Mossbauer Spectroscopic Studies on a Supersaturated Solid Solution of Fe-Cu Formed by Mechanical Alloying

Mechanical alloying (MA) was employed to produce supersaturated solid solutions of Fe1-xCux,which is virtually immiscible under an equilibrium condition at ambjent temperature. The X-ray diffraction results show that the solutions formed in the concentration ranges of x≤0.1 5 and x≥0.40 are of bcc structure of iron and fcc structure of copper. respectively. For the region in between.however, the alloy obtained is a mixture of bcc plus fcc phases. The Mossbauer spectrum of the solid solution of a single phase could be fitted by two sub-spectra with hyperfine magnetic fields of 200 and 250 kOe. respectively. suggesting that there must exist two forms of coordination in the solution. While to fit the spectrum for the solution with mixed structu re. three Sub-spectra. including a spectrum of α-Fe, should be used. The variation of the Mossbauer spectra of Fe60Cu40 with milling time as well as annealing temperature was systematically studied. This may be ascribed to the changes of the number of nearest neighboring atoms of iron in the processes of formation and decomposition of the solid solution during milling and annealing     

Mechanically Driven Alloying and Structural Evolution of Nanocrystalline Fe_(60)Cu_(40) Powder

Highly supersaturated nanocrystalline fcc Fe60Cu40 alloy has been prepared by mechanical alloying of elemental powders. The phase transformation is monitored by X-ray diffraction (XRD),Mossbauer spectroscopy and extended X-ray absorption fine structure (EXAFS). The powder obtained after milling is of single fcc structure with grain size of nanometer order. The Mossbauer spectra of the milled powder can be fitted by two subspectra whose hyperfine magnetic fields are 16 MA/m and 20 MA/m while that of pure Fe disappeared. EXAFS results show that the radial structure function (RSF) of Fe K-edge changed drastically and finally became similar to that of reference Cu K-edge, while that of Cu K-edge nearly keeps unchanged in the process of milling. These imply that bcc Fe really transforms to fcc structure and alloying between Fe and Cu occurs truly on an atomic scale. EXAFS results indicate that iron atoms tend to segregate at the boundaries and Cu atoms are rich in the fcc lattice. Annealing experiments show that the Fe atoms at the interfaces are easy to cluster to α-Fe at a lower temperature, whereas the iron atoms in the lattice will form γ-Fe first at temperature above 350℃, and then transform to bcc Fe     

Thermal Stability of Fe2O3 Nanowires

The thermal stability of α-Fe203 and γ-Fe2O3 nanowires was studied by post annealing the samples at different temperatures. Before and after annealing, the samples were characterized by X-ray diffraction and scanning electron microscopy. The α-Fe2O3 nanowires are stable at the temperatures up to 600℃, and the crystalline structure becomes more perfect after annealing. This behavior supplies a way to improve the quality of the α-Fe2O3 nanowires. The γ-Fe2O3 nanowires become unstable when annealed at 350℃. Raman spectra of both nanowires have been measured, which also indicate that the γ-Fe203 nanowires are transformed into α-Fe2O3 under the strong laser beam.     

β→α Transformation of γ-Phase in Sintered WC-Co Cemented Carbides

Varying the morphology and the structure of γ-phase (Co-base Co-W-C solid solution) by means of altering the cooling rate and the preparing method of liquid sintered WC-Co cemented carbides samples, the mechanism of fcc→hcp transformation of γ-phase in WC-Co alloy has been explored. The results show that, the cooling rate is an important affecting factor on fcc→hcp transformation of γ-phase and the fcc→hcp transformation is mainly a diffusive type when cooling WC-Co samples above room temperature     

Mechanical and Wear Properties of Nanostructured Surface Layer in Iron Induced by Surface Mechanical Attrition Treatment

A porosity-free and contamination-free surface layer with grain sizes ranging from nanometer to micrometer in Fe samples was obtained by surface mechanical attrition treatment (SMAT) technique. Mechanical and wear properties of the surface layer in the SMATed and annealed Fe samples were measured by means of nanoindentation and nanoscratch tests, respectively. Experimental results showed that the hardness of the surface layer in the SMATed Fe sample increased evidently due to the grain refinement. The elastic moduli of the surface layers in the SMATed and annealed Fe samples were unchanged, independent of grain size in the present grain size regime. Compared with the original Fe sample, the wear resistance enhanced and the coefficient of friction decreased in the surface layer of the SMATed Fe sample.     

