All the samples in the present work were prepared by conventional solid‐state reaction (SSR). Nb2O5 (99.99%), Ba(NO3)2 (≥99%), Sr(NO3)2 (≥99%), Co(NO3)2·6H2O (≥98%), KNO3 (≥99%), LiNO3 (99.99%), and Fe2O3 (99.995%) were purchased from Aldrich Ltd. and used as starting materials. For the preparation of the SBN, SBNC30, SBNC45, and SBNC60 samples, the corresponding chemicals were mixed homogeneously in stoichiometric ratios according to the formula Sr0.5Ba0.5Nb2‐xCoxO6‐δ (x = 0, 0.3, 0.45, 0.6). The mixed powders were first pressed into pellets under axial pressure (8 MPa) and calcinated at 700 °C for 2 h in air. After cooling down, these pellets were reground into fine powders and repressed into pellets under axial pressure (12 MPa). After sintering at 1150 °C for 12 h in air atmosphere, all the pellets were ground for 2 h before characterizations and electrochemistry tests. Sr0.5Ba0.5Fe0.45Nb1.55O6 denoted as SBNF45 and Sr0.4Ba0.4Co0.2Nb2CoO6 denoted as (SBC)N were also prepared under the same conditions. KNb0.775Co0.225O3 (KNC), LiNb0.925Co0.075O3 (LNC075), and LiNb0.775Co0.225O3 (LNC225) were prepared by following the same procedure except for their relatively lower final sintering temperature (1000 °C). Commercial IrO2 (99.9%) with a Brunauer–Emmett–Teller (BET) surface area of ≈32.5 m2 g−1 was also purchased from Aldrich Ltd. and tested after grinding.
Fe2o3
Manufactured by Merck Group
Sourced in Germany, United States, United Kingdom
Fe2O3 is a chemical compound composed of iron and oxygen. It is a reddish-brown powder that is commonly used as a raw material in various industrial and laboratory applications.
Automatically generated - may contain errors
Lab products found in correlation
Nb2o5, by Merck Group (3 mentions)
Srco3, by Merck Group (3 mentions)
Bi2o3, by Merck Group (3 mentions)
Caco3, by Merck Group (3 mentions)
Al2o3, by Merck Group (3 mentions)
Mn2o3, by Merck Group (2 mentions)
Co3o4, by Merck Group (2 mentions)
Agarose, by Thermo Fisher Scientific (2 mentions)
Boric acid, by Merck Group (2 mentions)
Sodium hydroxide (naoh), by Merck Group (2 mentions)
Hydrochloric acid (hcl), by Merck Group (2 mentions)
Lino3, by Merck Group (1 mentions)
Co no3 2 6h2o, by Merck Group (1 mentions)
Sr no3 2, by Merck Group (1 mentions)
N methyl pyrrolidone (nmp), by Merck Group (1 mentions)
Li2co3, by Merck Group (1 mentions)
La2o3, by Merck Group (1 mentions)
H2so4, by Merck Group (1 mentions)
Sm2o3, by Merck Group (1 mentions)
Eu2o3, by Merck Group (1 mentions)
38 protocols using fe2o3
1
Solid-State Synthesis of Perovskite Oxides
2
Graphite-based Electrode Fabrication
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The chemicals used were as follows: Graphite powder, Co3O4 powder (30 nm, 99%, Aldrich, Darmstadt, Germany), Fe2O3 (30 nm, 99%, Aldrich), sulfuric acid (95%), potassium permanganate (KMnO4), hydrochloric acid, hydrogen peroxide, Hydrazine, toluene, polyvinylidene fluoride (PVdF), N-methylpyrrolidone (NMP) (Sigma Aldrich, Darmstadt, Germany), copper foil (10 mm thickness, Schlenk Metallfolien, Germany), electrolyte 1M lithium hexafluorophosphate solution (LiPF6) in ethylene carbonate (EC): diethyl carbonate (DEC): ethyl methyl carbonate (EMC) (1:1:1, by weight, Danvec, Singapore) and Celgard 2320 separator.
3
Synthesis of Fe-Doped LLZO Garnets
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A series of Li7−3xFe3+xLa3Zr2O12 garnets with intended mole fractions (xint) of Fe3+ with xint=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.
4
Evaluating Interference Effects on Quartz Analysis
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To investigate the effect of the interference, synthetic air samples were prepared by mixing of pure α-quartz with a variety of other pure materials. Three materials, cristobalite (NIST CRM1879a), kaolinite (Ajax Chemicals Pty Ltd), and iron oxide (Fe2O3, Merck & Co. Inc.) were selected since they were detected as common matrices in the workplace samples.
The synthetic samples were prepared in two steps. At first, approximately 0.1 mg of pure α-quartz was deposited onto a filter by a plastic cyclone sampler following the same procedure as the standard air samples above and weighted. Then, one of the matrices was deposited onto the filter by the same procedure and reweighed. The total dust loadings for all samples were less than 1 mg. The matrix concentration against the total dust was calculated with these gravimetric results. The range of the matrix concentration was aimed to have a comparable range to the workplace samples. Any effect of the layering of the materials was considered to be negligible as the dust loadings were less than 1 mg (ISO, 2015 ; Skoog et al., 2017 ).
