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 epsilon-Fe2-3N particles existing in the amorphous matrix. it was found that the structure-relaxation 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 epsilon-Fe2-3N was almost completed at 673 K. It is considered that the formation of the ideal epsilon-Fe3N is originated from the ordering of the nitrogen atoms during the annealing in vacuum. On the other hand, gamma'-phase (Fe4N) was seen to precipitation of epsilon-phase at 723 K. Two possible modes are proposed in the precipitation of gamma'-phase, depending on the heating rate and crystallographic orientation relationships, i.e. [121](epsilon)//[001](gamma), (2(1) over bar0$)(epsilon)//(110)(gamma) and [100](epsilon)//[110](gamma), (001)(epsilon)//(111)(gamma). In addition, alpha-Fe particles were observed to form from the gamma'-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 gamma'-phase as depicted above. The results obtained in this work are in a good agreement with the assumption.

Highly efficient and stable electrooxidation of methanol and ethanol on 3D Pt catalyst by thermal decomposition of In2O3 nanoshells

In this paper In2O3nanoshells have been synthesized via a facile hydrothermal approach. The nanoshells can be completely cracked into pony-size nanocubes by annealing, which are then used as a support of Pt catalyst for methanol and ethanol electrocatalytic oxidation. The prepared In2O3and supported Pt catalysts (Pt/In2O3) were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field effect scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). Cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry and electrochemical impedance spectroscopy (EIS) were carried out, indicating the excellent catalytic performance for alcohol electrooxidation can be achieved on Pt/In2O3nanocatalysts due to the multiple active sites, high conductivity and a mass of microchannels and micropores for reactant diffusions arising from 3D frame structures compared with that on the Pt/C catalysts. © 2016 Science Press

Surface grain refinement mechanism of SMA490BW steel cross joints by ultrasonic impact treatment

Ultrasonic impact treatment (UIT) is a postweld technique for improving the fatigue strength of welded joints. This technique makes use of ultrasonic vibration to impact and plastically deform a weld toe and can achieve surface grain refinement of the weld toe, which is considered as the main reason for the improvement of fatigue strength. In this paper, the microstructure of the surface of a treated weld toe was observed by metallographic microscopy and transmission electron microscopy (TEM). The results show that UIT could produce severe plastic deformation on the surface layer of the weld toe and the maximum depth of plastic deformation extended to approximately 260 μm beneath the treated surface. Repeated processing could exacerbate the plastic deformation on the surface layer, resulting in finer grains. We can conclude that the surface grain refinement mechanism of SMA490BW welded joints is related to the high density of dislocation tangles and dislocation walls. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

Effects of pre-deformation on microstructure and properties of Al–Cu–Mg–Ag heat-resistant alloy

The effects of the pre-deformation on the microstructure, mechanical properties and corrosion resistance of Al–Cu–Mg–Ag alloys were investigated by means of hardness tests, tensile tests, intergranullar corrosion (IGC) tests and transmission electron microscopy (TEM), respectively. The results show that with the increase of deformation amount, the aging hardening rate increases while the strength of the alloy decreases and then increases. The sample with a pre-deformation of 6% possesses the highest tensile strength due to the refinedly and homogeneously distributed precipitations. The pre-deformation aging accelerates the heterogeneous nucleation of Ω and θ′ phases at dislocations, and also refines the precipitations both in the grains and along the grain boundaries. The precipitation of Ω phase is restrained while that of θ′ phase is accelerated in pre-deformed Al–Cu–Mg–Ag alloy compared with the sample without pre-deformation. In addition, the width of the precipitate free zone decreases with increasing the pre-deformation amount, leading to a narrower IGC passageway. This results in an enhanced IGC resistance of Al–Cu–Mg–Ag alloy treated by pre-deformation aging. © 2017, Central South University Press and Springer-Verlag GmbH Germany.

Effects of Yttrium on the Microstructures and Interfaces in a Low Expansion Superalloy

The forms and structures of the phases in Fe-Ni-Co-Nb-Ti-Si low expansion superal-loys have been studied using analytical electron microscopy, high resolution electron microscopy, chemical phase analysis, X-ray diffraction, etc. The effects of yttrium on the microstructures and properties in the superalloys have also been investigated. The results reveal that trace yttrium mainly located in the platelet precipitates makes the crystal structure changed. The platelet precipitates become smaller, denser and rather homogeneous with appropriate yttrium addition. Compared with the conventional low expansion superalloy, the misfit of the platelet phase with the matrix in the yttrium-containing low expansion superalloy decreases from 0.7% to 0.07%, which indicates very low stress at the interface.

