La2o3

Manufactured by Merck Group

Sourced in Germany

La2O3 is a rare earth oxide compound that serves as a key material in various laboratory applications. It has a high melting point and is commonly used in the production of specialty ceramics, glass, and refractory materials. La2O3 exhibits unique optical and electrical properties that make it suitable for specific research and development activities.

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29 protocols using la2o3

Synthesis of Perovskite Ceramics

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Ceramic
samples of nominal composition La_1/2+1/2xLi_1/2–1/2xTi_1–xAl_xO₃ (0.1
≤ x ≤
0.6) were synthesized from stoichiometric amounts of La₂O₃ (99.99% Aldrich), Li₂CO₃ (99.9%,
Aldrich), TiO₂ (99.99%), and Al(NO₃)₃·9H₂O (>98% Aldrich) by a solid-state reaction
as
previously described.^{32 (link)} These reagents
were ground together in an agate mortar and heated at 800 °C
for 12 h in highly dense alumina crucibles (La₂O₃ was previously dried at 700 °C for 4 h for decarbonation).
The reground powders were isostatically cold-pressed at 200 MPa and
heated at 1100 °C for 24 h. Finally, they were uniaxial-pressed
and heated again for 6 h at a temperature range of 1300–1400
°C depending on their composition and furnace-cooled to room
temperature. To avoid lithium losses, the heating rate in the thermal
treatment was 1 °C·min^–1.

Vezzù K., García-González E., Pagot G., Urones-Garrote E., Sotomayor M.E., Varez A, & Di Noto V. (2022). Effect of Relaxations on the Conductivity of La1/2+1/2xLi1/2–1/2xTi1–xAlxO3 Fast Ion Conductors. Chemistry of Materials, 34(12), 5484-5499.

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Chromite-Based Perovskite Synthesis

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Three different
compositions of chromite based perovskites were examined, see Table 1. Those were prepared
as follows via a modified Pecchini method:⁵⁴ Appropriate amounts of SrCO₃ (99.995% trace metals basis,
Aldrich) and La₂O₃ (99.99% trace metals basis,
Aldrich) were dissolved in HNO₃ (redistilled, 99.999% trace
metals basis, Aldrich); Cr(NO₃)₃·9(H₂O) (99.99% trace metals basis, Alfa Aesar) and, in case of
Ni containing perovskites, Ni(NO₃)·6(H₂O) (99.995% trace metals basis, Aldrich) were dissolved in double
distilled water. The cation solutions were merged, citric acid (99.9998%
trace metals basis, Aldrich) was added as a complexing agent in a
molar ratio of 1.2 with respect to the total amount of cations, and
the obtained solution was heated in a quartz beaker. After evaporation
of large parts of the solvent a darkish foam was formed, which spontaneously
decomposed upon further heating. The black residue was calcined at
750 °C in a box furnace, milled in a stainless steel mortar,
isostatically pressed (ca. 4 kbar), and finally sintered at 1400 °C
for 2 h in air to obtain targets for pulsed laser deposition (PLD).
La_0.6Sr_0.4FeO_3δ (LSF)
targets were prepared from commercial powder (purchased from Aldrich)
by isostatic pressing (ca. 4 kbar) and sintering at 1250 °C in
air.

Opitz A.K., Nenning A., Rameshan C., Kubicek M., Götsch T., Blume R., Hävecker M., Knop-Gericke A., Rupprechter G., Klötzer B, & Fleig J. (2017). Surface Chemistry of Perovskite-Type Electrodes During High Temperature CO2 Electrolysis Investigated by Operando Photoelectron Spectroscopy. ACS Applied Materials & Interfaces, 9(41), 35847-35860.

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Synthesis and Characterization of Ta and La-doped CCTO

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Before fabricating polycrystalline dense samples, Ta- and La-doped (Ca_1/4Cu_3/4)TiO₃ (equivalently, CaCu₃Ti₄O₁₂) powders were first synthesized via a conventional mixed oxide technique using CaCO₃ (99.995%, Aldrich), CuO (99.995%, Alfa Aesar), TiO₂ (99.8%, Aldrich), Ta₂O₅ (99.9%, Aldrich), and La₂O₃ (99.99%, Aldrich). The initial stoichiometry of 5%-Ta-doped powder was adjusted to be (Ca_1/4Cu_3/4)Ti_0.95Ta_0.05O₃ for the B-site doping. Based on a previous report showing the La substitution in the Ca site^{33 (link)}, a La-doped stoichiometric powder of (Ca_0.20La_0.05Cu_0.75)TiO₃ was prepared for 5% A-site doping. Both powder mixtures of the starting materials were ball-milled in ethyl alcohol for 24 h. The dried slurries were then calcined at 900 °C in air for 12 h. The calcined powders were ball-milled again for another 2 h to obtain fine particles. The Ta- and La-doped powders were both slightly pressed into disks and then isostatically pressed under 200 MPa to fabricate polycrystalline samples. The pellets were sintered in a tube-type furnace at 1150 °C in air for 12 h, and removed immediately to room temperature without any furnace cooling to obtain high-temperate equilibrium segregation.

