Energy Dispersive X-ray Diffraction Experiments Research Articles

Effect of calcium bentonite clay and fly ash on the stabilization of organic soil from Alberta, Canada

This paper presents findings of the effect of calcium bentonite (Ca-bentonite) and pulp mill fly ash (PFA) on the compressibility behavior, and microstructural evolution of organic soil. A natural soil consisting of 26% organic matter was collected from the wetlands in the Wabasca region, Northern Alberta, Canada. A various mix design was prepared for the laboratory tests with the addition of 5%, 8%, 10%, 12%, 15%, and 20% Ca-bentonite with constant 30% PFA. One-dimensional consolidation tests were carried out to evaluate compressibility behavior of the stabilized organic soil. In addition, fall cone tests were conducted to evaluate change in undrained shear streth of soil after stabilization. A series of scanning electron microscope (SEM) tests with energy dispersive X-ray (EDS) and X-ray diffraction (XRD) experiments were conducted to investigate the microstructural and chemical aspects of the organic soil treated with Ca-bentonite and PFA. The results showed that a mixture of 10% Ca-bentonite with 30% PFA was the optimum dosage for improving compressibility of organic soil regardless of the curing method. Microstructural and chemical analysis revealed that the mineralogical and morphological contents of the stabilized organic soil were affected due to the pozzolanic reaction. The results showed that Ca-bentonite and PFA were able to considerably improve the strength and compressibility of the selected organic soil.

Thermal expansion of liquid Fe-S alloy at high pressure

Local structure and density of liquid Fe-S alloys at high pressure have been determined in situ by combined angle and energy dispersive X-ray diffraction experiments in a multi-anvil apparatus, covering a large temperature and compositional range. Precise density measurements collected for increasing temperature allowed us to directly derive the thermal expansion coefficients for liquid Fe-S alloys as a function of composition. In turn, thermal expansion has been used to refine thermodynamic models and to address the crystallization regime of telluric planetary cores by comparing the adiabatic temperature gradient and the slope of the liquidus in the Fe-FeS system.For Fe-S cores of asteroids and small planetesimals, top-down solidification is the dominant scenario as the compositional domain for which the slope of the liquidus is greater than the adiabatic gradient is limited to a narrow portion on the Fe-rich side. However, bottom-up growth of the inner core is expected for S-poor cases, with this compositional domain expanding to more S-rich compositions with increasing pressure (size of the planetary body). In particular, bottom-up crystallization cannot be excluded for the Moon and Ganymede.

Probing High-Pressure Structural Evolution in Polyurea with In Situ Energy-Dispersive X-ray Diffraction and Molecular Dynamics Simulations

Polyurea, an elastomer with a phase-segregated microstructure, has been proven as an effective coating in defense applications. To gain a more complete understanding of the high-pressure atomic-level morphology of these phases and to validate molecular dynamics (MD) simulations, multi-angle energy-dispersive X-ray diffraction experiments were performed in situ up to pressures of ∼6 GPa at room temperature. Structure factors were obtained and compared to MD simulations with an average error of less than 5% between major peak positions. The first sharp diffraction peak shifted from 4.56 Å to lower d-spacing with pressure, indicating compression between hard segments. This was further supported by the behavior of a peak at ∼3.86 Å from the pair distribution function (PDF), suspected to represent π-stacking and separation between soft segments. Compression within the hard segments themselves is minimal as low-r peaks in the PDF are not greatly affected by pressure.

Experimental investigation of modified bentonite clay-crumb rubber concrete

This study was carried out to investigate the effects of jointly replacing cement and sand with bentonite clay and crumb rubber on the engineering properties of 25 MPa concrete. The materials used for the study were cement, bentonite clay, sand, crumb rubber, stone and water. Microstructural formation, elemental compositions and crystalline phases of cement, bentonite clay, sand, crumb rubber and stone were determined by using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD) experiments respectively. Geotechnical properties of fine aggregates (sand and crumb rubber) and coarse aggregate (stone) were determined from sieve analysis, fineness modulus, moisture content, apparent relative density and bulk density experiments. Water samples were evaluated with pH and conductivity tests. Mechanical properties of the modified bentonite clay-crumb rubber concrete were evaluated with slump, bulk density, compressive strength and tensile splitting strength tests. The microstructural formation and elemental composition of the concrete were also evaluated with the aid of SEM and EDS respectively. The results revealed that the constituent materials possessed adequate engineering requirements for the production of concrete. The modified bentonite clay-crumb rubber concrete showed comparable mechanical and microstructural properties to that of plain concrete and can be suitable for the construction of driveways, floors and walkways.

