High-resolution X-ray diffraction, DIFFaX, NMR and first principles study of disorder in the Li2MnO3-Li[Ni1/2Mn1/2]O2 solid solution

X-ray diffraction patterns of Li[Li_(1−2x)/3Ni_xMn_2/3−x/3]O₂ show reflections between 20° and 35°, 2θ (CuKα) due to Li₂MnO₃-like ordering of the transition metal (Ni, Mn and Li) layers. The ordering is rarely perfect, resulting in characteristic broadening and changes in the intensities of these reflections. ⁶Li MAS NMR studies of Li₂MnO₃ show that the [Li_1/3Mn_2/3] layers are well ordered, the disorder arising from the stacking of the layers in the c-direction. DIFFaX was used to model the Li₂MnO₃ XRD data and extract the stacking fault frequency. The results show that even well-ordered cation layers may show only weak or no superstructure reflections, if there is no or little ordering in the c-direction.     

Phosphate-intercalated Ca-Fe-layered double hydroxides: Crystal structure, bonding character, and release kinetics of phosphate

The nitrate-form of Ca-Fe-layered double hydroxide (Ca-Fe-LDH) was synthesized via co-precipitation method, and its phosphate-intercalates were prepared by ion-exchange reaction. According to X-ray diffraction analysis, the Ca-Fe-LDH-NO₃⁻ compound and its H₂PO₄⁻-intercalate showed hexagonal layered structures, whereas the ion-exchange reaction with HPO₄²⁻ caused a frustration of the layer ordering of LDH. Fe K-edge X-ray absorption spectroscopy clearly demonstrated that the Ca-Fe-LDH lattice with trivalent iron ions was well-maintained after the ion-exchange with HPO₄²⁻ and H₂PO₄⁻. Under acidic conditions, phosphate ions were slowly released from the Ca-Fe-LDH lattice and the simultaneous release of hydroxide caused the neutralization of acidic media. Fitting analysis based on kinetic models indicated a heterogeneous diffusion process of phosphates and a distinct dependence of release rate on the charge of phosphates. This study strongly suggested that Ca-Fe-LDH is applicable as bifunctional vector for slow release of phosphate fertilizer and for the neutralization of acid soil.     

Dispersion of laser generated surface waves in an epoxy-bonded layered medium

In this paper, the dispersion of laser generated surface wave in an epoxy bonded copper-aluminum layered specimen is studied. A laser ultrasonic experiment based on the point-source/point-receiver (PS/PR) technique was conducted to measure the surface wave signals in the layered specimen. The received wave signals were then processed in the frequency domain to obtain the dispersion relation of the fundamental surface wave mode. Theoretical calculations of the dispersion relations of the fundamental surface wave modes in two-layered and three-layered specimens were conducted to explore the influence of the bonding layer thickness on the dispersion relation. The experimental dispersion relation for the epoxy bonded copper-aluminum layered specimen is in good agreement with the calculated dispersion relation. The influence of the bonding layer thickness on the dispersion relation is studied and the potential application of the present results to the NDE of bonded layered media based on laser ultrasonics is also addressed.     

Synthesis and characterization of Cd-Cr and Zn-Cd-Cr layered double hydroxides intercalated with dodecyl sulfate

Cd-Cr and Zn-Cd-Cr layered double hydroxides (CdCr-LDH and ZnCdCr-LDH) containing alkyl sulfate as the interlamellar anion have been prepared through a coprecipitation technique. The resulting compounds were characterized using X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, and scanning electron microscopy. Magnetic property measurements indicate that antiferromagnetic interactions occur between the chromium ions in the two compounds at low temperatures. The introduction of zinc influences the ligand field of Cr^III and the Cr^III-Cr^III interactions in the LDH compound. It is found that both CdCr-LDH and ZnCdCr-LDH can be delaminated by dispersion in formamide, leading to translucent and stable colloidal solutions.     

The role of the trivalent metal in an LDH: Synthesis, characterization and fire properties of thermally stable PMMA/LDH systems

Two layered double hydroxides (LDHs), calcium aluminum undecenoate (Ca₃Al) and calcium iron undecenoate (Ca₃Fe), have been prepared by the co-precipitation method. XRD analysis of these LDHs reveals that they are layered materials and FT-IR and TGA confirmed the presence of the undecenoate anions in the material produced. The PMMA composites were prepared by bulk polymerization and the samples were characterized by XRD, TEM, TGA and cone calorimetry. Both additives greatly enhance the thermal stability of PMMA, while the calcium aluminum LDH gives better results when the fire properties were examined using the cone calorimeter.     

