Kinetics of synthesizing process for obtaining iron nanopowder by chemical-metallurgical method under isothermal conditions

2021 ◽  
pp. 72-77
Author(s):  
Tien Hiep Nguyen ◽  
◽  
Van Minh Nguyen ◽  

In this work the kinetics of synthesizing process of metallic iron nanopowder by hydrogen reduction from α-FeOOH hydroxide under isothermal conditions were studied. α-FeOOH nanopowder was prepared in advance by chemical deposition from aqueous solutions of iron nitrate Fe(NO3)3 (10 wt. %) and alkali NaOH (10 wt. %) at room temperature, pH = 11, under the condition of continuous stirring. The hydrogen reduction process of α-FeOOH nanopowder under isothermal conditions was carried out in a tube furnace in the temperature range from 390 to 470 °C. The study of the crystal structure and composition of the powders was performed by X-ray phase analysis. The specific surface area S of the samples was measured using BET method by low-temperature nitrogen adsorption. The average particle size D of powders was determined via the measured S value. The size characteristics and morphology of the particles were investigated by transmission and scanning electron microscopes. The calculation of the kinetic parameters of the hydrogen reduction process of α-FeOOH under isothermal conditions was carried out by the Gray-Weddington model and Arrhenius equation. It is shown that the rate constant of reduction at 470 °C is approximately 2.2 times higher than in the case at 390 °C. The effective activation energy of synthesizing process of iron nanopowder by hydrogen reduction from α-FeOOH was ~38 kJ/mol, which indicates a mixed reaction mode. In this case, the kinetics overall process is limited by both the kinetics of the chemical reaction and the kinetics of diffusion, respectively, an expedient way to accelerate the process by increasing the temperature or eliminate the diffusion layer of the reduction product by intensive mixing. It is show that Fe nanoparticles obtained by hydrogen reduction of its hydroxide at 410 °C, corresponding to the maximum specific rate of the reduction process, are mainly irregular in shape, evenly distributed, the size of which ranges from several dozens to 100 nm with an average value of 75 nm.

Author(s):  
Hieр Nguyen Tien

The kinetics of metallic cobalt nanopowder synthesizing by hydrogen reduction from Co(OH)2 nanopowder under isothermal conditions were studied. Co(OH)2 nanopowder was prepared in advance by chemical deposition from aqueous solutions of Co(NO3)2 cobalt nitrate (10 wt.%) and NaOH alkali (10 wt.%) at room temperature, pH = 9 under continuous stirring. The hydrogen reduction of Co(OH)2 nanopowder under isothermal conditions was carried out in a tube furnace in the temperature range from 270 to 310 °C. The crystal structure and composition of powders was studied by X-ray phase analysis. The specific surface area of samples was measured using the BET method by low-temperature nitrogen adsorption. The average particle size of powders was determined by the measured specific surface area. Particles size characteristics and morphology were investigated by transmission and scanning electron microscopes. Kinetic parameters of Co(OH)2 hydrogen reduction under isothermal conditions were calculated using the Gray–Weddington model and Arrhenius equation. It was found that the rate constant of reduction at t = 310 °C is approximately 1.93 times higher than at 270 °C, so the process accelerates by 1.58 times for 40 min of reduction. The activation energy of cobalt nanopowder synthesizing from Co(OH)2 by hydrogen reduction is ~40 kJ/mol, which indicates a mixed reaction mode. It was shown that cobalt nanoparticles obtained by the hydrogen reduction of its hydroxide at 280 °C are aggregates of equiaxed particles up to 100 nm in size where individual particles are connected to several neighboring particles by contact isthmuses.


2020 ◽  
Vol 96 (4) ◽  
pp. 47-55
Author(s):  
Tien Hiep Nguyen ◽  
◽  

In this work the kinetics of the hydrogen reduction process of nickel oxide nanopowder in non-isothermal conditions were studied. NiO nanopowder was prepared in advance by thermal decomposition at 300°C of nickel hydroxide Ni(OH)2. Ni(OH)2 nanopowder was prepared by chemical deposition from aqueous solutions of nickel nitrate Ni(NO3)2 (10 wt. %) and alkali NaOH (10 wt. %) at room temperature, pH=9, under the condition of continuous stirring. The hydrogen reduction process of NiO nanopowder in non-isothermal conditions was carried out in the linear heating mode at a rate of 5°C/min in the temperature range 25–400°C. The study of the crystal structure and composition of the powder samples was performed by X-ray phase analysis. The specific surface area S of the powders was measured using BET method by low-temperature nitrogen adsorption. The average particle size D of powder samples was determined via the measured S value. The size and shape of the particles were investigated by scanning electron microscopic method. The calculation of kinetic parameters of the reduction process of nickel oxide in non-isothermal conditions was carried out by the differential-difference method using the data of thermogravimetric analysis and the equation for non-isothermal kinetics. It was revealed that the hydrogen reduction process of NiO nanopowder in non-isothermal conditions occurs in the temperature range 240–300°С with a maximum specific rate of 13,045•10-8 kg/s recorded at 280°С. The activation energy for the reduction process of NiO nanopowder was estimated at ~59 kJ/mol, which confirms the kinetic mode of limiting the process. It is shown that an increase in temperature to 280 °С can effectively increase the rate of the overall hydrogen reduction process of NiO nanopowder while guaranteeing the quality of the reduction product. The obtained Ni nanoparticles mainly have a rounded shape, their size ranges from 40–80 nm. Keywords: kinetics, nickel, nanopowder, hydrogen reduction, non-isothermal conditions, activation energy.