Yoon H.I., Lee D.K., Bae H.B., Jo G.Y., Chung H.S., Kim J.G., Kang S.J, & Chung S.Y. (2017). Probing dopant segregation in distinct cation sites at perovskite oxide polycrystal interfaces. Nature Communications, 8, 1417.

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Synthesis of Fe-Doped LLZO Garnets

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A series of Li_7−3xFe³⁺_xLa₃Zr₂O₁₂ garnets with intended mole fractions (x_int) of Fe³⁺ with x_int=0.04–0.72 per formula unit (pfu) was synthesized by high-temperature sintering methods, as reported in our earlier study on Fe-bearing LLZO [11] (link). The starting materials were Li₂CO₃ (99%, Merck), La₂O₃ (99.99%, Aldrich), ZrO₂ (99.0%, Aldrich) and ⁵⁷Fe enriched Fe₂O₃. The latter was used to obtain well-resolved ⁵⁷Fe Mössbauer spectra (see below). Li₂CO₃ was mixed with the various oxides in the necessary proportions and they were ground intimately together. This mixture was calcinated at 900 °C, reground, pressed into pellets, and sintered at 1050 °C for 16 h and then removed from the furnace.

Rettenwander D., Geiger C.A., Tribus M., Tropper P., Wagner R., Tippelt G., Lottermoser W, & Amthauer G. (2015). The solubility and site preference of Fe3+ in Li7−3xFexLa3Zr2O12 garnets. Journal of Solid State Chemistry, 230, 266-271.

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Solid-state Synthesis of Ta-doped LLZTO

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The Ta-doped LLZTO powders were synthesized using a solid-state synthesis method with LiOH·H₂O (99.99%; Sigma-Aldrich), La₂O₃ (99.99%; Sigma-Aldrich), Ta₂O₅ (99.99%; Sigma-Aldrich), and ZrO₂ (99%; Sigma-Aldrich). Note that 20 weight (wt) % excess LiOH·H₂O was added to compensate for the volatile Li components during the sintering process. We combined the precursors at stoichiometry and calcined them at 900°C for 12 hours in an alumina crucible to form a cubic LLZTO phase. The obtained LLZTO powders were ball-milled at 200 rpm for 10 hours to attain a fine powder with a particle size of 5 to 10 μm. We pressed them into 10-mm-diameter pellets, which were sintered at 1100°C for 10 hours in air with 0.2 wt % γ-Al₂O₃ (99.9%; Sigma-Aldrich) as the sintering agent. The obtained pellets were polished with 600, 1500, and 2000 grit sandpaper to clean the surface and remove possible surface impurities. The final thickness of the LLZTO pellets was approximately 700 μm, and their relative density was approximately 93%.

Lee S., Lee K.S., Kim S., Yoon K., Han S., Lee M.H., Ko Y., Noh J.H., Kim W, & Kang K. (2022). Design of a lithiophilic and electron-blocking interlayer for dendrite-free lithium-metal solid-state batteries. Science Advances, 8(30), eabq0153.

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Synthesis of Photocatalytic Oxide Materials

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La₂O₃ (99.9%), TiO₂ (anatase, 99.9%), BiOCl
(98%), and Na₂SO₄ (99%) are purchased from Sigma-Aldrich.
Bi₂O₃ (99.9%) and acetone (pro analysis) are
purchased from Acros Organics
and Supelco, respectively. NaCl (99%), KCl (99.5%), and iodine (99%)
are purchased from VWR Chemicals.

Werner V., Aschauer U., Redhammer G.J., Schoiber J., Zickler G.A, & Pokrant S. (2023). Synthesis and Structure of the Double-Layered Sillén–Aurivillius Perovskite Oxychloride La2.1Bi2.9Ti2O11Cl as a Potential Photocatalyst for Stable Visible Light Solar Water Splitting. Inorganic Chemistry, 62(17), 6649-6660.

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Synthesis of La0.5Li0.5TiO3 Ceramic

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La_0.5Li_0.5TiO₃ samples were prepared by a conventional solid-state reaction. The reagents used for this study were as follows: Li₂CO₃ 99% (Merck KGAA, Berlin, Germany), La₂O₃ 99.99% (Sigma-Aldrich, Berlin, Germany), and TiO₂ 99% (Sigma-Aldrich, Germany). La₂O₃ was heated at 1000 °C and TiO₂ at 700 °C prior to weighing. Stoichiometric amounts of these reagents were ground together in an agate mortar and heated at 800 °C for 4 h in order to eliminate CO₂. The reground mixture was then cold-pressed at 150 MPa and heated at 1150 °C for 12 h. These powders were used to produce the composites.
To prepare sintered LLTO pellets, the powder was reground, pressed, and heated again at 1350 °C for 6 h. In order to avoid lithium losses, the heating rate used in all treatments was performed at 1 °C/min. Finally, the sample was quickly cooled from high temperature by immersion in liquid nitrogen.

