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- Chumakova, Natalia A., et al.
(författare)
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Properties of Graphite Oxide Powders and Membranes as Revealed by Electron Paramagnetic Resonance Spectroscopy
- 2018
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Ingår i: The Journal of Physical Chemistry C. - : American Chemical Society (ACS). - 1932-7447 .- 1932-7455. ; 122:39, s. 22750-22759
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Tidskriftsartikel (refereegranskat)abstract
- The spin probe technique was used to study graphite oxide (GO) powders swelled in polar liquids (CH3CN, CH3OH, and H2O) and liquid-free GO membranes (GOM). The nitroxide radicals TEMPO (2,2,6,6-tetramethylpiperidine-N-oxyl) and TEMPOL (4-hydroxy-2,2,6,6-tetramethylpiperidine-N-oxyl) readily penetrated into the interplane space of GO from the solution. Electron paramagnetic resonance (EPR) spectra of these radical probes were sensitive to molecular mobility and orientation ordering within the internal space of GO. The radicals embedded in swelled GO were in two states with different rotational mobilities. The small fraction of radicals located in the interplane space of GO and detected in the broad range of temperatures was in the state of fast rotation, similar to the same radicals dissolved in bulk liquids, thus providing experimental evidence of formation of a liquid-like media within the interplane space of GO. Such mobile media may be responsible for the unusual permeation properties of GOM, which is reported in the literature. Second, less-mobile fraction of radicals was found to be immobilized at the internal surface of GO and was sensitive to phase transformations in the swelled GO structures. The transformations were detected as anomalies at temperature dependences of rotational mobility of radicals. The detected dependence of EPR spectra of probe radicals on orientation of GOM, relative to the direction of magnetic field in the EPR spectrometer, was used for quantitative characterization of orientation alignment of GO planes within the membranes. Such an approach may serve as an elegant method to estimate the relative quality of membranes and other GO-layered structures.
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- Klechikov, Alexey, et al.
(författare)
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Multilayered intercalation of 1-octanol into Brodie graphite oxide
- 2017
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Ingår i: Nanoscale. - : Royal Society of Chemistry (RSC). - 2040-3364 .- 2040-3372. ; 9:20, s. 6929-6936
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Tidskriftsartikel (refereegranskat)abstract
- Multilayered intercalation of 1-octanol into the structure of Brodie graphite oxide (B-GO) was studied as a function of temperature and pressure. Reversible phase transition with the addition/removal of one layer of 1-octanol was found at 265 K by means of X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC). The same transition was observed at ambient temperature upon a pressure increase above 0.6 GPa. This transition was interpreted as an incongruent melting of the low temperature/high pressure B-GO intercalated structure with five layers of 1-octanol parallel to GO sheets (L-solvate), resulting in the formation of a four-layered structure that is stable under ambient conditions (A-solvate). Vacuum heating allows the removal of 1-octanol from the A-solvate layer by layer, while distinct sets of (00 l) reflections are observed for three-, two-, and one-layered solvate phases. Step by step removal of the 1-octanol layers results in changes of distance between graphene oxide planes by similar to 4.5 angstrom. This experiment proved that both L- and A-solvates are structures with layers of 1-octanol parallel to GO planes. Unusual intercalation with up to five distinct layers of 1-octanol is remarkably different from the behaviour of small alcohol molecules (methanol and ethanol), which intercalate B-GO structure with only one layer under ambient conditions and a maximum of two layers at lower temperatures or higher pressures. The data presented in this study make it possible to rule out a change in the orientation of alcohol molecules from parallel to perpendicular to the GO planes, as suggested in the 1960s to explain larger expansion of the GO lattice due to swelling with larger alcohols.
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- Korobov, Mikhail V., et al.
(författare)
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Sorption of polar organic solvents and water by graphite oxide : thermodynamic approach
- 2016
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Ingår i: Carbon. - : Elsevier. - 0008-6223 .- 1873-3891. ; 102, s. 297-303
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Tidskriftsartikel (refereegranskat)abstract
- Sorption of polar organic solvents CH3OH, C4H8O (THF), CH3CN, C3H7NO (DMF), C2H6OS (DMSO), C5H9NO (NMP) and water was quantitatively evaluated for Hummers (H-GO) and Brodie (B-GO) graphite oxides at T = 298K and at melting temperature (Tm) of the solvents. H-GO showed stronger sorption compared to B-GO for all studied solvents and the increase of sorption upon lowering temperature was observed for both H-GO and B-GO. Thermodynamic equations allowed to explain earlier reported "maximums" of swelling/sorption in the binary systems H-GO – solvent at Tm. The specific relation between the values of enthalpies of sorption and melting leads to the change of sign in enthalpies of sorption at Tm and causes maximal swelling/sorption. The same thermodynamic explanation was given for the "maximum" on the swelling vs. pressure dependence in B-GO and H-GO – H2O systems earlier reported at pressure of phase transition "liquid water-ice VI". Notably higher sorption of H2O was observed for H-GO compared to H-GO membrane (H-GOm) at high relative humidity (RH), RH > 0.75. Experimental sorption isotherm of H-GOm was used to simulate permeation rates of water through H-GOm and to estimate effective diffusion coefficient of water through the membrane.
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- You, Shujie, et al.
(författare)
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Selective Intercalation of Graphite Oxide by Methanol in Water/Methanol Mixtures
- 2013
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Ingår i: The Journal of Physical Chemistry C. - : American Chemical Society (ACS). - 1932-7447 .- 1932-7455. ; 117:4, s. 1963-1968
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Tidskriftsartikel (refereegranskat)abstract
- Graphite oxide is selectively intercalated by methanol when exposed to liquid water/methanol mixtures with methanol fraction in the range 20-100%. Insertion of water into the GO structure occurs only when the content of water in the mixture with methanol is increased up to 90%. This conclusion is confirmed by both ambient temperature XRD data and specific temperature variations of the GO structure due to insertion/deinsertion of an additional methanol monolayer observed upon cooling/heating. The composition of GO-methanol solvate phases was determined for both low temperature and ambient temperature phases. Understanding of graphite oxide structural properties in binary water/methanol mixtures is important for the unusual permeation properties of graphene oxide membranes for water and alcohols. It is suggested that graphite oxide prepared by Brodie's method can be used for purification of water using selective extraction of methanol from water/alcohol mixtures.
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- Talyzin, A V, et al.
(författare)
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Ferromagnetism in C60 polymers: pure carbon or contamination with metallic impurities?
- 2007
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Ingår i: J Nanosci Nanotechnol. - 1533-4880. ; 7:4-5, s. 1151-61
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Tidskriftsartikel (refereegranskat)abstract
- A review of ferromagnetism in C-60 polymeric materials synthesized by high pressure high temperature (HPHT) treatment is presented. Analysis of published data proves that the reported ferromagnetism cannot be assigned to polymeric structure in either perfect or defect states. Most recent experimental studies have not confirmed previously reported levels of magnetization in polymeric samples while it appears that ferromagnetism of "magnetic carbon" is preserved above the depolymerization point of any C-60 polymer. Identical ferromagnetic properties in some samples of fullerene polymer and graphite like hard carbon phase also show that the effect is most likely not connected to fullerenes at all. Most of the data published previously as an evidence of ferromagnetism in C-60 polymers synthesized at HPHT conditions can be explained by contamination with magnetic impurities. Formation of iron carbide (Fe3C) due to reaction of metallic iron with fullerene molecules allows to explain observed Curie temperature of similar to 500 K and levels of magnetization reported for ''magnetic carbon."
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