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Rates and activation parameters for the spontaneous cis to trans isomerization of the monoalkyl complexes (I) giving (II) are measured.
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ABSTRACT
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Polycrystalline powders of Na2xMn1−xPS3 have been synthesized from layered MnPS3 material by successive ion-exchange intercalation of potassium and sodium ions. Their x-ray photoelectron spectroscopy (XPS) and x-ray excited Auger... more
Polycrystalline powders of Na2xMn1−xPS3 have been synthesized from layered MnPS3 material by successive ion-exchange intercalation of potassium and sodium ions. Their x-ray photoelectron spectroscopy (XPS) and x-ray excited Auger spectroscopy spectra have been measured at room temperature using Mg Kα (1253.6 eV) x-ray source. In particular, the Mn, P, and S 2p and Na 1s and 2p core-level regions and the Na Auger KL23L23 transition have been investigated. All the analyzed XPS core-level spectra display a single-peak structure, suggesting the absence of nonequivalent atoms of Na, Mn, P, and S. The manganese XPS spectrum shows, as observed in MnPS3 and in its cesium and potassium intercalation compounds, typical shake-up satellites, suggesting that the Mn–S bond is yet mainly ionic in nature. The comparison with the XPS spectra relative to MnPS3 and its potassium intercalation compound (K2xMn1−xPS3) does not emphasize any relevant difference in the binding energy positions of the investigated core levels, indicating that sodium ion intercalation process does not alter the electronic properties of pure host matrix. Moreover, Na 2p core levels are discrete and well localized in agreement with the hypothesis of a weak link between the guest (the Na+ ions) and the host lattice (the negatively charged Mn1−xPS3 sheets). Such a hypothesis finds confirmation by the calculation of the Na modified Auger parameter.
Research Interests: Engineering, Chemistry, Applied Physics, X Rays, Mathematical Sciences, and 12 morePhysical sciences, Intercalation Chemistry, Potassium, Electronic properties, Spectrum, Room Temperature, Binding Energy, Porous Material, Ion Exchange, Electron Impact Ionization, X Ray Photoelectron Spectroscopy, and ionic bonding
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MALDI and ESI-MS have been applied to the characterization of the reaction products between the labile cis-[Pt(DMSO) 2 Cl 2 ] (1) and trans-[Pt(DMSO) 2 Cl(CH 3 )] (2) complexes with the simplest poly(amidoamine) ligand (PAMAM, G = 0,... more
MALDI and ESI-MS have been applied to the characterization of the reaction products between the labile cis-[Pt(DMSO) 2 Cl 2 ] (1) and trans-[Pt(DMSO) 2 Cl(CH 3 )] (2) complexes with the simplest poly(amidoamine) ligand (PAMAM, G = 0, 1,2-diaminoethane as core). The ...
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ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full... more
ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.
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Abstract Nanotherapeutics based on cyclodextrins (CD) have been designed to fight the antibiotic resistance and guarantee a successful outcome. Some of them are already on the market or are approaching the clinical phases. In this... more
Abstract Nanotherapeutics based on cyclodextrins (CD) have been designed to fight the antibiotic resistance and guarantee a successful outcome. Some of them are already on the market or are approaching the clinical phases. In this contribution, photo-independent/dependent strategies based on the use of CD nanocarriers delivering antibiotics/antibacterials, antivirals, antifungals, disinfectants, and antiseptics will be reviewed. Moreover nanophototherapeutics based on CD as antibacterials in photo-antimicrobial chemotherapy will be discussed. We will refer to the following nanosystems: (1) CD inclusion nanocomplexes; (2) nanoassemblies entirely composed by CD (i.e., vesicles, micelles, and nanospheres); (3) nanoparticles based on CD-polymer conjugates or CD inclusion complexes entrapped in polymeric matrixes; (4) nanoplatforms based on CD-carbon materials (i.e., carbon nanotubes or graphene derivatives); (5) silver decorated-CD nanostructures. CD-immobilized or cross-linked to fibers, textiles, or surface will not be reviewed in depth. These nanoantimicrobial systems will be reviewed with their in vitro and/or in vivo applications.
