scholarly journals Preparation procedure to obtain iron nanopowder under non-isothermal conditions

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.

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.


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.


Metals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 581
Author(s):  
Abdulhakim A. Almajid

This study is focused on the deformation mechanism and behavior of naturally aged 7010 aluminum alloy at elevated temperatures. The specimens were naturally aged for 60 days to reach a saturated hardness state. High-temperature tensile tests for the naturally aged sample were conducted at different temperatures of 573, 623, 673, and 723 K at various strain rates ranging from 5 × 10−5 to 10−2 s−1. The dependency of stress on the strain rate showed a stress exponent, n, of ~6.5 for the low two temperatures and ~4.5 for the high two temperatures. The apparent activation energies of 290 and 165 kJ/mol are observed at the low, and high-temperature range, respectively. These values of activation energies are greater than those of solute/solvent self-diffusion. The stress exponents, n, and activation energy observed are rather high and this indicates the presence of threshold stress. This behavior occurred as a result of the dislocation interaction with the second phase particles that are existed in the alloy at the testing temperatures. The threshold stress decreases in an exponential manner as temperature increases. The true activation energy was computed by incorporating the threshold stress in the power-law relation between the stress and the strain. The magnitude of the true activation energy, Qt dropped to 234 and 102 kJ/mol at the low and high-temperature range, respectively. These values are close to that of diffusion of Zinc in Aluminum and diffusion of Magnesium in Aluminum, respectively. The Zener–Hollomon parameter for the alloy was developed as a function of effective stress. The data in each region (low and high-temperature region) coalescence in a segment line in each region.


2007 ◽  
Vol 990 ◽  
Author(s):  
Hideaki Zama ◽  
Yuuji Nishimura ◽  
Michiyo Yago ◽  
Mikio Watanabe

ABSTRACTChemical vapor deposition (CVD) of copper using both a novel Cu(II) β-diketonate source and hydrogen reduction process was studied to fill contact vias with the smallest diameter in the 32nm and more advanced generation chip. Pure Cu films were grown under the condition with the product of hydrogen partial pressure and H2/Cu source molar ratio being over 1,000,000. We succeeded in filling the 40-nm-diameter contact vias by optimizing the growth condition of the Cu-CVD in both substrate temperatures and reaction pressures.


2018 ◽  
Vol 924 ◽  
pp. 333-338 ◽  
Author(s):  
Roberta Nipoti ◽  
Alberto Carnera ◽  
Giovanni Alfieri ◽  
Lukas Kranz

The electrical activation of 1×1020cm-3implanted Al in 4H-SiC has been studied in the temperature range 1500 - 1950 °C by the analysis of the sheet resistance of the Al implanted layers, as measured at room temperature. The minimum annealing time for reaching stationary electrical at fixed annealing temperature has been found. The samples with stationary electrical activation have been used to estimate the thermal activation energy for the electrical activation of the implanted Al.


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.


2019 ◽  
Vol 85 (5) ◽  
pp. 60-68
Author(s):  
Yuliay Pogorenko ◽  
Anatoliy Omel’chuk ◽  
Roman Pshenichny ◽  
Anton Nagornyi

In the system RbF–PbF2–SnF2 are formed solid solutions of the heterovalent substitution RbxPb0,86‑xSn1,14F4-x (0 < x ≤ 0,2) with structure of β–PbSnF4. At x > 0,2 on the X-ray diffractograms, in addition to the basic structure, additional peaks are recorded that do not correspond to the reflexes of the individual fluorides and can indicate the formation of a mixture of solid solutions of different composition. For single-phase solid solutions, the calculated parameters of the crystal lattice are satisfactorily described by the Vegard rule. The introduction of ions of Rb+ into the initial structure leads to an increase in the parameter a of the elementary cell from 5.967 for x = 0 to 5.970 for x = 0.20. The replacement of a part of leads ions to rubium ions an increase in electrical conductivity compared with β–PbSnF4 and Pb0.86Sn1.14F4. Insignificant substitution (up to 3.0 mol%) of ions Pb2+ at Rb+ at T<500 K per order of magnitude reduces the conductivity of the samples obtained, while the nature of its temperature dependence is similar to the temperature dependence of the conductivity of the sample β-PbSnF4. By replacing 5 mol. % of ions with Pb2+ on Rb+, the fluoride ion conductivity at T> 450 K is higher than the conductivity of the initial sample Pb0,86Sn1,14F4 and at temperatures below 450 K by an order of magnitude smaller. With further increase in the content of RbF the electrical conductivity of the samples increases throughout the temperature range, reaching the maximum values at x≥0.15 (σ573 = 0.34–0.41 S/cm, Ea = 0.16 eV and σ373 = (5.34–8.16)•10-2 S/cm, Ea = 0.48–0.51 eV, respectively). In the general case, the replacement of a part of the ions of Pb2+ with Rb+ to an increase in the electrical conductivity of the samples throughout the temperature range. The activation energy of conductivity with an increase in the content of RbF in the low-temperature region in the general case increases, and at temperatures above 400 K is inversely proportional decreasing. The nature of the dependence of the activation energy on the concentration of the heterovalent substituent and its value indicate that the conductivity of the samples obtained increases with an increase in the vacancies of fluoride ions in the structure of the solid solutions.


1967 ◽  
Vol 6 (48) ◽  
pp. 911-915 ◽  
Author(s):  
M. P. Hochstein ◽  
G. F. Risk

The activation energy ϵe1 of polar firn samples determined by D.C. resistivity measurements is a function of temperature and density. In the temperature range −2° C. to −10° C. ϵe1 decreases with decreasing temperature reaching a nearly constant value for temperatures colder than −10°C.; in the temperature range −10°C. to −21°C. ϵe1 was found to decrease with increasing density and to lie between 0.7 eV. and 0.4 eV.


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