ATOMIC SCALE MECHANISM OF RESTRAINED EMBRITTLEMENT IN AMORPHOUS Fe_(78)B_(13)Si_9 ALLOY BY ELECTRIC PULSE RAPID ANNEALING

The direct observations of the atomic arrangements in both conventional furnace annealed and electric pulse rapid annealed Fe78B13Si9 amorphous alloy have been conducted by the lattice imaging technique in a higt resolution electron microscope. The results showed that the embrittlement of the alloy was related to the extent of atomic rearrangements during the annealing processes. The embrittlement of the alloy after 1hour conventional furnace annealing at about 270℃ is caused by the sufficient atomic rearrangements which are characterized by the growth of some bct Fe3B-like atomic short range ordering regions already existed in the as-quenched structure. Electric pulse rapid annealing can effectively retard the above-mentioned atomic rearrangements and thus restrain the embrittlement. The embrittlement only occurs when certain amount of bcc α-Fe nanocrystals are precipitated in the amorphous matrix during electric pulse rapid annealing.

Nanometer Stripe Microstructure of Supersaturated Solid Solution in Fe-Cu Alloy

Strengthening due to precipitation of Cu in the a-Fe matrix is an important phenomenon utilized in the design of HSLA steels. In the present work, the microstructure of supersaturated solid solution in Fe-1.18%Cu binary alloy was investigated by means of high resolution electron microscopy. The results indicated that the solid solution was heterogeneous, there were lots of Cu atom clusters, which consisted of diffractive stripe microstructure similar to twin crystal. Orientation deviation was observed between two （110）o planes in diffractive stripes, which results in light and shade contrast. Furthermore, formation mechanisms of the nanometre stripe microstructure were discussed in terms of the interaction of Cu and Fe atoms in the Fe-Cu binary alloys.

One-pot synthesis and optical properties of In- and Sn-doped ZnO nanoparticles

Colloidal indium-doped zinc oxide (IZO) and tin-doped zinc oxide (ZTO) nanoparticles were successfully prepared in organic solution, with metal acetylacetonate as the precursor and oleylamine as the solvent. The crystal and optical properties were characterized by X-ray diffraction, UV−visible spectrophotometry, and fluorescence spectroscopy, respectively; the surface and structure morphologies were observed by scanning electron microscopy and transmission electron microscopy. The XRD patterns of the IZO and ZTO nanoparticles all exhibited similar diffraction peaks consistent with the standard XRD pattern of ZnO, although the diffraction peaks of the IZO and ZTO nanoparticles were slightly shifted with increasing dopant concentration. With increasing dopant concentration, the fluorescent emission peaks of the IZO nanoparticles exhibited an obvious red shift because of the difference in atomic radii of indium and zinc, whereas those of the ZTO nanoparticles exhibited almost no shift because of the similarity in atomic radii of tin and zinc. Furthermore, the sizes of the IZO and ZTO nanoparticles distributed in the ranges 20–40 and 20–25 nm, respectively, which is attributed to the difference in ionic radii of indium and tin. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

HREM Study on Sm(Co,Fe,Cu,Ti)_7 Alloy Aged under Different Conditions

The microstructures and defects of various aged Sm( Co, Fe,Cu,Ti)_7 alloys have been observed in several orientations by using high resolution electron microscopy.Experimental results indicate that the alloy is composed of Sm2(Co,Fe,Cu,Ti)_(17)(2:17) phase with a small amount of titanium and Sm(Co,Fe,Cu)5,(1:5) phase.The 2:17 phase is rich in iron and the 1.5 phase is rich in copper.At aging stages corresponding to the peak magnetic coercivity,the alloy has a cellular-like microstructure with fine cells of the 2:17 phase surrounded by thin boundaries of the 1:5 phase.The average size of the cells is about 33 nm.The orientation relationship of [0001]_(2:17)/[0001]1:5 and(1210)_(2:17)/(0110)_(1:5) has been found in this alloy.The high resolution images show coherence between 2:17 phase and 1:5 phase and very small mismatch in some phase boundaries.The cells of 2:17 phase are full of microtwins with twin plane perpendicular to caxis.The cells of 2:17 phase rapidly grow up,when the aging temperature rises and aging time prolongs.For the alloy aged at 850℃, the 2:17 phase and 1:5 phase transform from cellular-like into striplike microstructure,and a few of twin boundaries can be seen in the 2:17 phase.Besides the twin boundaries,antiphase boundaries are sometimes observed in the 2:17 phase of the alloy aged at 800℃,for 10 h.