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Research Interests: Chemistry and Counterion
... Furthermore, porphyrins can coordinate a large variety of metal ions in the central macrocycle, leading to the possibility of accessing the rich chemical properties of these derivatives (eg spectroscopic and redox properties, electron... more
... Furthermore, porphyrins can coordinate a large variety of metal ions in the central macrocycle, leading to the possibility of accessing the rich chemical properties of these derivatives (eg spectroscopic and redox properties, electron density, axial coordination). ...
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Lithium intercalate thin films have been obtained from MnPS3 starting material and characterized by the x-ray photoelectron spectroscopy technique. The regions of Mn 2p and 3p, P and S 2p, and Li 1s core levels have been investigated. The... more
Lithium intercalate thin films have been obtained from MnPS3 starting material and characterized by the x-ray photoelectron spectroscopy technique. The regions of Mn 2p and 3p, P and S 2p, and Li 1s core levels have been investigated. The analysis of the spectra has revealed the lack of nonequivalent atoms of Mn, P and S, and Li. The presence of shake-up-type satellites at the Mn 2p and 3p core levels suggests that Li2xMn1−xPS3 is a large-gap insulating Mn compound analogously to the parent MnPS3. After lithium intercalation no remarkable shift has been observed in the binding energy positions of the investigated core levels in comparison with the corresponding MnPS3 pure compound. On these bases, we assume that only an ion transfer accompanies the lithium intercalation process.
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Sodium intercalated manganese thiophosphate Na0.62Mn0.69PS3 powders have been synthesized by a two-step ion-exchange process. Dielectric measurements have been performed as a function of both temperature and frequency on the prepared... more
Sodium intercalated manganese thiophosphate Na0.62Mn0.69PS3 powders have been synthesized by a two-step ion-exchange process. Dielectric measurements have been performed as a function of both temperature and frequency on the prepared samples in the 20–106 Hz frequency range over the 78–350 K temperature range by using the autobalancing bridge method. The temperature dependence of the dielectric constant imaginary part reveals the presence of a loss peak at the low temperatures together with a strong dispersion at the low frequencies and at the highest investigated temperatures. While the loss peak presence is characteristic for dipolar polarization processes, the strong low frequency dispersion at not very high temperatures, observed also in the dielectric constant real part, is typical for system with hopping charge carriers. A hypothesis about the nature of such carriers has been formulated on the basis of both the ion-exchange intercalation process and the comparison with the die...
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ABSTRACT
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We study the emission properties of a high quality monolithic microcavity with an embedded ultrathin organic tetrakis(4-methoxyphenyl)porphyrin layer. Spectral and angle-resolved photoluminescence measurements show a well defined... more
We study the emission properties of a high quality monolithic microcavity with an embedded ultrathin organic tetrakis(4-methoxyphenyl)porphyrin layer. Spectral and angle-resolved photoluminescence measurements show a well defined polarized doublet at detection angles larger than 15°. The splitting energy ranges up to 70 meV. The usual employed mechanism, based on the mismatch between the center of the mirror stop band and the wavelength of the microcavity, accounts only for a small fraction of the observed splitting. A transfer matrix model taking into account the optical anisotropy of the organic layer, has been employed to reproduce the observed experimental results. The anisotropy of the organic layer, confirmed by optical absorption spectroscopy, origins from a local molecular order as inferred by atomic force microscopy measurements.
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Aggregation of small molecules on a polymeric matrix, driven by electrostatic interactions, provides a simple and attractive strategy for building well-defined supramolecular species. By choosing matrices of different nature and length... more
Aggregation of small molecules on a polymeric matrix, driven by electrostatic interactions, provides a simple and attractive strategy for building well-defined supramolecular species. By choosing matrices of different nature and length together with the proper experimental conditions (pH, ionic strength, etc.) it is possible to tune the extent of aggregation and/or the size of the aggregates and, thereby, the “macroscopic” properties (absorption and emission features, redox potentials, etc.) of the supramolecular complex. It turns out that porphyrins are particularly good “bricks” for building these complexes, given their well known and tunable electronic properties (i.e., through the insertion of different metal ions and/or substituents on the porphyrin ring), . Recently, it has been reported that the water-soluble anionic porphyrin, mesotetrakis 4-sulphonatophenyl)-porphyrin (H2TPPS) (Figure 1), interacts with the protonated form of polylysine leading to the formation of aggregates [1].