Crystallization and Hardness of Melt Spun Fe73Si13B9Nb4Cu1 Alloy

An alloy having composition Fe73Si13B9Nb4Cu1 was synthesized by melt spinning to investigate the kinetics of crystallization. Techniques of differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Mossbauer spectroscopy were employed to characterize the phases produced due to annealing at various temperatures. High temperature DSC revealed two stage crystallization reactions. First stage, crystallization occurs at temperature around 514℃ with the production of α-Fe (bcc) and Fe3Si phases. In the second stage, Fe2B and α-Fe (Si,Nb) phases were produced. Mossbauer results revealed the formation of Fe3Si, Fe13Si3 and Fe7Si1 in the first stage and Fe3Si, Fe13Si3, Fe2B and α-Fe (Si,Nb) phases in the second stage of crystallization. An abrupt change in average internal magnetic field was observed at 500℃. The maximum hardness value was found for the sample heat-treated at 500℃.     

Mechanical Properties Improvement of AlCrFeNi_2Ti_(0.5) High Entropy Alloy through Annealing Design and its Relationship with its Particle-reinforced Microstructures

High entropy alloy has attracted increasing attentions.However,to enhance the alloy strength often leads to impairment of the ductility,or vice versa.Here we reported a heat treatment approach on AlCrFeNi2Ti0.5 high entropy alloy,which can elevate the strength and ductility simultaneously.An ingot of AlCrFeNi2Ti0.5 weighing 2.5 kg was firstly fabricated by medium frequency induction melting.Then samples from the same height of the bulk ingot were annealed for 6 h at 600,700,800 and 1000 ℃,respectively.After 1000 ℃ annealing,an optimal microstructure was obtained by using our approach which can make some precipitation particles distribute homogeneously in the dendrite interior while keep the interdendrite structure as a single solid solution phase.The mechanical test on this AlCrFeNi2Ti0.5 alloy sample showed that,the compressive fracture strength σbc was increased by about600 MPa and the plastic strain ep was doubled,compared with those of the as-cast sample.Our approach can be readily adapted to large-scale industrial production of high entropy alloys with high strength and ductility by proper annealing treatment.     

High Resolution Electron Microscopy Observations of Structural Changes in Iron Nitride Films Annealed in Vacuum

Iron-nitride films were prepared by reactive sputtering, and the effect of annealing treatment on the structures was investigated by means of in-situ electron microscopy and high resolution electron microscopy (HREM). As-deposited films were observed to be a mixed structure of a few ultrafine ε-Fe2-3N particles existing in the amorphous matrix. lt was found that the structurerelaxation in the amorphous occurred at 473 K, and the ultrafine grains began to grow at the higher annealing temperatures. The transition of the amorphous to ε-Fe2-3N was almost completed at 673 K. It is considered that the formation of the ideal ε-Fe3N is originated from the ordering of the nitrogen atoms during the annealing in vacuum. On the other hand, γ'-phase (Fe4N) was seen to precipitation of ε-phase at 723 K. Two possible modes are proposed in the precipitation of γ'-phase, depending on the heating rate and crystallographic orientation relationships. i.e. [121]ε [001]γ, (210)ε(110)γ and [100]ε[110]γ, (001)ε(111)γ. In addition,α-Fe particles were observed to form from the γ'-phase at high temperatures. We assumed that these structural changes are due to the diffusion of nitrogen and iron atoms during the annealing,except for the case of the precipitation of the γ'-phase as depicted above. The results obtained in this work are in a good agreement with the assumption.     

