scholarly journals Heterostructural Mixed Oxides Prepared via ZnAlLa LDH or ex-ZnAl LDH Precursors—Effect of La Content and Its Incorporation Route

Materials ◽  
2021 ◽  
Vol 14 (8) ◽  
pp. 2082
Author(s):  
Katarzyna Antoniak-Jurak ◽  
Paweł Kowalik ◽  
Wiesław Próchniak ◽  
Robert Bicki ◽  
Grzegorz Słowik

The effect of La content and its incorporation route on physicochemical properties of ZnO/Zn(Al,La)2O4 or La2O3–ZnO/ZnAl2O4 mixed oxides with a spinel structure obtained from ZnAlLa Layered double hydroxides (LDHs) or ex-ZnAl LDH materials was investigated. The heterostructural nanocomposites with the similar Zn/Al molar ratio and varied La content were prepared by two techniques: via co-precipitation and thermal treatment of ZnAlLa LDHs at 500 °C or via incipient wetness impregnation of ex-ZnAl LDHs with aqueous solutions of lanthanum nitrate and subsequent thermal treatment. The obtained series of materials were characterized by the following techniques: X-ray fluorescence (XRF), N2 adsorption (BET), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), thermogravimetric analysis with evolved gas analysis (TG/DTG/EGA), scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and Fourier-transform infrared spectroscopy (FFT). The evaluation of activity toward the high-temperature water gas shift (HT-WGS) within the temperature range of 350–420 °C was carried out on the basis of rate constant measurements in the kinetic mode using a differential reactor. The co-precipitation technique allowed for a better distribution of La in bulk and on the spinel surface than in case of lanthanum incorporation via impregnation. ZnO/Zn(Al,La)2O4 or La2O3–ZnO/ZnAl2O4 mixed oxides were characterized by moderate activity in the HT-WGS reaction. The results reveal that introduction of lanthanum oxide over 2.4–2.8 wt% induces the phase separation of the ZnAl2O4 spinel, forming ZnO on the ZnAl2O4 spinel surface.

2010 ◽  
Vol 14 (06) ◽  
pp. 540-546 ◽  
Author(s):  
Lingling Zhang ◽  
Yongtao Lu ◽  
Yukou Du ◽  
Ping Yang ◽  
Xiaomei Wang

Meso-tetrakis(p-sulfonatophenyl)porphyrin (TPPS4) functionalized platinum nanocomposites were synthesized and characterized using ultraviolet-visible absorption spectroscopy (UV-vis), fluorescence spectroscopy (FL), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and X-ray diffraction (XRD) methods. The postulated configuration of TPPS4 functionalized platinum nanocomposite may be described as an antenna system containing a photoreceptive TPPS4 shell and a nanosize platinum core. Fluorescence and photoelectrochemistry studies of both TPPS4 and the platinum nanocomposites showed that efficient electron/energy transfer occurred from the TPPS4 donor to the metallic nanocore acceptor. TPPS4 functionalized platinum nanocomposites are photocatalytic active for water reduction to produce hydrogen. The turnover numbers (TONPt and TONTPPS4) and quantum yield of hydrogen (ϕH2) for the photocatalyst (nPt:nTPPS4= 250) were 44, 11056, and 1.8%, respectively, calculated on the basis of the total amount of H2 evolution for 12 h irradiation.


2005 ◽  
Vol 288-289 ◽  
pp. 191-194 ◽  
Author(s):  
X.D. Kong ◽  
Xue Min Wang ◽  
X. Yu ◽  
Fu Zhai Cui

Nanocomposites of hydroxyapatite-fibroin (HA-FB) were prepared using the biomimetic process. The Nanocomposites were detected with X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The FTIR results showed that chemical bond forms between HA nanocrystals and fibroin protein. The secondary structure of fibroin can be affected by the mineralization process. TGA results indicated the content of mineralized fibroin in the nanocomposites can be freely adjusted by changing the initial concentration of fibroin solution. TEM image showed that the diameter of the single mineralized nanofibrils is about 2-3 nm and the nanofibrils can aggregate into bundles with the size of 6-8 nm in width and 30-60 nm in length.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Quanguo Li ◽  
Yanhua Shen ◽  
Taohai Li

In this work, CaWO4nanoparticles have been synthesized by microwave-assisted method at a low temperature of 120°C. The as-prepared powders were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). It is found that the reaction time played an important role in the morphology controlling and crystallinity level of CaWO4crystals. The effects of photoluminescent properties have a great relationship with crystallinity.


2011 ◽  
Vol 239-242 ◽  
pp. 2839-2842
Author(s):  
Hong Mei Mu ◽  
Peng Fei ◽  
Bi Tao Su ◽  
Zi Qiang Lei

A series of Fe3+-dopped polyaniline (Fe3+/PANI) nanomaterials with different morphologies and a higher conductivity were successfully synthesized using a simple and static interfacial polymerization by using FeCl3 as both oxidant catalyst and dopant. The effect of surfactants CTAB and SDS and the concentration of FeCl3 on the morphology and conductivity of Fe3+/PANI nanomaterial were investigated. The samples were characterized by Transmission Electron Microscopy (TEM), SDY-4 probes conductivity meter, X-ray Diffractometry (XRD), Energy dispersive spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy techniques. TEM’s results showed that their morphologies changed with the type of the surfactant and the concentration of FeCl3. Introducing surfactants CTAB and SDS into Fe3+/PANI remarkably improved the conductivity of the material. The conductivities of CTAB/Fe3+/PANI and SDS /Fe3+/PANI nanomaterials were respectively about 4.8×10-2 and 1.3×10-2 S/cm while the conductivity of Fe3+/PANI was found to be 1.5×10-4 S/cm. The different morphology and high conductivity may be ascribed to the mutual effects of the surfactant and oxidant.