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Nowadays, novel less-expensive nanoformulations for in situ-controlled and safe delivery of photosensitisers (PSs) against opportunistic pathogens in body-infections areas need to be developed. Antimicrobial photodynamic therapy (aPDT) is... more
Nowadays, novel less-expensive nanoformulations for in situ-controlled and safe delivery of photosensitisers (PSs) against opportunistic pathogens in body-infections areas need to be developed. Antimicrobial photodynamic therapy (aPDT) is a promising approach to treat bacterial infections that are recalcitrant to antibiotics. In this paper, we propose the design and characterization of a novel nanophototherapeutic based on the trade cyclodextrin CAPTISOL® (sulfobutylether-beta-cyclodextrin, SBE-βCD) and 5,10,15,20-tetrakis(1-methylpyridinium-4-yl)porphine tetrakis(p-toluenesulfonate) (TMPyP) to fabricate efficient biocompatible systems for aPDT. Spherical nanoassemblies of about 360 nm based on CAPTISOL®/TMPyP supramolecular complexes with 1:1 stoichiometry and equilibrium binding constant (Kb ≅ 1.32 × 105 M-1) were prepared with entrapment efficiency of ≅ 100% by simple mixing in aqueous media and freeze-drying. These systems have been characterized by complementary spectroscopy and microscopy techniques. Time resolved fluorescence pointed out the strong interaction of porphyrin monomer within nanoassemblies (τ2 ≅ 11 ns with an amount of ca 90%) and scarce self-aggregation of porphyrins have been observed. Singlet oxygen comparative determination (ϕΔ CAPTISOL®/TMPyP = 0.58) assessed their photodynamic potential. Release and photostability studies have been carried out under physiological conditions pointing out the role of CAPTISOL® to sustain porphyrin release for more than 2 weeks and to protect PS from photodegradation. Finally, photoantimicrobial activity of nanoassemblies vs free porphyrin have been investigated against Gram-negative P. aeruginosa, E. coli and Gram-positive S. aureus. The proposed nanosystems were able to photokill both Gram-positive and -negative bacterial cells similarly to TMPyP at MBC90 = 6 µM of TMPyP and at 42 J/cm2 light dose. However, with respect to the less selective free TMPyP in biological sites, nanoassemblies exhibit sustained release properties and a higher photostability thus optimizing the PDT effect at the site of action. These results can open routes for in vivo translational studies on nano(photo)drugs and nanotheranostics based on less expensive formulations of CD and PS.
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When mixtures of D2 O/DCl are used to foster the self-assembly formation of TPPS4 porphyrin J-aggregates in aqueous solutions, an inverse kinetic isotope effect of 0.4 and an inverse equilibrium isotope effect of 0.6 are clearly detected.... more
When mixtures of D2 O/DCl are used to foster the self-assembly formation of TPPS4 porphyrin J-aggregates in aqueous solutions, an inverse kinetic isotope effect of 0.4 and an inverse equilibrium isotope effect of 0.6 are clearly detected. Most importantly, the addition of at least 10 % D2 O causes an inversion in the handedness of the final chiral J-aggregates, thus evidencing an important role of deuterium in driving the enantiomeric excess in the scalemic mixture of such supramolecular assemblies.
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The engineering of multifunctional nanoparticles carrying photosensitizer drugs (PS) and exposing binding groups for cellular receptors is of increasing interest in therapeutics and diagnostics applications. Natural and modified... more
The engineering of multifunctional nanoparticles carrying photosensitizer drugs (PS) and exposing binding groups for cellular receptors is of increasing interest in therapeutics and diagnostics applications. Natural and modified cyclodextrins (CDs) offer useful scaffolds to bind PS guests by supramolecular interactions. In particular, amphiphilic β-CDs, which form nanoaggregates of diverse shape and size according to the polarity of substituent groups on the rims, include in their different compartments as CD cavity, hydrophilic and hydrophobic portion, PS with different physicochemical properties. PS embedded in cationic amphiphilic CD nanoassemblies are effective in inducing photodynamic damage in cancer cells. For a carrier/PS system to be used in photodynamic therapy (PDT) or photodynamic diagnosis (PDD), the appropriate combination of the delivery characteristics with the preservation of the photodynamic activity of the PS is strictly required. Homogeneous multilayer films based on cationic amphiphilic β-CD entrapping anionic porphyrins can be constructed to exploit interfacial electrostatic interactions between the two components. The capability of CDs to generate restricted microenvironments for PS which can facilitate photoinduced energy transfer with suitable donor molecules was investigated for potential application in fluorescence diagnosis. Besides, recent findings suggest that PDT could represent a useful tool for properly addressing an alternative approach for killing pathogens and combating infections at a clinical level. Finally, modified CDs can bind gold nanoparticles, yielding hybrid organic/inorganic nanoparticles which were studied in water solution and after casting on solid substrates. These binary assemblies could further encapsulate PS or other conventional drugs, opening new intriguing routes on multimodal therapy.
