EFFECT OF NANOCRYSTALLIZATION ON OXIDATION RESISTANCE OF TiAl INTERMETALLIC COMPOUND

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Surface nanocrystallization of commercial pure titanium by shot peening

The surface nanostructures of commercial pure titanium was realized by the modified shot peening equipment commonly used in industry through the special treatment process. The results show that high-energy-shot-peening(HESP) commonly used to prepare nanostructured surface layers can be achieved by the increase of pill size, pill speed, and treatment time in the commercial shot peening equipment. XRD, SEM and TEM were used to characterize the surface layer microstructure of treated specimens. The analytic results show that the main deformation mode of commercial pure Ti is twinning. At the beginning of deformation, the dislocations are formed and twins occur within or on plane, then twins in intersection plane appear, and at last the twin characteristics disappear in the surface layer after longer treatment time. The deformation layer depth increases with treatment time in a certain period when the pill size and speed are unchanged. And in the severe plastic deformation (SPD) layer in which the twins are not identified easily by using SEM, the nanocrystalline microstructures are found under TEM. The finest grain size in the surface layer is about 40 nm, and the depth of nanostructured layers is over 60 μm. The microhardness of the nanostructured surface layers is enhanced significantly after shot peening compared with that of the initial simple.

Research on the dissolution behavior of cementite in the GCr15 steel surface layer induced by surface nanocrystallization

Dissolution of cementite was found in the surface layer of 1.0C-1.5Cr steel plates during the process of surface mechanical attrition treatment(SMAT),and its evolution was characterized by transmission electron microscope(TEM),three-dimensional atom probe(3DAP)and Mssbauer spectroscopy.The average grain size contained in the top surface of SMAT specimen was 10nm,and no diffraction ring corresponding to cementite grain was identified in the selected area election diffraction(SAED)pattern,which indicated the disappearance of cementite.3DAP analysis showed the average carbon concentration in ferrite(0.75 at%)after SMAT,which was almost 100 times higher than that in matrix(0.008 at%),which suggested cementite dissolve in the process of SMAT.The results of Mssbauer spectroscopy indicated that partial cementite dissolved in the process of SMAT,the saturation of cementite dissolution is about 47%.Evolution of cementite involved three sub-stages:①inoculation stage,in the first 5 min of treated duration,cementite fraction is reduced only by 0.4%;②dissolution stage,within the following 25 min cementite fraction significantly is reduced from 14.6% to 8.4%;③saturation stage,when treatment exceeds 30 min,the fraction of cementite nearly remains the same.

Surface nanocrystallization of Ti6AI4V induced by circulation rolling plastic deformation

A nanocrystallization surface layer was successfully obtained in a sample of Ti6Al4V. The microstructure features of the sample were characterized by using X-ray diffraction analysis(XRD), scanning electron microscopy(SEM) and transmission electron microscopy(TEM) observations. The average grain size in the top surface layer is about 10nm, and gradually increases with the distance from the surface increasing.

Surface Nanocrystallization of C45E4 Steel by Ultrafast Electropulsing-ultrasonic Surface Treatment

The effect of high-energy electropulsing-ultrasonic surface treatment（EUST） on the surface properties and the microstructure evolution of C45 E4 steel was investigated. Refined microstructure and reduced surface roughness were obtained owing to the surface nanocrystallization process. Compared with the ultrasonic surface treatment（UST）, the impact depth of the surface strengthened layer was increased by 40% to 700 μm after EUST. The average grain size of the surface nanocrystallization layer was reduced to 30-50 nm. The surface roughness of the C45 E4 steel was reduced to 0.25 μm, and the surface microhardness was dramatically enhanced to 460 HV. The improvement of microstructure and micro-hardness at ambient temperature was likely attributed to the acceleration of atomic diffusion and the enhancement of plastic deformation ability in the surface strengthened layer under the influence of electropulsing. Due to the electropulsing-assisted ultrasonic strengthening effect, the surface nanocrystallization in this ultrafast procedure was noticeably enhanced.

Surface Nanocrystallization of Steel 20 Induced by Fast Multiple Rotation Rolling

In order to expand the application of steel 20 in precision device,fast multiple rotation rolling( FMRR) is applied to fabricate a nanostructured layer on the surface of steel 20. The FMRR samples are then Cr-Rare earth-boronized under low-temperature. The microstructure of the top surface layer is characterized by transmission electron microscopy( TEM). Microhardness of the top surface is measured by a Vickers microhardness tester. The boride layer is characterized by using scanning electron microscopy( SEM).Experimental results show that a nanostructured layer with their grain size range from 200 to 400 nm is obtained in the top surface layer. The microhardness of FMRR sample changes gradiently along the depth from about274 HV in the top surface layer to about 159 HV in the matrix,which is nearly 1.7 times harder than that of the original sample. The penetrating rate is enhanced significantly when the FMRR samples are Cr-Rare earthboronized at 600 ℃ for 6 h. Thickness of the boride layer increases to around 20 μm,which is nearly twice thicker than that of the original sample.

