Pub Date : 2024-09-15DOI: 10.1134/s0036023624601788
K. F. Shumovskaya, M. E. Komshina, M. V. Sukhanov, S. D. Plekhovich, A. D. Plekhovich, P. A. Otopkova, O. Yu. Troshin, A. D. Bulanov
Abstract
Samples of amorphous silicon dioxide have been synthesized from silicon with natural isotope abundance; silicon highly enriched in silicon-28, silicon-29, or silicon-30 with a degree of enrichment from 99.29 ± 0.01 to 99.9980 ± 0.0010 at %; and silicon being a mixture of silicon-28 and silicon-30. The samples were studied by IR spectroscopy. The IR spectra of the samples demonstrate a low-frequency shift of the known stretching and bending vibration absorption bands for the silicon-29 and silicon-30 isotopes by 0.1–30.1 cm–1 compared to silicon-28. For the silicon dioxides containing a mixture of silicon-28 and silicon-30 isotopes and with natural isotope composition, there is a deviation from the linear dependence of the vibration frequency of monoisotopic samples. The positions of the absorption band maxima in the model IR spectrum of silicon dioxide have been calculated by the DFT method. The results obtained correlate with experimental data with high accuracy. The reduced mass and force constant of vibrating groups of atoms in silicon dioxide were determined, and the influence of these factors on the isotopic shift in the IR spectrum of silicon dioxide, depending on the type of vibration, was established.
{"title":"Isotope Effect in IR Spectra of Highly Enriched Amorphous Silicon Dioxide ASiO2 (A = 28, 29, 30)","authors":"K. F. Shumovskaya, M. E. Komshina, M. V. Sukhanov, S. D. Plekhovich, A. D. Plekhovich, P. A. Otopkova, O. Yu. Troshin, A. D. Bulanov","doi":"10.1134/s0036023624601788","DOIUrl":"https://doi.org/10.1134/s0036023624601788","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Samples of amorphous silicon dioxide have been synthesized from silicon with natural isotope abundance; silicon highly enriched in silicon-28, silicon-29, or silicon-30 with a degree of enrichment from 99.29 ± 0.01 to 99.9980 ± 0.0010 at %; and silicon being a mixture of silicon-28 and silicon-30. The samples were studied by IR spectroscopy. The IR spectra of the samples demonstrate a low-frequency shift of the known stretching and bending vibration absorption bands for the silicon-29 and silicon-30 isotopes by 0.1–30.1 cm<sup>–1</sup> compared to silicon-28. For the silicon dioxides containing a mixture of silicon-28 and silicon-30 isotopes and with natural isotope composition, there is a deviation from the linear dependence of the vibration frequency of monoisotopic samples. The positions of the absorption band maxima in the model IR spectrum of silicon dioxide have been calculated by the DFT method. The results obtained correlate with experimental data with high accuracy. The reduced mass and force constant of vibrating groups of atoms in silicon dioxide were determined, and the influence of these factors on the isotopic shift in the IR spectrum of silicon dioxide, depending on the type of vibration, was established.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-09-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142251740","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-15DOI: 10.1134/s003602362460179x
D. N. Grishchenko, M. A. Medkov
Abstract
Bioglass 45S5 was doped with bismuth oxide in concentrations up to 40 wt %. The amorphism of the synthesized glasses was confirmed by X-ray powder diffraction. The influence of Bi2O3 on the properties of the bioactive glass was studied. In a series of samples containing 0 to 40 wt % bismuth oxide, the glass characteristics change as follows: pH in the model medium decreases from 7.84 to 7.46 upon glass leaching; radiopacity increases from 1150 HU to values above 11 000 HU; percent chemical degradation drops from 1.299% to 0.424%; bioactivity decreases in the range 0–10 wt % Bi2O3 and is absent in the range 20–40 wt % Bi2O3. The bioactive glasses containing up to 10 wt % Bi2O3 can find application in reconstructive surgery. They have radiopaque and bioactive properties. The bioactive glasses containing 20–40 wt % Bi2O3 have high radiopacity and chemical durability, and only weakly affect pH when dissolved. They may be candidate radiomodifier materials for the radiation therapy of malignant neoplasms.
