Fabrication of PES-based nanofiltration membrane modified by composite PAA-co-PMMA-g-ZnA nanoparticles

In the current research, nanocomposite polyethersulfone-based nanofiltration membranes were prepared by composite PAA-co-PMMA-g-ZnA nanoparticles. NF membranes were fabricated by phase inversion through casting solution technique. The effect of composite PAA-co-PMMA-g-ZnA nanoparticles concentration into the casting solution on physicochemical characteristics of membrane was studied. Scanning optical microscopy images showed uniform particle distribution for the membranes. Scanning electron microscopy images also demonstrated that membrane porosity was enhanced by increase in nanoparticles content ratio. The membrane surface 3D images showed smooth surface for the membranes filled with 0.05, 0.1 and 0.5 wt% nanoparticles. The contact angle results exhibited that membrane hydrophilicity was improved significantly by using of NPs in membrane matrix. The contact angle was decreased from 65.38° for PES membrane to 48.33° for membrane filled with 0.5 wt% nanoparticles. The water permeability was reduced initially by addition of 0.05 wt% nanoparticles into the casting solution and then increased by more nanoparticles loading rate (0.1 wt%). The water permeability was decreased again by more increase in nanoparticles loading range from 0.5 to 1 wt%. The salt rejection was improved strongly from 68.4 % for PES to 88.58 % for membrane filled with 0.5 wt% nanoparticles. The membranes mechanical strength was increased sharply from 2835.5 to 3337.3 kPa with addition of nanoparticles into the casting solution.     

Enhancement of catalytic activity in dehydrogenation ofn-dodecane over nano-structured Pt-Sn/SBA-16 catalysts by microwave drying

In the present investigation, experimental results from a study of cubic SBA-16-supported Pt-Sn bimetallic catalysts used to investigate dehydrogenation ofn-dodecane to 1-dodecene are presented. Pt (1 wt%)-Sn (1 wt%)/SBA-16 catalyst is synthesized using a simple co-impregnation (CI) method. Further, the impregnated catalysts are dried separately using microwave drying (MW-D) and conventional electrical drying (CE-D) techniques. The microwave-mediated drying of Pt (1%)-Sn (1%)/SBA-16 shows a better catalytic performance and time-on-stream activity for the target reaction.     

Formation and Physical Stability of Zanthoxylum bungeanum Essential Oil Based Nanoemulsions Co-Stabilized with Tea Saponin and Synthetic Surfactant

The purpose of this work was to evaluate the possibility of adding tea saponin (TS) to reduce the synthetic surfactant concentration, and maintain or improve the shelf stability of nanoemulsions. The Zanthoxylum bungeanum essential oil (2.5 wt%) loaded oil-in-water nanoemulsions were co-stabilized by Tween 40 (0.5–2.5 wt%) and TS (0.1–5 wt%). A combination of several analytical techniques, such as dynamic laser scattering, interfacial tension, zeta potential, and transmission electron microscope, were used for the characterization of nanoemulsions. Low levels of TS (0.1–0.5 wt%) with Tween 40 had significant effects on the emulsification, and a nanoemulsion with the smallest droplet diameter of 89.63 ± 0.67 nm was obtained. However, in the presence of high TS concentration (0.5–5 wt%), micelles generated by the non-adsorbed surfactants in the aqueous lead to droplets growth. In addition, the combinations of Tween 40 and TS at the high level (>3.5 wt%) exerted a synergistic effect on stabilizing the nanoemulsions and preventing both Ostwald ripening and coalescence. The negative charged TS endowed the droplets with electrostatic repulsion and steric hinderance appeared to prevent flocculation and coalescence. These results would provide a potential application of natural TS in the preparation and stabilization of nanoemulsions containing essential oil.     