Effect of Annealing Atmosphere on the Mechanical Property of Free-cutting Phosphor Bronze Alloy

The present work is focused on the influence of annealing atmosphere on the microstructure and mechanical property of free-cutting phosphor bronze alloy.The annealing of the alloy was conducted in the three kinds of annealing atmosphere such as air,vacuum and nitrogen.After annealing,a discernable difference in recystallized grain size and lead particle size was not appeared with different annealing atmosphere.The tensile strength of the alloy annealed in air or nitrogen atmosphere was higher than that of those annealed in vacuum atmosphere.In thecase of the alloy annealed in vacuum atmosphere,the mechanical strength was reduced by vaporization of zinc.In the case of annealing in nitrogen and in air atmosphere,the sweating of lead was occurred.However,the inverse segregation of lead was suppressed by copper oxide layer on the surface annealed in air.This copper oxide layer leads to a decrease of the yield during fabrication process. Therefore,annealing of the alloy in nitrogen atmosphere is favorable in terms of the mechanical strength and yield.     

Effect of Annealing on the Optical Properties of GaN Films Grown by Pulsed Laser Deposition

In the present study,gallium nitride thin films were grown by using pulsed laser deposition.After the growth samples were annealed at 400 and 600℃in the nitrogen atmosphere.Surface morphology of the as-grown and annealed samples was observed by atomic force microscopy.Post-growth annealing results in an improved surface roughness of the films.Chemical analysis of the samples was performed by X-ray photoelectron spectroscopy.Stoichiometric gallium nitride thin films were obtained for the samples annealed at 600℃.Optical measurements of the samples were performed to measure the band gap and optical constants of the films.Effect of annealing on the band gap and optical constants of the films was studied.     

Synthesis and Room Temperature d~o Ferromagnetic Properties of α-MoO_3 Nanofibers

Herein,we report the magnetic properties of α-MoO_3 nanofibers synthesized via a hydrothermal method.X-ray photoelectron and Raman spectroscopic studies have been employed to evidence the presence of oxygen vacancy defects in the α-MoO_3 nanofibers.To elucidate the oxygen vacancy related ferromagnetism,post-thermal annealing in oxygen and vacuum was performed.The UV emission band of α-MoO_3 nanofibers reveals a red shift from oxygen annealed to vacuum annealed,indicating a bandedge reduction.The saturation magnetization of oxygen annealed nanofibers decreases while that of vacuum annealed nanofibers increases.These results strongly confirm that the oxygen vacancies play a significant role in inducing ferromagnetism.The origin of ferromagnetism may be due to the exchange interactions among localized electron spin moments resulting from oxygen vacancies of α-MoO_3 nanofibers.The presence of such defects was further supported by the photoluminescence measurements.     

Ordering of the α-Fe(Si) Crystallization Phase in Annealed Fe_(73.5)Cu_1Mo_3Si_(13.5)B_9 Alloy

The ordering of the α-Fe(Si) crystallization phase in annealed Fe73.5Cu1Mo3Si13.5B9 alloy has been studied using XRD method. The α-Fe(Si) phase in Fe73.5Cu1Mo3Si13.5B9 alloy annealed at 460℃ for 1 h consists of the DO3-type ordered region with spherical shape and disordered region. The size of DO3 ordered region increases with the annealing temperature. When the annealing temperature is 560℃, the size of the ordered region in the α-Fe(Si) grain is 14.0nm,which is nearly as large as that of the α-Fe(Si) grain (14.2 nm) and the degree of order of the α-Fe(Si) phase is about 0.78. When Fe73.5Cu1 Mo3Si13.5B9 amorphous alloy is annealed at 520℃, with the increment of the annealing time, the shape of the DO3 ordered region in the α-Fe(Si) phase is spheroidal at the beginning of the annealing and becomes spherical and has asize of 12.8 nm when the annealing time is 60 min. In addition, the DO3 superlattice lines of the α-Fe(Si) phase will vanish if Fe73.5Cu1Mo3Si13.5 B9 amorphous alloy is annealed for 1 h at 750℃.     

