Citrate Sol Gel Method Research Articles

Effects of Er3+ concentration on the structure and optical properties of the MgAl2O4/MgO/Sr3Al2O6/SrAl2O4 mixed phases prepared by the citrate sol gel method

The mixed phases of the un-doped MgAl2O4/MgO/Sr3Al2O6/SrAl2O4 (MMSS), MgAl2O4/MgO (MM) Sr3Al2O6/SrAl2O4 (SS), and the doped MMSS:x% Er3+ (0 ≤ x ≤ 1.8) nanopowders were synthesized using the citrate sol-gel method. The effect of Er3+ concentration on the structure, morphology and optical properties were investigated. X-ray powder diffraction (XRD) analysis indicated the cubical MgAl2O4, MgO and Sr3Al2O6; and monoclinic SrAl2O4 phases. The scanning electron microscopic images revealed the transformation of irregular particles to rod-like structure with an increase in Er3+ concentration. Transmission electron microscope indicated the nanosized particles depends on Er3+ concentration. Severals distinct absorption bands located at 444, 546, 653 and 704 nm under UV excitation (285 nm) corresponding to the defects states of the MgAl2O4, MgO, SrAl2O4, and Sr3Al2O6 phases were observed. There were traces of emission peaks at 546 and 653 nm attributed to the 4S3/2 → 4I15/2 and 4F9/2 → 4I15/2 transitions of Er3+ ion. An exponential decrease in luminescence was observed with an increase in Er3+ concentration.

The Novel Synthesis of CaMnO3 Perovskite Type-Oxide and its Catalytic Activity for Degradation of Dye

The CaMnO3 perovskite type-oxide has been synthesized using a citrate sol-gel method using two different MnO2 precursors and calcium carbonate. The cryptomelane-type manganese oxide precursor produced well-crystalline CaMnO3 perovskite, whereas pyrolusite-type manganese oxide (commercial) generated mixtures of CaMnO3 perovskite and un-reacted MnO2 using the same CaCO3 as other precursor. The CaCO3/MnO2 mole ratio seems to play a crucial role to obtain high purity of the CaMnO3 perovskite. The CaMnO3 perovskite proves to have high catalytic activity for the degradation of methylene blue (MB) using hydrogen peroxide as an oxidant. This Fenton catalyst is able to degrade 98.5% of MB within 20 minutes of degradation times at pH 2.

Magnetic properties of Sr0.95Nd0.05Fe12-xScxO19 hexaferrite nanoparticles

Sr0.95Nd0.05Fe12-xScxO19 (0 ≤ x ≤ 1.56) nanocrystallites, 50–100 nm thick, were obtained by citric sol-gel method. Single P63/mmc phase with lattice parameters increasing continuously with x was proved by X-ray diffraction. Scanning electron microscope control of the microstructure shows a decrease in particle size with increasing x from 1000 to ∼250 nm. Saturated hysteresis loops were obtained in field of 5 T and magnetization switching via curling mode was observed for crystallites with sizes from 1000 to ∼600 nm. For smaller particles magnetization was switched via coherent reorientation. The effect of doping on magnetic properties was apparent in samples containing more than one Sc3+ ion substituting Fe3+ pro one unit cell (x ≥ 0.60). The saturation magnetization was found to increase on cooling from 300 K and for samples with x ≥ 0.60 exhibits local maximum at Tcone temperatures considerably lower in comparison with those of bulk counterparts. The appearance of conical magnetic order is reflected in temperature dependences of extrinsic magnetic properties, coercivity and remanence, which decrease also on doping. Temperature variation of magnetization in zero field cooling/field cooling modes shows that Tcone is shifted downwards with increasing field.

Citrate sol-gel synthesis of BaAl2O4:x% Cu2+ (0 ≤ x ≤ 1) nano-phosphors: Structural, morphological and photoluminescence properties