{"title":"Bi2O3-Doped Bioglass 45S5 for Medical Use","authors":"D. N. Grishchenko, M. A. Medkov","doi":"10.1134/s003602362460179x","DOIUrl":"https://doi.org/10.1134/s003602362460179x","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Bioglass 45S5 was doped with bismuth oxide in concentrations up to 40 wt %. The amorphism of the synthesized glasses was confirmed by X-ray powder diffraction. The influence of Bi<sub>2</sub>O<sub>3</sub> on the properties of the bioactive glass was studied. In a series of samples containing 0 to 40 wt % bismuth oxide, the glass characteristics change as follows: pH in the model medium decreases from 7.84 to 7.46 upon glass leaching; radiopacity increases from 1150 HU to values above 11 000 HU; percent chemical degradation drops from 1.299% to 0.424%; bioactivity decreases in the range 0–10 wt % Bi<sub>2</sub>O<sub>3</sub> and is absent in the range 20–40 wt % Bi<sub>2</sub>O<sub>3</sub>. The bioactive glasses containing up to 10 wt % Bi<sub>2</sub>O<sub>3</sub> can find application in reconstructive surgery. They have radiopaque and bioactive properties. The bioactive glasses containing 20–40 wt % Bi<sub>2</sub>O<sub>3</sub> have high radiopacity and chemical durability, and only weakly affect pH when dissolved. They may be candidate radiomodifier materials for the radiation therapy of malignant neoplasms.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-09-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142251742","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-15DOI: 10.1134/s0036023624601715
E. P. Simonenko, A. S. Mokrushin, I. A. Nagornov, S. A. Dmitrieva, T. L. Simonenko, N. P. Simonenko, N. T. Kuznetsov
Abstract
The process of modification Ti2CTx MXene multilayer by hydrothermal synthesis of bulk hierarchically organized formations of Co(CO3)0.5(OH)⋅0.11H2O has been studied. It is shown that under the chosen conditions the MXene is partially oxidized to form aggregates of titanium dioxide nanoparticles with a diameter of ~3–10 nm on its surface. The sensing properties of the obtained composite material at room temperature and relative humidity 65 ± 3% to a wide range of gaseous analytes (50 ppm CO, benzene, acetone, ethanol, 2500 ppm H2, CH4, 5% O2, and 40 ppm NH3, NO2) have been investigated. Increased sensitivity has been found for the detection of 40 ppm NH3 and NO2: the responses have been found to be 91 and 63%, respectively. Some aspects of the detection mechanism are discussed. The results obtained show promising modification of multilayer MXene with semiconducting metal oxides and hierarchically formed bulk formations in order to improve its chemoresistive properties.
{"title":"Preparation and Chemosensory Properties of Nanocomposite Obtained by Hydrothermal Modification of Ti2CTx with Hierarchically Organized Co(CO3)0.5(OH)⋅0.11H2O","authors":"E. P. Simonenko, A. S. Mokrushin, I. A. Nagornov, S. A. Dmitrieva, T. L. Simonenko, N. P. Simonenko, N. T. Kuznetsov","doi":"10.1134/s0036023624601715","DOIUrl":"https://doi.org/10.1134/s0036023624601715","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>The process of modification Ti<sub>2</sub>CT<sub><i>x</i></sub> MXene multilayer by hydrothermal synthesis of bulk hierarchically organized formations of Co(CO<sub>3</sub>)<sub>0.5</sub>(OH)⋅0.11H<sub>2</sub>O has been studied. It is shown that under the chosen conditions the MXene is partially oxidized to form aggregates of titanium dioxide nanoparticles with a diameter of ~3–10 nm on its surface. The sensing properties of the obtained composite material at room temperature and relative humidity 65 ± 3% to a wide range of gaseous analytes (50 ppm CO, benzene, acetone, ethanol, 2500 ppm H<sub>2</sub>, CH<sub>4</sub>, 5% O<sub>2</sub>, and 40 ppm NH<sub>3</sub>, NO<sub>2</sub>) have been investigated. Increased sensitivity has been found for the detection of 40 ppm NH<sub>3</sub> and NO<sub>2</sub>: the responses have been found to be 91 and 63%, respectively. Some aspects of the detection mechanism are discussed. The results obtained show promising modification of multilayer MXene with semiconducting metal oxides and hierarchically formed bulk formations in order to improve its chemoresistive properties.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-09-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142251748","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-15DOI: 10.1134/s0036023624602034
N. M. Khaidukov, M. N. Brekhovskikh, N. Yu. Kirikova, V. A. Kondratyuk, V. N. Makhov
Abstract