A M■ssbauer Study on the Mechanically Alloyed Cu-Sn Alloys

Nanocrystalline E and η electron compounds and supersaturated solid solution of the Cu-Sn system have been prepared by mechanical alloying of elemental Cu and Sn powders. The atomie alloying and microstructure of the resultant alloys have been investigated by XRD, DSC and 119Sn Mossbauer spectroscopy. A little amount of SnO2 was detected by Mossbauer spectroscopy, although no trace of diffiaction peaks occurred in the XRD pattern. Thus the spectra for all the milled samples should be fitted using two quadrupole-splitting doublets: one corre sponding to SnO2, the other corresponding to the resultant alloys. The composition dependence of the hyperfine parameters has been eXtensively discussed and explained well with respect to oxidation, sudece effect resulting from grain refinement, coordination environment asymmetry and distortion caused or/and induced by mechanical alloying.     

Mechanism on the Effect of Al upon the γ→ε Martensite Transformation in the Fe-Mn Alloys

The structure of the solid solution treated and deformed Fe-25Mn-(0-3.11)Al-0.15C alloys was examined by means of metallograph and X-ray diffraction, which has confirmed that Al restrains the γ→ε transformation in the Fe-Mn alloys. The mechanism on the restraining effect of Al has been discussed on the basis of the efFect of Al upon the stacking fault energy in the Fe-Mn alloys.Aluminium increases thermodynamically the stability of the Fe-Mn austenite and the driving force limit necessitated to be overcome for the γ→ε transformation, because the thermodynamicalcalculation indicates that Al increases the stacking fault energy in the Fe-Mn alloys at 300 K.Al will decrease the number and the size for the ε-martensite nucleus according to the stacking fault mechanism of the ε-martensite nucleation     

Effect of residual dissolved oxygen on the corrosion behavior of low carbon steel in 0.1 M NaHCO3 solution

The effect of residual dissolved oxygen(DO)on the corrosion behavior of carbon steel in 0.1 M Na HCO_3solution was investigated by electrochemical measurements,corrosion mass loss test,scanning electron microscopy(SEM)and X-ray diffraction(XRD).In the initial immersion stage,the increase of the dissolved oxygen concentration led to the change of from a reductive state of active dissolution to an oxidizing state of pseudo passivation in low carbon steel.While in the final stage,all the steels transformed into the steady state of pseudo passivation.In the anaerobic solution,the formation ofα-Fe OOH was attributed to the chemical oxidization of the ferrous corrosion products and the final cathodic process only included the reduction ofα-Fe OOH,while in the aerobic solution,it included the reduction of oxygen andα-Fe OOH simultaneously.As the main corrosion products,the content ofα-Fe OOH was increased while that of Fe_6(OH)_(12)CO_3was decreased with increasing concentration of dissolved oxygen.The total corrosion mass loss of the steel was promoted with the increase of dissolved oxygen concentration.     

Giant Stress—impedance Effect in Amorphous and Current Annealed Fe73.5Cu1Nb3Si13.5B9 Ribbons

The giant stress-impedance(GSl) effect in amorphous and current annealed Fe73.5Cu1Nb3Si13.5B9 ribbons has been investigated .The results showed that the GSl effect changed drastically with annealing techniques and the maximum stress impedance ratio of 350% was obtained after optimal conditions of current annealing .The behaviors of the stress impedance vary with densities of annealing current and the stress longitudinally applied during current annealing.The maximum change of stress impedance existed in the sample annealed by high-current-density electropulsing under applied stress of 100MPa.     

Annealing Effect on Transport and Magnetic Properties of La_(0.67)Sr_(0.33)MnO_3 Thin Films Grown on Glass Substrates by RF Magnetron Sputtering

The manganite La0.67Sr0.33MnO3(LSMO) thin films were grown on glass substrates in a mixed argon and oxygen atmosphere by using RF magnetron sputtering.The structural characteristics,transport behaviors and magnetic properties of LSMO films were studied by annealing the films in air at 550 and 620 ℃.The out-of-plane lattice parameter a LSMO contracted after annealing and was close to that of bulk LSMO abulk,indicating that the internal strain was fully relaxed.Nanocrystalline grains were observed in the annealed films.Enhanced saturation magnetization and metal-to-insulator transition temperature(TMI=268 K) were also obtained.Curie temperatures(Tc) of the as-grown films was 340 K with the same as that of annealed at 550 ℃,but dropped to 315 K when the annealing temperature increased to 620 ℃,which can be attributed to the oxygen release during annealing in atmosphere.     

