectric phase over a wide temperature range (nearly 82 °C) followed by a paraelectric phase for 13.7 °C. It is found to display very fast switching between 243 and 45 μs at the driving voltage of 3.2 V/μm in the SmC*A phase. At 20 °C, the mixture exhibits a moderately high spontaneous polarization (137 nC/cm2), low viscosity (1.01 Pa s) and fast switching (240μs). The formulated mixture is thus expected to be suitable for use in fast-response AFLC-based display devices.

In situ characterisation for studying nucleation and growth of nanostructured materials and thin films during liquid-based synthesis

Knowledge about the nucleation, growth, and formation mechanisms during materials synthesis using sol-gel and solution-based methods is important to design a material with desired properties. We used aqueous chemical synthesis as an environmentally friendly and highly flexible route to tailored and reproducible synthesis of oxide nanomaterials and thin films. For studies of hydrothermal synthesis an in situ cell using synchrotron X-ray diffraction was used to investigate the formation mechanisms of SrxBa1-xNb2O6 piezoelectrics. Aqueous chemical solution deposition of phase pure oriented piezoelectric thin films demands strong control of processing parameters. An in situ cell for synchrotron X-ray diffraction studies of the annealing and crystallisation steps during aqueous chemical solution deposition was used to understand the nucleation and crystallisation of Ba0.85Ca0.15Zr0.1Ti0.9O3 (BCZT). We discuss how the knowledge about nucleation and growth obtained by in situ characterisation can be used to design the optimal procedure for fabrication of oxide materials with desired properties.Graphical abstract