Abstract This paper reports on the effects of varying the Cu2+ doping concentration on the structure, morphology and optical properties of the BaAl2O4 phosphor. BaAl2O4:x% Cu2+ (0 ≤ x ≤ 1) series were successfully synthesized via citrate sol-gel method. The X-ray diffraction (XRD) results revealed that the prepared phosphor sample consist of a single phase hexagonal structure. The presence of Ba, Al, O and Cu were confirmed by the energy dispersive X-ray spectroscopy (EDS). Scanning electron microscope (SEM) revealed that the morphology of the prepared samples highly depends on the Cu2+ concentration. Transmission electron microscopy (TEM) results revealed the hollow tubular and nano-nature of the crystallite sizes. When the un-doped sample was excited at 283 nm, the photoluminescence (PL) results revealed six emission peaks located at 420, 435, 457, 521, 612 and 722 nm, which were attributed to the intrinsic intra band gap defects within the BaAl2O4 (host). The emission at 425 nm observed for the BaAl2O4:Cu2+ samples was attributed to the 3d84s1 → 3d9 transition in Cu2+ ion. The optimum doping Cu2+ concentration was found to be 0.075% Cu2+. Critical energy transfer distance (Rc) of Cu2+ ions was found to be 12.01 A, which suggested that the multipole-multipole interaction was the main reason for the luminescence quenching. The International Commission on Illumination (CIE) colour showed that the bluish emission colour of the prepared samples depends on the excitation wavelength and Cu2+ concentration. Thermo stimulated luminescence (TSL) of the host material showed the presence of both the swallow and deep traps respectively located at 75 and 240 °C.

Graphene influence on the structure, magnetic, and optical properties of rare-earth perovskite

Perovskite-graphene nanocomposites of rare-earth LaFeO3-rGO and LaFeO3 nanoparticles are synthesized and characterized. The preparation was done by citrate sol-gel method. The structural characterization has been performed using XRD and FT-IR. Scanning electron microscope (SEM) and atomic force microscope (AFM) were used to analyze the morphology of the prepared nanocomposite. Vibrating sample magnetometer (VSM) was used to study the magnetic properties of the investigated samples. Introducing graphene to the structure results increase in MS. Also, the optical and thermal properties have been measured and discussed, and the effect of graphene is observed where it decreases the band gap than reported for pure LaFeO3 nanoparticles.

Copper-Containing Films Obtained by the Simple Citrate Sol–Gel Route for NO2 Detection: Adsorption and Kinetic Study

The citrate sol–gel method was utilized for the fabrication of copper-containing films sensitive to NO2 gas. Effect of annealing temperature on the film phase composition, morphology, and sensor response was studied. X-ray diffraction reveals the formation of Cu2Cl(OH)3 phase at 250 °C and the CuO phase at 350 and 500 °C. It was found out that the films annealed at 250 °C and 350 °C showed the best sensor characteristics. The influence of thermal degradation on the probability of percolation effect in films and its connection to a decrease of gas sensitivity was studied. The kinetics of the NO2 gas adsorption on the film’s surface was described following the Elovich model. Activation energy estimated from the ln(S) vs. 1/T plots was 252 and 30 kJ/mol for the films annealed at 250 and 350 °C, respectively.

Application of nanostructured aluminium titanate (Al2TiO5) photocatalyst for removal of organic pollutants from water: Influencing factors and kinetic study

In this study, aluminum titanate (Al2TiO5)-based nanostructure with the outstanding photocatalytic performance was prepared via the simple citrate sol-gel method. The effects of thee operational variables such as pH, temperature, catalyst dosage, and initial dye concentration on the photodegradation efficiency of methylene blue (MB) were explored in some details. The results showed that compared to TiO2, AT benefits a superior photocatalytic activity due to its narrow band gap (2.88 eV) and low recombination rate of charge carriers. Increasing the wastewater temperature from 25 to 60 °C can improve the degradation percent from 22.15 to 52%. Based on the thermokinetic calculations, the Arrhenius activation energy, ΔH, and ΔS values were also estimated as +24.69 kJ mol−1, 21.78 J mol−1, and 222.48 J K−1.mole−1, respectively. According to the Langmuir-Hinshelwood kinetic model, the photocatalyst follows a first-order equation in a wide range of temperatures. In addition, escalating the pH value from 4 to 9.5 may noticeably enhance the photodegradation efficiency from 7.1 to 46.6%. The enhanced photocatalytic activity at alkaline media was mainly attributed to the excessive generation of hydroxyl ions, improved adsorption of cationic dye on the catalyst surfaces, and effective separation of involved charge carriers. The maximum performance was obtained for the AT dosage of 20 mg/lit and MB concentration of 2.5 mg/lit. Finally, the recycling experiments after 6 runs verified the high stability of the photocatalyst.

