Thermoanalytical investigations on kinetics and mechanism of deamination of tris(ethylenediamine)copper(II) sulphate

Nair, C.G.R.; Mathew, Suresh; Ninan, K. N.

doi:10.1007/bf01913732

Cited by 9 publications

(4 citation statements)

References 25 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The polycondensation reaction performed at 150°C for 2-60 min did not lead to the complete reduction of Cu 2+ ions and, therefore, the reflections associated with Cu 0 , as well as with Cu 2 O and CuO 2 [26][27][28][29], were observed in the XRD patterns (Fig. 5).…”

Section: Resultsmentioning

confidence: 99%

“…For instance, due to the higher content of the crystalline phase, the intensity of the amorphous halo in the samples obtained at 150°C is significantly lower than in the sample prepared at 200°C. In addi tion, the reflections corresponding to copper nano particles [23] and, depending on conditions [24,25], copper oxides Cu 2 O/CuO 2 [26][27][28][29] were identified in the diffractograms. The IR heating of a sample must take place in argon atmosphere at 250-350°C for 5 min in a nanocomposite material containing only nanoparticles of zero valent copper of 2 to 6 nm diam eter according to the TEM images (Fig.…”

Section: Resultsmentioning

confidence: 99%

See 1 more Smart Citation

Synthesis, structure, and properties of new Cu/polydiphenylamine metallopolymer nanocomposites

et al. 2011

View full text Add to dashboard Cite

EXPERIMENTALCommerically available solvents and chemicals were used without further purification unless other wise stated. Ammonium persulfate and toluene were additionally subjected to crystallization [16] and frac tional distillation [17], respectively. The monomer and other reagents were prepared as described earlier [13]. The oligomers of polydiphenylamine were synthesized by the interphase (water/toluene) oxidative polymeri zation of diphenylamine monomer ([M] = 0.2 M) using ammonium persulfate ([(NH 4 ) 2 S 2 O 8 ]/[M] = 1.25) and hydrochloric acid ([M]/[HCl] = 1/5) [13].The synthesis of Cu/polydiphenylamine nano composites was performed by dissolving diphe nylamine oligomers (2 wt %) in DMFA solution con taining 5-30 wt % of copper acetate monohydrate (with respect to M w of oligomers) followed by the removal of the solvent in vacua at 85°C. The residue was then treated at 150-350°C for 2-60 min under an Ar atmosphere using an automated IR heating machine [18].The FTIR spectra were recorded using a Specord M-82 spectrophotometer with Soft Spectra software package over the region 4000-400 cm -1 on samples prepared in KBr pellets. An X ray analysis of obtained materials was performed with a Rigaku dif fractometer in a continuous mode (FeK α source, Bragg-Brentano geometry). Transmission scanning microscopy (EM-301, acceleration voltage 60-80 kV, Phillips) was used to study the microstructure of Cu/polydiphenylamine nanocomposites, while atomic adsorption spectroscopy (AAS 30, Carl Zeiss Jena) was applied for quantitative copper analysis of the fabricated samples.A thermogravimetric analysis (TGA) was carried out using a Netzsch TG 209 F1 thermomicrobalance under the dynamic mode in a stream of nitrogen or air in the temperature range 30-820°C. The sample was thermostated first at 30°C for 15 min and then for the second time at 820°C for 30 min. The TG experimen tal parameters were as follows: a heating rate of 10°C/min, a nitrogen flow rate of 50 ml/min, a sample weight of 100 mg, and a standard alumina made cru cible.The calorimetric measurements were performed using a TA-4000 differential scanning calorimeter (Mettler) equipped with a DSC-30 heating cell at a heating rate of 10°C/min under N 2 in the temperature range 20-350°C. RESULTS AND DISCUSSIONA comparison of the IR spectra of the starting oli gomers and the obtained Cu/polydiphenylamine nanocomposites (Fig. 1) revealed an increase in the intensity of the adsorption bands associated with the deformation vibration of aromatic C-H groups (812 cm -1 ) and valent oscillations of C=N bonds in the quinonoid like structures (1650 cm -1 ) [13,[19][20][21] as a result of the growth of the polymeric chain and the increase in the oxidation level of the product.It was shown that the thermal Cu induced poly condensation [22] of crystalline oligomers of dipheny lamine is accompanied by a release of hydrogen, which consequently leads to the reduction of Cu 2+ ions to nanoscale particles of Cu 0 (Fig. 2a).Abstract-It was found that the Cu induced thermal polycondens...

show abstract

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Synthesis, structure, and properties of new Cu/polydiphenylamine metallopolymer nanocomposites

et al. 2011

View full text Add to dashboard Cite

show abstract

“…The PXRD diffraction pattern of the tubes obtained corresponded to that of CuO as identified from JCPD file. 56 To obtain pure copper tubes, Figure 7, the coaxial fibers were first calcined at 550 °C for 2 h under air atmosphere followed by another 1 h under 6% H 2 in N 2 gas. Hydrogen gas was used to facilitate the reduction of CuO to Cu tubes.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…This was due to the oxidation reaction that takes place upon heating copper metal in presence of oxygen. The PXRD diffraction pattern of the tubes obtained corresponded to that of CuO as identified from JCPD file . To obtain pure copper tubes, Figure , the coaxial fibers were first calcined at 550 °C for 2 h under air atmosphere followed by another 1 h under 6% H 2 in N 2 gas.…”

Section: Resultsmentioning

confidence: 99%

Electrically Conducting Polymers As Templating Interfaces for Fabrication of Copper Nanotubes

et al. 2012

View full text Add to dashboard Cite

Submicrometer tubes have been fabricated by a polymer-based template approach using electroless deposition. The copper was deposited on polystyrene fibers functionalized with an interfacial electrically conducting polyaniline thin film layer. Thermal degradation of the functionalized fiber templates resulted in copper tubes of diameter 1600 ± 50 nm with wall thicknesses ranging between 100 and 200 nm. The morphology and elemental analysis of copper coaxial fibers was analyzed using SEM and EDS. Electrical properties were analyzed using FTIR and PXRD was used to study crystal structure of copper nanotubes.

show abstract

Contribution of HRTEM to the characterization of silica-incorporated copper-oxide catalysts prepared by the Sol-Gel technique

Benaı̈ssa¹,

Díaz²

1998

Microsc. Res. Tech.

View full text Add to dashboard Cite

Thermoanalytical investigations on kinetics and mechanism of deamination of tris(ethylenediamine)copper(II) sulphate

Cited by 9 publications

References 25 publications

Synthesis, structure, and properties of new Cu/polydiphenylamine metallopolymer nanocomposites

Synthesis, structure, and properties of new Cu/polydiphenylamine metallopolymer nanocomposites

Electrically Conducting Polymers As Templating Interfaces for Fabrication of Copper Nanotubes

Contribution of HRTEM to the characterization of silica-incorporated copper-oxide catalysts prepared by the Sol-Gel technique

Contact Info

Product

Resources

About