Bifunctional electrode performance for zinc-air flow cells with pulse charging

Bifunctional air electrodes with tuned composition consisting of two precious metal-free oxide catalysts are manufactured for application in rechargeable zinc-air flow batteries and electrochemically tested via long-term pulse charge and discharge cycling experiments at 50mAcm−2 (mean). NiCo2O4 spinel, synthesized via direct impregnation on carbon nanofibers or nickel powder and characterized by energy dispersive X-ray spectroscopy and X-ray diffraction experiments, shows high activity toward oxygen evolution reaction with low charge potentials of < 2.0 V vs. Zn/Zn2+. La0.6Sr0.4Co0.2Fe0.8O3 perovskite exhibits bifunctional activity and outperforms the NiCo2O4 spinel in long-term stability tenfold. By combining the catalysts in one bi-catalyzed bifunctional air electrode, stable performances of more than 1000h and 450 cycles are achieved when supplied with oxygen and over 650h and 300 cycles when supplied with synthetic air. In addition, the pulse charging method, which is beneficial for compact zinc deposition, is successfully tested on air electrodes during long-term operation. The oxygen evolution potentials during pulse, i.e. at tripled charge current density of 150mAcm−2, are only 0.06–0.08V higher compared to constant charging current densities. Scanning electron microscopy confirms that mechanical degradation caused by bubble formation during oxygen evolution results in slowly decreasing discharge potentials.

Energy Dispersive X-ray Diffraction (EDXRD) of Li1.1V3O8 Electrochemical Cell

ABSTRACTIn this study, we conducted the first energy dispersive x-ray diffraction (EDXRD) experiments on Li/Li1.1V3O8 coin cells discharged to different lithiation levels in order to investigate the phase transitions upon electrochemical reduction. The phase transformation from layered Li-poor α to Li-rich α to defect rock-salt β phase was confirmed with cells of different lithiation stages. No spatial localization of phase formation was observed throughout the cathodes under the conditions of this measurement.

Strength and texture of Pt compressed to 63 GPa

Angle- and energy-dispersive X-ray diffraction experiments in a radial geometry were performed in the diamond anvil cell on polycrystalline platinum samples at pressures up to 63 GPa. Observed yield strength and texture depend on grain size. For samples with 70–300-nm particle size, the yield strength is 5–6 GPa at ∼60 GPa. Coarse-grained (∼2-μm particles) Pt has a much lower yield strength of 1–1.5 GPa at ∼60 GPa. Face-centered cubic metals Pt and Au have lower strength to shear modulus ratio than body-centered cubic or hexagonal close-packed metals. While a 300-nm particle sample exhibits the 〈110〉 texture expected of face-centered-cubic metals under compression, smaller and larger particles show a weak mixed 〈110〉 and 〈100〉 texture under compression. Differences in texture development may also occur due to deviations from uniaxial stress under compression in the diamond anvil cell.

Preparation and characterisation of copper inorganic antibacterial material containing holmium

A new inorganic antibacterial material was synthesised by the sol–gel method using copper ion as antibacterial ion, holmium nitrate as additive and white carbon black as carrier. The structure and properties of the inorganic antibacterial material were characterised by inductively coupled plasma atomic emission spectroscopy, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM) techniques, energy dispersive spectrum (EDS) analysis, X-ray diffraction (XRD) and antibacterial experiments (Escherichia coli as experimental bacteria). The result showed that the bacteriostasis rate of this new material was higher than that of the general Cu antibacterial white carbon black (without containing holmium); the bacteriostasis rate was over 90%. The form of the inorganic antibacterial material was investigated by XRD. The difference between the new inorganic antibacterial material and white carbon black was studied by FT-IR. Scanning electron microscopy and EDS were used to detect the holmium ion in the material.