Ceramic samples of europium-doped multi-component fluorides Na3CaMg3AlF14 and NaCaMg2F7 were prepared by high-temperature solid-phase reactions. The prepared compounds both have cubic pyrochlore structures. A comparison of the X-ray diffraction patterns for the prepared compounds confirms that Na3CaMg3AlF14 was prepared as a new polymorph with a cubic pyrochlore structure, which differs from its rhombohedral phase described in the literature. The addition of NH4(HF2) before the last annealing provided reducing conditions for the stabilization of europium ions exclusively in the 2+ charge state. The Eu2+ ions in the synthesized fluoride matrices luminesce with a band peaking at about 395 nm due to 4f65d–4f7 interconfiguration transitions. The Eu2+ ions doped into these matrices form predominantly a single type of optical center, which provides for a fairly narrow width (FWHM ~ 30 nm) of the 4f65d–4f7 emission band. Also, the Eu2+ ions in the prepared ceramics emit narrow-line luminescence with the major line at about 362 nm, associated with 4f7–4f7 intraconfiguration transitions from the lowest excited state 6P7/2 to the ground state 8S7/2. The prepared ceramics exhibit a good thermal stability of 4f65d–4f7 luminescence of Eu2+ with the thermal quenching temperature T1/2 equal to 504 and 543 K for Na3CaMg3AlF14:Eu2+ (1.0 at %) and NaCaMg2F7:Eu2+ (0.5 at %), respectively. This property may be of interest for the practical application of these phosphors. Additional annealing of the ceramics under an argon atmosphere with the addition of NaHF2 instead of NH4(HF2) led to a partial conversion of europium ions from the divalent to trivalent state. As a result, a series of narrow luminescence lines appeared in the red region of the spectrum due to 4f6–4f6 (5D0 → 7FJ) intraconfiguration transitions in Eu3+.
{"title":"Luminescence Features of Multicomponent Cubic Fluoride Pyrochlores Doped with Europium Ions","authors":"N. M. Khaidukov, M. N. Brekhovskikh, N. Yu. Kirikova, V. A. Kondratyuk, V. N. Makhov","doi":"10.1134/s0036023624602034","DOIUrl":"https://doi.org/10.1134/s0036023624602034","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Ceramic samples of europium-doped multi-component fluorides Na<sub>3</sub>CaMg<sub>3</sub>AlF<sub>14</sub> and NaCaMg<sub>2</sub>F<sub>7</sub> were prepared by high-temperature solid-phase reactions. The prepared compounds both have cubic pyrochlore structures. A comparison of the X-ray diffraction patterns for the prepared compounds confirms that Na<sub>3</sub>CaMg<sub>3</sub>AlF<sub>14</sub> was prepared as a new polymorph with a cubic pyrochlore structure, which differs from its rhombohedral phase described in the literature. The addition of NH<sub>4</sub>(HF<sub>2</sub>) before the last annealing provided reducing conditions for the stabilization of europium ions exclusively in the 2+ charge state. The Eu<sup>2+</sup> ions in the synthesized fluoride matrices luminesce with a band peaking at about 395 nm due to 4<i>f</i> <sup>6</sup>5<i>d</i>–4<i>f</i> <sup>7</sup> interconfiguration transitions. The Eu<sup>2+</sup> ions doped into these matrices form predominantly a single type of optical center, which provides for a fairly narrow width (FWHM ~ 30 nm) of the 4<i>f</i> <sup>6</sup>5<i>d</i>–4<i>f</i> <sup>7</sup> emission band. Also, the Eu<sup>2+</sup> ions in the prepared ceramics emit narrow-line luminescence with the major line at about 362 nm, associated with 4<i>f</i> <sup>7</sup>–4<i>f</i> <sup>7</sup> intraconfiguration transitions from the lowest excited state <sup>6</sup>P<sub>7/2</sub> to the ground state <sup>8</sup>S<sub>7/2</sub>. The prepared ceramics exhibit a good thermal stability of 4<i>f</i> <sup>6</sup>5<i>d</i>–4<i>f</i> <sup>7</sup> luminescence of Eu<sup>2+</sup> with the thermal quenching temperature <i>T</i><sub>1/2</sub> equal to 504 and 543 K for Na<sub>3</sub>CaMg<sub>3</sub>AlF<sub>14</sub>:Eu<sup>2+</sup> (1.0 at %) and NaCaMg<sub>2</sub>F<sub>7</sub>:Eu<sup>2+</sup> (0.5 at %), respectively. This property may be of interest for the practical application of these phosphors. Additional annealing of the ceramics under an argon atmosphere with the addition of NaHF<sub>2</sub> instead of NH<sub>4</sub>(HF<sub>2</sub>) led to a partial conversion of europium ions from the divalent to trivalent state. As a result, a series of narrow luminescence lines appeared in the red region of the spectrum due to 4<i>f</i> <sup>6</sup>–4<i>f</i> <sup>6</sup> (<sup>5</sup>D<sub>0</sub> → <sup>7</sup>F<sub>J</sub>) intraconfiguration transitions in Eu<sup>3+</sup>.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-09-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142251737","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-29DOI: 10.1134/s0036023624601338