Ethanol sensing characteristics of Au and Cl-comodified ZnO nanoparticles

Au and Cl-comodified ZnO nanoparticles were prepared by a citric sol–gel method. XRD and TEM showed that the simultaneous introduction of gold and chlorine resulted in smaller crystallite and particle size than the pristine ZnO. XPS revealed that chlorine existed in the form of chloride, while gold was in the mixed states of Au3+ ions and Au0 atoms. Compared with the pristine ZnO, Au-ZnO and Cl-ZnO, the Au,Cl-ZnO nanoparticles exhibited the best and stable ethanol sensing performance, including higher gas response (19.64–100 ppm), sensitivity and selectivity at comparatively lower prime working temperature of 220 °C. The improved ethanol sensing performance was ascribed to the higher surface coverage of adsorbed oxygen species resulting from the substitution of Au3+ for Zn2+ ions and Cl- for O2– ions in the ZnO lattice which increased the concentration of electrons and number of adsorption sites, as well as from the spillover effect of metallic gold with the highly effective dissociation catalytic ability.

Effect of Boron and Aluminum Doping on the Reflectivity of Samarium Compounds

The precursor was prepared by citrate sol-gel combustion method, and the nanocrystals were calcined at high temperature. The morphology and structure of the material were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and Fourier Transform Infrared Spectrometer (FTIR). The reflectance of the sample material was tested by UV-Vis NIR spectrophotometer (UVPC). The results showed that the sample material was nanocrystal, the particle size was uniform, and agglomerated to form microparticles. The material with the highest reflectance at 1064 nm wavelength was 54.58% of SmB0.5Al0.5O3 material, and the reflectivity of the powder with the lowest reflectivity at the wavelength of 1064 nm was 43.36% of that of SmB0.3Al0.7O3. Among them, the lowest reflectance at 1060–1090 nm was 32.65% at 1080 nm of SmBO3.

Electrical and optical studies on tungsten-substituted bismuth molybdates

Abstract This manuscript highlights the structural, electrical and optical properties of Bi2Mo1-xWxO6 (x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) compounds. These compounds were prepared employing the citrate sol-gel method. These compositions were characterized using thermo-gravimetric and differential scanning calorimetry, X-ray diffraction and infrared techniques. The Rietveld refinements of X-ray powder diffraction data determined and confirmed the crystal structure of the compositions. DC electrical conductivity indicated the conduction behaviour and diffuse reflectance spectroscopy confirmed the semiconducting nature of the compounds. Room temperature photoluminescence results exhibited two type of emission namely blue-green and green emission in the visible region.

Characteristics of new Mg0.5(Zr1-xSnx)2(PO4)3 NASICON structured compound as solid electrolytes

Mg0.5(Zr1-xSnx)2(PO4)3 with 0.0 ≤ x ≤ 1.0 compounds were synthesized using water-based citrate sol-gel method. X-ray diffraction and its Rietveld refinement analysis for x ≤ 0.6 confirmed the formation of a monoclinic NASICON structured compound with a space group P21/n upon sintering at 800 °C for 24 h. The total conductivity value obtained for Mg0.5ZrSn(PO4)3 is 2.47 × 10-5 S cm-1 at 500 °C which is two order of magnitude higher compared to the pristine Mg0.5Zr2(PO4)3. The activation energy value for pristine Mg0.5Zr2(PO4)3 and Mg0.5ZrSn(PO4)3 are Ea = 0.84 ± 0.05 eV and Ea = 0.79 ± 0.04 eV respectively. Furthermore, exponent s(T) behaviour was found to increase with rising temperature and is in good agreement with the correlated barrier hopping model. It seems that Mg0.5ZrSn(PO4)3 achieved higher conductivity and lower activation energy than the pristine Mg0.5Zr2(PO4)3, indicates that the Sn4+ ion substituted compound make a desirable solid electrolytes for magnesium power storage.

Ethanol sensing characteristics of (La,Ba)(Fe,Ti)O3 nanoparticles with impurity phases of BaTiO3 and BaCO3

