Sorption study of an anionic dye - benzopurpurine 4B - on calcined and uncalcined Mg-Al layered double hydroxides

In this paper, the elimination from aqueous solution of the pollutant benzopurpurine 4B by Mg-Al-CO₃ hydrotalcite and its modified form Mg-Al-500 has been studied. Mg-Al-CO₃²⁻ layered double hydroxide with an Mg/Al molar ratio of 2.0 was synthesized by the co-precipitation method, and its modification was carried out by calcination. The affinity of these materials with a mixture of benzopurpurine 4B was studied as a function of dye-adsorbent contact time, initial pH of the solution, initial dye concentration and temperature. The results indicate that HDLs were effective in removing benzopurpurine 4B anionic dye. Their saturated adsorption capacities are very high, particularly for the calcined material Mg-Al-500 compared to the standard one Mg-Al-CO₃²⁻.The characterisation of the solid Mg-Al-500, both fresh and after removal of the dye by X-ray diffraction and infrared spectroscopy, shows that the benzopurpurine 4B adsorption on this calcined phase is enhanced by reconstruction of a matrix hydrotalcite intercalated by the dye, with basal spacing of 23.77 Å, which is larger than that of Mg-Al-CO₃²⁻ LDHs (7.57 Å).     

Chitin-humic acid hybrid as adsorbent for Cr(III) in effluent of tannery wastewater treatment

Adsorption of Cr(III) from both synthetic and real samples of tannery wastewater treatment's effluent on chitin-humic acid (chitin-HA) hybrid has been carried out. Rate constant and capacity of adsorption of Cr(III) from the synthetic sample were investigated and removal of Cr(III) from the real sample was tested at optimum medium acidity equivalent to pH 3.5. Characterization using Fourier transform infra red (FT-IR) spectroscopy revealed that both COO⁻ and N-acetyl originated from respectively humic acid (HA) and chitin were involved on the adsorption of Cr(III), and hence the Freundlich's multilayer and multi-energy adsorption model was more applicable to treat the adsorption data than the Langmuir's monolayer and mono-energy model. The quantification of adsorption capacity and rate constant using Freundlich isotherm model and first order adsorption reaching equilibrium yielded values of 6.84 × 10⁻⁴ mol g⁻¹ (35.57 mg g⁻¹) and 1.70 × 10⁻² min⁻¹, respectively. Removal test for the real wastewater treatment's effluent showed that the maximum amount of Cr(III) could be removed by 1 g of chitin-HA hybrid was 2.08 × 10⁻⁴ mol or equivalent to 10.82 mg.     

Binding of rare earth metal complexes with an ofloxacin derivative to bovine serum albumin and its effect on the conformation of protein

The water-soluble Pr (Ⅲ) and Nd (Ⅲ) complexes with an ofloxacin derivative have been prepared and characterized. The single-crystal X-ray diffraction showed that the Pr (III) and Nd (III) complexes have the similar molecular structure. Under physiological pH condition, the effects of [PrL(NO₃)₂(CH₃OH)](NO₃) and [NdL(NO₃)₂(CH₃OH)](NO₃) on bovine serum albumin (BSA) were examined using fluorescence spectroscopy in combination with UV-vis absorbance and circular dichroism (CD) spectra. The result reveals that the quenching mechanism of fluorescence of BSA by two complexes is a static quenching process and the number of binding sites is about 1 for both. The thermodynamic parameters (ΔH=−14.52 kJ mol⁻¹, ΔS=56.54 J mol⁻¹ K⁻¹ for [PrL(NO₃)₂(CH₃OH)](NO₃) and ΔH=−24.63 kJ mol⁻¹, ΔS=22.07 J mol⁻¹ K⁻¹ for [NdL(NO₃)₂(CH₃OH)](NO₃)) indicate that hydrophobic and electrostatic interactions are the main binding force in the complexes-BSA system. The binding average distance between complexes and BSA was obtained on the basis of Förster's theory. In addition, it was proved by the CD spectra that the BSA secondary structure was changed in the presence of complexes in an aqueous solution.     