Pushpanjali Singh, Amit K. Sharma, Pawan Kumar, Dharm Veer, Devendra Kumar, Deshraj Singh, Ram S. Katiyar
Abstract
Solid acid composites of (1 – x)NaH2PO4/xCeP2O7 (x = 0.1–0.4) with different molar weight ratio of NaH2PO4 (SDP) and CeP2O7 were synthesized and characterized. The characterization of solid acid composites was carried out to determine the structures, thermal stability, and conductivity, utilizing X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray analysis (EDX), thermogravimetric analysis (TGA), differential thermal analysis (DTA), and conductivity measurements. The electrolyte pellets of composite powder were prepared for the determination of ionic conductivity. The presence of CeP2O7 in the composite had a large impact on the conductivity measurements and increased the ionic conductivity of NaH2PO4. The thermal stability of the solid acid composites for dehydration, melting, and decomposition was investigated in the temperature range of 50 to 500°C under open atmospheric environments.
{"title":"Role of Pyrophosphate Source for Improving Proton Conductivity and Stability of Sodium Dihydrogen Phosphate","authors":"Pushpanjali Singh, Amit K. Sharma, Pawan Kumar, Dharm Veer, Devendra Kumar, Deshraj Singh, Ram S. Katiyar","doi":"10.1134/s0036023624601338","DOIUrl":"https://doi.org/10.1134/s0036023624601338","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Solid acid composites of (1 – <i>x</i>)NaH<sub>2</sub>PO<sub>4</sub>/<i>x</i>CeP<sub>2</sub>O<sub>7</sub> (<i>x</i> = 0.1–0.4) with different molar weight ratio of NaH<sub>2</sub>PO<sub>4</sub> (SDP) and CeP<sub>2</sub>O<sub>7</sub> were synthesized and characterized. The characterization of solid acid composites was carried out to determine the structures, thermal stability, and conductivity, utilizing X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray analysis (EDX), thermogravimetric analysis (TGA), differential thermal analysis (DTA), and conductivity measurements. The electrolyte pellets of composite powder were prepared for the determination of ionic conductivity. The presence of CeP<sub>2</sub>O<sub>7</sub> in the composite had a large impact on the conductivity measurements and increased the ionic conductivity of NaH<sub>2</sub>PO<sub>4</sub>. The thermal stability of the solid acid composites for dehydration, melting, and decomposition was investigated in the temperature range of 50 to 500°C under open atmospheric environments.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142201208","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-29DOI: 10.1134/s0036023624601521
I. U. Muzaddadi, A. Murugan, M. Hemamalini, M. N. Tahir, N. Raman, B. Bezbaruah, B. Ahmed, A. Manohar, A. Kulandaisamy, M. F. Hussain, T. Rajkumar
Abstract
Meso 5,10,15,20-tetrakis(3,4,5-trimethoxyphenyl)porphyrin [H2T(3,4,5-OCH3)PP] and its Ni complex [T(3,4,5-OCH3)PP Ni] (complex 1) have been prepared. Its oxidation characteristics were examined using diverse analytical techniques, such as UV-visible spectrophotometry (UV-Vis), electron paramagnetic resonance (EPR), cyclic voltammetry (CV), and nuclear magnetic resonance (NMR) with antimony pentachloride (SbCl5) or trifluoroacetic acid (TFA). The structure of the titled compound has been confirmed by single-crystal analysis. Cyclic voltammetry study of complex 1 provides that NiII is converted to NiIII porphyrin through π-cation radical formation which is further EPR supported by IR spectrum peaks at 1276 cm–1 with the addition of SbCl5. The confirmation of formation of the π-cation radical has been established by the emergence of a novel peak at 649.5 nm in the UV-visible spectrum. This peak, indicative of oxidation, was observed at the central Ni ion, distinguishing it from the porphyrin macrocycle. Additionally, the EPR spectrum informed the formation of Ni(III) from Ni(II) porphyrin which is oxidized with SbCl5 or CF3COOH (TFA) as (d_{z}^{2}) orbital has a single electron with high spin, S = 3/2 ground state in complex 1. Crystallographic analysis and Hirshfeld surface analysis, show hydrogen bonding and molecular packing in the crystal lattice. DFT calculation and experimental HOMO–LUMO gap in solvent closely align with the theoretically determined HOMO–LUMO energy difference (0.92 eV) for complex 1.
