scholarly journals Structural Transformations of Hydrolysates Obtained from Ti-, Zr-, and Ti, Zr-Solutions Used for Clay Pillaring: Towards Understanding of the Mixed Pillars Nature

Materials ◽  
2018 ◽  
Vol 12 (1) ◽  
pp. 44 ◽  
Author(s):  
Krzysztof Bahranowski ◽  
Agnieszka Klimek ◽  
Adam Gaweł ◽  
Katarzyna Górniak ◽  
Alicja Michalik ◽  
...  

Structural characteristics of hydrolysates formed from the aqueous Ti-, Zr-, and Ti, Zr-pillaring solutions prepared from inorganic precursors (TiCl4 and ZrOCl2), was investigated and compared with that of precipitates obtained from the same solutions after a slight alkalization of pH to the values reported for the conditions of clay pillaring. The materials were recovered by lyophilization and subsequently subjected to calcination at 500, 800 and 1000 °C. Of special interest was the effect of pH on the possible formation of mixed Ti, Zr-oxide species. Powder X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscope/energy dispersive spectrometer (SEM/EDS) analysis showed that even a relatively moderate alteration of pH in Ti-, Zr-, or Ti, Zr-precursor solutions caused substantial changes in the outcome of hydrolytic transformations, manifested by different phase and/or chemical composition of the resulting hydrolysates. Analysis of thermal evolution of hydrolysates showed that alkalization facilitated the transformation of anatase into rutile in materials obtained from Ti-pillaring solution, but retarded tetragonal to monoclinic zirconia conversion in samples derived from Zr-pillaring agent. The most striking effect was observed for the mixed Ti, Zr-pillaring solution, where an increase of pH enabled the formation of zirconium titanate as the only crystalline phase, rather than a multiphase mixture of anatase, monoclinic zirconia and zirconium titanate obtained from the more acidic precursor. The finding supports the model of mixed Ti-O-Zr network in props generated in Ti, Zr-pillared montmorillonites.

Author(s):  
R. Gronsky

The phenomenon of clustering in Al-Ag alloys has been extensively studied since the early work of Guinierl, wherein the pre-precipitation state was characterized as an assembly of spherical, ordered, silver-rich G.P. zones. Subsequent x-ray and TEM investigations yielded results in general agreement with this model. However, serious discrepancies were later revealed by the detailed x-ray diffraction - based computer simulations of Gragg and Cohen, i.e., the silver-rich clusters were instead octahedral in shape and fully disordered, atleast below 170°C. The object of the present investigation is to examine directly the structural characteristics of G.P. zones in Al-Ag by high resolution transmission electron microscopy.


Catalysts ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 678
Author(s):  
Stefano Alberti ◽  
Irene Basciu ◽  
Marco Vocciante ◽  
Maurizio Ferretti

In this contribution, the photoactivity upon activation by simulated sunlight of zinc oxide (ZnO) obtained from two different synthetic pathways (Acetate and Nitrate) is investigated for water purification. Different reagents and processes were exploited to obtain ZnO nanoparticles. Products have been characterized by means of X-Ray Diffraction, Scanning Electron Microscopy along with Energy Dispersive Spectrometer, Dynamic Light Scattering, and Diffuse Reflectance Measurements, to highlight the different outcomes ascribable to each synthesis. A comparison of characteristics and performances was also carried out with respect to commercial ZnO. Nanoparticles of this semiconductor can be obtained as aggregates with different degrees of purity, porosity, and shape, and their physical-chemical properties have been addressed to the specific use in wastewater treatment, testing their effectiveness on the photocatalytic degradation of methylene blue (MB) as a model pollutant. Excluding the commercial sample, experimental results evidenced a better photocatalytic behavior for the ZnO Nitrate sample annealed at 500 °C, which was found to be pure and stable in water, suggesting that ZnO could be effectively exploited as a heterogeneous photocatalyst for the degradation of emerging pollutants in water, provided that thermal treatment is included in the synthetic process.


Minerals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 533 ◽  
Author(s):  
Xin Zhang ◽  
Guanghui Li ◽  
Jinxiang You ◽  
Jian Wang ◽  
Jun Luo ◽  
...  