Author(s):  
Тиен Хиеп Нгуен ◽  
Ван Минь Нгуен ◽  
Мань Хунг Нгуен ◽  
Виталий Николаевич Данчук

The kinetics for the procedure of preparing iron nanopowder from α-FeOOH by hydrogen reduction under non-isothermal conditions were studied. The reduction of α-FeOOH nanopowder was shown to occur within the temperature range from 180 to 550 °С, with a maximum specific rate value attained at 500 °С. The activation energy for the reduction process α-FeOOH nanopowder was measured to be ~43 kJ/mol, evidencing a mixed reaction mode. Performing the reduction of α-FeOOH at 500 °С accelerated the process while ensuring the required properties of the product obtained. The Fe nanoparticles thus prepared were of rounded shape, the size ranging from 70 to 100 nm.


2019 ◽  
Vol 956 ◽  
pp. 55-66
Author(s):  
Bei Lei Yan ◽  
Wei Wei Meng ◽  
San Chao Zhao

In this work, a thermal reduction process via ultrafine titanium powder as the reducing agent under argon atmosphere is firstly used to prepare Ti4O7. Compared with the conventional method, this experiment process reduces the sintering temperature to 850°C. The phase transformation and the morphology of the as-prepared powders are examined by X-Ray diffraction (XRD) and scanning electron microscopy (SEM). Besides, it is found that the Ti4O7 powders obtained by titanium thermal reduction method exhibited the crystal structure, distinctly possessing an average particle size around 750 nm. The as-prepared Ti4O7 nanoparticles are used as anode active material in lithium battery. The results demonstrate that the anode with Ti4O7 calcined at 850°C by titanium thermal reduction method exhibited insertion/extraction lithium ion property.


1988 ◽  
Vol 121 ◽  
Author(s):  
G. H. Bogush ◽  
G. L. Dickstein ◽  
P. Lee ◽  
K.C. ◽  
C. F. Zukoski

ABSTRACTWe report here an experimental technqiue based on changes in reaction medium volume which we have used to observe the kinetics of hydolysis and polymerization of TEOS in aqueous ethanol solutions containing NH3. Our results show that there are three distinct reaction regions. By combining these results with determinations of change in reaction medium conductivity and average particle size, we are able to link the short and long time regions to TEOS hydrolysis and particle growth respectively. The intermediate reaction time region is not associated with hydrolysis, loss of ionic species due to condensation or to particle growth.


2021 ◽  
Vol 3 (1) ◽  
pp. 27
Author(s):  
Joseph Ogbezode ◽  
Olufemi Ajide ◽  
Soji Ofi ◽  
Oluleke Oluwole

In the present work, an attempt is made to use non-contact charcoal in the reduction of run-off mine goethite ore at heating temperatures above 570 °C. The reduction mechanism was adopted, following Levenspiel’s relations for the shrinking core model at different stages of reduction. The non-contact charcoal reduction approach is adopted to maximize the benefit of using CO/CO2 gases from charcoal for reduction without the need for beneficiation and concentration. The rate-controlling steps for the reduction kinetics of average particle sizes 5, 10, 15, and 20 mm at 570, 700, 800, 900, and 1000 °C were studied after heat treatment of the ore-wood charcoal at a total reduction time of 40 min using activated carbon reactor. Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analyses were done to investigate the spectrometric phase change and metallic components of the ore sample after reduction, respectively. The average percentage of the metallic iron content (56.6, 60.8, and 61.7%) and degree of metallization (91.62, 75.96, and 93.6%) are achieved from the SEM/EDX analysis of the reduced ore sample at reduction temperatures of 570, 800, and 1000 °C, respectively. The results indicate the tendency for high carbon deposit at the wustite stage of the reduction process at the lowest of temperature 570oC and the residence time of at 10 min. This study demonstrates that diffusion through the ash layer is the controlling resistance of the overall reduction process.