Hydriding and microstructure nanocrystallization of ZK60 Mg alloy by reaction milling in hydrogen

The hydriding of as-cast Mg-5.5%Zn-0.6%Zr(ZK60 Mg)(mass fraction)alloy was achieved by room-temperature reaction milling in hydrogen,with the mechanical energy serving as the driving force for the process.The hydriding progress during milling was examined by hydrogen absorption measurement,and the microstructure change was characterized by X-ray diffraction analysis(XRD),scanning electron microscopy(SEM),and transmission electron microscopy(TEM),respectively.The results show that,by room-temperature reaction milling in hydrogen,the as-cast ZK60 Mg alloy can be fully hydrided to form a nanocrystalline MgH_(2) single-phase microstructure.In particular,the average grain size of the MgH_(2) phase obtained by room-temperature reaction milling in hydrogen for 16.2 h is about 8-10 nm,and the average particle size of the as-milled hydrided powders is 2-3μm.

Nanocrystallization behaviour of a ternary amorphous alloy during isothermal annealing： a Monte Carlo simulation

The nanocrystallization behaviour of Zr70Cu20Ni10 metallic glass during isothermal annealing is studied by employing a Monte Carlo simulation incorporating with a modified Ising model and a Q-state Potts model. Based on the simulated microstructure and differential scanning calorimetry curves, we find that the low crystal-amorphous interface energy of Ni plays an important role in the nanocrystallization of primary Zr2Ni. It is found that when T〈T1max （where T1max is the temperature with maximum nucleation rate）, the increase of temperature results in a larger growth rate and a much finer mierostrueture for the primary Zr2Ni, which accords with the microstructure evolution in ＂flash annealing＂. Finally, the Zr2Ni/Zr2Cu interface energy σG contributes to the pinning effect of the primary nano-sized Zr2Ni grains in the later formed normal Zr2Cu grains.

Effect of Surface Nanocrystallization Induced by Fast Multiple Rotation Rolling on Cr-Rare Earth-Boronizing for Steel 45 under Low-Temperature

In this paper,fast multiple rotation rolling( FMRR) is applied to fabricate a nanostructured layer on the surface of steel 45. The FMRR samples are then Cr-Rare earth-boronized under low-temperature. The boride layer is characterized by using Scanning electron microscopy( SEM) and X-ray diffraction( XRD).Experimental results indicate that the thickness of the boride layer is greatly increased by surface nanocrystallization. The boride layer with relatively continuous structure instead of the zigzag teeth structure is obtained,and the penetrating rate is enhanced by 2. 5-3. 7 times when the FMRR samples are Cr-Rare earthboronized at the temperature of 570 ℃,600 ℃ and 650 ℃ for 6 h. The boride layer fabricated on the FMRR sample consists of single phase Fe2 B. Severe plastic deformation with the grain size of approximately 100 nm in the top surface layer of steel 45 is observed,and the thickness of the plastic deformation layer is about 30 μm.The microstructure in the top surface layer is characterized by Transmission electron microscopy( TEM). Grain boundaries are largely increased with high stacking fault energy after FMRR, leading to a significant enhancement of RE boron-chromizing speed.

Surface Nanocrystallization of Magnesium Alloy AZ91D by High-Energy Shot Peening

High-energy shot peening （HESP）, a method to produce severe plastic deformation by high velocity flying balls, was applied on die cast magnesium alloy AZ91D. Effects of surface nanocrystallization by HESP and heat treatment at different temperatures were investigated. The mi- crostructure evolution was conducted using X-ray diffraction （XRD） and field emission scanning electronic microscopy （FESEM）. The hardness was measured by microhardness tester. The experimental results show that surface nanocrystrallization of AZ91D obtained by HESP would lead to the increase of microhardness. Low temperature heated at 100℃ for 1 h do not change the property obviously. However, both the microstructure and microhardness vary greatly after heat treatment at 400℃ for 1 h.

Optimization Design of an Embedded Multi-Cell Thin-Walled Energy Absorption Structures with Local Surface Nanocrystallization

Bymeans of the local surface nanocrystallization that enables to change the material on local positions,an innovative embedded multi-cell(EMC)thin-walled energy absorption structures with local surface nanocrystallization is proposed in this paper.The local surface nanacrystallization stripes are regarded as the moving morphable components in the domain for optimal design.Results reveal that after optimizing the local surface nanocrystallization layout,the specific energy absorption(SEA)is increased by 50.78%compared with the untreated counterpart.Besides,in contrast with the optimized 4-cell structure,the SEA of the nanocrystallized embedded 9-cell structure is further enhanced by 27.68%,in contrast with the 9-cell structure,the SEA of the nanocrystallized embedded clapboard type 9-cell structure is enhanced by 3.61%.Thismethod provides a guidance for the design of newenergy absorption devices.

