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Herein we report a facile method for the synthesis of N-doped crystalline mesoporous titanium dioxide (NMT) with ordered structure. Structural characterization and HR-TEM studies revealed that NMT exhibits pure anatase phase with highly crystalline ordered mesoporous structure in NMT. The N2 isotherms are of type IV with an H1 hysteresis loop and a pronounced capillary condensation step at high relative pressure for NMT, suggesting the presence of well-ordered mesoporous structure. The reflectance spectrum of NMT shows stronger absorption in the visible region above 400 nm, owing to the substitution of the lattice oxygen by nitrogen. XPS results proved the doping of nitrogen in to oxygen in TiO2 lattice, which confirmed by the presence of peak at 401 eV for N1s. The efficiency of photocatalyst was evaluated by the degradation of Rhodamine-B and antibacterial activity against E. coli under visible-light irradiation. N-doped mesoporous TiO2 shows superior photocatalytic and anti-bacterial activity compared to pure TiO2 under visible-light irradiation. The enhanced photocatalytic activity of NMT is attributed to synergistic effect of NMT that is N-doping and well ordered crystalline mesoporous structure with high surface area of NMT. These findings suggest that N-doped mesoporous TiO2 has potential application in many areas such as degradation of hazardous pollutants, anti-bacterial agents, fuel cells, battery electrode, sensors, opto electronic devices, photo active self-cleaning surfaces.

An enhanced visible light photocatalytic performance of band-gap engineered bismuth titanate photocatalyst by tin and carbon (Sn&C) codoping is being reported in the present work. The photocatalyst sample was synthesized by the Pechini route and characterized by powder XRD, micro-Raman, XPS and HR-TEM studies. The photocatalytic performance of co-doped bismuth titanate was evaluated by the degradation of malachite green under the irradiation of natural sunlight. The photocatalytic results showed that Sn&C codoped bismuth titanate degraded the pollutant in 3 h whereas pristine bismuth titanate takes longer irradiation time (>5 h) for the complete degradation of malachite green. The improved visible light photocatalytic performance of Sn&C codoped bismuth titanate can be attributed to the significant decrease in the band gap energy (1.8 eV) relative to the pristine bismuth titanate (3.05 eV) coupled with high porosity, larger surface area and nanowire like morphology.

Livestock is one of the major contributors to nitrogen emission in the environment. Small portions of nitrogen, such as ammonia, nitrous oxide, nitric acid, and nitrate, constitute the reactive forms and produce the greenhouse gas effects. Buildup of reactive nitrogen in environment has led to poor air/water quality causing ailments in plants, humans, and animals. Cattle, buffaloes, sheep, goat, pigs, and poultry have the largest share in manure nitrogen production. Cattle and buffaloes are the largest contributors of ammonia accounting for 56.1% and 23.6%, respectively, followed by goat (10%), sheep (6%), and remaining 4.3% from rest of the species. Mitigation measures include maintaining optimum livestock numbers with better production efficiency, balanced feeding, optimizing protein and amino acids quality of diet, and reducing fecal nitrogen excretion through precision feeding. Eco-friendly manure management such as anaerobic composting, lime acidification, and biogas production will help in reduced nitrogen emission to the environment. Harnessing the benefits of abundantly available nitrogen for productive purposes would lead to safer environment and better nitrogen use efficiency.

This work focuses on the structure, morphology and photocatalytic performance of pure TiO2 and IO3--doped TiO2 nanoparticles. The photocatalytic activity IO3--doped TiO2 nanoparticles in the decomposition of monocrotophos (MCP) are illustrated and discussed in comparison with standard Degussa P-25. Furthermore, IO3--doped TiO2 showed high relative photonic efficiency compared with some of the commercial photocatalysts. The obtained results show a significant dependence of the degradation performance on IO3--doped TiO2 nanoparticles’s structural, morphological and composition properties. In particular, smaller particle size, large surface area and the formation of mixed phases of TiO2 by the addition of iodic acid have a beneficial influence to enhance the photocatalytic activity of IO3--doped TiO2 nanoparticles for the degradation as well as mineralization of MCP.