The synthetic samples were prepared in two steps. At first, approximately 0.1 mg of pure α-quartz was deposited onto a filter by a plastic cyclone sampler following the same procedure as the standard air samples above and weighted. Then, one of the matrices was deposited onto the filter by the same procedure and reweighed. The total dust loadings for all samples were less than 1 mg. The matrix concentration against the total dust was calculated with these gravimetric results. The range of the matrix concentration was aimed to have a comparable range to the workplace samples. Any effect of the layering of the materials was considered to be negligible as the dust loadings were less than 1 mg (ISO, 2015 ; Skoog et al., 2017 ).
5
Hematite and Titanium Dioxide Nanocomposite
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All chemicals were of reagent grade and used without purification. MB (C16H18ClN3S, >97%) was manufactured by Kemika (Zagreb, Croatia); H2SO4 (95–97%) was provided from Merck (Darmstadt, Germany); NaOH (ZorkaPharm, Šabac, Serbia); Fe2O3 (commercial nanopowder, grain sizes <50 nm, Merck, Germany), Fe2O3(1) (synthesized hematite nanoparticles by [26 (link)], Fe2O3(2) (synthesized hematite nanoparticles by [27 (link)]). Commercial TiO2(1) (Hombikat, CAS No 13463-67-7, surface area 35–65 m2/g and 21 nm primary particle size, anatase, Sigma-Aldrich Chemie GmbH, Steinheim, Germany) and TiO2 (Molar Chemicals KFT, Halásztelek, Hungary) were also used for the synthesis of the nanocomposite. All solutions were prepared using ultrapure water. The aqueous stock solution of MB had a concentration of 2.45 × 10−2 mM.
6
Synthesis of RSrCoFeO6 Perovskites
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The RSrCoFeO6 (R =
Sm, Eu) samples were prepared by using the solid-state
reaction process. First, the precursor oxides Sm2O3 (Alfa Aesar, 99.9% REO), Eu2O3 (Alfa
Aesar, 99.9% REO), SrCO3 (Merck), Co2O3 (Merck, >99%), and Fe2O3 (Merck, >99%)
were
mixed in the proper stoichiometric ratio. Afterward, we placed the
mixture together with 20 zirconia balls (∼5 mm diameter) in
a Retsch PM100 planetary ball mill at 450 rpm for 30 min (dry without
a medium). Finally, the powder was thermally treated for 12 h at 1100
°C in an air atmosphere, thus obtaining the final compounds.
Sm, Eu) samples were prepared by using the solid-state
reaction process. First, the precursor oxides Sm2O3 (Alfa Aesar, 99.9% REO), Eu2O3 (Alfa
Aesar, 99.9% REO), SrCO3 (Merck), Co2O3 (Merck, >99%), and Fe2O3 (Merck, >99%)
were
mixed in the proper stoichiometric ratio. Afterward, we placed the
mixture together with 20 zirconia balls (∼5 mm diameter) in
a Retsch PM100 planetary ball mill at 450 rpm for 30 min (dry without
a medium). Finally, the powder was thermally treated for 12 h at 1100
°C in an air atmosphere, thus obtaining the final compounds.
7
Synthesis and Characterization of NaCu0.2Fe0.3Mn0.5O2
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The NaCu0.2Fe0.3Mn0.5O2 compound was synthesized using a solid-state reaction. The precursors, of Na2CO3 (99%), CuO (99%), Fe2O3 (99%) and Mn2O3 (99%) were obtained from Sigma-Aldrich, and were mixed in proportional ratios. The obtained powder was burned at 500 °C for 16 h, and then, the sample was ground, pressed into pellets and transferred to an oven at 850 °C for 24 h.
To determine the purity of the sample, powder XRD was performed using a Bruker D8 Discover with Twin/Twin optics, at room temperature, with Cu Kα radiation (λ = 1.5406 Å, 10° ≤ 2θ ≤ 80°). To precisely determine the optical properties of the prepared sample, a Shimadzu UV-3101 PC scanning spectrophotometer was used at room temperature, with a wavelength range of 200–800 nm, with a sample pellet of 0.5 mm of diameter. Finally, the electrical property measurements were obtained using complex impedance spectroscopy with a Solartron SI 1260 impedance/gain phase analyzer in the temperature and frequency ranges of 333–453 K and 10−1 to 106 Hz, respectively, with a sample pellet with a thickness of 1 mm and a diameter of 8 mm.