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ABSTRACT A series of salts of the type [Pt(terpy)Me]X (X = Cl, NO3, PF6, ClO4, B(C6H5)(4)) containing a new organometallic complex cation of platinum(II) with 2,2':6',2 ''-terpyridine (terpy) were... more
ABSTRACT A series of salts of the type [Pt(terpy)Me]X (X = Cl, NO3, PF6, ClO4, B(C6H5)(4)) containing a new organometallic complex cation of platinum(II) with 2,2':6',2 ''-terpyridine (terpy) were synthesized and characterized by H-1, C-13, and Pt-195 NMR spectroscopy. No evidence for fluxionality of the terpyridine ligand was obtained, indicating that it is terdentate. The fourth position in the coordination plane is occupied by a methyl group. The resulting cation is unreactive toward substitution and is stable in aqueous solutions under mild conditions. The planarity and electron delocalization of the terpy moiety lead to extensive stacking interactions, forming dimers in dilute aqueous solution and larger aggregates when the concentration and/or the ionic strength increase. UV/vis and H-1 NMR spectra show characteristic dependencies on the concentration of the complex, the temperature, the solvent, and the ionic strength. Analysis of the absorption spectral data gives a value of 10 (+/-8) x 10(3) M(-1) (T = 298 K; mu = 0.101 mol L(-1)) for the dimerization equilibrium constant. Resonance light-scattering spectra, measured for the first time on a metal-containing noncyclic substrate, provide evidence for the tendency of the complex to form large self-aggregates even under low ionic strength conditions. The interaction of the cationic complex ion with calf thymus DNA was investigated by UV/vis, CD spectroscopy, resonance light-scattering, thermal denaturation, and gel electrophoresis mobility assays. At high r(f) ratios the complex seems to form extended aggregates on the surface of the nucleic acid, but at lower r(f) ratios evidence was obtained for intercalation.
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Under acidic conditions and at high ionic strength or in the presence of templating species, 5,10,15,20-tetrakis(4-sulfonatophenyl)porphyrin (TPPS[Formula: see text] self-organizes into J-aggregates. In these species, the porphyrins align... more
Under acidic conditions and at high ionic strength or in the presence of templating species, 5,10,15,20-tetrakis(4-sulfonatophenyl)porphyrin (TPPS[Formula: see text] self-organizes into J-aggregates. In these species, the porphyrins align in a general edge-to-edge geometry, responsible for their peculiar optical properties. The self-assembling process is hierarchical, and the kinetics are strongly dependent on the mixing protocols. In the case of sigmoidal profiles, the kinetic data have been treated using a model proposed in the literature by R.F. Pasternack. Accordingly, an autocatalytic growth with the formation of an [Formula: see text]-mer of porphyrin units is the rate-determining step (RDS) leading to the eventual J-aggregates whose size spans from nano- up to the micro-scale. The impact of different experimental parameters, together with inorganic counter-anions, and various cationic and anionic species (organic anions, metal ions, porphyrins, and metal complexes) will be reviewed.
