Obtainment of α-Tricalcium Phosphate by Solution Combustion Synthesis Method Using Urea as Combustible

2008 ◽  
Vol 396-398 ◽  
pp. 591-594 ◽  
Author(s):  
Tiago M. Volkmer ◽  
L.L. Bastos ◽  
V.C. Sousa ◽  
L.A. Santos

The aim of this work is the synthesis of α-tricalcium phosphate by solution combustion synthesis using urea as combustible in the stoichiometric ratio and with excess of combustible. The salts Ca(O3)2.4H2O and (H4)2HPO4 were used as reaction precursors with Ca/P ratio of 1.5. The pH adjustment was made adding nitric acid. A porous foam composed by β-tricalcium phosphate, hydroxyapatite and α or β-dicalcium pyrophosphate were obtained as reaction product. X-ray diffraction was used to identify the phases. The obtainment of α-TCP was possible after a heat treatment where the material was held at 1250°C for 15 hours followed by quenching. Smaller particle size was obtained when four times the stoichiometric ratio of combustible was used in the reaction. α-TCP samples were immersed in SBF in order to verify the biocompatibility.

2012 ◽  
Vol 485 ◽  
pp. 473-477
Author(s):  
Gui Yang Liu ◽  
Jun Ming Guo ◽  
Li Li Zhang ◽  
Jing Wang ◽  
Bao Sen Wang ◽  
...  

LiAl0.1Mn1.9O4 materials were prepared by a solution combustion synthesis method. In order to improve the purity of the products, the effect of further calcination time was investigated. The phase compositions of the as-prepared products were determined by X-ray diffraction (XRD). The electrochemical performance of the products was tested by using a coin-type half battery versus lithium metal foil as anode material. XRD results suggested that the main phase of the products was LiAl0.1Mn1.9O4, and there was a trace amount Mn2O3 impurity in some of the products. The purity, crystallinity and grain size of the LiAl0.1Mn1.9O4 were increased with increasing further calcination time. Electrochemical experiments demonstrate that the initial discharge capacities of the products with further calcination time of 0, 6, 12 and 24h were 93.7, 105.7, 114.0 and 120.6mAh/g, and about 89.8, 89.5, 89.2 and 88.3% of the initial capacities were retained after 25 cycles, respectively. Further calcination time can enhance the initial capacity, but is not favorable for the cycle ability of the products.


2012 ◽  
Vol 625 ◽  
pp. 251-254 ◽  
Author(s):  
Gui Yang Liu ◽  
Bao Sen Wang ◽  
Ying He ◽  
Jun Ming Guo

In this paper, LiNixMn2−xO4 materials were prepared by solution combustion synthesis method using acetic salts as raw materials and acetic acid as fuel. The phase structures are characterized by X-ray diffraction (XRD). Electrochemical performances of the materials are investigated by galvanostatic charge/discharge methods. XRD results revealed that the main phase of the products with increasing Ni3+ content is LiMn2O4, and there is a trace amount of Mn3O4 found in the product with Ni3+ content of 0.05. Electrochemical experiments showed that the capacity and the cyclability of the LiNixMn2−xO4 materials decrease with increasing Ni3+ content. Ni3+ doping has no significantly improvement for the capacity and the cyclability of the LiMn2O4 spinel.


Materials ◽  
2018 ◽  
Vol 11 (12) ◽  
pp. 2385 ◽  
Author(s):  
Siyong Gu ◽  
Mingli Qin ◽  
Houan Zhang ◽  
Jidong Ma

This work reports the preparation of La2O3 uniformly doped Mo nanopowders with the particle sizes of 40–70 nm by solution combustion synthesis and subsequent hydrogen reduction (SCSHR). To reach this aim, the foam-like MoO2 precursors (20–40 nm in size) with different amounts of La2O3 were first synthesized by a solution combustion synthesis method. Next, these precursors were used to prepare La2O3 doped Mo nanopowders through hydrogen reduction. Thus, the content of La2O3 used for doping can be accurately controlled via the SCSHR route to obtain the desired loading degree. The successful doping of La2O3 into Mo nanopowders with uniform distribution were proved by X-ray photon spectroscopy and transmission electron microscopy. The preservation of the original morphology and size of the MoO2 precursor by the La2O3 doped Mo nanopowders was attributed to the pseudomorphic transport mechanism occurring at 600 °C. As shown by X-ray diffraction, the formation of Mo2C impurity, which usually occurs in the direct H2 reduction process, can be avoided by using the Ar calcination-H2 reduction process, when residual carbon is removed by the carbothermal reaction during Ar calcination at 500 °C.