Here we report, for the first time, the synthesis of highly crystalline novel mesoporous carbon/nitrogen ( C / N )-codoped TiO 2 (MCNT) using ethylene diamine and carbon tetrachloride as the source for nitrogen and carbon, KIT-6 as the template, and titanium tetraisopropoxide as the TiO 2 source. The obtained material has been unambiguously characterized by various sophisticated techniques. XRD and TEM analysis revealed that the MCNT material possesses highly crystalline 3D structure with a continuous network of mesoporous channels as well as structure corresponding to TiO 2. UV-DRS analysis indicated that light absorption shifted to lower energy and stronger absorption in the visible light region. XPS revealed that C and N were doped effectively and C or N dopants might be present in the chemical environment of Ti – O – N or Ti – O – C . It has been found that the material is highly crystalline and possesses high surface area, pore volume and uniform pore size distribution. Owing to its textural characteristics, it could be useful for various applications, such as photocatalysis, fuel cells, bulky biomolecule adsorption and nanotechnology.

A novel nitrogen-doped mesoporous carbon with three-dimensional (3D) body centered Ia over(3, ̄) d structure (N-MCK6) has been successfully prepared for the first time by employing KIT-6 mesoporous silica as a hard template with aniline molecule as a carbon precursor. The polymerization of aniline molecules inside the mesochannels of KIT-6 template has been performed by ammonium peroxydisulfate. The obtained material has been unambiguously characterized by powder X-ray diffraction, nitrogen adsorption at -196 °C, high resolution transmission electron microscopy (HRTEM), electron energy loss spectroscopy (EELS), and X-ray photoelectron spectroscopy (XPS). XRD analysis revealed that N-MCK6 possesses 3D cubic structure with an enatiomeric pair of independently interpenetrating 3D continuous networks of mesoporous channels that are mutually intertwined and separated by carbon walls. HRTEM images of N-MCK6 display highly ordered mesoporous structure with linear array of mesopores, which are arranged in regular intervals. It has been found that the material is partially graphitic and possesses high surface area, pore volume and uniform pore size distribution. XPS, CHN and EELS analysis confirm that the nitrogen atom can be successfully doped in the carbon nanostructure. XPS results also revealed that the sample mainly possesses graphitic carbon atoms which are bonded to nitrogen in the form of imine and amine groups. This simple method can offer material with a considerable amount of nitrogen in the carbon lattice, which can be applied for many electrical and electronic, and energy storage applications. Refereed/Peer-reviewed

La-doped ZnO nano particles with different La contents were prepared by co-precipitation method using the precursors of zinc and lanthanum. The XRD results indicated that the particle size of La-doped ZnO is much smaller as compared to that of pure ZnO and decreases with increasing La loading. The effect of La loading on the photocatalytic activity of La-doped ZnO in the degradation of 2,4,6-trichlorophenol (TCP) was studied and the results are compared with the pure ZnO and TiO2. The results showed that the rate of degradation of TCP over La-doped ZnO is much higher as compared to that of pure ZnO and TiO2 and increases with increasing La loading upto 0.8 wt% and then decreases. Moreover, the relative photonic efficiency value of La-doped ZnO is relatively higher as compared to undoped ZnO. Among the catalyst studied, 0.8 wt% La-doped ZnO was the most active, showing high relative photonic efficiencies and high photocatalytic activity for the degradation of TCP. La doping in ZnO is highly effective and can significantly enhance the photocatalytic degradation and mineralization of TCP. The enhancement of photocatalytic activity of La-doped ZnO samples is mainly due to their smaller particle size and capability for reducing the electron hole pair recombination. Moreover, the increase of the TCP adsorption over La-doped ZnO samples may also be related for their high photocatalytic activity.

A simple wet-impregnation method and controlled calcination process was used for preparing nano-sized silicotungstic acid (STA) supported on zirconia embedded inside the various mesoporous silicas such as SBA- 15, MCM-41 and MCM-48. Catalysts with different (%) STA loadings were also synthesized and characterized by XRD, N-2 adsorption-desorption, TEM (29) Si-MAS NMR, FT-Raman spectroscopic techniques. The acidic behavior of the catalysts was studied by TPD of ammonia and FT-IR pyridine adsorption technique. The effect of calcination temperature on the textural parameters of the catalysts and the integrity of STA on the surface of the catalyst were also examined. Moreover, the performance of these catalysts was investigated in the esterification of isoamyl alcohol (IAA) with acetic acid (AA). Catalytic activities were correlated with the acidity of the catalysts. Effects of reaction parameters such as mole ratio of reactants, reaction temperature, catalyst concentration and reusability of the catalyst were studied to get higher substrate conversions and product selectivities. Among the catalysts, 15 wt.% STA/22.4 wt.% ZrO2/SBA-15 calcined at 1123 K was found to be the most active and acidic catalyst, showing higher conversion and selectivity than neat 15 wt.% STA/ZrO2 in esterification of lAA by AA. The reaction was found to be heterogeneously catalyzed and no contribution from homogeneous (leached) STA into the medium under the reaction conditions was observed. (C) 2007 Elsevier B.V. All rights reserved.