Hybrid of chitin and humic acid as high performance sorbent for Ni(II)

Hybrid of humic acid (HA) and chitin has been synthesized and the hybrid material (chitin-HA) was then applied as sorbent to adsorb Ni(II). The HA was extracted from peat soil of Gambut District, South Kalimantan, Indonesia, according to the procedure recommended by IHSS (International Humic Substances Society). The chitin was isolated from crab shell waste of sea food restaurants through deproteination using NaOH 3.5% (w/v) and followed by removal of inorganic impurities using HCl 1 M. The synthesis of chitin-HA was performed by reacting gelatinous chitin solution in HCl 0.5 M and HA solution in NaOH 0.5 M. Parameters investigated in this work consists of effect of medium acidity on the sorption, sorption rate (k_s) and desorption rate (k_d) constants, Langmuir (monolayer) and Freundlich (multilayer) sorption capacities, and energy (E) of sorption. The k_s and k_d were determined according to a kinetic model of first order sorption reaching equilibrium, monolayer sorption capacity (b) and energy (E) were determined according to the Langmuir isotherm model, and multilayer sorption capacity (B) was determined based on the Freundlich isotherm model.Sorption of Ni(II) on both chitin and chitin-HA was maximum at pH 8.0. The kinetic expression resulted from the proposed kinetic model has been shown to be more applicable than the commonly known Lagergren equation obtained from the pseudo-first order sorption model. The application of the proposed model revealed that the presence of HA increased the k_s from 0.018 min⁻¹ for chitin to 0.031 min⁻¹ for chitin-HA. As for k_s, the value of b was also bigger in the presence of HA, i.e. 7.42 × 10⁻⁵ mol/g for chitin and 9.93 × 10⁻⁵ mol/g for the chitin-HA. Unlike k_s and b, the value of E slightly decreased from 23.23 to 21.51 kJ/mol for the absence and presence of HA, respectively. It can also be deduced that the presence of HA on chitin contributed more to the additional layer of Ni(II) sorbed on sorbent. Without HA, B for chitin was only 6.17 times higher than b, while with the presence of HA, the enhancement of the sorption capacity from the multilayer (B) to the monolayer (b) was 19.40. The increase of k_s, b, B, and the decrease of E would be very benefit in the real application of chitin-HA for the recovery of Ni(II) from aqueous samples.     

Removal of nickel(II) ions from aqueous solutions using the natural clinoptilolite and preparation of nano-NiO on the exhausted clinoptilolite

The natural zeolite tuff (clinoptilolite) from a Serbian deposit has been studied as adsorbent for Ni(II) ions from aqueous solutions. Its sorption capacity at 298 K varies from 1.9 mg Ni g⁻¹ (for the initial solution concentration of 100 mg Ni dm⁻³) to 3.8 mg Ni g⁻¹ (for C₀ = 600 mg Ni dm⁻³) and it increases 3 times at 338 K. The sorption is best described by the Sips isotherm model. The sorption kinetics follows the pseudo-second-order model, the activation energies being 7.44, 5.86, 6.62 and 6.63 kJ mol⁻¹ for C₀ = 100, 200, 300 and 400 mg Ni dm⁻³, respectively. The sorption involves a film diffusion, an intra-particle diffusion, and a chemical cation-exchange between the Na⁺ ions of clinoptilolite and the Ni²⁺ ions. The sorption is endothermic (ΔH° being 37.9, 33.4, 30.0, 27.7 and 24.3 kJ mol⁻¹ for C₀ = 100, 200, 300, 400 and 600 mg Ni dm⁻³, respectively) and spontaneous in the 298-338 K temperature range. Thermal treatment of the Ni(II)-loaded clinoptilolite results in the formation of spherical nano-NiO particles of approx. 5 nm in diameter which are randomly dispersed in the clinoptilolite lattice.     

Synthesis and utilization of chitin-humic acid hybrid as sorbent for Cr(III)