2011 ◽  
Vol 142 ◽  
pp. 209-212
Author(s):  
Gui Yang Liu ◽  
Jun Ming Guo ◽  
Li Li Zhang ◽  
Bao Sen Wang ◽  
Ying He

To improve the cyclability of spinel LiMn2O4, Al3+doped LiAlxMn2−xO4(x=0, 0.01, 0.05 and 0.10) materials are prepared using a solution combustion synthesis method using acetic salts as raw materials and acetic acid as fuel. Their phase structures are characterized by X-ray diffraction (XRD). Electrochemical performances of the materials are investigated by galvanostatic charge/discharge methods. XRD results reveal that the purity of the samples increases with increasing Al3+content. Electrochemical experiments demonstrate that the charge/discharge cyclability of the LiAlxMn2-xO4increases with increasing Al3+content. Compared with the pristine LiMn2O4, the Al-doped LiAlxMn1−xO4show the obviously improved cyclability, especially for the sample LiAl0.1Mn1.9O4.


2011 ◽  
Vol 186 ◽  
pp. 7-10 ◽  
Author(s):  
Gui Yang Liu ◽  
Jun Ming Guo ◽  
Bao Sen Wang ◽  
Ying He

Single phase Al3+ doped LiMn2O4 has been prepared by flameless solution combustion synthesis method at 600oC for 1h. X-ray diffraction (XRD) and scanning electric microscope (SEM) were used to determine the phase composition and micro morphology of the products. XRD analysis indicates that the purities increase and the lattice parameters of the products decrease with increasing Al3+ content. Electrochemical test indicates that the cycling performance of the products with Al3+ doping are better than that of the product without Al3+ doping. The product LiAl0.10Mn1.90O4 gets the best electrochemical performance. At the current density of 30mA/g, the initial discharge capacity of LiAl0.10Mn1.90O4 is 124.8mAh/g, and after 20 cycles, the capacity retention is more than 89%. SEM investigation indicates that the particles of LiAl0.10Mn1.90O4 are sub-micron in size and well dispersed.


2020 ◽  
Vol 32 (3) ◽  
pp. 501-507
Author(s):  
Krushitha Shetty ◽  
B.S. Prathibha ◽  
Dinesh Rangappa ◽  
K.S. Anantharaju ◽  
H.P. Nagaswarupa ◽  
...  

MgFe2O4 nanoferrites were synthesized by sol-gel and solution combustion synthesis (SCS) methods through green and chemical methods. Green and chemical methods for sol-gel were processed with use of lemon extract and citric acid, respectively. A green and chemical method for solution combustion synthesis was followed by using Phyllanthus acidus leaf extract and urea, respectively. The influence of synthesis approach on the behaviour of prepared nanoferrites were studied using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and UV visible spectroscopy, vast variation in particle size, crystallinity, electrochemical and photocatalytic activity of the nanoferrites synthesized by various methods were witnessed. Powder X-ray diffraction (PXRD) result of prepared nanoferrites acquired by green and chemical approaches clarified phase structure as spinel and the crystalline size found to be around 11-24 nm. The spinel surface morphology was witnessed for the synthesized nanoferrites. The tetrahedral and octahedral sites of the prepared nanoferrites were confirmed by FTIR spectra. MgFe2O4 nanoferrites synthesized by green sol-gel approach exposed superior electrochemical activity by possessing very less charge transfer resistance. The results of EIS were correlated with the photocatalytic degradation of Rose Bengal dye. Photocatalytic property of the prepared nanoferrites was examined for photodegradation of Rose Bengal dye under UV-light.


2013 ◽  
Vol 802 ◽  
pp. 84-88
Author(s):  
Sagulthai Kahatta ◽  
Nopsiri Chaiyo ◽  
Chesta Ruttanapun ◽  
Wicharn Techitdheera ◽  
Wisanu Pecharapa ◽  
...  

The microwave-assisted solution combustion synthesis was applied to the initial synthesizing of Ca3Co2O6powder using glycine as a fuel and nitrate as an oxidant. The as-synthesized powders were calcined at 700-1,000ºC for 4h. Product characterization was performed using Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD) and Scanning electron microscope (SEM). The fuel-to-oxidizer molar ratio was found to affect the combustion reaction and character of the powder obtained. The phase composition of powder after calcination at various temperatures has shown that the formation of Ca3Co2O6occurs directly. The calcined powder possesses a rhombohedral crystal structure with an X-ray diffraction pattern that could be matched with the Ca3Co2O6JCPDS: 89-0629. This method is a simple way of synthesizing fine Ca3Co2O6powder with a low calcination temperature.