High-pressure behavior and thermoelastic properties of niobium studied by in situ x-ray diffraction

In situ synchrotron energy dispersive x-ray diffraction (XRD) experiments on Nb have been conducted at pressures up to 6.4 GPa and temperatures up to 1073 K. From the pressure-volume-temperature measurements, thermoelastic parameters were derived for the first time for Nb based on the thermal pressure (ΔPth) equation of state (EOS), modified high-T Birch-Murnaghan EOS, and Mie-Grüneisen-Debye EOS. With the pressure derivative of the bulk modulus KT′ fixed at 4.0, we obtained the ambient isothermal bulk modulus KT0 = 174(5) GPa, the temperature derivative of bulk modulus at constant pressure (∂KT/∂T)P=−0.060(8) GPa K−1 and at constant volume (∂KT/∂T)V=−0.046(8) GPa K−1, the volumetric thermal expansivity αT(T)=2.3(3)×10−5+0.3(2)×10−8T (K−1), as well as the pressure dependence of thermal expansion (∂α/∂P)T=(−2.0±0.4)×10−6 K−1 GPa−1. Fitting the present data to the Mie-Grüneisen-Debye EOS with Debye temperature Θ0 = 276.6 K gives γ0 = 1.27(8) and KT0 = 171(3) GPa at a fixed value of q = 3.0. The ambient isothermal bulk modulus and Grüneisen parameter derived from this work are comparable to previously reported values from both experimental and theoretical studies. An in situ high-resolution, angle dispersive XRD study on Nb did not indicate any anomalous behavior related to pressure-induced electronic topological transitions at ∼5 GPa as has been reported previously.

Thick Ni based amorphous composite coating with good erosion wear resistance

A thick Ni based amorphous composite coating was prepared by the laser cladding technology. The microstructure, phase composition, hardness and erosion wear resistance of the coatings were characterised by means of scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction and erosion wear experiments in this study. The results showed that the amorphous and nanocrystal composite coatings had dense structure, low porosity and metallurgical bonding with the substrate. The addition of TiB2 played a significant role in improving both the amorphous content and the mechanical behaviours of the coatings. With the increasing content of B, the hardness, erosion and wear resistance of the coatings increased. The overall performance showed better for the Ni based coating containing 20%TiB2, due to the superior combined efforts of amorphous and nanocrystallines. The hardness of the coating was about 6·5 times better than that of the 304 steel, and the erosion rate, especially at high impact angles, is superior to the commercial NiCr/Cr3C2 coating.

Investigation of the structural organization of cationic nanoemulsion/antisense oligonucleotide complexes

Atomic force microscopy image analysis and energy dispersive X-ray diffraction experiments were used to investigate the structural organization of cationic nanoemulsion/oligonucleotide complexes. Oligonucleotides targeting topoisomerase II gene were adsorbed on cationic nanoemulsions obtained by means of spontaneous emulsification procedure. Topographical analysis by atomic force microscopy allowed the observation of the nanoemulsion/oligonucleotide complexes through three-dimensional high-resolution images. Flattening of the oil droplets was observed, which was reduced in the complexes obtained at high amount of adsorbed oligonucleotides. In such conditions, complexes exhibit droplet size in the 600nm range. The oligonucleotides molecules were detected on the surface of the droplets, preventing their fusion during aggregation. A lamellar structure organization was identified by energy dispersive X-ray diffraction experiments. The presence of the nucleic acid molecules led to a disorganization of the lipid arrangement and an expansion in the lattice spacing, which was proportional to the amount of oligonucleotides added.

Aluminum-1,4-cyclohexanedicarboxylates: High-Throughput and Temperature-Dependent in Situ EDXRD Studies

The system AlCl3·6H2O/cis-H2CDC/trans-H2CDC/solvent was systematically investigated with high-throughput methods to study the influence of the two 1,4-cyclohexanedicarboxylate isomers (cis- and trans-H2CDC) as flexible aliphatic linker molecules on the formation of new crystalline compounds. Using the cis-isomer, the layered inorganic-organic hybrid compound [Al(OH)(cis-CDC)] (1) is formed. The use of trans-H2CDC leads to the microporous MOF [Al(OH)(trans-CDC)]·H2O (2) denoted CAU-13. Its framework is related to the well-known MIL-53, which was previously described for trivalent cations and rigid terephthalate linker molecules. The crystal structures of 1 and 2 were derived from powder X-ray diffraction data. Temperature-dependent in situ energy dispersive X-ray diffraction (EDXRD) experiments for the synthesis of 2 were carried out at HASYLAB, DESY, Hamburg. The kinetic analysis, applying the Gualtieri model to the experimental data, revealed Arrhenius activation energies of 76 kJ/mol for both the nucleation and the growth process. These values do not differ much from the activation energies reported for MOFs with aromatic rigid linker molecules.