To determine the purity of the sample, powder XRD was performed using a Bruker D8 Discover with Twin/Twin optics, at room temperature, with Cu Kα radiation (λ = 1.5406 Å, 10° ≤ 2θ ≤ 80°). To precisely determine the optical properties of the prepared sample, a Shimadzu UV-3101 PC scanning spectrophotometer was used at room temperature, with a wavelength range of 200–800 nm, with a sample pellet of 0.5 mm of diameter. Finally, the electrical property measurements were obtained using complex impedance spectroscopy with a Solartron SI 1260 impedance/gain phase analyzer in the temperature and frequency ranges of 333–453 K and 10−1 to 106 Hz, respectively, with a sample pellet with a thickness of 1 mm and a diameter of 8 mm.
8
Synthesis and Characterization of BCFO Thin Films
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Pellets with 10% bismuth excess were synthesized by mixing Bi2O3 (99.9%), CaO (99.995%) and Fe2O3 (99.9%) powders (Sigma-Aldrich) with different xCas. The pellets were pressurized to form 1-inch-diameter button-shaped targets. They were calcinated at 800 °C for 8 h in ambient conditions. After the calcination, the pellets were ground into fine powders, and formed into the same shape as the previous targets. Then, they were sintered at 850 °C for 8.5 h under ambient conditions. The epitaxial BCFO thin films (xCa = 0.1–0.6) were deposited on a SrTiO3 (001) substrate (CrysTec GmbH) using pulsed laser deposition with a KrF excimer laser (λ = 248 nm). The heater T during film growth was 665 °C in an oxygen environment of 0.07 Torr. Laser fluence and repetition rate were set to be ~1 J cm−2 and 10 Hz. All the films were in-situ cooled down to room T at a rate of 10 °C min−1 under an oxygen environment of 500 Torr. The c-axis lattice parameters of the as-grown BCFO thin films were characterized using a four-circle X-ray diffractometer (PANalytical X’Pert PRO MRD) with Cu Kα1 radiation. We measured 2θ−ω X-ray scans from 10° to 60° at an interval of 0.1°. We also performed reciprocal space maps and line scans using a synchrotron source (Beamline 3A, PLS II) in Pohang Accelerator Laboratory.
9
Solid-State Reactive Sintering of CSO-FeCo2O4
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Commercial powders of Ce0.8Sm0.2O2−δ (CSO, Kceracell, Korea), Fe2O3 and Co3O4 (Sigma-Aldrich, Germany) were used for solid-state reactive sintering. Respective amounts of powders were weighed for nominal CSO-FeCo2O4 compositions with a weight percent ratio of 60:40. The powder mixture was ball milled in ethanol for 48 h on a roller bench with 175 rpm. After drying in ambient air at 70 °C the powder mixture was pressed with an uniaxial press in disc-shaped membranes with d = 20 mm. The discs were sintered with a heating rate of 5 K/min to 1200 °C and a dwell time of 5 h. At the sintering temperature, the spinel is partially reduced into a high-temperature monoxide phase with rock salt structure. Therefore, a slow rate of 0.5 K/min between 900 and 800 °C is implemented in the cooling cycle in order to enable complete re-oxidation of the high-temperature Co/Fe monoxide to the respective spinel phase according to the Fe3−xCoxO4 phase diagram [10 (link)].
For electrical conductivity measurements, the samples were burnished using sanding paper (1200 graining). For KFPM measurements, the samples were embedded in epoxy resin and polished to mirror using diamond polishing paste. The roughness of the polished samples was around 50 nm.
For electrical conductivity measurements, the samples were burnished using sanding paper (1200 graining). For KFPM measurements, the samples were embedded in epoxy resin and polished to mirror using diamond polishing paste. The roughness of the polished samples was around 50 nm.
10
Pulsed Laser Deposition of STFO and GDC Thin Films
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The GDC target (Ce0.8Gd0.2O2 − δ) for pulsed laser deposition was prepared from powder (Treibacher, Austria) by isostatical pressing and subsequent sintering at 1550 °C for 5 h. The STFO (SrTi0.7Fe0.3O3 − δ) powder was prepared by solid state reaction from SrCO3 (99.99% pure, Sigma-Aldrich), TiO2 (99.99% pure, Sigma Aldrich), and Fe2O3 (99.98% pure, Sigma Aldrich). The educts were thoroughly mixed, calcined at 800 °C, ground, again calcined at 1000 °C, and—after a further grinding step—isostatically pressed and sintered at 1250 °C. The phase purity of both targets was confirmed by X-ray diffraction. STFO and GDC thin films were deposited on (100)-oriented yttria stabilized zirconia single crystals (YSZ, 9.5 mol% Y2O3 in ZrO2, supplier: CrysTec, Germany) by pulsed laser deposition (PLD) using a KrF excimer-laser (Lambda COMPexPro 201 F, 248 nm wavelength). The deposition of 200 nm thin films was carried out in 4 × 10− 2 mbar of pure oxygen with a pulse repetition rate of 5 Hz and a nominal pulse energy of 400 mJ. The substrate temperature during the deposition was controlled by a pyrometer (Heitronics, Germany) and was 650 °C.
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