To further improve the ethanol sensing performance of LaFeO3 (LFO) nanoparticles, the co-doping of acceptor and donor at La and Fe sites at equal mole amount was designed to increase the oxygen adsorbing ability of the resultant nanoparticles. A series of (La,Ba)(Fe,Ti)O3 nanoparticles, with the designed mole ratios of Ba/La (Ti/Fe) as 0, 0.25, 0.33, 0.50, and 1.0, were prepared by a citric sol–gel method. XRD confirmed the main phase of orthorhombic LFO, and the impurity phases of cubic BaTiO3 (BTO) and orthorhombic BaCO3. The incorporation of Ba and Ti into the LFO lattice was verified by the increased unit cell volume of LFO upon more doping. TEM, BET, and XPS measurements indicated that the appropriate co-doping of Ba and Ti into the LFO lattice and the simultaneous existence of BTO and BaCO3 resulted in smaller grain size, larger BET surface area, and thus higher concentration of adsorbed oxygen species than those in the pristine LFO nanoparticle. Among all (La,Ba)(Fe,Ti)O3 sensors, the sensor based on the (La,Ba)(Fe,Ti)O3 nanoparticles with the designed Ba/La = 0.50 exhibited the highest gas response and sensitivity toward ethanol at the prime working temperature of 132 °C, which was ascribed to the higher surface oxygen coverage contributed by the synergistic effect of co-doping and impurity phases on the number of surface active sites and oxygen adsorbing ability.

Preparation of nitrogen-doped aluminium titanate (Al2TiO5) nanostructures: Application to removal of organic pollutants from aqueous media

Recently, aluminum titanate (Al2TiO5)-based nanostructures have been proved to serve as an efficient photocatalytic material with satisfactory photodegradation capacity. In this study, the citrate sol–gel method was used to synthesize these nanostructures and inspect the significant impacts of nitrogen-doping-originated crystalline defects on their photocatalytic performance in some details for the first time. The results indicated that the penetration of nitrogen atoms into AT crystal lattice, depending on the nitriding time and temperature, can induce a great deal of the residual stress and result in propagating the existing cracks and breaking down the particles. The XPS and FTIR results confirmed the formation of some new bonds in the crystal structure (including O-Ti-N and Ti-N), the substitutional and interstitial replacement of nitrogen atoms with oxygen atoms, oxygen vacancies, and the attachment of nitrogen species at superficial oxygen sites. These events may vary the bandgap values from 2.88 eV for pristine AT to 2.73 eV for the nitrided one, thereby manipulating the charge carrier recombination rate and activation of superficial catalytic reactions in the particles. Numerically, the band structure variations can efficiently increase the photodegradation efficiency of methylene blue (MB) and apparent rate constant (k) by 1.4 times (from 38.9 to 55.9%) and 1.8 times (from 0.0038 to 0.0068 min−1), respectively. Finally, the results show that the synthesized photocatalyst can successfully compete with TiO2-based photocatalysts in terms of photocatalytic performance.

Electrical and optical studies on tungsten-substituted bismuth molybdates

Abstract This manuscript highlights the structural, electrical and optical properties of Bi2Mo1-xWxO6 (x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) compounds. These compounds were prepared employing the citrate sol-gel method. These compositions were characterized using thermo-gravimetric and differential scanning calorimetry, X-ray diffraction and infrared techniques. The Rietveld refinements of X-ray powder diffraction data determined and confirmed the crystal structure of the compositions. DC electrical conductivity indicated the conduction behaviour and diffuse reflectance spectroscopy confirmed the semiconducting nature of the compounds. Room temperature photoluminescence results exhibited two type of emission namely blue-green and green emission in the visible region.

Optimization of structural and luminescent properties with intense red emitting thermally stable Sm3+ doped CaBiVO5 phosphors for w-LED applications

Sm3+ doped CaBiVO5 (CBV: Sm3+) phosphors synthesized namely by solid-state reaction (SSR), combustion (CB) and citrate sol-gel (SG) method to optimize the synthesis procedure and also to enhance the luminescent properties for the first time. X-ray powder diffraction patterns and scanning electron micrographs recorded for the synthesized CBV: Sm3+ phosphors to analyse structural and morphological aspects, respectively. The excitation spectra measured by monitoring emission at 649 nm for CBV: Sm3+ phosphors reveal significant absorption in ultraviolet (UV), near (n)-UV and blue spectral regions. The comparative photoluminescence (PL) spectra measured under 343 nm excitation for differently synthesized CBV: Sm3+ phosphors, which exhibit significantly enhanced emission intensity for SG derived phosphor than other adopted methods. The PL spectra for SG derived 1.0 mol% Sm3+ doped CBV phosphor at λex = 275 and 343 nm exhibit sharp peaks located at 566, 606 and 649 nm along with weak host emission broadband and for λex = 406 nm, similar sharp peaks of Sm3+ transitions are observed without any host emission. Unlike mostly explored Sm3+ doped phosphors, emission peak in red spectral region (649 nm) is more intense as compared to the emission peak in orange region (599 nm) in the present work. The energy transfer mechanism responsible for concentration quenching in CBV phosphors is discussed in detail. The CBV: Sm3+ phosphors manifest color tunability from orange to orange-red region by modulating excitation from 275 nm (0.567, 0.404) to 343 nm (0.591, 0.399) and finally to 406 nm (0.620, 0.376). The temperature-dependent PL studies indicate appreciable thermal stability of as-prepared phosphor. Above mentioned results suggest that CBV: Sm3+ phosphor has great potential for use in white light-emitting diode (w-LED) applications.