New types of hybrid material have been synthesized by using four different methods of immobilization of humic acid (HA) on chitin. The most stable hybrid material toward the change of medium acidity was then utilized as sorbent for Cr(III).The HA was extracted from peat soil of Gambut District, South Kalimantan, Indonesia, using the recommended procedure of International Humic Substances Society (IHSS), while the chitin was isolated from crab shell waste through deproteination using 3.5% (w/v) NaOH and followed by removal of inorganic impurities using 1 M HCl. The four methods of immobilization of HA on chitin were (i) Method A: chitin powder (4 g) was gently poured into the stirred solution of 0.4 g HA in 40 mL of 0.01 M NaOH. After overnight stirring, the solid was separated, washed with water, and dried in oven at 70 °C. (ii) Method B: gelatinous chitin (40 g) in 250 mL of 0.5 M HCl was reacted with HA (4 g) in 500 mL of 0.5 M NaOH and aged for 24 h. The product was washed with water and dried. (iii) Method C: HA powder (0.5 g) was mixed with the stirred gel of chitin (2.5 g) in 60 mL of CaCl₂ saturated methanol and the mixture was then washed with the mixed solution of 25 mL of 2 M sodium citrate and ethylene glycol 1:1. The solid was separated, washed with water, and dried. (iv) Method D: the solution of HA (0.056 g) in 10 mL of 0.01 M NaOH was reacted with the gel of chitin (0.2 g) in 10 mL of CaCl₂ saturated methanol. After 24 h stirring, the solid was separated from the reaction medium, washed with the mixed solution of 2 M sodium citrate and ethylene glycol 1:1, and followed by washing with water and drying. Parameters investigated in this study consisted of the stability test of the immobilized HA, as well as the rate constant (k₁), capacity (b), and energy (E) of sorption as well as the rate constant of desorption (k₋₁). The k₁ and k₋₁ were determined according to a kinetic model of first order sorption reaching equilibrium, while the b and E were determined according to the Langmuir isotherm model.Compared to HA, Methods, A, C, and D; Method B produced the most stable immobilization of HA on chitin. The hybrid material (Chitin-HA) synthesized through Method B was stable in the acidity range that equivalent to pH 2.0-11.0. At the acidity giving maximum sorption, i.e. pH 5, the presence of immobilized HA on the Chitin-HA enhanced more than three times the k₁ and k₋₁, i.e. from 0.057 min⁻¹ and 8.51 × 10⁻⁴ (min⁻¹) (mol/L) for chitin to 0.183 min⁻¹ and 3.27 × 10⁻³ (min⁻¹) (mol/L) for the Chitin-HA. On the contrary, the presence of HA on Chitin-HA only gave small increase on b and small decrease on E. The values of b and E for Cr(III) on chitin were 1.45 × 10⁻² mol/g and 23.12 kJ/mol, respectively, while those on Chitin-HA were 1.78 × 10⁻² mol/g and 19.95 kJ/mol, respectively.     

Influence of cetyltrimethylammonium bromide on the morphology of AWO4 (A = Ca, Sr) prepared by cyclic microwave irradiation

AWO₄ (A = Ca, Sr) was prepared from metal salts [Ca(NO₃)₂·4H₂O or Sr(NO₃)₂], Na₂WO₄·2H₂O and different moles of cetyltrimethylammonium bromide (CTAB) in water by cyclic microwave irradiation. The structure of AWO₄ was characterized by X-ray diffraction (XRD) and selected area electron diffraction (SAED). Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) revealed the presence of nanoparticles in clusters with different morphologies; spheres, peaches with notches, dumb-bells and bundles, influenced by CTAB. Six Raman vibrational peaks of scheelite structure were detected at 908, 835, 793, 399, 332 and 210 cm⁻¹ for CaWO₄ and 917, 833, 795, 372, 336 and 192 cm⁻¹ for SrWO₄, which are assigned as ν₁(A_g), ν₃(B_g), ν₃(E_g), ν₄(B_g), ν₂(A_g) and ν_f.r.(A_g), respectively. Fourier transform infrared (FTIR) spectra provided the evidence of W-O stretching vibration in [WO₄]²⁻ tetrahedrons at 793 cm⁻¹ for CaWO₄ and 807 cm⁻¹ for SrWO₄. The peaks of photoluminescence (PL) spectra were at 428-434 nm for CaWO₄, and 447-451 nm for SrWO₄.     

Cationic starch as a precursor to prepare porous activated carbon for application in supercapacitor electrodes

Three activated carbons (ACs) for the electrodes of supercapacitor were prepared from cationic starch using KOH, ZnCl₂ and ZnCl₂/CO₂ activation. The BET surface area, pore volume and pore size distribution of the ACs were evaluated using density functional theory method, based on N₂ adsorption isotherms at 77 K. The surface morphology was characterized with SEM. Their electrochemical performance in prototype capacitors was determined by galvanostatic charge/discharge characteristics and cyclic voltammetry, and compared with that of a commercial AC, which was especially prepared for use in supercapacitors. The KOH-activated starch AC presented higher BET surface area (3332 m² g⁻¹) and larger pore volume (1.585 cm³ g⁻¹) than those of the others, and had a different surface morphology. When used for the electrodes of supercapacitors, it exhibited excellent capacitance characteristics in 30 wt% KOH aqueous electrolytes and showed a high specific capacitance of 238 F g⁻¹ at 370 mA g⁻¹, which was nearly twice that of the commercial AC.     