Surface Nanocrystallization of Commercial Pure Titanium Induced by SMAT and Its Properties

In this paper the preparation technique of surface nanocrystallization in commercial pure titanium was carried out by surface mechanical attrition treatment (SMAT). The mean grain size was calculated by using X-ray diffraction (XRD) and transmission electron microscope (TEM), and the results showed that the mean grain size of the surface was refined to nm Ievel after SMAT treatment. Nanocrystallized surface layers were formed after treated for 5, 15, 30 and 60 min. Microhardness experimental results implied the microhardness obviously increased on the surface layer and it also showed the variation of microhardness at the cross section. Corrosion test results showed the corrosion resistance of the surfaces in the original commercial pure titanium treated by SMAT was not improved in HCI solution. The corrosion micrographs were observed by scanning electron microscope (SEM).

Nanocrystallization of Cementite in 0.4C-1Cr Steel During High-Power Surface Processing

The microstructures of the nanocrystalline surface layer of a quenched and high temperature tempered 0. 4C- 1Cr steel induced by high-power surface processing （HPSP） technique were characterized by scan- ning eleetron microscopy and transmission electron microscopy. The results indicate that a nanocrystalline layer was fabricated on the surface of the steel 19 using HPSP treatment. The mean grain size in the surface layer is about 11 nm. The nanocrystallization of cementite is prior to that of the matrix phase, ferrite.

Surface nanocrystallization of 7A52 aluminum alloy welded joint

As a means of surface modification process, metal surface nanocrystallization （MSN） has attracted widespread attention and enjoyed a great prospect. However, currently little research is carried out regarding MSN of welded joint. The processes of high energy shot peening （HESP） technology and ultrasonic impact treatment （UIT） were carried out to achieve joint surface nanocrystallization. The grain size of before and after the welded joint surface nanocrystallization were comparatively analyzed with X-ray diffractometer, the surface deformation layer thickness of before and after the welded joint surface nanocrystallization were comparatively analyzed with optical microscopy, the surface hardness of before and after the welded joint surface nanocrystallization were comparatively analyzed with micro hardness machine. The results show that both of the processes can achieve welded joint surface nanocrystaUization and the weld after HESP have smaller grain size, larger deformation layer thickness and higher hardness values than those after UIT. However, HESP is restrained by the shapes and sizes of welding materials, so the UIT process is preferred to use in the general engineering practical applications.

Magnetothermal Analysis of Nanocrystallization of Amorphous and Relaxations of Nanocrystalline Materials

For a few years it has been realized that nanocrystalline phases can be formed during crystallization of amorphous alloys annealed isothermally below the crystallization temperature of usual heating experiments. Data of this transformation monitored by the measurement of magnetic susceptibility are presented. A method using a magnetic balance with electronic stabilisation and combined computer facilities is applied. Constant heating and cooling rates as well as isothermal heat treatments are used. Magnetic measurements are able to detect the onset of the transformation of amorphous NI-P alloys much earlier than was possible with differential scanning calorimetry. The transformation kinetics can be analyzed by means of the Avrami plot based on the Johnson-Mehl-Avrami equation. The kinetics of solid state reactions in the nanostructured material can be investigated similarly. Formation of a Ni-phase in a nanostructured Hf-Ni alloy could be detected in a very early stage, where calorimetric methods are not sensitive. Segregation phenomena could be detected from the experiments even after long time. The sensitivity of the applied method is not dependent on the heating rate as the sensitivity of scanning calorimetry is.

Nanocrystallization of Amorphous Fe_(73.5)Cu_1Nb_3Si_(13.5)B_9 Irradiated by Laser

The surface nanocrystallization of amorphous Fe73.5 Cu1Nb3Si13.5B9 radiated by CO2 laser was studied by means of M（oe）ssbauer spectroscopy, transmission electro iroscope and X-ray diffraction. The result shows that under certain technical conditions, nanocrystalline is fiound on the surface of amorphous Fe73.5 Cu1Nb3Si13.5B9 radiated by laser; the crystallization phase is α-Fe（Si） crystalline, and its size is about 10-20 nm; the nanocrystalline is uniformly distributed on amorphous base to keep the amorphous and crystallized phase in balance; the a mount of crystallization reaches 23% when the laser power is 300 W, the diameter of light spot is 20 mm, and the radiation speed is 20 mm/s. The phase balance can be controlled by adjusting the laser technology parameter. Laser radiation on the amorphous Fe73.5 Cu1Nb3Si13.5B9 alloy is an important technique for surface nanocrystallization of the amorphous alloys.