Three-dimensional cage type iron substituted mesoporous silica with different iron contents (FeSBA-1) was synthesized in a highly acidic media using cetyltriethylammonium bromide and tetraethylorthosilicate as a template and a silica source, respectively. Acylation of toluene with acetic anhydride (AA) was carried out over FeSBA-1 mesoporous catalysts with different n(si)/n(le) ratios in the temperature range 80-180 degrees C for a time-on-stream of 1-6 h under liquid phase conditions. The important factors affecting the conversion and the selectivity of the reaction, such as the reaction temperature, feed ratio, catalyst weight and time-on-stream were studied and the results are discussed in detail. The reaction conditions were optimized and the N-AA/n(Toluene) ratio of 2 and catalyst weight of 0.1 g (3.3 wt% of total reaction mixture) were maintained for all catalytic runs. It was found that the catalytic activity is strongly influenced by the amount of tetrahedral iron in the catalysts. Among the catalysts used in the present study, FeSBA-1(36) showed a high toluene conversion and selectivity to p-methylacetophenone (p-MAP) under the optimized reaction conditions. It was also found that the selectivity for p-MAP was always higher than in-NIAP and o-MAP for all the catalysts and the activity of the catalysts changes in the following order: FeSBA1(36) > FeSBA-1(90) > FeSBA-1(120). (c) 2006 Elsevier Inc. All rights reserved.

Mesoporous carbon nitride materials have been synthesized using SBA-15 by pore filling technique whereas mesoporous boron nitride and boron carbon nitride have been prepared by elemental substitution technique using mesoporous carbon as template. The obtained materials have been unambiguously characterized by sophisticated techniques such as XRD, HRTEM, EELS, XPS, FT-IR and N2 adsorption. The textural parameters of the materials are quite higher as compared to the respective nonporous nitrides. These materials could offer great potential for the applications, such as catalytic supports, gas storage, biomolecule adsorption and drug delivery.

In spite of its high protein content, castor cake is not used as livestock feed due to the presence of toxic factors—ricin, ricinine and allergen. Of the three, ricin is the most detrimental to the animals. In order to detoxify the cake, a number of physical and chemical methods were employed. Soaking (3, 6 and 12 h), steaming (30 and 60 min), boiling (30 and 60 min), autoclaving (15 psi, 30 min; 15 psi, 60 min) and heating (100 °C 30 min; 120 °C 25 min) were the physical methods employed, while the chemical methods consisted of ammonia (7.5, 12.5 ml/kg of castor cake), formaldehyde (5, 10 g/kg), lime (10, 20 and 40 g/kg), sodium chloride (5, 10 and 20 g/kg), tannic acid (5, 10 g/kg) and sodium hydroxide (2.5, 5 and 10 g/kg). The efficacy of the treatments was assessed, based on the qualitative and quantitative changes in ricin content. Of all the methods employed, autoclaving (15 psi., 60 min) and lime treatment (40 g/kg) completely destroyed the toxin.

Photochemically stable catalysts for complete degradation of organic dyes are yet to be developed. Most of the proposed systems suffer from loss of activity with use, at varying extent. In the present investigation, the photoactivity of TiβCD in the visible region is studied using the organic dye (Nile red). This system is relatively inexpensive, reproducible, extremely stable and efficient in complete degradation of dye in aqueous solution. In order to obtain maximum information about the performance of TiβCD catalyst, we varied the components of the system for dye degradation. The dependence of the degradation percentage on the amount of catalysts and concentration of the dye has been studied. In addition to the above, a comparative study on the photocatalytic activities of colloidal TiO 2 in the presence of the Nile red was also made.