Adsorption of N/S heterocycles in the flexible metal–organic framework MIL-53(FeIII) studied by in situ energy dispersive X-ray diffraction

The adsorption of N/S-containing heterocyclic organic molecules in the flexible iron(III) terephthalate MIL-53, Fe(III)(OH)(0.6)F(0.4)(O2C-C6H4-CO2)·(H2O), from the liquid phase was studied with in situ energy dispersive X-ray diffraction (EDXRD), in order to follow the adsorption-induced expansion of the structure. For comparison with the diffraction data, liquid phase adsorption isotherms were recorded for uptake of benzothiophene, benzothiazole and indole in isopropanol and in heptane. The solvent not only influences pore opening but is also a competing guest. The in situ EDXRD experiments allow the kinetics of guest uptake and the competition with solvent to be monitored directly. Indole uptake is limited; this adsorbate is barely capable of opening the closed, either hydrated or dehydrated, MIL-53(Fe) structure, or of penetrating the isopropanol-containing material in the concentration range under study. When isopropanol is used as a solvent, the guest molecules benzothiophene and benzothiazole must be present at a certain threshold concentration before substantial adsorption into the metal-organic framework takes place, eventually resulting in full opening of the structure. The fully expanded structures of benzothiophene or benzothiazole loaded MIL-53(Fe) materials have Imcm symmetry and a unit cell volume of ca. 1600 Å(3), and upon uptake of the guest molecules by the closed form (unit cell volume ~1000 Å(3)) no intermediate crystalline phases are seen. Successful uptake by MIL-53(Fe) requires that the adsorbate is primarily a good hydrogen bond acceptor; additionally, based on UV-visible spectroscopy, a charge-transfer interaction between the S atoms of benzothiophene and the aromatic rings in the MOF pore wall is proposed.

Structural, optical and electrical properties of RuS2 ± x films, prepared by reactive magnetron sputtering

Thin layers of ruthenium sulfide (RuS2±x, laurite) were deposited on a heated substrate by reactive magnetron sputtering using a metallic ruthenium target and H2S as reactive gas. The balanced magnetron plasmas were excited by a direct-current (DC) or a radio-frequency (RF, 27MHz) power supply, respectively. To comprehensively study the influence of substrate temperature, H2S partial pressure and total pressure of Ar–H2S mixtures of different ratio on film composition, density, film structure, morphology and optical as well as electrical properties series of layers were deposited on different substrates such as titanium foil, glassy carbon and oxidized silicon wafers. Highest density of 5.5 to 5.6gcm−3 in films of 600nm thickness deposited on glassy carbon was found using a total sputtering pressure in the sputter chamber of 0.5–1.5Pa, a DC sputter power of 100W and an Ar:H2S ratio=3:1 at a substrate temperature Tsub=360°C.Layers deposited on glassy carbon at a pressure>1Pa were sulfur rich with a S-to-Ru ratio of 2.1. To elucidate phase formation during film growth in-situ energy dispersive X-ray diffraction experiments were performed employing Ti foil and thermally oxidized Si wafers as substrates. In both cases ruthenium rich (S:Ru=1.7) seed layers were formed prior to the growth of nearly stoichiometric laurite crystallites. Evaluating the width of the diffraction peaks 111 and 200 a growth of laurite grains from 20 to 40nm was inferred when increasing the substrate temperature from 150 to 450°C. The formation of larger grains is correlated with an increase in resistivity. Absorption spectra obtained from laurite layers deposited under RF sputter conditions at substrate temperatures of 360 and 430°C indicate a direct band gap of 1.8eV and a high number of defect states in the band gap.

The structure of liquid N-methyl pyrrolidone probed by x-ray scattering and molecular simulations

The structural properties of liquid N-methyl pyrrolidone have been investigated by combining energy dispersive x-ray diffraction experiments and molecular dynamics simulations with generalized AMBER force field. A very good agreement between theoretical and experimental diffraction patterns was achieved. The analysis of the radial distribution functions shows that the methyl-carbonyl H-bond network observed in the crystal structure is partly preserved in the liquid structure.