Iron and chromium-based oxides for residual methane abatement under realistic conditions: A study on sulfur dioxide poisoning and steam-induced inhibition

A series of iron and chromium-based oxides were used as catalysts for the total oxidation of residual methane under realistic after-treatment conditions. This study operated with sulfur dioxide, steam and methane concentrations similar to those typically found in natural gas turbines and natural gas-powered vehicle exhausts (around 4.6 ppmV of sulfur dioxide and 10%vol of steam alongside 312 ppmV of methane balanced in air). The catalysts were synthesised using the citrate sol-gel method and characterised by BET, XRD, TPR, in situ UV–vis, in situ DRIFTS, SEM, EDX, TEM and TGA under flowing air. The performance of the catalysts was tested at atmospheric pressure and operating temperatures between 450 °C and 550 °C using three different reactant mixtures: i) 366 ppmV of methane balanced in air, ii) 347 ppmV of methane and 5.1 ppmV of sulfur dioxide balanced in air, iii) 312 ppmV of methane, 4.6 ppmV of sulfur dioxide and 10%vol steam balanced in air. This study revealed that the iron:chromium ratio has a profound impact on the performance of the catalysts. The XRD characterisation revealed that the iron and chromium-based oxides are solid solutions of hematite and eskolaite. Furthermore, the iron oxide-rich catalysts (60%mol to 80%mol iron content) contain an additional phase, which was identified as a metastable FeCr2O4 mixed oxide with spinel structure. In terms of catalytic activity, resistance to sulfur poisoning and sensitivity towards steam inhibition, these two catalysts were superior to pure iron oxide and comparable to pure chromium oxide. Under dry conditions, these two catalysts achieved higher methane conversion levels than pure chromium oxide, suggesting that the metastable FeCr2O4 spinel gives rise to improved catalytic performance. Finally, this study has proven that the sulfur resistance characteristic of chromium oxide is maintained in iron and chromium-based oxides with a chromium oxide loading as low as 20%mol, resulting in similarly effective catalysts with a lower cost, a reduced environmental impact and a considerable reduction in the health hazards associated with the exposure to chromium.

Fabrication, microstructure and optical properties of Ga2O3 transparent ceramics

In this paper, Ga2O3 transparent ceramics were successfully prepared using the ceramic method. First, Ga2O3 sub-micro powders which possessed good dispersibility were synthesized by a citrate sol-gel method and the particle sizes of the synthesized powders calcined at 500 °C were approximately less than 1 μm. Next, the Ga2O3 ceramics were sintered via SPS at 980 °C for 5 min under a pressure of 90 MPa. The resulting Ga2O3 transparent ceramics were β-Ga2O3 with monoclinic structure and achieved a relative density as high as 99.1%. Furthermore, the transmittance was greater than 40% in the wavelength range between 396 nm and 667 nm and the highest transmittance was 45.5% at a wavelength of 494 nm. This Ga2O3 transparent ceramic exhibited two excitation peaks, one at 263.5 nm and the other at 378 nm. The fluorescence emission spectrum had two emission peaks with one located at 388 nm with an excitation wavelength of 263.5 nm and the other at 420 nm with an excitation wavelength of 378 nm. These photoluminescence properties can mainly be attributed to the recombination between donors and acceptors. Ga2O3 transparent ceramics have promising applications as transparent conductive materials and inorganic scintillators.

Activity improvement of acid treatment on LaFeO3 catalyst for CO oxidation

The rational design of low-cost catalysts with excellent catalytic activity is one of the most significant topics in heterogeneous catalysis. LaFeO3 (LFO) perovskite was synthesized by the citrate sol-gel method and followed through a selective dissolution method by acid solutions. The surface element percentage, chemical states and pore structure of LFO were tuned. The acid-treated catalyst (LFO-H) showed higher activity in CO oxidation than the raw LFO. In terms of various characterizations, the exposed La ions of the LFO were slightly etched by dilute nitric acid, but the LFO-H still preserved the original perovskite framework. The corresponding surface area, surface oxygen vacancies and reducibility were also improved after acid treatment, accounting for its higher catalytic activity. Moreover, the LFO-H also exhibited excellent thermal stability because the perovskite structure remains after acid treatment.