The present investigation was carried out to study the affect of feeding urea ammoniated neem kernel meal on carcass characteristics and organoleptic properties of the meat in goats. Eight local weaned kids of 3-4 months age with mean body weight of 7.85±0.42 kg were assigned to two groups of four each in a completely randomised design and were offered diets containing isonitrogenous concentrate mixtures containing either peanut meal or urea ammoniated neem (Azadirachta indica) seed kernel meal (UANSKM) along with ad libitium oat hay or green sorghum as roughage for 13 fortnights. The animals were slaughtered at the end of the experimental period and the carcass characteristics and organoleptic evaluation of the meat was carried out. The carcass characteristics in terms of dressing percentage, meat bone ratio, percent edible and inedible did not differ between the treatments. Similarly the organoleptic characteristics and cooking loss were comparable between the treatments implying that UANSKM can be substituted for peanut meal in goat diets to alleviate the shortage and high cost of peanut meal without affecting meat quality. (Asian- Aust. J. Anim. Sci. 2003. Vol 16, No. 10 : 1451-1454)

The effect of urea treatment on chemical composition of neem seed kernel cake (NSKC) was investigated by soaking the cake in 2.1% urea solution (1.2 l kg -1 NSKC) for five days. The effect on utilisation of nutrients by replacing groundnut cake (GNC) (30%) with urea-treated neem seed kernel cake (UTNSKC) (33%) in a concentrate mixture fed to meet 70% of the protein requirements of lambs (8 males and 8 females), was monitored in a digestibility study. Following urea treatment of NSKC only 9.5% of urea was hydrolysed and the crude protein content of the cake was increased by 6.65%. The tannin content in depulped neem seeds was 37% catechin equivalent. Whereas feeding UTNSKC had no effect on intake of dry matter (72.5 vs 66.3 g/kg BW 0.75 day -1 ) and digestibility of crude fibre (41.3 vs 43.4%), the cake depressed (p

The performance of 12 male and 12 female Mandya × Merino lambs weighing between 5.4 and 12.4 kg was investigated by feeding neem seed kernel cake (NSKC) after treatment with 2.5% urea. Lambs of each sex were allotted randomly to concentrate mixture containing either 30% groundnut cake (GNC) or 33% urea-treated neem seed kernel cake (UTNSKC). Over a period of 182 days the concentrate mixtures fed, to meet 70% of the protein requirements of the lambs, were given with oat hay offered ad libitum. Replacement of GNC by UTNSKC in the concentrate mixture depressed (P 0.05) in lambs fed UTNSKC (74.0 g) and GNC (80.3 g). More DM (7.08 vs. 8.04 kg kg−1) and CP (1.10 vs. 1.23 kg kg−1) were required for growth on the ration containing UTNSKC. Feeding UTNSKC had no effect on blood profile, wool growth and carcass characteristics. Kidneys from animals fed UTNSKC were enlarged (P

A growth trial was undertaken to study the feasibility of total replacement of deoiled groundnut cake (DGNC) with urea ammoniated neem (Azadirachta indica) seed kernel meal (UANSKM). Isonitrogenous control (22% DGNC) and experimental (22.5% UANSKM) concentrate mixtures were fed to 12 male and 12 female goats to meet 90% of the CP requirements for 50 g daily gain. Ad libitum oat (Avena sativa) hay up to 8 fortnights or green sorghum (Sorghum vulgare) for the rest of period was also provided. The total body weight gain (kg), average daily gain (g), feed conversion efficiency (feed/gain) and feed cost (Rs.) per kg gain in the control group were 6.0 ± 0.56, 32.8 ± 3.20, 8.7 ± 0.55 and 29.8 ± 1.83, respectively. The corresponding figures in the experimental group were 5.6 ± 0.59, 31.0 ± 3.25, 9.1 ± 0.57 and 25.6 ∓ 1.62, respectively. The nutritive values of the consumed diets were comparable between the control and experimental group. Dietary variation did not significantly influence the efficiency of DM (8.7 vs 9.1 g), protein (1.2 vs 1.2 g CP) and energy (22.9 vs 22.8 kcal ME) utilization per unit gain. Feed cost per kg gain of the experimental diet was cheaper than the control diet by 14.2%. The concentration of blood biochemical constituents (haemoglobin, glucose and urea nitrogen) and the activity of various enzymes (transaminases and alkaline phosphatase) did not differ significantly between the treatments. The feeding cost per unit weight gain and average daily gain in males was marginally superior to females, though not significant. Glucose concentrations were higher (P < 0.01) in males, whereas the other blood constituents did not differ between the sexes. It is concluded that urea ammoniated neem seed kernel meal can be a satisfactory, economical and wholesome substitute to totally replace deoiled groundnut cake in rations of growing goats.