添加Al2O3对Ni0.5Zn0.5Fe2O4纳米纤维结构和磁性能的影响

采用静电纺丝技术制备了添加0～20wt%Al2O3的Ni0.5Zn0.5Fe2O4纳米纤维。通过XRD、FESEM、TEM和VSM对样品的物相结构、形貌和磁性能进行了表征。结果表明,所合成的复合纳米纤维的直径都分布在40～150 nm之间,添加到纤维中的Al2O3主要以非晶态形式分布于铁氧体晶粒边界;随着Al2O3添加量的增加,可观察到γ-Fe2O3相逐渐析出,Ni-Zn铁氧体的晶格常数单调减小,说明有一些Al2O3进入到尖晶石晶格中取代了B位的Fe3+离子,Ni-Zn铁氧体的平均晶粒尺寸先增大后减小,在Al2O3添加量为8wt%时达到最大值39.2 nm;比饱和磁化强度和矫顽力随Al2O3添加量的增加呈现出相同的变化规律,先减小后增大,当Al2O3添加量超过5wt%时又开始变小。     

Ce0.1+xTi0.5-xAl0.2Y0.1La0.1O1.8材料的制备及在三效催化剂中的应用

采用共沉淀法制备了Ce0.1+xTi0.5-xAl0.2Y0.1La0.1O1.8(0≤x≤0.4)材料, 并对所制备的材料进行了X射线衍射(XRD)和X射线光电子能谱(XPS)的表征, 测定了材料的比表面积(BET法)和储氧量(OSC), 同时采用氢气程序升温还原(H2-TPR)和氨气程序升温脱附(NH3-TPD)研究了材料的还原性能和表面酸性. 研究结果表明, Ce/Ti摩尔比大于1∶2的材料能形成立方萤石结构的固溶体, Ce/Ti摩尔比为1时, 材料表面Ce4+/Ce3+摩尔比达到最大; 随着Ce/Ti摩尔比的增大, 材料的储氧能力先增大后减小, 而TPR还原峰温则是先减小后增大, 当Ce/Ti摩尔比为1时, 材料的储氧量达到最大, 为660 μmol/g; 还原峰峰温最低, 为616 ℃. 以制备的材料为载体制备了一系列Pt/Ce0.1+xTi0.5-xAl0.2Y0.1La0.1O1.8三效催化剂, 并对催化剂进行了活性评价. 活性测试结果表明, 以Ce/Ti比为1的载体材料制成的催化剂对C3H8, CO和NO的起燃温度分别为236, 147和228 ℃, 表现出了优异的温度特性.     

LiNi0.5-xAl2xMn1.5-xO4的制备、结构及电化学特征

采用喷雾干燥法合成了LiNi0.5-xAl2xMn1.5-xO4(0≤2x≤0.15)正极材料,研究Al掺杂对LiNi0.5Mn1.5O4材料结构与电化学性能的影响.通过X射线衍射(XRD)、扫描电子显微镜(SEM)、电感耦合等离子体-原子发射光谱(ICP-AES)、傅里叶红外光谱(FTIR)、循环伏安(CV)和充放电测试等手段对其结构及电化学性能进行表征.结果表明,Al取代Ni和Mn使材料的晶体结构发生了转变,空间群由P4332转变为Fd3m,同时增大了锂离子的扩散速率,提高了材料的倍率性能.在室温下,LiNi0.4 5Al0.1Mn1.45O4表现了最好的倍率性能,当放电电流为0.5 C时,放电容量为126 mA.h/g,当放电电流增加到5 C时,放电容量为109 mA.h/g,保持率达到了87%.此外,Al取代Ni和Mn有效降低了材料在高温下的Mn溶解量,从而有效改善了材料在高温大倍率下的循环性能.LiNi0.45Al0.1Mn1.45O4材料在50℃,倍率为3 C时,放电容量为121.7mA.h/g,循环50次后,仍可保留初始容量的94%.     

Microporous 3D aluminum MOF doped into chitosan‐based mixed matrix membranes for ethanol/water separation

An aluminum metal–organic framework (Al‐MOF), [Al(OH)(BPDC)] (DUT‐5; BPDC = Biphenyl‐4,4′‐dicarboxylate), was synthesized using solvothermal reactions. The high surface area and micropores (approximately 1.2 nm) of DUT‐5 were characterized using N₂ gas sorption measurements. The thermal stability of DUT‐5 and its phase purity were also investigated. The different amounts of DUT‐5 (0.1, 0.15, and 0.2 wt%) were successfully incorporated into the chitosan (CS) polymer to prepare a mixed matrix membrane (MMM) for the pervaporation of water/ethanol at 25°C. In particular, when 0.15 wt% of DUT‐5 was loaded, the DUT‐5@CS MMMs displayed excellent permeability and selectivity in ethanol/water separation. The results indicated that compared with pristine chitosan membranes, the flux of DUT‐5@CS membranes with 0.15 wt% loading significantly increased from 315 to 378 (g/m² h^?1) and the separation factor from 347 to 3,429. These promising results of the microporous Al‐MOF doped into chitosan MMMs reveal its good application potential for the bio‐ethanol separation processes.     

