金属材料表面纳米化研究与进展

大多数金属材料的失效都是从其表面开始的,进而影响整个材料的整体性能。研究表明,在金属材料表面制备纳米晶,实现表面纳米化,可以提升材料的表面性能,延长其使用寿命。金属材料表面纳米化是指利用反复剧烈塑性变形让表层粗晶粒逐步得到细化,材料中形成晶粒沿厚度方向呈梯度变化的纳米结构层,分别为表面无织构纳米晶层、亚微米细晶层、粗晶变形层和基体层,这种独特的梯度纳米结构对金属材料表面性能的大幅度提升效果显著。根据国内外表面纳米化的研究成果,首先对表面涂层或沉积、表面自纳米化以及混合纳米化3种金属表面纳米化方法进行了简要概述,阐述了各自优缺点,总结了表面自纳米化技术的优势,在此基础上重点分析了位错和孪晶在金属材料表面自纳米化过程中所起的关键作用,提出了金属材料表面自纳米化机制与材料结构、层错能大小有着密不可分的联系,对金属材料表面自纳米化机制的研究现状进行了归纳;阐明了表面纳米化技术在金属材料性能提升上的巨大优势,主要包括对硬度、强度、腐蚀、耐磨、疲劳等性能的改善。最后总结了现有表面强化工艺需要克服的关键技术,对未来的研究工作进行了展望,并提出将表面纳米化技术与电镀、气相沉积、粘涂、喷涂、化学热处理等现有的一些表面处理技术相结合,取代高成本的制造技术,制备出价格低廉、性能更加优异的复相表层。

医用钛合金表面纳米化组织与性能研究

针对近β型TLM钛合金试样表面进行了不同时间的高能喷丸处理,采用金相显微镜(OM)、扫描电子显微镜(SEM)、X射线衍射仪(XRD)以及显微硬度仪等对不同喷丸处理后的试样进行了组织观察和性能测试。研究发现,在喷丸的近表层发生了纳米化,形成了一定厚度的纳米晶层。喷丸处理时间越长,最表层的平均晶粒尺寸越小,晶粒尺寸沿着厚度方向有梯度变化,距喷丸表面越远,晶粒尺寸就会越大。同时纳米晶层的显微硬度相对于基体组织有大幅提高,显微硬度距表面距离越远,显微硬度越低,硬度的提升主要是由于表面晶粒细晶强化的作用所致。

Strengthening-softening transition and maximum strength in Schwarz nanocrystals

Recently,a Schwarz crystal structure with curved grain boundaries(GBs)constrained by twin-boundary(TB)networks was discovered in nanocrystalline Cu through experiments and atomistic simulations.Nanocrystalline Cu with nanosized Schwarz crystals exhibited high strength and excellent thermal stability.However,the grainsize effect and associated deformation mechanisms of Schwarz nanocrystals remain unknown.Here,we performed large-scale atomistic simulations to investigate the deformation behaviors and grain-size effect of nanocrystalline Cu with Schwarz crystals.Our simulations showed that similar to regular nanocrystals,Schwarz nanocrystals exhibit a strengthening-softening transition with decreasing grain size.The critical grain size in Schwarz nanocrystals is smaller than that in regular nanocrystals,leading to a maximum strength higher than that of regular nanocrystals.Our simulations revealed that the softening in Schwarz nanocrystals mainly originates from TB migration(or detwinning)and annihilation of GBs,rather than GB-mediated processes(including GB migration,sliding and diffusion)dominating the softening in regular nanocrystals.Quantitative analyses of simulation data further showed that compared with those in regular nanocrystals,the GB-mediated processes in Schwarz nanocrystals are suppressed,which is related to the low volume fraction of amorphous-like GBs and constraints of TB networks.The smaller critical grain size arises from the suppression of GB-mediated processes.

医用钛合金表面喷丸后微米压痕研究

采用高能喷丸强化(HESP)对医用钛合金进行了表面处理,并采用SEM、AFM、TEM和微米压痕对处理过程的微观组织演变及其微观力学性能进行了研究。结果表明,经过HESP处理,在材料表面形成了梯度组织,并且材料表面粗糙度随着冲击时间的增加而先增加后降低,逐渐趋于稳定;TEM分析显示材料表面经过处理形成了纳米晶。通过微米压痕分析发现,强化后的样品弹性模量随加工时间的增加而减小,最小值出现在处理60 min的表面位置,约为59.026 GPa,相对于未处理样品下降了15.78%,且随着喷丸时间的增加,屈服强度和应变硬化指数逐渐增加。

Gd对冷旋锻制备纳米晶镁合金的影响

通过显微硬度测试、拉伸试验和透射电镜手段研究Gd元素对冷旋锻过程镁合金纳米化的影响。结果表明,由于纯镁中很难形成位错阵列,旋锻不能实现纯镁纳米化。相比之下,单独添加Gd,旋锻后镁合金晶粒可得到显著细化。在旋锻早期阶段,纯镁和Mg−Gd合金中都形成孪晶片层。随着增加旋锻变形的继续,相比纯镁,更多的非基面位错在Mg−Gd合金中形成,这促进了Mg−Gd合金中位错阵列的形成,导致合金纳米化。随着Gd含量的增加,Mg−Gd合金晶粒细化效果显著提升,晶粒细化至100 nm以下的临界Gd含量约为5.4%(质量分数)。

EFFECT OF NANOCRYSTALLIZATION ON OXIDATION RESISTANCE OF TiAl INTERMETALLIC COMPOUND

ＥＦＦＥＣＴＯＦＮＡＮＯＣＲＹＳＴＡＬＬＩＺＡＴＩＯＮＯＮＯＸＩＤＡＴＩＯＮＲＥＳＩＳＴＡＮＣＥＯＦＴｉＡｌＩＮＴＥＲＭＥＴＡＬＬＩＣＣＯＭＰＯＵＮＤ①ＴａｎｇＺｈａｏｌｉｎ，ＷａｎｇＦｕｈｕｉ，ＷｕＷｅｉｔａｏＮａｔｉｏｎａｌＫｅｙＬａｂｏｒａｔｏ...

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 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 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 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.

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.

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.

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.

Effect of surface nanocrystallization and PPEC time on complex nanocrystalline hard layer fabricated by plasma electrolysis

Size distribution of nano-carbides produced by duplex treatments of surface nanocrystallization(by surface severe plastic deformation) and plasma electrolytic carburizing on CP-Ti was investigated.Skewness and kurtosis of Gussian shape distribution curves were studied and the effect of time was determined.The usage of longer time is more suitable for achieving less size of complex nano-carbides.Surface roughness of treated samples was measured.It is observed that there is an optimum level for time on surface roughness increasing(difference between two measured data).

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.

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).

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.

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.