Two metabolism trials (experiments 1 and 2) were conducted to examine the effect of the organic S compound, sodium 3-mercapto-1-propane sulfonic acid (MPS) on feed intake, fiber digestibility, rumen fermentation and abundance of cellulolytic rumen microorganisms in cattle fed low S (

The monoclinic cell of di­cyclo­hexyl­ammonium 2,4-di­chloro­phenoxy­acetate contains four C12H24N+·C5H8Cl2O3− ion pairs. The ammonium N atom is hydrogen bonded to the oxy­gen ends of two carboxyl groups to form a 12-membered O—C—O⋯HNH⋯O—C—O⋯HNH ring. In (2,4-di­chloro­phenoxy­lacetato)­bis­(tri­phenyl­phosphine)silver(I), [Ag(C8H5Cl2O3)(C18H15P)2], the carboxyl CO2 unit chelates to the Ag atom in an anisobidentate manner [Ag—O = 2.436 (2) and 2.517 (2) A]; the Ag atom shows distorted tetrahedral geometry.

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Iron porphyrins are widespread in nature, being found as the active sites in hemoglobin, myoglobin and a wide range of cytochromes1. The most common porphyrin is Protoporphyrin IXiron(II)/(III) [PPIXFe(II)/(III)] (haem), however this complex is difficult to crystallise and its chemistry is often modelled using man made porphyrins. We have previously studied [FeIIIPPIXCl]2 by high pressure Mossbauer spectroscopy and found evidence of a change of spin from high spin state to a spin admixed state S = +/− 3/2, +/− 5/2.

Background: Psoriasis is a chronic inflammatory disease of the skin and joints with an increased cardiovascular risk. Previous studies have shown a higher prevalence of metabolic syndrome (MS) in psoriatic patients. Objective: To investigate the prevalence of MS in patients with psoriasis and healthy controls, and to determine the relation between disease severity and the presence of MS. Materials and Methods: We performed a hospital-based case-control study on 118 adult patients with psoriasis vulgaris and 120 controls matched for age, sex and body mass index. MS was diagnosed by the presence of three or more of the South Asian Modified National Cholesterol Education Program's Adult Panel III criteria. Results: MS was significantly more common in psoriatic patients than in controls (44.1% vs. 30%, P value = 0.025). Psoriatic patients also had a higher prevalence of triglyceridemia (33.9% vs. 20.8%, P value = 0.011), abdominal obesity (34.7% vs. 32.5%, P value = 0.035) and elevated blood sugar. There was no difference in the high density lipoprotein (HDL) levels and presence of hypertension among patients with psoriasis and normal controls. There was no correlation between the severity and duration of psoriasis with MS. Conclusion: MS is frequent in patients with psoriasis. We have found no relationship between disease severity and presence of MS. Hence, we suggest that all patients must be evaluated for the MS, irrespective of the disease severity.

Here we demonstrate a facile synthesis of 3D mesoporous carbon nitride with Ia3d symmetry (MCN-6) using mesoporous silica KIT-6 with 3D porous structure and different pore diameters as hard templates, and ethylenediamine and carbon tetrachloride as the sources for N and C, and C, respectively. The obtained materials possess bimodal pores that can be controlled with a simple adjustment of the pore diameter of the KIT-6 templates. The lower angle powder X-ray diffraction (XRD) patterns and high resolution transmission electron microscope (HRTEM) images confirm that the MCN-6 materials possess a well-ordered mesoporous 3D structure with a highly interwoven and a branched pore structure. The textural parameters such as the specific surface areas and specific pore volumes of the materials can also be controlled by tuning the pore diameter of the hard template. The specific surface area and the specific pore volume of the samples increase with increasing the pore diameter of the hard template. The C/N ratio of the MCN-6 is ca. 4.3 which is similar to that obtained for MCN-1 prepared from SBA-15 as template. FT-IR and XPS spectroscopy results reveal that samples contain a CN network with a lot of free NH 2 groups which are originated from ethylenediamine and can offer the basic sites. The temperature programmed desorption of CO 2 confirms that the samples are highly basic and the basicity of the sample is 0.195 mmol of CO 2 per g which is higher than that of MCN-1 (0.14 mmol of CO 2 per g). We tested the performance of MCN-6 materials in the base-catalyzed Knoevenagel condensation of benzaldehyde and malononitrile. The catalysts exhibit excellent activity and afford a high yield of the corresponding α,β-unsaturated nitrile in a short reaction time even at room temperature. In addition, catalysts are highly stable and can be recyclable several times without affecting their activity. Refereed/Peer-reviewed