Systematic Investigation of Zinc Aminoalkylphosphonates: Influence of the Alkyl Chain Lengths on the Structure Formation

With the high-throughput (HT) methodology, the bifunctional aminoalkylphosphonic acids (AAPA) linker molecules 2-aminoethyl- (AEPA), 3-aminopropyl- (APPA), and 4-aminobutylphosphonic acid (ABPA) [HO(3)P-C(n)H(2n)-NH(2) (n = 2-4)] and zinc nitrate were used to synthesize new metal phosphonates in order to investigate the influence of the alkyl chain length on the structure formation. The systematic investigations led to one known (ZnO(3)PC(2)H(4)NH(2)) and six new compounds: one using AEPA, three using APPA, and two using ABPA. The crystal structures of five compounds were determined by single crystal X-ray diffraction, using X-ray powder diffraction (XRPD) data as well as structure modeling employing force field methods. For compound 1, Zn(O(3)P-C(2)H(4)-NH(3))(NO(3))(H(2)O) (monoclinic, Cc, a = 4.799(1) Å, b = 29.342(6) Å, c = 5.631(1) Å, β = 91.59(3)°, V = 792.7(3) Å(3), Z = 4), and compound 2, Zn(2)(OH)(O(3)P-C(3)H(6)-NH(3))(NO(3)) (monoclinic, P2/c, a = 12.158(2) Å, b = 5.0315(10) Å, c = 13.952(3) Å, β = 113.23(3)°, V = 784.3(3) Å(3), Z = 2), the structures were determined using single crystal X-ray diffraction data. The crystal structures of [Zn(O(3)P-C(3)H(6)-NH(2))]·H(2)O (3) (monoclinic, P2(1)/c, a = 9.094(2) Å, b = 5.0118(7) Å, c = 16.067(4) Å, β = 90.38(2)°, V = 732.3(2) Å(3), Z = 4) and Zn(O(3)P-C(4)H(8)-NH(2)) (5) (monoclinic, P2(1)/c, a = 8.570(7) Å, b = 8.378(4) Å, c = 9.902(6) Å, β = 90.94(5)°, V = 710.9(8) Å(3), Z = 4) were determined using XRPD data. The structural model for compound 6, Zn(O(3)P-C(4)H(8)-NH(3))(NO(3))(H(2)O), was established using lattice parameters from XRPD data and following crystal structure modeling employing force field methods. The structures depend strongly on the alkyl chain length n. For n = 2 and 4 isoreticular compounds are observed, while n = 3 leads to new structures. Larger amounts of all compounds were obtained employing scale-up syntheses in a conventional oven as well as in a microwave reactor system. In addition, in situ energy dispersive X-ray diffraction (EDXRD) experiments at 130 °C were performed at beamline F3 at HASYLAB, DESY, Hamburg, to investigate the formation of compounds 2 and 3 as well as the phase transformation of 2 into 3 upon addition of NaOH. All compounds were characterized in detail using X-ray powder diffraction, IR/Raman spectroscopy, and thermogravimetric and elemental analysis.

Synthesis of isoreticular CAU-1 compounds: effects of linker and heating methods on the kinetics of the synthesis

Two isoreticular aluminium containing metal–organic frameworks, CAU-1-NH2 and CAU-1-(OH)2, have been synthesized solvothermally using 2-aminoterephthalic and 2,5-dihydroxyterpththalic acid to elucidate the product formation depending on the functionalized carboxylic acids. Here, we focus on the product formation kinetics of the amino-functionalized CAU-1, i.e.CAU-1-NH2. The reactions were studied by in situ energy dispersive X-ray diffraction (EDXRD) experiments in the temperature range of 115–145 °C. Both conventional electric (CE) and microwave (MW) -assisted heating were employed. The latter led to shorter induction periods as well as shorter crystallisation times compared to the conventional synthesis. In analogy with the previously reported results of the EDXRD studies of the formation of CAU-1-(OH)2, similar crystal growth rates were observed for both CAU-1-NH2 and CAU-1-(OH)2 using CE heating. In contrast, MW-assisted synthesis of CAU-1-NH2 led to a shorter induction period as well as an acceleration of the crystal growth compared to CAU-1-(OH)2. The acceleration in the crystal growth stage of CAU-1-NH2 can be attributed to a larger pre-exponential factor (about three times that of CAU-1-(OH)2) derived from the Arrhenius plot. However, the activation energy of the crystal growth exhibits similar values for both MW-assisted and CE synthesis of CAU-1-NH2 and CAU-1-(OH)2.