Ludwigite ore is a typical low-grade boron ore accounting for 58.5% boron resource of China, which is mainly composed of magnetite, lizardite and szaibelyite. During soda-ash roasting of ludwigite ore, the presence of lizardite hinders the selective activation of boron. In this work, lizardite and szaibelyite were prepared and their soda-ash roasting behaviors were investigated using thermogravimetric-differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), and scanning electron microscope and energy dispersive spectrometer (SEM-EDS) analyses, in order to shed light on the soda-ash activation of boron within ludwigite ore. Thermodynamics of Na2CO3-MgSiO3-Mg2SiO4-Mg2B2O5 via FactSage show that the formation of Na2MgSiO4 was preferential for the reaction between Na2CO3 and MgSiO3/Mg2SiO4. While, regarding the reaction between Na2CO3 and Mg2B2O5, the formation of NaBO2 was foremost. Raising temperature was beneficial for the soda-ash roasting of lizardite and szaibelyite. At a temperature lower than the melting of sodium carbonate (851 °C), the soda-ash roasting of szaibelyite was faster than that of lizardite. Moreover, the melting of sodium carbonate accelerated the reaction between lizardite with sodium carbonate.


Minerals ◽  
2019 ◽  
Vol 9 (9) ◽  
pp. 507 ◽  
Author(s):  
Maxim Rudmin ◽  
Elshan Abdullayev ◽  
Alexey Ruban ◽  
Ales Buyakov ◽  
Bulat Soktoev

We investigated the mechanochemical synthesis of complex slow release fertilizers (SRF) derived from glauconite. We studied the effectiveness of the mechanical intercalation of urea into glauconite using planetary and ring mills. The potassium-nitric complex SRFs were synthesized via a mechanochemical method mixing glauconite with urea in a 3:1 ratio. The obtained composites were analyzed using X-ray diffraction analysis, scanning electron microscopy, X-ray fluorescence analysis, and infrared spectroscopy. The results show that as duration of mechanochemical activation increases, the mineralogical, chemical, and structural characteristics of composites change. Essential modifications associated with a decrease in absorbed urea and the formation of microcrystallites were observed when the planetary milling time increased from 5 to 10 min and the ring milling from 15 to 30 min. Complete intercalation of urea into glauconite was achieved by 20 min grinding in a planetary mill or 60 min in a ring mill. Urea intercalation in glauconite occurs much faster when using a planetary mill compared to a ring mill.


2014 ◽  
Vol 975 ◽  
pp. 207-212
Author(s):  
Dayse I. dos Santos ◽  
Olayr Modesto Jr. ◽  
Luis Vicente A. Scalvi ◽  
Americo S. Tabata

Metal oxide nanocomposites were prepared by two different routes: polyol and sol-gel. Characterization by X ray diffraction showed that the first process produces directly a two-phase material, while the sol-gel powder never showed second phase below 600°C. Light spectroscopy of the treated powders indicated similarities for the processed materials. Although the overall material compositions are about the same, different structural characteristics are found for each processing. With the exception of Ti-Zn materials, all the double metal oxide powders showed higher absorbance than either TiO2 powder.


2015 ◽  
Vol 70 (3) ◽  
pp. 183-190 ◽  
Author(s):  
Gerhard Sohr ◽  
Nina Ciaghi ◽  
Klaus Wurst ◽  
Hubert Huppertz

AbstractSingle crystals of the hydrous cadmium borate Cd6B22O39·H2O were obtained through a high-pressure/high-temperature experiment at 4.7 GPa and 1000 °C using a Walker-type multianvil apparatus. CdO and partially hydrolyzed B2O3 were used as starting materials. A single crystal X-ray diffraction study has revealed that the structure of Cd6B22O39·H2O is similar to that of the type M6B22O39·H2O (M=Fe, Co). Layers of corner-sharing BO4 groups are interconnected by BO3 groups to form channels containing the metal cations, which are six- and eight-fold coordinated by oxygen atoms. The compound crystallizes in the space group Pnma (no. 62) [R1=0.0379, wR2=0.0552 (all data)] with the unit cell dimensions a=1837.79(5), b=777.92(2), c=819.08(3) pm, and V=1171.00(6) Å3. The IR and Raman spectra reflect the structural characteristics of Cd6B22O39·H2O.