Syntactic Intergrowth Structure in the Calcium-Rare Earth Fluorocarbonate Minerals

The microstructural characteristics of syntactic polycrystal in the calcium rare earth fluorocarbonate minerals from Southwest China have been studied by means of selected area electron diffraction and high resolution electron microscopy(HREM). The complication of the heterogeneous fabric of the minerals have been revealed by HREM. The results show that the crystal structure of the minerals was formed by a disorder stacking of the unit layers of bast naesite and synchisite in the calcium rare earth fluorocarbonate minerals along c direction. The stacking fault and other crystal defects in the syntactic polycrystal have been discussed.

FINE STRUCTURES OF BOTH INTERFACES AND INTERFACIAL REACTION PRODUCTS

The characteristic of interface depending on the atomic structure exerts an inportant,and sometime controlling,influence on performance of the interacial materials. The present paper reviews the main studies on fine structure of both the materials inter- faces and interfacial reaction products in semiconductor uperlattice,metal multilayer ceram- ics and composite materials by mean of selected area electron doffraction patterns and high resolution electron microscopy. The following features of interfaces are reviewed:the orientation relationships;the char- acteristic of steps,facets and ronghness of interfaces;atomic bonding across the interface;the degree of coherency,the structure of misfit dislocations and elastic relaxations at the inter- faces:the presence of defects at the onterfaces:the structure of the interfacial reaction prod- ucts as well as the reaction kinetics and reaetion mechanism.

HRTEM Study of Three New Regularly Mixed-layer Structures of B_8S_6 Type in Ca-RE Fluorocarbonate Minerals

The microstructural features of clacium rare earth(Ca RE) fluorocarbonate minerals from Southwest China were studied by using selected area electron diffraction(SAED) and high resolution transmission electron microscopy(HRTEM). Three new regularly mixed layer structures of B 8S 6 type with long period and different stacking sequence, i.e. B 8S 6 Ⅰ, B 8S 6 Ⅱ, and B 8S 6 Ⅲ, were found in the derived polycrystal of parisite, in which their structural symmetry, cell parameters, chemical formulas of crystal and stacking models of structural unit layer, etc. were determined. The results of this study also show that these new regularly mixed layer structrues were formed by order stacking unit layer of bastnaesite(B) and synchisite(S) in varying proportion along c axis. The observation under HRTEM reveals that in the three new regularly mixed layer structures there are different distribution modes of Ce F ion layers, CO 2- 3 ion groups between the Ce F ion layers, and CO 2- 3 ion groups between Ce F and Ca 2+ ion layers, and there are some heterogeneous textures, such as disorder interlayer and stacking fault. It further proves the complexity of the crystal structure of the Ca RE fluorocarbonate minerals.

HREM STUDY OF GRAIN BOUNDARY PHASES IN Fe-Ni-Co-Nb-Ti SUPERALLOY

The microstructures of the grain boundary phases in Fe-Ni-Co-Nb-Ti superalloy have been studied by high resolution electron microscopy (HREM).Besides the Laves phase,three other grain boundary phases have been found and analyzed. The ε phase particles are needle-like with some stacking faults along the(0001) direction. The dominant phase at the grain boundaries is the orthorhombic phase that is also rod-like. High reselution image also confirms the existence of the triclinic phase at the grain boundaries that is irregular and scarce.

Influence of tribofilm on superlubricity of highly-hydrogenated amorphous carbon films in inert gaseous environments

In this study,we mainly focus on the structural morphology and inter-atomic bonding state of tribofilms resulting from a highly-hydrogenated amorphous carbon(a-C:H) film in order to ascertain the underlying mechanisms for its superlubric behavior(i.e.,less than 0.01 friction coefficient).Specifically,we achieved superlubricity(i.e.,friction coefficients of down to 0.003) with this film in dry nitrogen and argon atmospheres especially when the tribo-pair is made of an a-C:H coated Si disk sliding against an a-C:H coated steel ball,while the a-C:H coated disk against uncoated ball does not provide superlubricity.We also found that the state of superlubricity is more stable in argon than in nitrogen and the formation of a smooth and uniformly-thick carbonaceous tribofilm appears to be one of the key factors for the realization of such superlubricity.Besides,the interfacial morphology of sliding test pairs and the atomic-scale bond structure of the carbon-based tribofilms also play an important role in the observed superlubric behavior of a-C:H films.Using Raman spectroscopy and high resolution transmission electron microscopy,we have compared the structural differences of the tribofilms produced on bare and a-C:H coated steel balls.For the a-C:H coated ball as mating material which provided superlow friction in argon,structural morphology of the tribofilm was similar or comparable to that of the original a-C:H coating;while for the bare steel ball,the sp^2-bonded C fraction in the tribofilm increased and a fingerprint-like nanocrystalline structure was detected by high resolution transmission electron microscopy(HRTEM).We also calculated the shear stresses for different tribofilms,and established a relationship between the magnitude of the shear stresses and the extent of sp^3-sp^2 phase transformation.