{"title":"Investigation of Oxidative Behaviour and Structural Insights of (3,4,5-Trimethoxyphenyl)Porphyrin Ni(II) Complex: Experimental and Theoretical Study","authors":"I. U. Muzaddadi, A. Murugan, M. Hemamalini, M. N. Tahir, N. Raman, B. Bezbaruah, B. Ahmed, A. Manohar, A. Kulandaisamy, M. F. Hussain, T. Rajkumar","doi":"10.1134/s0036023624601521","DOIUrl":"https://doi.org/10.1134/s0036023624601521","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p><i>Meso</i> 5,10,15,20-tetrakis(3,4,5-trimethoxyphenyl)porphyrin [H<sub>2</sub>T(3,4,5-OCH<sub>3</sub>)PP] and its Ni complex [T(3,4,5-OCH<sub>3</sub>)PP Ni] (complex <b>1</b>) have been prepared. Its oxidation characteristics were examined using diverse analytical techniques, such as UV-visible spectrophotometry (UV-Vis), electron paramagnetic resonance (EPR), cyclic voltammetry (CV), and nuclear magnetic resonance (NMR) with antimony pentachloride (SbCl<sub>5</sub>) or trifluoroacetic acid (TFA). The structure of the titled compound has been confirmed by single-crystal analysis. Cyclic voltammetry study of complex <b>1</b> provides that Ni<sup>II</sup> is converted to Ni<sup>III</sup> porphyrin through π-cation radical formation which is further EPR supported by IR spectrum peaks at 1276 cm<sup>–1</sup> with the addition of SbCl<sub>5</sub>. The confirmation of formation of the π-cation radical has been established by the emergence of a novel peak at 649.5 nm in the UV-visible spectrum. This peak, indicative of oxidation, was observed at the central Ni ion, distinguishing it from the porphyrin macrocycle. Additionally, the EPR spectrum informed the formation of Ni(III) from Ni(II) porphyrin which is oxidized with SbCl<sub>5</sub> or CF<sub>3</sub>COOH (TFA) as <span>(d_{z}^{2})</span> orbital has a single electron with high spin, <i>S</i> = 3/2 ground state in complex <b>1</b>. Crystallographic analysis and Hirshfeld surface analysis, show hydrogen bonding and molecular packing in the crystal lattice. DFT calculation and experimental HOMO–LUMO gap in solvent closely align with the theoretically determined HOMO–LUMO energy difference (0.92 eV) for complex <b>1</b>.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142201207","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-23DOI: 10.1134/s0036023624601156
I. A. Shentseva, K. A. Tagiltsev, A. N. Usol’tsev, N. A. Korobeynikov, V. R. Shayapov, M. N. Sokolov, S. A. Adonin
Abstract
New antimony complexes, (3-Br-1-EtPy)3[Sb2I9] (1) and (1,2-Me2Py)4[Sb8I28] (2) have been prepared by the reaction of SbI3 with iodides of the corresponding cations in organic solvents. The features of the crystal structure of the compounds have been determined by X-ray diffraction. The complexes are thermally stable at least up to 200°C and have a band gap of ~2.2 eV.