Synthesis, Structural Transformation, Thermal Stability, Valence State, and Magnetic and Electronic Properties of PbNiO3 with Perovskite- and LiNbO3-Type Structures

We synthesized two high-pressure polymorphs PbNiO(3) with different structures, a perovskite-type and a LiNbO(3)-type structure, and investigated their formation behavior, detailed structure, structural transformation, thermal stability, valence state of cations, and magnetic and electronic properties. A perovskite-type PbNiO(3) synthesized at 800 °C under a pressure of 3 GPa crystallizes as an orthorhombic GdFeO(3)-type structure with a space group Pnma. The reaction under high pressure was monitored by an in situ energy dispersive X-ray diffraction experiment, which revealed that a perovskit-type phase was formed even at 400 °C under 3 GPa. The obtained perovskite-type phase irreversibly transforms to a LiNbO(3)-type phase with an acentric space group R3c by heat treatment at ambient pressure. The Rietveld structural refinement using synchrotron X-ray diffraction data and the XPS measurement for both the perovskite- and the LiNbO(3)-type phases reveal that both phases possess the valence state of Pb(4+)Ni(2+)O(3). Perovskite-type PbNiO(3) is the first example of the Pb(4+)M(2+)O(3) series, and the first example of the perovskite containing a tetravalent A-site cation without lone pair electrons. The magnetic susceptibility measurement shows that the perovskite- and LiNbO(3)-type PbNiO(3) undergo antiferromagnetic transition at 225 and 205 K, respectively. Both the perovskite- and LiNbO(3)-type phases exhibit semiconducting behavior.

Structural stability of Zn 3N 2 under high pressure

In situ high-pressure energy dispersive X-ray diffraction experiment on Zn 3N 2 has been performed by using a diamond anvil cell instrument with synchrotron radiation at room temperature. The results showed that the structure of Zn 3N 2 is stable in the experimental pressure range up to 25.2 GPa. According to the Birch−Murnaghan equation of state determined from the relationship of unit cell volume and pressure, assuming B′ 0=4, the bulk modulus B 0=228(2) GPa has been obtained.

Li intercalation and anion/cation substitution of transition metal chalcogenides: Effects on crystal structure, microstructure, magnetic properties and Li+ ion mobility

Abstract We investigated experimentally the effect of Li intercalation on the structural, microstructural and magnetic properties as well as on the Li ion diffusivity of the complex chalcogenides Cr5−yTiySe8. In addition, the effect of anion substitution in TiS2−zSez on the Li diffusion parameters was studied by 7Li nuclear magnetic resonance (NMR) spin-lattice relaxation measurements. For Cr5−yTiySe8 the Li+ insertion is accompanied by an irreversible phase transition from monoclinic to trigonal symmetry which is electronically driven. The maximal Li content in the host material depends on the Ti content and decreases with increasing y in Cr5−yTiySe8. The intercalated materials can be deintercalated and the minimal Li content in the residual compound increases with Ti abundance. The intercalation process is accompanied by drastic changes of the microstructure. Electrochemical discharge curves depend significantly on the Ti. According to the results of XANES investigations performed on Cr4TiSe8, Ti is first reduced during Li uptake and Cr atoms accept electrons at later stages of the intercalation reaction. In-situ energy dispersive X-ray diffraction experiments show that the Li intercalation at room temperature proceeds via two different mechanisms while intercalation at 60 °C is faster and is dominated by one mechanism. 7Li MAS NMR measurements revealed a variety of transition metal environments around the Li sites corresponding to the Cr/Ti disorder. The NMR studies also indicate fast Li dynamics. The magnetism of the educts is dominated by strong antiferromagnetic exchange interactions in the high temperature region and by spin-glass behavior in the low temperature range. Intercalation of Li weakens the antiferromagnetic exchange and for fully intercalated materials ferromagnetic exchange is observed. The interpretation of the experimental results is supported by accompanying band structure calculations. In layer-structured LixTiS2−zSez (x ≈ 0.7) the Li diffusivity was investigated by various NMR techniques and compared with results obtained for the pure end members LixTiS2 and LixTiSe2. In particular, anion substitution clearly influences the slopes of the low-T flanks of the diffusion induced NMR relaxation-rate peaks. The corresponding activation barriers characterizing local hopping processes are reduced in the mixed samples with 0