Crystallization behaviors and optical properties of isotactic polypropylene: comparative study of a trisamide and a rosin-type nucleating agent

The effects of concentrations of N, N’, N”-tris- tert. butyl- 1,3,5- benzene- tricarboxamide (NA) and a hemiacid of dehydroabietic acid (1:1 K) on the optical properties of iPP were compared with each other. It revealed that the NA was an effective transparent nucleating agent for iPP. The NA had advantage at very concentration (0.02 wt%), while the 1:1 K had some advantage at high concentrations (0.3 wt%～0.5 wt%), The optimal concentration range of the NA was 0.1 wt% to 0.4 wt%, while the value for 1:1 K was 0.3 wt% to 0.5 wt%. The absence of detectable spherulites in nucleated iPP was confirmed by SEM and POM. This was an important reason why the nucleated iPPP showed improved optical properties. The results of WAXD showed that preferential growth along the b-axis during crystallization and more disordered structures were formed in the nucleated samples. The results of DSC disclosed increased crystallization peak temperature and melting temperature in the nucleated samples.     

Ti-doped LiAlH4 for hydrogen storage: synthesis, catalyst loading and cycling performance

The direct synthesis of LiAlH(4) from commercially available LiH and Al powders in the presence of TiCl(3) and Me(2)O has been achieved for the first time. The effects of TiCl(3) loadings (Ti/Al = 0, 0.01, 0.05, 0.2, 0.5, 1.0 and 2.0%) and various other additives (TiCl(3)/Al(2)O(3), metallic Ti, Nb(2)O(5), and NbCl(5)) on the formation and stability of LiAlH(4) have been systematically investigated. The yield of LiAlH(4) initially increases, and then decreases, with increasing TiCl(3) loadings. LiH + Al → LiAlH(4) yields above 95% were obtained when the molar ratios of Ti/Al were 0.05 and 0.2%. In the presence of a very tiny amount of TiCl(3) (Ti/Al = 0.01%), LiAlH(4) is still generated, but the yield is lower. In the complete absence of TiCl(3), LiAlH(4) does not form. Addition of metallic Ti, Nb(2)O(5), and NbCl(5) to commercial LiH and Al does not result in the formation of LiAlH(4). Preliminary tests show that TiCl(3)-doped LiAlH(4) can be cycled, making it a suitable candidate for hydrogen storage.     

Application of ion-exchange cartridge clean-up in food analysis. II. Determination of benzylpenicillin, phenoxymethylpenicillin, oxacillin, cloxacillin, nafcillin and dicloxacillin in meat using liquid chromatography with ultraviolet detection.

A multiresidue analytical method was developed for the simultaneous determination of benzylpenicillin (PCG), phenoxymethylpenicillin (PCV), oxacillin (MPIPC), cloxacillin (MCIPC), nafcillin (NFPC) and dicloxacillin (MDIPC) in meat. The method involves the use of an ion-exchange cartridge for sample clean-up followed by ion-pair high-performance liquid chromatography with ultraviolet detection. The recoveries of PCG, PCV, MPIPC, MCIPC, NFPC and MDIPC from pork muscle spiked at levels of 0.5, 0.1 and 0.05 mg/kg were in the range of 77-90, 73-95 and 80-93% with coefficients of variation of 0.5-1.7, 1.6-4.4 and 3.2-6.6%, respectively. For beef muscle spiked at levels of 0.5, 0.1 and 0.05 mg/kg, the recoveries of these compounds were 83-92, 71-86 and 77-90% with coefficients of variation of 1.7-4.4, 2.6-7.0 and 3.9-6.4%, respectively. The detection limits for each penicillin were 0.02 mg/kg in meat.     