Boyano I., Mainar A.R., Blázquez J.A., Kvasha A., Bengoechea M., de Meatza I., García-Martín S., Varez A., Sanz J, & García-Alvarado F. (2020). Reduction of Grain Boundary Resistance of La0.5Li0.5TiO3 by the Addition of Organic Polymers. Nanomaterials, 11(1), 61.

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Synthesis of Solid-State Cubic LLZO Electrolytes

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Li₂CO₃ (99.9%), La₂O₃ (99.9%), ZrO₂ (99.9%), Al₂O₃ nanopowder (<50 nm particle size), Ta₂O₅ (99.9%) were purchased from Sigma-Aldrich and used as received. Garnet-structured cubic LLZO solid electrolytes with the desired amounts of doping elements (only Al, only Ta, or both Al and Ta) was prepared through a solid-state reaction. The whole precursor materials were weighed according to the stoichiometry and mixed by planetary ball-milling in isopropyl alcohol at 200 rpm for 10 h. No excess Li was added into the mixture. After drying the mixture, the collected powder was calcined at 1000 ˚C for 2–4 h to obtain the cubic LLZO powder. The calcined LLZO powder was reground and pressed into a pellet at 50 MPa. Finally, the pellet was sintered at 1200 ˚C from 1 to 24 h to ensure the formation of well-dense body. In the sintering step, the pellet was covered with the mother LLZO power to minimize the Li loss at high temperature. During the synthesis of cubic LLZO powder and the sintering of pellet, Al₂O₃ crucible with boron nitride (BN) coating was used to prevent the unintentional Al doping.

Shin D.O., Oh K., Kim K.M., Park K.Y., Lee B., Lee Y.G, & Kang K. (2015). Synergistic multi-doping effects on the Li7La3Zr2O12 solid electrolyte for fast lithium ion conduction. Scientific Reports, 5, 18053.

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Synthesis of Calcium-Rare Earth Manganates

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We apply a standard
solid-state reaction (SSR) routine to synthesize Ca_2–xR_xMnO₄ compounds
with x = 0.01, 0.05, 0.10, and 0.15, where R = Y
or La. The pure oxide powders, CaCO₃ (Reag. Ph Eur, Merck),
MnO₂ (≥99%, Sigma-Aldrich), and Y₂O₃ (99.99%, Strem Chemicals) or La₂O₃ (99.99%,
Sigma-Aldrich), are weighed in the proper stoichiometric ratios and
milled by a mortar and pestle. Finally, the powder mixtures undergo
four 24 h SSR steps with increasing temperatures applying a 100 K
h^–1 heating rate at 1273, 1373, 1473, and 1573 K.
Prior to each step, the powders are thoroughly milled to increase
the surface area for the reaction. Subsequently, disk-shaped specimens
are prepared for each compound by uniaxial pressing of the powder
at 700 MPa and sintering of the green body at 1573 K in air for 24
h.^{12 (link),13 (link),19 (link)}

Azulay A., Wahabi M., Natanzon Y., Kauffmann Y, & Amouyal Y. (2020). Enhanced Charge Transport in Ca2MnO4-Layered Perovskites by Point Defect Engineering. ACS Applied Materials & Interfaces, 12(44), 49768-49776.

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Synthesis and Characterization of La2Sn2-xTixO7

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Samples in the system La₂Sn_2–xTi_xO₇ were prepared in two batches, the first batch consisting
of 11 samples from x = 0 to x =
2, in steps of 0.2. Subsequently, a second batch of samples from x = 1.8 to x = 1.95 (with x varying in steps of 0.05) was prepared. Both sets of samples were
prepared under identical conditions, using stoichiometric amounts
of La₂O₃ (Sigma-Aldrich 99.9%), TiO₂ (Sigma-Aldrich 99%), and SnO₂ (Sigma-Aldrich 99.9%),
which were predried overnight to remove CO₂ and H₂O before weighing. These powders were then ball milled for 16 h in
isopropanol with zirconia media, dried, sieved and (uniaxially) pressed
into pellets. The pellets were then heated at 1673 K for 48 h, with
a ramp rate of 5 K min^–1. After cooling, the samples
were ground for both X-ray diffraction and MAS NMR analysis.

Fernandes A., McKay D., Sneddon S., Dawson D.M., Lawson S., Veazey R., Whittle K.R, & Ashbrook S.E. (2016). Phase Composition and Disorder in La2(Sn,Ti)2O7 Ceramics: New Insights from NMR Crystallography. The Journal of Physical Chemistry. C, Nanomaterials and Interfaces, 120(36), 20288-20296.

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