{"title":"Di- and Octanuclear 1,2-Dimethylpyridinium and 3-Bromo-1-Ethylpyridinium Iodoantimonates(III): Crystal Structure and Physicochemical Properties","authors":"I. A. Shentseva, K. A. Tagiltsev, A. N. Usol’tsev, N. A. Korobeynikov, V. R. Shayapov, M. N. Sokolov, S. A. Adonin","doi":"10.1134/s0036023624601156","DOIUrl":"https://doi.org/10.1134/s0036023624601156","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>New antimony complexes, (3-Br-1-EtPy)<sub>3</sub>[Sb<sub>2</sub>I<sub>9</sub>] (<b>1</b>) and (1,2-Me<sub>2</sub>Py)<sub>4</sub>[Sb<sub>8</sub>I<sub>28</sub>] (<b>2</b>) have been prepared by the reaction of SbI<sub>3</sub> with iodides of the corresponding cations in organic solvents. The features of the crystal structure of the compounds have been determined by X-ray diffraction. The complexes are thermally stable at least up to 200°C and have a band gap of ~2.2 eV.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-08-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142201212","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-23DOI: 10.1134/s0036023624700554
G. S. Zakharova, N. V. Podval’naya, T. I. Gorbunova, M. G. Pervova, A. N. Enyashin
Abstract
Hexagonal h-WO3-based substitutional solid solutions of general formula h-W1–xFexO3, where 0.01 ≤ x ≤ 0.06 were prepared by hydrothermal synthesis. The crystal lattice of the prepared h-W1–xFexO3 compounds is stabilized by ({text{NH}}_{4}^{ + }) ions in hexagonal channels. Quantum-chemical calculations showed that dopant iron ions replace cations in the tungsten sublattice, and are not intercalated into lattice channels. The dopant is not an independent participant in reactions involving h-W1–xFexO3, but only causes the reorganization of the near-Fermi states of the h-WO3 matrix. The extent of the dopant homogeneity range of the solid solution is determined by the pH of the working solution. The h-W0.94Fe0.06O3 prepared at pH 2.3 has the largest specific surface area, equal to 108 m2/g. Its photocatalytic activity in 1,2,4-trichlorobenzene (TCB) photodegradation is several times that of m-W0.94Fe0.06O3.
{"title":"Hydrothermal Synthesis and Photocatalytic Properties of Iron-Doped Tungsten Oxide","authors":"G. S. Zakharova, N. V. Podval’naya, T. I. Gorbunova, M. G. Pervova, A. N. Enyashin","doi":"10.1134/s0036023624700554","DOIUrl":"https://doi.org/10.1134/s0036023624700554","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Hexagonal <i>h</i>-WO<sub>3</sub>-based substitutional solid solutions of general formula <i>h-</i>W<sub>1–<i>x</i></sub>Fe<sub><i>x</i></sub>O<sub>3</sub>, where 0.01 ≤ <i>x</i> ≤ 0.06 were prepared by hydrothermal synthesis. The crystal lattice of the prepared <i>h-</i>W<sub>1–<i>x</i></sub>Fe<sub><i>x</i></sub>O<sub>3</sub> compounds is stabilized by <span>({text{NH}}_{4}^{ + })</span> ions in hexagonal channels. Quantum-chemical calculations showed that dopant iron ions replace cations in the tungsten sublattice, and are not intercalated into lattice channels. The dopant is not an independent participant in reactions involving <i>h</i>-W<sub>1–<i>x</i></sub>Fe<sub><i>x</i></sub>O<sub>3</sub>, but only causes the reorganization of the near-Fermi states of the <i>h</i>-WO<sub>3</sub> matrix. The extent of the dopant homogeneity range of the solid solution is determined by the pH of the working solution. The <i>h</i>-W<sub>0.94</sub>Fe<sub>0.06</sub>O<sub>3</sub> prepared at pH 2.3 has the largest specific surface area, equal to 108 m<sup>2</sup>/g. Its photocatalytic activity in 1,2,4-trichlorobenzene (TCB) photodegradation is several times that of <i>m</i>-W<sub>0.94</sub>Fe<sub>0.06</sub>O<sub>3</sub>.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-08-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142201216","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-23DOI: 10.1134/s003602362460117x
M. N. Smirnova, O. N. Kondrat’eva, G. E. Nikiforova, A. D. Yapryntsev, A. A. Averin, A. V. Khoroshilov
Abstract