New perovskite Ba0.7La0.3Ti0.55Fe0.45O3-δ prepared by citric sol-gel method: From structure to physical properties

A new material Ba0.7La0.3Ti0.55Fe0.45O3-δ (BLTFO) has been prepared via the citric sol gel method. The correlation between structural, vibrational, and electric properties of BLTFO have been investigated using different technique. The XRD study showed that BLTFO perovskite was a single phase that crystallize in the cubic system with a space group Pm3̅m (a = 3.94 Å). The nanometric average crystallite size (D) was calculated from the XRD peaks using the two Scherrer and the Halder-Wagner methods. The particle sizes observed by SEM (70–140 nm) are several times larger than those calculated by XRD, indicating that each particle observed by SEM consists of several crystallites domains. The sphericity of each element present in this composition was studied by the Atomic Hirshfeld Surfaces (AHS) analysis in order to prove the obtained phase. Furthermore, this investigation proved that the BLFTO is stabilized by covalent, ionic and van Der Waals interactions. All stretching and bending vibrations were studied by IR and Raman. Moreover, the Mössbauer technique revealed the presence of Iron in the (+III) oxidation state. The electrical conductivity was measured in the frequency range from 20Hz to 2 MHz and temperatures between 520 and 700 K using impedance spectroscopy. The latter confirmed that an equivalent parallel Rg//C//CPE circuit can be connected. Besides, the analysis of Nyquist plots revealed the contribution of two electrically active regions The DSC analysis confirmed that this new material presented a phase transition at T = 600 K.

The Development of High-Throughput Methods in the Study of Solid State Li-Electrolytes

High-throughput experimentation is a fast and efficient methodology for materials discovery, screening, and optimization. It has, therefore, garnered a lot of attention from battery researchers as a potential way to accelerate the development of next-generation Li-ion batteries and battery systems beyond Li-ion. However, its successful use in battery materials discovery has been extremely limited due to a variety of challenges including: (i) difficulties in synthesizing mg-scale samples that are comparable to bulk samples made by industrial methods, (ii) limited high-throughput characterization acting like a bottleneck even after high throughput synthesis is developed, and (iii) high cost of commercially available high-throughput instrumentation. Here, we develop high throughput techniques for solid-state electrolytes.First, a novel synthesis approach is used to make 64 mg-scale solid electrolytes simultaneously. The powder samples are prepared by a citrate sol-gel method using an automated dispensing system. These powders were formulated into sixty-four pellets using a home-made high-throughput pellet press die. The samples are then sintered at high temperature to yield the solid electrolytes. The proof of concept here is performed on the Li-La-Ti-O pseudo-ternary system that includes the perovskites Li3xLa2/3-xTiO3, considered candidates for solid-state electrolytes for high energy lithium-ion batteries. Given that vacancies and other defects play an essential role in ionic conductivity, the screening of complete phase diagrams has the potential to reveal phases with optimized defect contents and thus yield improved solid electrolytes.We have therefore developed a high-throughput characterization suite for solid electrolytes. First, we use a high throughput X-ray diffractometer capable of producing Rietveld quality patterns for mg-scale samples in 10 min such that 64 patterns can be obtained in under 12 h. This system is readily used to produce structural phase diagrams in ternary or even quaternary systems. Next, a high throughput electrochemical impedance spectrometer is used to map the ionic conductivities onto the phase diagrams. Finally, high throughput electrochemistry is used to determine the stability window of the electrolytes. All aspects of this workflow are demonstrated on the Li-La-Ti-O system. This now permits the synthesis and full characterization of approximately 192 compositions per week with one researcher only. This approach is well suited to determine the structure-property relations in complex composition spaces.The complete ternary Li-La-Ti phase diagram synthesized at 1150 °C with slow cooling was determined and will be presented in detail. The total (ionic + electronic) conductivity of the phase diagram was mapped by the electrochemical impedance spectroscopy. Quenching was performed to verify that transformations during slow cooling are moderate in this system. Consequences for the development of other solid electrolytes will also be discussed.