Erratum Erratum to ‘‘Photocatalytic degradation of 2,4,6-trichlorophenol using lanthanum doped ZnO in aqueous suspension” [Catalysis Communications 8 (9) (2007) 1377–1382] S. Anandan , A. Vinu *, T. Mori , N. Gokulakrishnan , P. Srinivasu , V. Murugesan , K. Ariga b Nano-ionics Materials Group, Fuel Cell Materials Center, National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan b Supermolecules Group, Advanced Materials Laboratory, National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044, Japan Department of Chemistry, Anna University, Chennai 600 025, India

Microstructural development in sintered uranium dioxide pellets was studied with reference to (1) origin of the powder and (2) time, temperature and other conditions of sintering. Changes in the microstructure of the sintered pellets when reheated at temperatures below and above sintering temperature for various periods of time have also been studied. It was found that a judicious choice of the powder with desired characteristics and a judicious choice of optimum conditions for sintering of the powder have to be utilized to attain controlled microstructure. The grain size can be increased and grain development made more perfect by an appropriate thermal treatment of the sintered pellets.

It was shown earlier that uranium dioxide derived from different compounds exhibited variations in the sintering behaviour and to attain maximum densification, the sintering should be carried out within a temperature range, specific for each of the powders.In the present work, the sintering behaviour of uranium dioxide derived from ammonium diuranate prepared by different methods, was studied in an atmosphere of hydrogen. Significant differences in the sintering (densification) behaviour of the powders was noted under identical sintering (firing) treatments. The influence of variations in sintering treatment, such as rates of heating or soaking periods, on the densification of the samples of different origins was studied. It was found that the sintering behaviour depended on both the powder characteristics and the sintering treatment. Attempts were made to relate the origin and thermal history of the UO2 with its powder characteristics; and its sintering behaviour to its powder characteristics and the fir...

The investigation is aimed at a study of the relations between powder properties, sintering treatments and the densification and microstructure development in urania pellets. Urania powders for this study were prepared from ammonium diuranate by decomposition and reduction at various temperatures, namely, 400°, 600°, 900°, 1200° and 1500°C. Pellets prepared from these powders were sintered at temperatures in the range of 1200° to 1700°C with different soaking periods.The influence of (i) sintering temperatures, (ii) soaking periods at different temperatures, (iii) intermediate soaks at varying time periods at various temperatures, (iv) reheating of prepared sintered pellets and (v) rates of heating during sintering, on the density and microstructure development of pellets was studied in this investigation.The study revealed that urania pellets of specified density and grain development can be prepared by first attempting to achieve densification and then continuing the thermal treatments to attain the des...

As reported earlier, electrical conductivity of sintered uranium dioxide pellets depended on the calcination temperature and the sintering treatments, and could be related to the microstructure attained. The highest sintering temperature studied was 1700° C. In the present study, high density pellets prepared by sintering at 1500° C were refired at 1800°, 1900° and 2000°C. Though there were no significant changes in the densities, the electrical conductivity of the samples varied considerably showing a minima at a refiring temperature of 1900°C. Attempts were made to correlate the changes in electrical conductivity to the microstructural changes which still seem to be influenced by the thermal history of the samples.

In an earlier investigation, it was reported that the electrical conductivity of sintered compacts of urania powders depended on the calcination temperature and the sintering treatments. In the present study, the conductivity of the samples sintered at temperatures between 1100°C to 1700°C were studied. Attempts were made to correlate the changes in the conductivity with the microstructure of the samples. The details of the microstructure were studied by electron microscopy.