Author(s):  
Van Minh Nguyen ◽  
Tien Hiep Nguyen ◽  
Stanislav V. Gorobinsky

In this work, nanopowders (NP) Co(OH)2 were obtained by chemical precipitation from aqueous solutions of cobalt nitrate Co(NO3)2 and alkali NaOH (10 wt. %) using surfactants: sodium dodecyl sulfate (SDS) and cetylpyridinium chloride (CPC) (0.1 wt. %). It was shown that Co(OH)2 NP with 0.1% SDS is the best quality product, since its dispersion increases more than 2 times compared to the samples with 0.1% CPC and without surfactants. In this case, the Co(OH)2 NP has the form of flakes with an irregular shape and a nanometer size (about 100 nm) with an average thickness of 30 nm. It was found that the average particle size of Co NP obtained by hydrogen reduction of Co(OH)2 NP with 0.1% SDS at 280°C has a maximum on the distribution histogram shifted to the interval 41–50 nm, which is characterized by a narrow particle size distribution and represents spherical particles sintered with each other.


2020 ◽  
Vol 20 (6) ◽  
pp. 3770-3779 ◽  
Author(s):  
Umar Farooq ◽  
Farheen Naz ◽  
Ruby Phul ◽  
Nayeem Ahmad Pandit ◽  
Sapan Kumar Jain ◽  
...  

This paper reports the attempt to develop an efficient heterostructure photocatalyst by employing SrZrO3 as ferroelectric substrate with deposited nanostructured CdS semiconductor on the surface. Primarily bare SrZrO3 and CdS nanoparticles were synthesized by using polymeric citrate precursor and co-precipitation routes, respectively. The chemical deposition technique was used to develop the CdS over the surface of the pre-synthesized SrZrO3 nanoparticles. The synthesized bare nanoparticles and their heterostructure were characterized by XRD which shows the formation of orthorhombic and face centred cubic (FCC) phases of SrZrO3 and CdS, respectively. TEM was used to estimate the morphology and particle size of as-synthesized nanoparticles, which shows the average particle size of 14, 24 and 25 nm for SrZrO3, CdS and SrZrO3/CdS, respectively. The BET surface area of SrZrO3, CdS and SrZrO3/CdS samples was found to be 299, 304 and 312 m2/g respectively. Methylene blue was used as model pollutant to determine the photocatalytic activity of the synthesized nanomaterials. The heterostructure shows an enhanced activity as compared to bare nanoparticles. Dielectric constant and dielectric loss of the nanoparticles was investigated as a function of frequency at room temperature and as a function of temperature at 500 kHz. The room temperature dielectric constant for SrZrO3, CdS and SrZrO3/CdS was found to be 13.2, 17.8 and 25.5 respectively at 100 kHz.


1990 ◽  
Vol 5 (10) ◽  
pp. 2056-2065 ◽  
Author(s):  
Nae-Lih Wu ◽  
Ta-Chin Wei ◽  
Shau-Y Hou ◽  
S-Yen Wong

The kinetics of the solid-state reaction Y2BaCuO5 + 3BaCuO2 + 2CuO ⇉ 2YBa2Cu3O6.5−x + xO2 was studied by using x-ray diffractometric and thermogravimetric analyses. Both analyses established that the reaction was well described by the kinetic equation: 1 − 3(1 − F)2/3 + 2(1 − F) = k0 exp(− E/RT)t, where F is the fractional conversion of a calcined powder, E is 520 kcal/molc and, for a rcactant mixture with an average particle size of 3 μm, k0 is 2.03 ⊠ 1092 min−1. An unreacted-core shrinking model was proposed to obtain the particle-size dependence of the reaction, and predicted that the pre-exponential constant k0 changed with reactant particle size by k0 = 2.03 ⊠ 1092(3/d)2 exp(4/d − 4/3), where d is the average reactant particle size in μm.


2019 ◽  
Vol 12 (06) ◽  
pp. 1951003 ◽  
Author(s):  
Yu Zhang ◽  
Yiyang Wang ◽  
Yalong Liao ◽  
Muyuan Guo ◽  
Gongchu Shi

Nano Pd-Ni/[Formula: see text]-Al2O3 bimetallic catalyst was prepared by chemical precipitation method enhanced with ultrasonic wave. The influence of dosage of dispersant, ultrasonic intensity and mass ratio of Pd to Ni on the dechlorination property of the catalyst obtained was investigated in detail. The appearance morphology, composition and structure of the catalysts prepared were characterized with X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and nitrogen adsorption, while the specific surface area was determined using the Brunauer–Emmett–Teller (BET) isotherm and the chemical composition of active gradients was tested with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Results indicate that the nano Pd-Ni/[Formula: see text]-Al2O3 bimetallic catalyst prepared has uniform distribution of active ingredients with an average particle size of 4.91[Formula: see text]nm, and the chlorine content of shellac dechlorinated with the catalyst obtained is 0.34[Formula: see text]wt.% which is lower than that reported in the literature, meaning the perfect dechlorination property of the catalyst.


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