Nano-Twinning and Martensitic Transformation Behaviors in 316L Austenitic Stainless Steel During Large Tensile Deformation

The evolutions of nano-twins and martensitic transformation in 316L austenitic stainless steel during large tensile deformation were studied by electron backscatter diffraction(EBSD)technology and transmission electron microscopy(TEM)in detail.The results show that due to the low stacking fault energy of the steel,phase transformation induced plasticity(TRIP)and twinning induced plasticity(TWIP)coexist during the tensile deformation.The deformation firstly induces the formation of deformation twins,and dislocation pile-up is caused by the reduction of the dislocation mean free path(MFP)or grain refinement due to the twin boundaries,which further induces the martensitic transformation.With the increase of tensile deformation,a large number of nano-twins andα’-martensite appear,and the width of nano-twins decreases gradually,meanwhile the frequency of the intersecting deformation twins increases.The martensitic transformation can be divided into two types:γ-austenite→α’-martensite andγ-austenite→ε-martensite.α’-martensite is mainly distributed near the twin boundaries,especially at the intersection of twins,whileε-martensite and stacking faults exist in the form of transition products between the twins and the matrix.

Preparation of nanodiamonds by laser irradiation of graphite

Graphite powders were irradiated by pulsed laser at room temperature and normal pressure and then boiled in perchloric acid. Samples were characterized by high-resolution transmission electron microscopy (HRTEM), electron diffraction pattern (EDP), X-ray diffraction (XRD) pattern, and Raman spectroscopy. The analyses on the HRTEM images, EDP, and XRD show that the diamond particles with a size of about 5 nm are obtained. The shifting and broadening of the diamond peak in Raman spectrum indicate that there are high defect density and residual internal stress in synthetic diamond.

FePO4-coated Li[Li0.2Ni0.13Co0.13Mn0.54]O2 with improved cycling performance as cathode material for Li-ion batteries

Li[Li0.2Ni0.13Coo.13Mn0.54]O2 cathode materials were synthesized by carbonate-based co-precipitation method, and then, its surface was coated by thin layers of FePO4. The prepared samples were characterized by X-ray diffraction （XRD）, field emission scanning electron micro- scope （FESEM）, energy-dispersive spectroscopy （EDS）, and transmission electron microscopy （TEM）. The XRD and TEM results suggest that both the pristine and the coated materials have a hexagonal layered structure, and the FePO4 coating layer does not make any major change in the crystal structure. The FePO4-coated sample exhibits both improved initial discharge capacity and columbic efficiency compared to the pristine one. More significantly, the FePO4 coating layer has a much positive influence on the cycling perfor- mance. The FePO4-coated sample exhibits capacity reten- tion of 82 % after 100 cycles at 0.5℃ between 2.0 and 4.8 V, while only 28 % for the pristine one at the same charge-discharge condition. The electrochemical impe- dance spectroscopy （EIS） results indicate that this improved cycling performance could be ascribed to the presence of FePO4 on the surface of Li[Li0.2Ni0.13Co0.13Mno.54102 par- ticle, which helps to protect the cathode from chemical attacks by HF and thus suppresses the large increase in charge transfer resistance.

Fabrication of single-crystalline ZnSe multipod-based structures

ZnSe multipod-based structures,including tetrapod-like microrods,long microwires,and short nanorods,are selectively prepared by atmospheric pressure thermal evaporation of ZnSe nanoparticles without using any catalyst.The morphologies could be well controlled by simply adjusting the deposition position.The phase structures,morphologies,and optical properties of the products are investigated by X-ray diffraction(XRD),scanning electron microscopy(SEM),high-resolution transmission electron microscopy(TEM),and photoluminescence(PL) spectroscopy.A vapor-liquid mechanism is proposed for the formation of ZnSe multipod-based structures.The presented route is expected to be applied to the synthesis of other Ⅱ-Ⅵ groups or other group's semiconductor materials with controllable morphologies.