The use of a polymer inclusion membrane in a paper-based sensor for the selective determination of Cu(II)

A disposable paper-based sensor (PBS) is described for the determination of Cu(II) in natural and waste waters at approximately 2 cents per measurement. The device makes use of a polymer inclusion membrane (PIM) to provide the selectivity for Cu(II). The PIM consists of 40 wt% di(2-ethlyhexyl) phosphoric acid (D2EHPA) as the carrier, 10 wt% dioctyl phthalate (DOP) as a plasticizer, 49.5 wt% poly(vinyl chloride) (PVC) as the base polymer and 0.5 wt% (m m⁻¹) 1-(2′-pyridylazo)-2-naphthol (PAN) as the colourimetric reagent. High selectivity under mildly acidic conditions (HCl, pH 2.0) is achieved for Cu(II) in the presence of frequently encountered metal ions in natural and waste waters such as Fe(III), Al(III), Zn(II), Cd(II), Pb(II), Ca(II), Mg(II), and Ni(II).     

Al-Ni2P/SBA-15催化剂的制备、表征及加氢脱硫催化性能

以磷酸氢二铵为磷源,硝酸镍为镍源,硝酸铝为助剂铝源,制备了n_P/n_Ni=0.8,Al含量为1.06wt%~6.35wt%的一系列Al-Ni₂P/SBA-15催化剂。采用XRD、TEM和N₂吸脱附等技术对催化剂的结构进行了表征研究,以二苯并噻吩(DBT)作为模型化合物,在微型固定床反应器上对催化剂的加氢脱硫(HDS)性能进行了评价。结果表明,Al修饰的Al-Ni₂P/SBA-15催化剂仍然保持介孔结构,当Al含量低于5.29wt%时,催化剂的物相主要是Ni₂P,当Al含量在5.29wt%-6.35wt%之间时,催化剂的物相为Ni₂P和Ni₁₂P₅。Al含量为4.24wt%的3-Al-Ni₂P/SBA-15催化剂具有最好的二苯并噻吩加氢脱硫催化活性,在反应温度为360 ℃,反应压力为3.0 MP的条件下,3-Al-Ni₂P/SBA-15催化剂对二苯并噻吩的转化率可达99.0%。     

Genipin‐crosslinked gelatin hydrogel incorporated with PLLA‐nanocylinders as a bone scaffold: Synthesis,characterization, and mechanical properties evaluation

Nowadays, despite remarkable progress in developing bone tissue engineering products, the fabrication of an ideal scaffold that could meet the main criteria, such as providing mechanical properties and suitable biostability as well as mimicking the bone extracellular matrix, still seems challenging. In this regard, utilizing combinatorial approaches seems more beneficial. Here, we aim to reinforce the mechanical characteristics of gelatin hydrogel via a combination of Genipin‐based chemical cross‐linking and incorporation of the poly l ‐lactic acid (PLLA) nanocylinders for application as bone scaffolds. Amine‐functionalized nanocylinders are prepared via the aminolysis procedure and incorporated in gelatin hydrogel. The nanocylinder content (0, 1, 2, 3, and 4 wt%) and cross‐linking density (0.1, 0.5, and 1 wt/vol%) are optimized to achieve suitable morphology, swelling ratio, degradation rate, and mechanical behaviors. The results indicate that hydrogel scaffold cross‐linking by 0.5 wt% of Genipin shows optimized morphological feathers with a pore size of around 300 to 500 μm as well as an average degradation rate (40.09% ± 3.08%) during 32 days. Besides, the incorporation of 3 wt% PLLA nanocylinders into the cross‐linked gelatin scaffold provides an optimized mechanical reinforcement as compressive modulus, and compressive strength show a 4‐ and 2.6‐fold increase, respectively. 3‐(4,5‐dimethylthiazol‐2‐yl)‐2,5‐diphenyltetrazolium bromide assay indicates that the scaffold does not have any cytotoxicity effect. In conclusion, gelatin composite reinforced with 3 wt% PLLA nanocylinders cross‐linked via 0.5 wt/vol% Genipin is suggested as a potential scaffold for bone tissue engineering applications.     