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Research Interests: Pharmacology, Biochemistry, Chemistry, Medicine, Multidisciplinary, and 9 morePhotodynamic Therapy, Ps, SC, Singlet Oxygen, Acd, Langmuir, Oh, BODIPY, and O
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Abstract We report a hybrid nanoassembly based on gold colloids decorated with a new thiolated amphiphilic cyclodextrin complexing dopamine (AuNPs@SC16SH/DA). The novel amphiphilic β-cyclodextrin SC16SH, bearing on average one thiol group... more
Abstract We report a hybrid nanoassembly based on gold colloids decorated with a new thiolated amphiphilic cyclodextrin complexing dopamine (AuNPs@SC16SH/DA). The novel amphiphilic β-cyclodextrin SC16SH, bearing on average one thiol group at the end of an oligoethylene glycol chain per CyD unit, was obtained in a multi-step synthesis and fully characterized by NMR spectroscopy and MALDI analysis. The AuNPs@SC16SH hybrid assembly was prepared by mixing AuNPs and SC16SH in aqueous solution and investigated by UV/Vis and TEM measurements. The AuNPs@SC16SH/DA supramolecular assembly, bearing both thiol-stabilized gold nanoparticles and the neurotransmitter dopamine, has been conceived as stimuli-responsive delivery system able to control the release of dopamine upon proper stimuli. Two redox functionalities (i.e. the Au-S bond and the redox behaviour of dopamine) have been exploited to detach SC16SH/DA complex from the AuNPs@SC16SH/DA progenitor platform, using dithiothreitol (DTT), and to detect the complex by cyclic voltammetry (CV). Following, dopamine was finally released from the SC16SH/DA assembly upon treatment with Brij® S20 and the free dopamine was monitored by CV. Overall, our hybrid nanoassemblies turned out to be able to release dopamine, upon combined action of redox and digestion agents in medium emulating biological environment.
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The development of cyclodextrin nanoassemblies as useful carriers for photosensitizer drugs (PS) delivery in biological environment is a topic of increasing interest. In this paper, we present a spectroscopic investigation on a nanosystem... more
The development of cyclodextrin nanoassemblies as useful carriers for photosensitizer drugs (PS) delivery in biological environment is a topic of increasing interest. In this paper, we present a spectroscopic investigation on a nanosystem based on an amphiphilic cationic β-cyclodextrin derivative (CD-N) and an anionic porphyrin (TPPS). Nanoassemblies were prepared by hydration of an organic film containing the two species. The system was characterized by complementary techniques such as UV-vis, stationary and time-resolved fluorescence, and Dynamic Light Scattering (DLS) at different TPPS/CD-N molar ratios. Time-resolved fluorescence data showed that, at all the investigated molar ratios, TPPS is present both as self-aggregated species and monomers forming supramolecular adducts with CD-N. Moreover, DLS measurements evidenced families of aggregates having hydrodynamic radii ranging between 50 and 350 nm and the size distribution profile depending on the TPPS/CD-N molar ratio. At the...
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A series of polyamidoamine dendrimers (generations 1.5–4.0, with ethylenediamine as the central core) has been investigated in methanol solution by means of the small-angle X-ray scattering technique. The comparative analysis of the... more
A series of polyamidoamine dendrimers (generations 1.5–4.0, with ethylenediamine as the central core) has been investigated in methanol solution by means of the small-angle X-ray scattering technique. The comparative analysis of the structural properties of integer and half-integer generations of the dendrimers seems to be dominated by rather different trends. While the integer generations, bearing terminal amino groups, approach a
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ABSTRACT Li2xMn1-xPS3 films have been synthesized by exfoliating MnPS3 through the successive intercalations of K+ and Li+ ions. Their dielectric response has been measured from 80 to 350 K in the frequency range of (102–106) Hz. The... more
ABSTRACT Li2xMn1-xPS3 films have been synthesized by exfoliating MnPS3 through the successive intercalations of K+ and Li+ ions. Their dielectric response has been measured from 80 to 350 K in the frequency range of (102–106) Hz. The obtained data have been analyzed in terms of both complex permittivity ε* and the ac conductivity σ ac . The frequency dependence of σ ac has been interpreted in terms of the Jonscher’s law, whose exponent n decreases by increasing temperature. The n values lie between 0.479 and 0.501 and are typical of materials in which the ac conductivity is due to multiple hops of carriers. By analyzing the σ dc temperature dependence, the observed dielectric response has been attributed to the intercalated lithium ions, and the Li2xMn1-xPS3 films have been classified as hopping charge carrier systems.