Surface nanocrystallization in AISI 52100 steel induced by surface mechanical grinding treatment(SMGT)

Surface nanocrystallization(SNC) has proved to be an effective approach to improve the overall properties of bulk metallic materials.Recently,a new surface nanocrystallization technique,i.e.,surface mechanical grinding treatment(SMGT),was developed.In this work,a gradient nano-micro structure was achieved in the surface layer of the AISI 52100 steel by using SMGT.We obtained a minimum grain size of about 7nm in the top surface layer.The total thickness of the deformed layer is over 200 micrometer.Meanwhile the surface roughness is rather low. Ferrite grains were deformed to different extents varying with depth from the top surface.Gradient grain sizes were formed from top surface to deep matrix which offered a great opportunity to study the refinement process of the ferrite grains.It is found that dislocation activities play a dominant role in the process.At the initiate stage, dislocations accumulated and interacted to form dense dislocation walls and cells.Increasing strain and strain rate induced more dislocation walls in cells,forming finer cells.This procedure continued until nanograins formed at the top most surface. The existence of cementite particles in ferrite matrix greatly facilitates the ferrite refinement process.Boundaries between ferrites and cementites offered many dislocation sources which accelerate the propagation of dislocations. Dislocation walls were blocked by cementites which certainly lead to finer dislocation cells.The existence of cementites makes it easier to generate fresh dislocation walls in sub-micron grains.A strain gradient was formed from a cementite particle to surrounding ferrite grains.This strain gradient gives rise to more geometric necessary dislocations. As ferrite grain size decreased less than that of cementite particles,fragmentation occurred in cementites.Hard second phase was usually considered as brittle.In this work,evidences of deformation(traces of dislocation activities) in cementites were distinct.Since the stress concentration in the phase boundary(especially triple junction) excesses the shear modulus of cementite,dislocation emission was triggered.It is found in this work that dislocations tend to slip along parallel planes,possibly on(001),(01 0),(100),(110),(10 1 ) and(011) planes,depending upon as the load directions.

Effect of surface nanocrystallization on the electrochemical hydrogen evolution behavior of IF steel

Cathodic polarization curve and electrochemical impedance spectroscopy in 30% NaOH solution were utilized to investigate the hydrogen evolution （HE） behavior of interstitial free （IF） steel surface nanocrystallized （SNC） via ultrasonic particulate peening （USPP）. The surface morphology and grain size of the steel were analyzed by scanning electronic microscope （SEM） and X-ray diffraction （XRD）. It was found that the IF steel treated by SNC and SNC ＋ 1% roiling got reductions of 200 mV and 300 mV in HE over-potentials ,respectively. Their real surface areas are enlarged by about 20 times and the hydrogen evolution reaction activation flee energies are about 50% of the original IF steels＇ s activation free energy.

Enhanced oxidation resistance of Ce by addition of Ga and nanocrystallization

Ce is prone to catastrophic oxidation at room temperature and its oxidation resistance is difficult to be improved by alloying.Herein,we found that the oxidation resistance of active metal Ce can be significantly improved by the addition of 20 at.%Ga.Focused ion beam lift-out technique and scanning transmission electron microscopy analysis disclosed that a discontinuous Ga-rich layer was generated beneath the oxide layer in the coarse-grained Ce-Ga alloy.The Ga-rich layer formed by selective oxidation of Ce acts as a diffusion barrier for Ce outward diffusion and ceases the O/M interfacial reaction when a critical concentration of Ga(75 at.%)is reached.After nanocrystallization,uniform distribution of Ga was achieved.After oxidation,a relatively continuous Ga-rich layer was formed which further enhanced the oxidation resistance.The introduction of noble elements combining with nanocrystallization may provide a novel strategy for the protection of metals with high activity and poor oxidation resistance.

Stress-induced CsPbBr3 nanocrystallization on glass surface:Unexpected mechanoluminescence and applications

In this work,we discovered an unexpected mechanoluminescence (ML) phenomena occurring when transforming amorphous into crystalline,due to the stress-induced precipitation of CsPbBr3 perovskite nanocrystals on glass surface.It is revealed that,unlike the conventional thermal-induced phase transformation mechanism,the breakage of bonding of glass network provides the energy for nucleation and growth,and the shear stress avoids the long-range migration of structural units for crystallization.Such unique ML phenomenon enables the visualization of dynamical force that is inaccessible by common strategy,and so,opens up some novel applications,such as the pressure-sensitive "glassy pencil" to learn people's writing habits,and the pb^2+-detection with good sensitivity and selectivity.These findings not only demonstrate an effective route for the preparation of perovskite materials in a green,time-saving,low cost,and scalable way,enrich the knowledge of glass crystallization mechanism,but also exploit a useful avenue to quantitatively visualize the dynamical force.