Thermochemical behavior of metallic citrate precursors for the production of pure LaAlO3

Pure LaAlO₃ nanoparticles were synthesized, using a citrate-precursor technique. La(NO₃)₃, Al(NO₃)₃, and C₃H₄(OH)(COOH)₃, in a molar ratio of 1:1:4.5, were dissolved in deionized water. The pH of the aqueous solution was adjusted using NH₄OH. After drying, the citrate precursors were charred at 350 °C, followed by calcination at different temperatures. The thermochemical behavior of the charred citrate precursor to form LaAlO₃ was investigated using X-ray diffractometry, infrared spectroscopy, thermogravimetric analysis, and differential thermal analysis. While the charred specimen obtained at pH=2 (without NH₄OH addition) was composed of LaAl(OOCH₂)₃, the charred specimens obtained at pH>2 were composed of LaAlO_3−x−y(CO₃)_x(OH)_2y. All these metallic salts were decomposed at temperatures between 600 and 780 °C to form crystalline LaAlO₃ but calcining the specimens in air at ?800 °C were required to remove all residual chars to produce pure LaAlO₃. At 900 °C, the citrate-derived particles obtained at pH>2 were composed of LaAlO₃ crystallites with an average size of ∼30 nm.     

OH-absorption properties of the optical damage region in codoped In/Mg:LiNbO3 crystals with various Li/Nb ratios

OH-absorption properties of the optical damage region in a series of codoped In/Mg:LiNbO₃ crystals with various Li/Nb ratios have been investigated. The OH⁻-associated vibrational peak at 3507 cm⁻¹ is confirmed to occur in crystals with Li/Nb ratio of 0.94. For codoped In/Mg:LiNbO₃ crystals with Li/Nb ratio of 1.05 and 1.20, the OH⁻-associated vibrational peaks are detected at 3536 and 3507 cm⁻¹ as well. A new peak at 3518 cm⁻¹ attributed to a (In_Nb)²⁻-OH⁻-(Mg_Nb)³⁻ defect center is revealed in crystals with Li/Nb ratio 1.38. When the “In-Mg threshold” concentration is reached, the optical damage resistance ability of codoped In/Mg:LiNbO₃ crystals is greatly improved.     

Low-temperature oxidation of SiGe by liquid-phase deposition

Low-temperature silicon dioxide (SiO₂) films were grown on silicon germanium (SiGe) surfaces using the liquid-phase deposition (LPD) method. The growth solutions of LPD-SiO₂ are hydrofluorosilicic acid (H₂SiF₆) and boric acid (H₃BO₃). It was found that the growth rate increases with increasing temperature and concentration of H₃BO₃. The Auger electron spectroscopy profile shows that no pileup of Ge atoms occurs at the interface of SiO₂/SiGe after the LPD-SiO₂ growth. Al/LPD-SiO₂/p-SiGe MOS capacitors were prepared to determine capacitance-voltage (C-V) and current-voltage (I-V) characteristics. In our experiments, a low leakage current density of 8.69 × 10⁻⁹ A/cm² under a 2 MV/cm electric field was observed. Such a value is much smaller than those of plasma- and thermal-oxides as a result of no plasma damage and a lower growth temperature. Moreover, lower oxide charges and interface charge densities of 3.82 × 10¹⁰ cm⁻² and 1.12 × 10¹¹ eV⁻¹ cm⁻², respectively, were achieved in our LPD-SiO₂ compared to direct photochemical-vapor-deposition-SiO₂.     

Preparation and characterization of carbons for the retention of halogens in the condenser vacuum system of a thermonuclear plant