This work reports on the possibility of producing oxide InGaMgO4 by two-stage heat treatment of glycine-, starch- and PVA-nitrate precursors. The products formed as a result of their heating at low temperatures (≈ 90°С) were studied by powder X-ray diffraction. It was found that the powder formed from the glycine-nitrate precursor contains nanocrystalline In2O3, and drying of the polymer-nitrate compositions leads to the production of a thermally stable X-ray amorphous product. Its annealing at temperatures above 800°C allows synthesizing powder InGaMgO4 free of impurity phases. High-temperature treatment of the powder formed from the glycine-nitrate precursor also leads to the production of InGaMgO4, but does not remove the In2O3 impurity. Using scanning electron microscopy, it was found that single-phase InGaMgO4 powders synthesized from polymer-nitrate precursors have a similar grain structure but differ in grain size distribution. Presumably, this difference is due to the structural features of starch and PVA macromolecules used for the preparation of precursors. Oxide InGaMgO4 was characterized using differential scanning calorimetry, Raman and diffuse reflectance spectroscopy. The value of its band gap energy Eg was determined using the Tauc method.
{"title":"Features of Synthesis of InGaMgO4 from Nitrate-Organic Precursors and Study of Its Physical Properties","authors":"M. N. Smirnova, O. N. Kondrat’eva, G. E. Nikiforova, A. D. Yapryntsev, A. A. Averin, A. V. Khoroshilov","doi":"10.1134/s003602362460117x","DOIUrl":"https://doi.org/10.1134/s003602362460117x","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>This work reports on the possibility of producing oxide InGaMgO<sub>4</sub> by two-stage heat treatment of glycine-, starch- and PVA-nitrate precursors. The products formed as a result of their heating at low temperatures (≈ 90°С) were studied by powder X-ray diffraction. It was found that the powder formed from the glycine-nitrate precursor contains nanocrystalline In<sub>2</sub>O<sub>3</sub>, and drying of the polymer-nitrate compositions leads to the production of a thermally stable X-ray amorphous product. Its annealing at temperatures above 800°C allows synthesizing powder InGaMgO<sub>4</sub> free of impurity phases. High-temperature treatment of the powder formed from the glycine-nitrate precursor also leads to the production of InGaMgO<sub>4</sub>, but does not remove the In<sub>2</sub>O<sub>3</sub> impurity. Using scanning electron microscopy, it was found that single-phase InGaMgO<sub>4</sub> powders synthesized from polymer-nitrate precursors have a similar grain structure but differ in grain size distribution. Presumably, this difference is due to the structural features of starch and PVA macromolecules used for the preparation of precursors. Oxide InGaMgO<sub>4</sub> was characterized using differential scanning calorimetry, Raman and diffuse reflectance spectroscopy. The value of its band gap energy <i>E</i><sub><i>g</i></sub> was determined using the Tauc method.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-08-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142201211","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-23DOI: 10.1134/s0036023624601107
A. V. Egorysheva, S. V. Golodukhina, K. R. Plukchi, L. S. Razvorotneva, A. V. Khoroshilov, O. G. Ellert
Abstract
Subsolidus phase equilibria in the La2O3–(Ni/Со)O–Sb2O5 systems have been studied. A previously unknown compound La4Sb2O11 was found to exist in the La2O3–Sb2O5 system. La4Sb2O11 has been shown to decompose at 1060°C to form La3SbO7 and LaSbO4. Two ternary oxides (LaNi2SbO6 and La2NiSb2O9) have been discovered in the La2O3–NiO–Sb2O5 system. These new compounds are stable and do not undergo polymorphic transformations throughout the range of temperatures studied (25–1350°C). The existence of previously known ternary oxides, namely perovskite La3Ni2SbO9 and rosiaite LaNi1/3Sb5/3O6, has been verified. In the La2O3–CoO–Sb2O5 system, two new compounds (LaCo2SbO6 and La2CoSb2O9) have been found along with previously known perovskite La3Co2SbO9, rosiaite LaCo1/3Sb5/3O6, and rhombohedral pyrochlore La3Co2Sb3O14. These new compounds are isostructural to those found in the nickel oxide system. La2CoSb2O9, unlike its nickel analogue, decomposes at 990°C. For LaCo2SbO6, no thermal events associated with polymorphic transitions or melting have been detected on DSC curves up to 1350°C. An inspection of diffuse reflectance spectra of the newly synthesized LaNi2SbO6, La2NiSb2O9, LaCo2SbO6, and La2CoSb2O9 phases showed that the oxidation state of nickel and cobalt in them is 2+. The 1050°C isothermal sections of La2O3–(Ni/Co)O–Sb2O5 systems have been constructed.