Polysulfonylamine. CLXV [1] Kristallstrukturen von Metall‐di(methansulfonyl)amiden. 14 [1] Cs3Ag[(MeSO2)2N]4 und CsAg[(MeSO2)2N]2: Ein dreidimensionales und ein schichtförmiges Koordinationspolymer mit Bis(dimesylamido‐N)argentat‐Baugruppen

Polysulfonylamines. CLXV. Crystal Structures of Metal Di(methanesulfonyl)amides. 14. Cs₃Ag[(MeSO₂)₂N]₄ and CsAg[(MeSO₂)₂N]₂: A Three‐Dimensional and a Layered Coordination Polymer Containing Bis(dimesylamido‐N)argentate Building Blocks Serendipitous formation pathways and low‐temperature X‐ray structures are reported for the coordination compounds Cs₃A₂[AgA₂] ( 1 ) and Cs[AgA₂] ( 2 ), where A^— represents the pentadentate dimesylamide ligand (MeSO₂)₂N^—. Both phases (monoclinic, space group C2/c, Z′ = 1/2) contain inversion‐symmetric bis(dimesylamido‐N)argentate units displaying exactly linear N—Ag—N cores and short, predominantly covalent Ag—N bonds [ 1 : 213.5(2), 2 : 213.35(12) pm]; in each case, the coordination number of the silver ion is extended to 2 + 6 by four internal and two external Ag···O secondary interactions. The three‐dimensional coordination polymer 1 is built up from alternating layer substructures [{Cs(1)}{A}_4/2]^— with Cs(1) lying on twofold rotation axes and [{Cs(2)}₂{AgA₂}_4/4]⁺ with Cs(2) occupying general positions. Within the substructural layers, both types of cesium cation have approximately planar O₄ environments, whereas the final coordination spheres including interlayer bonds are extended to O₆ for Cs(1) and to O₈N for Cs(2). Compound 2 , in contrast, forms a genuine layer structure. The layers are constructed from Cs⁺ chains located on twofold rotation axes, alternating with [AgA₂]^— stacks reinforced by Ag···O secondary interactions and weak C—H···O hydrogen bonds; Cs⁺ is embedded in an O₈ environment. Both structures are pervaded by a three‐dimensional C—H···O network.     

层状纳米光催化复合材料H0.8Fe0.8Ti1.2O4/TiO2的合成及性质

用固相合成法制备出K0.8Fe0.8Ti1.2O4,并用离子交换反应制备出H0.8Fe0.8Ti1.2O4;通过C3H7NH2层间膨胀,TiO2粒子的插入和紫外光分解等反应,合成出一种新的层状光催化纳米复合材料-H0.8Fe0.8Ti1.2O4/TiO2.X射线衍射和漫反射等表征结果表明 该样品的层间高度为0.47nm,禁带能隙为2.18和2.88eV.用(>400 nm的光照射30 min,0.4 g样品可使甲基橙溶液(20 mg/L)的降解率达到22.1%.而同样条件下标准TiO2(P-25)仅为6.2%,表明所研制的层状纳米复合材料具有较高的光催化活性.     

Stabilization of Co in layered double hydroxides (LDHs) by microwave-assisted ageing

Co-containing layered double hydroxides at different pH have been prepared, and aged following different routes. The solids prepared have been characterized by element chemical analysis, powder X-ray diffraction, thermogravimetric and differential thermal analyses (both in nitrogen and in oxygen), FT-IR and Vis-UV spectroscopies, temperature-programmed reduction and surface area assessment by nitrogen adsorption at −196 °C. The best conditions found to preserve the cobalt species in the divalent oxidation state are preparing the samples at controlled pH, and then submit them to ageing under microwave irradiation.     

层状固体模板组装有机/无机纳米结构材料

主要介绍了几种有机／无机层状固体模板组装纳米功能材料的研究进展，对模板的类型、制备、纳米结构材料的产生及其应用前景进行了综述。     

Evidences for decarbonation and exfoliation of layered double hydroxide in N,N-dimethylformamide-ethanol solvent mixture

The behavior of a Hydrotalcite-like material (carbonate-containing Mg,Al-layered double hydroxide) in N,N-dimethylformamide (DMF)-ethanol mixture, at ambient temperature, has been investigated. The releasing of CO₂ and production of a formate-containing material occurred mainly for 1:1 (v/v) solvent mixture. Decarbonation of Hydrotalcite is promoted by DMF hydrolysis followed by neutralization of brucite-like layers through HCOO⁻ intercalation. Translucent colloidal dispersion of LDH nanoparticles from the formate-containing phase was characterized by transmission electron (TEM) and atomic force (AFM) microscopies. The absence of (00?) reflection at X-ray diffraction (XRD) pattern for dried colloidal dispersion indicated delamination of Hydrotalcite. The restacked sample exhibited broad reflections and typical hydroxide ordered layers non-basal (110) diffraction peaks. A LDH-HCOO⁻ material was also prepared and characterized by FTIR and FT-Raman spectroscopies. Decarbonation and exfoliation of Hydrotalcite in N,N-dimethylformamide-ethanol mixed solvent provide an interesting method for preparation of new intercalated LDH materials.