Activated carbons were prepared by air and carbon dioxide activation, from almond tree pruning, with the aim of obtaining carbons that reproduce the textural and mechanical properties of the carbons currently used in the filtering system of the condenser vacuum installation of a Thermonuclear Plant (CNA; Central Nuclear de Almaraz in Caceres, Spain), produced from coconut shell. The variables studied in non-catalytic gasification series with air were the temperature (215-270 °C) and the time (1-16 h) and the influence of the addition of one catalyst (Co) and the time (1-2 h) in catalytic gasification. In the case of activation with CO₂, the influence of the temperature (700-950 °C) and the time (1-8 h) was studied. The resulting carbons were characterized in terms of their BET surface, porosity, and pore size distribution. The N₂ adsorption isotherms at 77 K for both series showed a type I behaviour, typical of microporous materials. The isotherms showed that with both gasificant agents the temperature rise produced an increase in the carbon porosity. With regards to the activation time, a positive effect on the N₂ adsorbed volume on the carbons was observed. The best carbons of each series, as well as the CNA (carbon currently used in the CNA), were characterized by mercury porosimetry and iodine solution adsorption isotherms. The results obtained allowed to state that several of the carbons produced had characteristics similar to the carbon that is target of reproduction (which has S_BET of 741 m² g⁻¹, V_mi of 0.39 cm³ g⁻¹ and a iodine retention capacity of 429.3 mg g⁻¹): carbon C (gasification with CO₂ at 850 °C during 1 h), with S_BET of 523 m² g⁻¹, V_mi of 0.33 cm³ g⁻¹ and a iodine retention capacity of 402.5 mg g⁻¹, and carbon D (gasification with CO₂ at 900 °C during 1 h), whose S_BET is 672 m² g⁻¹, V_mi is 0.28 cm³ g⁻¹ and has a iodine retention capacity of 345.2 mg g⁻¹.     

Fabrication and application of highly ordered mesoporous Co3O4, NiO, and their metals

Highly ordered mesoporous Co₃O₄, NiO, and their metals were synthesized by nanocasting method using there corresponding mesoporous SBA-15 silica as a template. The obtained porous metal oxides have high surface areas, large pore volume, and a narrow pore size distribution. The N₂-adsorption data for mesoporous metal oxides have provided the BET area of 257.7 m² g⁻¹ and the total pore volume of 0.46 cm³ g⁻¹. The mesoporous metals were employed as a catalyst in the synthesis of (S)-3-pyrrolidinol from chiral (S)-4-chloro-3-hydroxybutyronitrile, and a high yield to (S)-3-pyrrolidinol-salt was obtained on the mesoporous Co metal catalyst.     

Characterization of MeWO4 (Me = Ba, Sr and Ca) nanocrystallines prepared by sonochemical method

Metal tungstates (MeWO₄, Me = Ba, Sr and Ca) were successfully prepared using the corresponding Me(NO₃)₂·2H₂O and Na₂WO₄·2H₂O in ethylene glycol by the 5 h sonochemical process. The tungstate phases with scheelite structure were detected with X-ray diffraction (XRD) and selected area electron diffraction (SAED). Their calculated lattice parameters are in accord with those of the JCPDS cards. Transmission electron microscopy (TEM) revealed the presence of nanoparticles composing the products. Their average sizes are 42.0 ± 10.4, 18.5 ± 5.1 and 13.1 ± 3.3 nm for Me = Ba, Sr and Ca, respectively. Interplanar spaces of the crystals were also characterized with high-resolution TEM (HRTEM). Their crystallographic planes are aligned in systematic array. Six different vibration wavenumbers were detected using Raman spectrometer and are specified as ν₁(A_g), ν₃(B_g), ν₃(E_g), ν₄(B_g), ν₂(A_g) and free rotation. Fourier transform infrared (FTIR) spectra provided the evidence of scheelite structure with W-O anti-symmetric stretching vibration of [WO₄]²⁻ tetrahedrons at 786-883 cm⁻¹. Photoluminescence emission of the products was detected over the range of 384-416 nm.     

Growth and characterization of two new NLO materials from the amino acid family: l-Histidine nitrate and l-Cysteine tartrate monohydrate

Single crystals of organic nonlinear optical (NLO) materials l-Histidine nitrate (C₆H₁₀N₃O₂)⁺ · (NO₃)⁻ and l-Cysteine tartrate monohydrate (C₃H₈NO₂S)⁺ · (C₄H₅O₆)⁻ · H₂O were grown by submerged seed solution method. Characterization of the crystals was made using single crystal X-ray diffraction. Fourier transform infrared (FTIR) spectroscopic studies, optical behaviour such as UV-visible-NIR absorption spectra and second harmonic generation (SHG) conversion efficiency were investigated to explore the NLO characteristics of the above materials. Microhardness measurements and dielectric studies of the compounds were also carried out.     