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Publisher Summary This chapter outlines the structural characterization of colloidal cyclodextrins. Noncovalent interactions, such as hydrogen and iconic bonding, and hydrophobic and Van der Walls interactions are supposed to be the... more
Publisher Summary This chapter outlines the structural characterization of colloidal cyclodextrins. Noncovalent interactions, such as hydrogen and iconic bonding, and hydrophobic and Van der Walls interactions are supposed to be the driving forces in the formation of CD supramolecular aggregates. The chapter focuses on the self-organization of amphiphilic CD, which forms colloidal systems with specific functionalities. The potential aggregation of CD nanoaggregates and their nanostructural complexes with different guests in drug delivery will be mentioned. Light scattering and fluorescent techniques are presented in order to characterize in detail their structure in aqueous solution. The heterotopic colloids of amphiphilic cyclodextrins and photosensitizers are shown as potential novel systems for targeted photodynamic therapy of tumours (PDT).
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Properly functionalized amphiphilic cyclodextrins (CDs) can act as capping agents for gold colloids in solution (Mazzaglia, A.; et al. J. Phys. Chem. C 2008, 112, 6764). In the present work, we report a study on a hybrid gold... more
Properly functionalized amphiphilic cyclodextrins (CDs) can act as capping agents for gold colloids in solution (Mazzaglia, A.; et al. J. Phys. Chem. C 2008, 112, 6764). In the present work, we report a study on a hybrid gold nanoparticles/amphiphilic CD supramolecular system ...
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Cesium ions have been intercalated by ion exchange into layered manganese thiophosphate to produce Cs2xMn1−xPS3. Investigations have been conducted by x-ray diffraction analysis, IR absorption spectroscopy, x-ray photoemission... more
Cesium ions have been intercalated by ion exchange into layered manganese thiophosphate to produce Cs2xMn1−xPS3. Investigations have been conducted by x-ray diffraction analysis, IR absorption spectroscopy, x-ray photoemission spectroscopy (XPS), and dielectric spectroscopy. The XPS spectra, recorded at room temperature and at the Mn, P, and S 2p, Mn 3p, and Cs 3d and 4d core-level regions, indicate that no charge transfer occurs from guest species (Cs+) to pure host lattice (MnPS3). The presence of shake-up satellites at the Mn 2p and 3p core levels suggests that the cesium intercalation does not alter the nature of the Mn–S bond which is mostly ionic. Dielectric measurements, carried out between 260 and 375K and in the 20Hz–1MHz frequency range, classify Cs2xMn1−xPS3 as hopping charge carrier systems. The nature of such carriers can be hypothesized on the basis of both the intercalation process by cationic substitution and the comparison with the observed dielectric response of th...
Research Interests: Engineering, Chemistry, Applied Physics, Manganese, Mathematical Sciences, and 13 moreDielectric Spectroscopy, Absorption spectroscopy, Physical sciences, Intercalation Chemistry, Photoemission Spectroscopy, Ion, Room Temperature, Ion Exchange, Charge transfer, X Ray Diffraction Analysis, X Ray Photoelectron Spectroscopy, Caesium, and ionic bonding
ABSTRACT Intercalation of 9-aminoacridine (9AA: C13H10N2) in thin films of exfoliated Li2x−yMn1−xPS3 has been performed by means of a solution approach starting from the hydrochloride salt of the organic species (9AAHCl: C13H10N2·HCl).... more
ABSTRACT Intercalation of 9-aminoacridine (9AA: C13H10N2) in thin films of exfoliated Li2x−yMn1−xPS3 has been performed by means of a solution approach starting from the hydrochloride salt of the organic species (9AAHCl: C13H10N2·HCl). The resulting nanocomposite Li2x−yMn1−xPS3(C13H11N2)y films have been investigated by X-ray photoemission spectroscopy (XPS), at room temperature, in the regions of the Mn, P, S and Cl 2p, Li, C and N 1s and Mn 3p core levels. The XPS analysis has been also carried out on the 9-aminoacridine hydrochloride films whose XPS spectra have been compared with those of the Li2x−yMn1−xPS3(C13H11N2)y films to obtain information about the nature of the interaction between the guest species (9AAH+) and the matrix (Li2x−yMn1−xPS3 −).