Thermal,mechanical and water barrier properties of graphene oxide/polyvinyl alcohol/polyol composite films

The novel polymer composite of polyvinyl alcohol (PVA), polyol(PO) and graphene oxide (GO) was used to prepare the PVA/PO and GO/PVA/PO with different weight percents of GO (0.5 and 1% denoted as (0.5 wt%)GO/PVA/PO and (1 wt%)GO/PVA/PO, respectively) through solution casting blend technique. The structure–properties of all used films were confirmed by scanning electron microscope (SEM), Transmission Electron Microscope (TEM), X-ray powder diffraction (XRD), thermogravimetric analysis (TGA) and mechanical properties. The SEM results exhibited the uniform and homogeneous dispersion of GO in the PVA/PO blend matrix. The TEM and XRD analysis confirmed the structure and exfoliation of GO nanosheets, respectively. Thermal stability suggested that (0.5 wt%)GO/PVA/PO and (1 wt%) GO/PVA/PO films are more stable than PVA/PO. The tensile strength of (0.5 wt%)GO/PVA/PO and (1 wt%)GO/PVA/PO films reached 270.5% and 1349.6%, respectively, which are higher than that of the PVA/PO film. The decrease in the water absorption (WA) of GO/PVA/PO was found from 110.5 to 38.4%. The physico-mechanical properties of used films suggested that the prepared GO/PVA/PO blend composite films can be applied in food packaging areas.     

Solvothermal synthesis and characterization of a series of lanthanide thiostannates(IV): the first examples of inorganic-organic hybrid cationic lanthanide thiostannates(IV)

A series of new lanthanide thiostannates(IV), [Y(2)(dien)(4)(μ-OH)(2)]Sn(2)S(6) (1, dien = diethyl-enetriamine), (tetaH)(2)[Ln(2)(teta)(2)(tren)(2)(μ-Sn(2)S(6))]Sn(2)S(6) [Ln = Eu (2), Sm (3); teta = triethylenetetramine; tren = tris(2-aminoethyl)amine] and [Eu(2)(tepa)(2)(μ-OH)(2)(μ-Sn(2)S(6))](tepa)(0.5)·H(2)O (4, tepa = tetraethylene-pentamine) were solvothermally synthesized and structurally characterized. 1 consists of a binuclear [Y(2)(dien)(4)(μ(2)-OH)(2)](4+) cation and a discrete dimeric [Sn(2)S(6)](4-) anion. Both 2 and 3 are isostructural and composed of [Ln(2)(teta)(2)(tren)(2)(μ-Sn(2)S(6))](2+) cations, protonated triethylenetetramines (tetaH), and discrete dimeric [Sn(2)S(6)](4-) anions. A Sn(2)S(6)(4-) anion bridges two [Ln(teta)(tren)](3+) cations via the trans-S(t) (t = terminal) atoms to form the first examples of inorganic-organic hybrid thiostannate cations [Ln(2)(teta)(2)(tren)(2)(μ-Sn(2)S(6))](2+). 4 consists of one-dimensional (1-D) neutral chains [Eu(2)(tepa)(2)(μ-OH)(2)(μ-Sn(2)S(6))](n) built up from the linkage of dinuclear complex cations [Eu(2)(tepa)(2)(μ(2)-OH)(2)](4+) and bridging anions [Sn(2)S(6)](4-), free tepa molecules, and lattice water molecules. The present compounds exhibit wide-band gap semiconducting properties with absorption band edges between 2.40 and 2.91 eV.     

Structural Investigation of Mixed Nitrided Galloaluminophosphates “AlGaPON” by EELS, XAS, and XPS Spectroscopies

Amorphous nitrided galloaluminophosphates “AlGaPON” catalysts with nitrogen contents varying from 0 to 23.3 wt% N were obtained by nitriding an Al_0.5Ga_0.5PO₄ precursor under ammonia flow at 750°C in a tubular furnace. The structural changes induced by this treatment were investigated by electron energy loss spectroscopy (EELS), X-ray absorption spectroscopy (XAS), and X-ray photoelecton spectroscopy (XPS). XANES and XPS results indicate that the first-coordination spheres of P, Ga, and Al atoms are modified by nitridation. In particular, the comparison of the P XANES spectra recorded on “AlGaPON” and on a PON phosphorus oxynitride (reference of mixed PO₂N₂ tetrahedra) reveals that mainly PO₂N₂ tetrahedra are present in highly nitrided samples. Moreover, the replacement of oxygen by nitrogen probably concerned P-O-Ga bonds rather than P-O-Al. EELS investigation reveals that the precursor is homogeneous at the used probe scale, but indicates that nitridation is accompanied by a loss of homogeneity of the material.     