Preparation and Characterization of Some Ferrites from CuO-ZnO-Fe_2O_3 Mixtures

The ferrites of Cuo-ZnO-Fe2o3 solid solution series near the molar ratio of ZnxCu1-x were prepared by direct heating of their coprecipitated hydroxides using NH4OH as precipitating agent where x=0.0, 0.2, 0.5, 0.8 and 1.0. Additional amounts of Cu and Zn sulphates were added to compensate the loss during the coprecipitation of the hydroxides. The ferritized samples were characterized by chemical analysis, XRD. DTA, TGA and SEM. XRD of both Zn0.2Cu0.8Fe2O4 and Zn0.5Cu0.5 Fe2O4 that indicates the formation of a heterogeneous ferrite material of ZnFe2O4 and CuFe2O4 mixed with variable amounts of α-Fe2O3. Zn and Cu ferrites were observed only in Zn0.8Cu0.2Fe2O4.From TGA-time relation, the activation energy of the different transformation phases were calculated. It is found that, the activation energy of ZnFe2O4 is slightly equal to 3/2 of that for CuFe2O4. Dielectric measurements show that the electrical behaviour depends on the ordering and disordering of the phases.     

Microstructure of the Ductile Phase in Intermetallic Compound Ni_(50)Al_(20)Fe_(30)

The microstructure of the single hot extruded and annealed Ni50Al20Fe30Y0.003 intermetallic compound alloys has been examined by means of high resolution electron microscopy (HREM). In these extruded and annealed alloys. the ductile phase is of a mixture of the disordered fcc γ matrix and or dered γ' precipitates. This fact well interprets the reason why the degree of annealing treatment can influence the strength and ductility of these alloys. The HREM observation revealed directly that there was some strain concentration at γ'-γ interfaces, due to the presence of more iron atoms in these two phases. The fixed orientation relationship between the γ phase and γ' precipitates was identified to be {001}γ{00 }γ' and <100 >γ < 100 > γ'     

Formation Mechanism of Chunky Graphite and Its Preventive Measures

The formation mechanism of chunky graphite has been reviewed and studied. The study consisted of a unidirectional solidification method, a small droplet method and a furnace cooling method. Four kinds of iron samples were prepared, namely, the pure Fe-C, Fe-C-S, Fe-C-Ce and Fe-C-Si-Ce alloys, and three kinds of nickel samples, namely the Ni-C, Ni-C-S and Ni-C-Mg alloys. The results of the unidirectional solidification of the Ni-C alloys showed that spheroidal graphite is not observed in the continuous solidified region, in which only flake-like graphite is observed, while spheroidal graphite is usually observed in the quenched liquid region. The existence of spheroidal graphite in the solidified phase is recognized only in the discontinuous growth mode of the Ni-C-Mg alloy solidified at 150 mm/h. This means that the spheroidal graphite is directly crystallized from the melt and entrapped by the flake-like chunky graphite that is formed by the continuous growth mode. In the small droplet method, a small piece of the Fe-C or Fe-C-Ce sample was melted on a pure graphite plate then cooled at a different cooling rate in a He-3%H2 atmosphere. The graphite in the Fe-C-Ce alloy is usually spherical. Nevertheless, the graphite morphology of the final solidified area changed from spherical to chunky and chunky to ledeburite with an increase in the cooling rate. This means that the chunky graphite is formed in the residual liquid region by the solidification into Fe-graphite system. The sample was cooled in a furnace, and the graphite morphology changes from spherical to chunky and chunky to ledeburite with the decrease in the Si content. These phenomena can be confirmed by the cooling curves of these samples.