2011 ◽  
Vol 685 ◽  
pp. 367-370 ◽  
Author(s):  
Min Qi ◽  
Da Yi Yang ◽  
Jing Ying Zhang ◽  
Hong Jun Ai

In order to improve the osteoblast growth and bacteria resistance, Zn-containing hydroxyapatite (Zn-HA) and titanium oxide (TiO2) composite coatings were prepared to improve binding between coating and Ti substrate. TiO2 film was prepared on the surface of Ti by micro-arc oxidation (MAO) and Zn-HA coating was deposited on TiO2 using sol–gel technique. Phase structure, composition and microstructure of the surface coatings were analyzed by X-ray diffraction (XRD) and Energy Dispersive Spectrometer (EDS), respectively. The adhesion strength between the coatings with different Zn content was measured by tensile testing. The results showed that there was no significant influence of Zn content on adhesion strength between coating and Ti substrate.


2015 ◽  
Vol 817 ◽  
pp. 278-282 ◽  
Author(s):  
Yong Jin Wang ◽  
Ren Bo Song ◽  
Ya Ping Li ◽  
Ruo Ling Bi

Formed in the semi-solid state, materials can obtain unconventional microstructures and properties compared with traditional method. In this paper, semi-solid billet of 9Cr18 steel was obtained through a wavelike sloping plate. Microstructure analysis of the semi-solid billet was conducted through scanning electron microscopy (SEM) and energy dispersive spectrometer (EDS). X-ray diffraction (XRD) test and microhardness test were also used to analyze the properties. The results showed that the structure of 9Cr18 semi-solid billet contained globular primary austenite and secondary austenite-Cr7C3 eutectic. Globular primary austenite grains were first formed during partial solidification in the sloping plate, and then the rest liquid metal formed secondary austenite and Cr7C3 eutectic structure surrounding the primary grains. Cr atoms had a concentration in the rest liquid side, which along with C atoms contributed to the formation of the Cr7C3 carbide. Hardness in the primary solid grain area and the eutectic area was about 330 HV and 650 HV, respectively. These specific properties were important for subsequent thixoforming of the functional graded materials.


Cerâmica ◽  
2002 ◽  
Vol 48 (305) ◽  
pp. 38-42 ◽  
Author(s):  
M. I. B. Bernardi ◽  
E. J. H. Lee ◽  
P. N. Lisboa-Filho ◽  
E. R. Leite ◽  
E. Longo ◽  
...  

The synthesis of TiO2 thin films was carried out by the Organometallic Chemical Vapor Deposition (MOCVD) method. The influence of deposition parameters used during growth on the final structural characteristics was studied. A combination of the following experimental parameters was studied: temperature of the organometallic bath, deposition time, and temperature and substrate type. The high influence of those parameters on the final thin film microstructure was analyzed by scanning electron microscopy with electron dispersive X-ray spectroscopy, atomic force microscopy and X-ray diffraction.


2006 ◽  
Vol 530-531 ◽  
pp. 683-688 ◽  
Author(s):  
Valter Ussui ◽  
Dolores Ribeiro Ricci Lazar ◽  
Nelson Batista de Lima ◽  
Ana Helena A. Bressiani ◽  
José Octavio A. Pascoal

A process for synthesis of fine zirconium titanate powders by chemical route is described. Zirconium/titanium molar ratio was varied from 0.67 to 1.5 and the powders produced were analyzed. The precipitation process comprises the mixture of zirconium and titanium metal salt solutions to ammonium hydroxide solution, followed by washing of the precipitate, calcination and grinding to result in zirconium titanate. The ceramic powder is then uniaxially pressed as cylindrical samples and sintered at 1400°C for 5 hours. The microstructure of fractured and thermally etched ceramic was observed by scanning electron microscopy, and crystal phase identifications were done by X-ray diffraction. At least two different zirconium titanate phases, ZrTiO4 and Zr5Ti7O24, were identified. Ceramic hardness was measured by Vickers indentation.


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