Catalytic Influence of Bimetallic Bifunctional Ni-Pd/H-β and H-Mordenite Nanoporous Catalysts for Hydroisomerisation of <Emphasis Type="Italic">n</Emphasis>-Octane

Zeolite-β and mordenite were impregnated with 0.1 wt% Pd and varying the amount (0.1–0.5 wt%) of Ni. The prepared nanoporous catalyst were characterized by various physico-chemical techniques such as XRD, nitrogen adsorption–desorption isotherm (BET), NH₃-TPD and TPR, XPS and TEM. Hydroisomerisation of n-octane was carried out in the temperature range from 200 to 450 °C in the presence of flowing H₂ gas under 1 atm. Finally we found that Ni addition up to 0.3 and 0.2 wt% over 0.1 wt% Pd/H-β and H-mordenite enhances the n-octane conversion and isomerisation selectivity. As the Ni amount exceeds the threshold values, the conversion decreases with increase in cracked products, and also, the selectivity of mono and dibranched isomers were improved suggestion operation of PCP intermediate mechanism. The bimetallic catalysts were more selective to the formation of dibranched isomers with higher octane number, when compared with monometallic catalysts. Ni-Pd loaded zeolite-β supports always show higher activity and selectivity than mordenite supports. Moreover, we achieved higher conversion (74.9 %) and isomerisation selectivity (92.5 %) at low Ni loading (0.3 Ni wt% over 0.1 Pd wt%/Hβ) for the first time.     

Dependence of mechanical properties on β‐form content and crystalline morphology for β‐nucleated isotactic polypropylene

As part of a continuous effort to develop high performance isotactic polypropylene (iPP) based on β‐form crystalline and morphological change induced by rare earth nucleator (WBG), various WBG contents (from 0.025 to 1.0 wt%) were adopted to prepare β‐nucleated iPP at a fixed final molten temperature (240°C) in this study. The crystallinity, polymorphic composition, and crystalline morphology were inspected in detail by a series of crystallographic characterizations, including calorimeter, X‐ray diffraction, polarized light microscopy (PLM), and electron microscopy. Furthermore, the self‐organization and re‐crystallization behavior of β‐nucleating agent occurred during cooling was characterized by rheometry. Finally, the dependence of mechanical properties, including tensile strength, elongation at break, and impact strength, on WBG content was discussed based on the variations in β‐form content and crystalline morphology. Interestingly, it is found that while the WBG content is below 0.1 wt%, the toughness of β‐nucleated iPP increases with increase in WBG content due to additional β‐form content; as the WBG content is in range of 0.1–0.5 wt%, the toughness increases at a lower rate with increase in WBG content due to β‐crystalline morphological change. However, a decrease in toughness is observed while nucleator content is above 0.5 wt% as WBG remains undissolved in iPP upon the adopted processing conditions. The result of this study provides valuable information for potential industrial applications. Copyright © 2010 John Wiley & Sons, Ltd.     

尖晶石型LiMn1.9Al0.1O3.95F0.05材料的制备及其增强的倍率性能

通过溶胶-凝胶和高温固相掺杂反应可控合成了形貌均匀、结晶性好的尖晶石型LiMn_1.9Al_0.1O_3.95F_0.05正极材料,探究了Al部分取代Mn、F部分取代O后对结构的影响,测试并比较了电极材料的倍率性能和循环充放电性能. 结果表明,尖晶石型LiMn_1.9Al_0.1O_3.95F_0.05和LiMn₂O₄有同样的晶型,但电极较传统的LiMn2O4电极倍率稳定性有显著提高. 在连续混合（如0.1C、0.5C和1C）充放电150次后,LiMn_1.9Al_0.1O_3.95F_0.05电极的容量仍能保持90%以上.     

Differential thermal analysis of the Al+20% (Fe-50%B) system

In the present study, aluminium and mechanically alloyed (36 h) Fe/B (50 wt%) are mixed. Al+20 (wt%) Fe/B mixture has been studied by differential thermal analysis to determine the aluminium quantity that is supposed to melt and afterwards does not solidify as it reacts with Fe/B powder. The different areas between endothermic reaction (melting peak) and exothermic reaction (solidification peak) allow in knowing the quantity of aluminium that reacts with Fe/B and the amount of intermetallic phases formed at high temperature. In order to follow the process, compacts were sintered at different temperatures (700, 800, 900, 1000 and 1200 °C), in N₂/10H₂/0.1CH₄ atmosphere. Microstructure was evaluated by image analysis and the results obtained by both techniques are compared.