Clay Minerals ◽  
2004 ◽  
Vol 39 (4) ◽  
pp. 391-404 ◽  
Author(s):  
J. E. F. C. Gardolinski ◽  
G. Lagaly ◽  
M. Czank

AbstractKaolinite and synthetic γ-Al(OH)3 (gibbsite or hydrargillite) were reacted with phenylphosphonic, phenylphosphinic and 2-nitrophenol-4-arsonic acids. The products were studied by powder X-ray diffraction, transmission electron microscopy/selected area electron diffraction/ energy dispersive X-ray/Fourier transform infrared and simultaneous thermogravimetric/differential thermal analysis. The acids were not intercalated but, instead, easily destroyed the structure of the minerals. Lamellar Al phenylphosphonate and aluminium phenylphosphinate and phenylarsonate with polymeric linear-chain structures were formed from kaolinite. The reaction between gibbsite and the same acids yielded almost identical products. No evidence of formation of grafted kaolinite derivatives after the reaction with phenylphosphonic acid was found.


1999 ◽  
Vol 564 ◽  
Author(s):  
J. Y. Phillip Wang ◽  
Hong Zhang ◽  
Imran Hashim ◽  
Girish Dixit ◽  
Fusen Chen

AbstractThis paper reports an extensive interfacial study of Cu deposited on Ta and TaN barrier layers. It has been reported that the Cu/Ta interface develops a uniform and thin amorphous layer at the interface upon thermal treatment[l]. However, our high resolution transmission electron microscopy (HRTEM) analysis shows atomically sharp interfaces for all conditions without any amorphous layer at the interfaces, especially for the ones which underwent one hour annealing at 400°C and 500°C. The “amorphization” effect is only observed if the Cu/Ta TEM specimen is exposed to oxygen. It exists usually at the thinner regions of the TEM specimen or if the specimen is left in air for > 24 hours. Energy dispersion x-ray (EDX) analysis of the “amorphized” region shows that it is a mixture of Cu, Ta, and O.


2015 ◽  
Vol 19 (56) ◽  
Author(s):  
Muflihatun ◽  
Siti Shofiah ◽  
Edi Suharyadi

Nanopartikel Nikel Ferit (NiFe2O4) telah disintesis dengan metode kopresipitasi dengan memvariasi konsentrasi NaOH dan suhu sintesis. Struktur kristal, ukuran partikel, dan morfologi dari sampel dianalisa menggunakan X-ray diffraction (XRD) dan transmission electron microscopy (TEM). Ukuran butir pada konsentrasi NaOH 3, 5, dan 10 M masing-masing adalah 5,7; 4,3; dan 4,2 nm, sedangkan pada suhu 60, 80, dan 150°C berturut-turut adalah 4,2; 4,9; dan 5,5 nm. Analisa fourier transform infrared (FTIR) menunjukkan dua puncak serapan pada rentang ~400-600 cm-1 yang terkait dengan site oktahedral dan tetrahedral pada struktur NiFe2O4. Sifat magnetik NiFe2O4 hasil analisa vibrating sample magnetometer (VSM) menunjukkan bahwa sampel berperilaku ferromagnetik dengan nilai koersivitasnya pada rentang 42-47 Oe. Sampel dengan variasi konsentrasi NaOH, koersivitasnya cenderung menurun dengan menurunnya ukuran partikel. Sementara sampel dengan variasi suhu, semakin kecil ukuran partikel, koersivitasnya cenderung meningkat. Pada 15 kOe, nilai magnetisasi terbesar (6,17 emu/g) diperoleh pada sampel dengan rasio fasa α-Fe2O3 paling rendah.


2021 ◽  
pp. 1-11
Author(s):  
Yan Zhang ◽  
Changqiu Wang ◽  
Yan Li ◽  
Anhuai Lu ◽  
Fanlu Meng ◽  
...  

Abstract Calcification within breast cancer is a diagnostically significant radiological feature that generally consists of hydroxylapatite. Samples from 30 cases of breast carcinoma with calcification were investigated using optical microscopy, energy-dispersive X-ray analysis, transmission-electron microscopy, Fourier-transform infrared spectroscopy, Raman spectroscopy, synchrotron radiation X-ray diffraction and X-ray fluorescence. Under optical microscopy, the calcifications were found to consist of either irregular aggregates with widths > 200 μm or spherical aggregates similar to psammoma bodies with an average diameter of 30 μm. Transmission-electron microscopy showed that short columnar or dumbbell-shaped crystals with widths of 10–15 nm and lengths of 20–50 nm were the most common morphology; spherical aggregates (~1 μm in diameter) with amorphous coatings of fibrous nanocrystals were also observed. Results indicated that hydroxylapatite was the dominant mineral phase in the calcifications, and both CO32– and cation substitutions (Na, Mg, Zn, Fe, Sr, Cu and Mn) were present in the hydroxylapatite structure. Fourier-transform infrared spectra show peaks at 872 and 880 cm–1 indicating that CO32– substituted both the OH– (A type) and PO43– (B type) sites of hydroxylapatite, making it an A and B mixed type. The ratio of B- to A-type substitution was estimated in the range of 1.1–18.7 from the ratio of peak intensities (I872/I880), accompanied with CO32– contents from 1.1% to 14.5%. Trace arsenic, detected in situ by synchrotron radiation X-ray fluorescence was found to be distributed uniformly in the calcifications in the form of AsO43– substituting for PO43–. It is therefore proposed that identifying these trace elements in breast cancer calcifications may be promising for future clinical diagnostics.


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