{"title":"Subsolidus Phase Equilibria in the La2O3–(Ni/Со)O–Sb2O5 Systems","authors":"A. V. Egorysheva, S. V. Golodukhina, K. R. Plukchi, L. S. Razvorotneva, A. V. Khoroshilov, O. G. Ellert","doi":"10.1134/s0036023624601107","DOIUrl":"https://doi.org/10.1134/s0036023624601107","url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>Subsolidus phase equilibria in the La<sub>2</sub>O<sub>3</sub>–(Ni/Со)O–Sb<sub>2</sub>O<sub>5</sub> systems have been studied. A previously unknown compound La<sub>4</sub>Sb<sub>2</sub>O<sub>11</sub> was found to exist in the La<sub>2</sub>O<sub>3</sub>–Sb<sub>2</sub>O<sub>5</sub> system. La<sub>4</sub>Sb<sub>2</sub>O<sub>11</sub> has been shown to decompose at 1060°C to form La<sub>3</sub>SbO<sub>7</sub> and LaSbO<sub>4</sub>. Two ternary oxides (LaNi<sub>2</sub>SbO<sub>6</sub> and La<sub>2</sub>NiSb<sub>2</sub>O<sub>9</sub>) have been discovered in the La<sub>2</sub>O<sub>3</sub>–NiO–Sb<sub>2</sub>O<sub>5</sub> system. These new compounds are stable and do not undergo polymorphic transformations throughout the range of temperatures studied (25–1350°C). The existence of previously known ternary oxides, namely perovskite La<sub>3</sub>Ni<sub>2</sub>SbO<sub>9</sub> and rosiaite LaNi<sub>1/3</sub>Sb<sub>5/3</sub>O<sub>6</sub>, has been verified. In the La<sub>2</sub>O<sub>3</sub>–CoO–Sb<sub>2</sub>O<sub>5</sub> system, two new compounds (LaCo<sub>2</sub>SbO<sub>6</sub> and La<sub>2</sub>CoSb<sub>2</sub>O<sub>9</sub>) have been found along with previously known perovskite La<sub>3</sub>Co<sub>2</sub>SbO<sub>9</sub>, rosiaite LaCo<sub>1/3</sub>Sb<sub>5/3</sub>O<sub>6</sub>, and rhombohedral pyrochlore La<sub>3</sub>Co<sub>2</sub>Sb<sub>3</sub>O<sub>14</sub>. These new compounds are isostructural to those found in the nickel oxide system. La<sub>2</sub>CoSb<sub>2</sub>O<sub>9</sub>, unlike its nickel analogue, decomposes at 990°C. For LaCo<sub>2</sub>SbO<sub>6</sub>, no thermal events associated with polymorphic transitions or melting have been detected on DSC curves up to 1350°C. An inspection of diffuse reflectance spectra of the newly synthesized LaNi<sub>2</sub>SbO<sub>6</sub>, La<sub>2</sub>NiSb<sub>2</sub>O<sub>9</sub>, LaCo<sub>2</sub>SbO<sub>6</sub>, and La<sub>2</sub>CoSb<sub>2</sub>O<sub>9</sub> phases showed that the oxidation state of nickel and cobalt in them is 2+. The 1050°C isothermal sections of La<sub>2</sub>O<sub>3</sub>–(Ni/Co)O–Sb<sub>2</sub>O<sub>5</sub> systems have been constructed.</p>","PeriodicalId":762,"journal":{"name":"Russian Journal of Inorganic Chemistry","volume":null,"pages":null},"PeriodicalIF":2.1,"publicationDate":"2024-08-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142201209","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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