2012 ◽  
Vol 485 ◽  
pp. 465-468
Author(s):  
Li Li Zhang ◽  
Gui Yang Liu ◽  
Jun Ming Guo ◽  
Bao Sen Wang ◽  
Ying He

Spinel LiMn2O4 have been prepared by the solution combustion synthesis method using acetate salts as raw materials and acetic acid as fuel. The phase compositions of the as-prepared products were determined by X-ray diffraction (XRD). The electrochemical performance of the products was tested by using a coin-type half battery versus lithium metal foil as anode material. XRD results suggested that the purities of the products prepared at 500oC are higher than these of the products prepared at 600oC. For the products prepared at 500oC, the purities of the products increase with increasing acetic acid ratios. But for the products prepared at 600oC, the purities of the products decrease with increasing acetic acid ratios. The performance tests indicated that the electrochemical performances of the products prepared at 500oC are better than these of the products prepared at 600oC. The product prepared at 500oC with the acetic acid ratio of 1.0 gets the best performance. The initial capacity of it reaches to 124.8mAh/g at the current density of 75mA/g, and after 50 cycles, the capacity retention is 93.7%.


Author(s):  
Valentin I. Romanovsky ◽  
Alexander A. Hort ◽  
Kirill B. Podbolotov ◽  
Nikolay Yu. Sdobnyakov ◽  
Vladimir S. Myasnichenko ◽  
...  

In this work, we studied possibility to obtain bimetallic nanopowders by our modified solution combustion synthesis method using citric acid as a fuel. Stoichiometric amounts of metal nitrates with metal to metal ratios 1:1 and 1:2 and fuels with final oxidizer to fuel ratio of 1.75 were used as initial components to prepare aqueous solutions. The almost complete absence of metal oxide phases was confirmed by energy-dispersive X-ray spectroscopy. The X-ray diffraction analysis of obtained materials showed that all samples are pure bimetallic nanopowders with distorted cubic crystal structure of each metal. According to high resolution transmission electron microscopy the mean diameter of metallic particles are about 10 nm for all nanopowders. The calculated interplanar distances of crystals of metal particles as well as detailed scanning transmission electron microscopy studying showed uniform distribution of different metal spices into nanoparticles. Thus, we can conclude the nanopowders are bimetallic particles with co-integrated crystal structures of different metalic spices. We suppose, the possibility of solution combustion synthesis of bimetallic nanopowder in the air environment is due to a combination of type and amount of the fuels as well as technological conditions of the synthesis. These lead to rapid combustion process at low temperature. In addition, protective inert atmosphere appears above freshly synthesized metal nanopowders during thermal decompositions of the fuels that eventually prevent metal oxidation. Modified SCS method could be successfully used for one-step synthesis of complex oxide-oxide and metal-oxide core-shell nanostructures. For citation: Romanovskii V.I., Khort A.A., Podbolotov K.B., Sdobnyakov N.Y., Myasnichenko V.S., Sokolov D.N. One-step synthesis of polymetallic nanoparticles in air invironment. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2018. V. 61. N 9-10. P. 42-47


2021 ◽  
Vol 10 (2) ◽  
pp. 93-103
Author(s):  
Fitria Hidayanti ◽  
Kiki R. Lestari ◽  
Nano Sujani ◽  
Jarot Raharjo

A study on the synthesis of black powder (La2NiO4) material using the solution combustion synthesis method at a variation of synthesis temperature of 60, 70, and 80°C was carried out. It produces a mass of black powder of 2 grams by four times of synthesis process. Then, material characterization was performed on the black powder samples obtained by using X-ray Diffraction (XRD) to determine the phases formed, Scanning Electron Microscopy - Energy Dispersive X-ray Spectroscopy (SEM-EDS) to determine the morphology and analyze the composition elemental on the microscale and Fourier Transform Infra-Red (FTIR) to determine chemical bonds. From the whole black powder sample, XRD analysis showed the phases of Dilantanum Nickel Tetraoxide (La2NiO4), Nickel Oxide (NiO), Lanthanum Oxide (La2O3), and Lanthanum Oxide Ht x-form (La2O3 Ht (x-form)). In addition, it was seen from the visible compositions of the phases that the NiO phase looks more dominant and the variation of the synthesis temperature shows that the La2O3 phase was increasing. This was supported by the EDS analysis, which showed that the EDS spectrum contains elements La, Ni, and O where the element O indicates that oxidation occurs in the elements Ni and La. On the other hand, the SEM analysis results confirm that the black powder sample contains the elements La and Ni, based on the high and low electron images contained in the morphology of the black powder sample. In addition, it was also known that the particles in the black powder sample were micron size and had porous morphology. This occurs due to rapid thermal decomposition events and excessive gas development. In addition, FTIR analysis showed that the O-H bond had been reduced and there are still C-O and C-H bonds indicating the presence of organic elements possessed by glycine.


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