Preparation of activated carbons from cherry stones by activation with potassium hydroxide

Using cherry stones, the preparation of activated carbon has been undertaken in the present study by chemical activation with potassium hydroxide. A series of KOH-activated products was prepared by varying the carbonisation temperature in the 400-900 °C range. Such products were characterised texturally by gas adsorption (N₂, −196 °C), mercury porosimetry, and helium and mercury density measurements. FT-IR spectroscopy was also applied. The carbons prepared as a rule are microporous and macroporous solids. The degree of development of surface area and porosity increases with increasing carbonisation temperature. For the carbon heated at 900 °C the specific surface area (BET) is 1624 m² g⁻¹, the micropore volume is 0.67 cm³ g⁻¹, the mesopore volume is 0.28 cm³ g⁻¹, and the macropore volume is 1.84 cm³ g⁻¹.     

Solvothermal synthesis and characterization of CdSe nanocrystals with controllable phase and morphology

Zinc blende (ZB) CdSe hollow nanospheres were solvothermally synthesized from the reaction of Cd(NO₃)₂·4H₂O with a homogeneously secondary Se source, which was first prepared by dissolving Se powder in the mixture of ethanol and oleic acid at 205 °C. As Se power directly reacted with Cd(NO₃)₂·4H₂O in the above mixed solvents, wurtzite (W) CdSe solid nanoparticles were produced. Time-dependent experiments suggested that the formation of CdSe hollow nanospheres was attributed to an inside-out Ostwald ripening process. The influences of reaction time, temperature and ethanol/oleic acid volume ratio on the morphology, phase and size of the hollow nanospheres were also studied. Infrared (IR) spectroscopy investigations revealed that oleic acid with long alkene chains behaved as a reducing agent to reduce Se powder to Se²⁻ in the synthesis. Photoluminescence (PL) measurements showed that the ZB CdSe hollow nanospheres presented an obvious blue-shifted emission by 42 nm, and the W CdSe solid nanoparticles exhibited a band gap emission of bulk counterpart.     

Preparation of organic acid anion-modified magnesium hydroxides by coprecipitation: A novel material for the uptake of heavy metal ions from aqueous solutions

New layered magnesium hydroxides whose brucite layers had been bridged with malate²⁻ and tartrate²⁻ were prepared by dropwise addition of Mg(NO₃)₂ to malate and tartrate solutions at a constant pH of 10.5. Malate²⁻ and tartrate²⁻ may have been also absorbed on the surfaces of hydroxides. In the case of using citrate solution, Mg(OH)₂ absorbed with citrate³⁻ was produced. These materials were found to take up Cu²⁺ rapidly from an aqueous solution at pH 5.0. Copper uptake by precipitates is attributed to the formation of chelate complexes of Cu²⁺ with citrate³⁻, malate²⁻, and tartrate²⁻.     

Hierarchically porous nanoflowers from TiO2–B nanosheets with ultrahigh surface area for advanced lithium-ion batteries

In this work, hierarchically porous TiO₂–B nanoflowers have been successfully synthesized via a facile solvothermal method followed by calcination treatment. The TiO₂–B nanoflowers are constructed by thin nanosheets, presenting ultrahigh specific surface area, up to 214.6 m² g⁻¹. As anode materials for Li-ion batteries, the TiO₂–B sample shows high reversible capacity, excellent cycling performance and superior rate capability. The specific capacity of TiO₂–B could remain over 285 mA h g⁻¹ at 1 C and 181 mA h g⁻¹ at 10 C rate after 100 cycles. We believe that the pseudocapacitive mechanism, ultrahigh surface area and scrupulous nanoarchitecture of the TiO₂–B are responsible for the enhancement of electrochemical properties.     

Porous LiNi0.75Co0.25O2 microspheres prepared via a hydrothermal process as cathode material for lithium ion batteries

Porous LiNi_0.75Co_0.25O₂ microspheres are successfully prepared by a simple hydrothermal process by using H[Ni_0.75Co_0.25OOH]₃ and LiOH as starting materials in the presence of urea for the first time. The synthesized samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), specific surface area (S_BET), and electrochemical performance. The synthesized LiNi_0.75Co_0.25O₂ has a good electrochemical performance with an initial discharge capacity of 169.3 mA g⁻¹ and good capacity retention of 96.7% after 50 cycles at 0.2 C (25 mA g⁻¹). The electrochemical lithium ion insertion/extraction process is quite reversible even at 5 C. Furthermore, the structure in the charge-discharge process is stable and the impedance increased slowly during cycling.