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Mechanical characterization and strain-rate sensitivity measurement of Ti-7333 alloy based on nanoindentation and crystal plasticity modeling

更新时间:2016-07-05

1.Introduction

Near β titanium has become widely accepted as the metal of choice for manufacturing aircraft components due to its superior properties[1,2].Ti-7333(Ti-7Mo-3Nb-3Cr-3Al,wt%)alloy is a newly developed near β titanium alloy owning outstanding mechanical properties such as high strength,excellent fatigue crack growth resistance,as well as good hardenability[3,4].Establishing the composition-microstructureperformance relationship is of great significance for predicting the mechanical properties of titanium alloys.Therefore,it is essential to obtain elastic and plastic properties of single phase as the basis of further investigation for polycrystalline aggregation.Plastic deformation in polycrystalline microstructures of titanium alloys is strongly dependent on the grain morphology and crystallographic lattice orientation[5].

水力压裂技术产生的裂缝长度通常可达100 m,宽度和长度分别为0.01 m和1 m。为了对油层进行分布式测量,微纳传感节点混在携砂液中(含石英砂)随压裂进程进入裂缝,其在裂缝中的位置因而是随机分布的[4]。体积和功率较大的锚节点通常布置于井筒内部,由外部电源供电,可直接与裂缝内的传感器节点进行磁感应通信,锚节点同时通过磁感应方式为传感节点提供电能;微纳尺寸的传感器节点具有全向线圈天线,同时配置超级电容器储存耦合电能。考虑到供电及传感器通信能力等因素,在面向油藏裂缝的地下无线传感网络中,锚节点和传感节点之间通信(下行链路)是单跳方式,传感节点与锚节点之间通信(上行链路)采用多跳方式[5]。

Nanoindentation has a distinct advantage to mechanically characterize individual phase in titanium alloys with significantly less effort and equipment comparing to micropillars and cantilever beams which require the focused ion beam(FIB)techniques to prepare samples[6].Thanks to its precise load-controlling and displacement-sensing capabilities,nanoindentation has been increasingly used to study the mechanical response of materials such as hardness,elastic modulus,creep parameters and strain-hardening exponent [7]. In addition,nanoindentation, combined with electron backscattered diffraction(EBSD)scan,has been widely applied to investigate deformation mechanism of grains with different orientations and confirmed that the anisotropic mechanical response is consistently observed across various titanium alloys[6,8–10].

Beyond the typical hardness tests,the strain-rate sensitivity(SRS)measurement based on dynamic nanoindentation becomes possible now.Although the local strain field around the indentation is much more complex than the conventional macroscopic Engineering ratesensitivity measurement,nanoindentation test allows investigating the mechanical response to strain rate with different microstructures,such as the ultrafine-grained and nanocrystalline materials[11,12],the fully lamellar microstructures[8]and the multilayered films[13].

UPS的配置应根据发信台设备的用电功率以结合其他因素做精确计算后进行配置,经统计,目前发信台正在运行的设备及所需功率如表2。

In the past few years,the crystal plasticity finite element(CPFE)method achieved great success in modeling and simulating the plastic deformation process of various microstructures,thus building up the relationship between microstructure and mechanical properties[14,15].The predictive capability of CPFE models mostly relies on the accuracy of constitutive laws,which express the slip rate on crystallographic slip planes in terms of resolved shear stress and other solution dependent state variables.Compared to the limitations in generating real samples with various microstructures,it is easier to establish different models with detailed characterization of microstructure features from single crystal to polycrystalline aggregate[16–18].Furthermore,the CPFE method also can provide credible validation for the experimental results,be instructive to predict mechanical performance of materials,and investigate detailed information about slip systems beyond the limitation of experimental conditions.

The purpose of this study is to investigate the micromechanical behavior and SRS properties of β phase in Ti-7333 alloy,using nanoindentation experiments combined with crystal plasticity modeling.The authors believe that the comparative analysis between experimental and numerical nanoindentation results could provide supportive information about mesoscopic mechanical behavior investigation and performance prediction.

2.Nanoindentation simulation and experiments

2.1.Nanoindentation tests

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To reveal the relationship between hardness and orientations the locations of indentations were carefully selected in the middle of grains away from boundaries for specific orientations identified by EBSD map,using a ZEISS SUPRA 55 Scanning Electron Microscope equipped with EBSD detector.The nanoindentation experiments were carried out using Hysitron TI-950 nanoindentation tester equipped with a Berkovich indenter.The spacing between adjacent indentations was over 20 times the maximum width of indentations to make sure that the deformation of one indentation was not interfered by the others.The loading procedure divided into three parts: firstly, loading to the maximum load(2000 μN)in 5 s,then holding for 2 s,and unloading to 0 μN in 5 s.

in which K is a constant with a value of 24.56 for perfect Berkovich indenter,and hc is the contact depth.In addition to the typical nanoindentation tests measuring static hardness,the CSM approach enables the investigation of the SRS properties of β phase in Ti-7333 alloy by the displacement oscillation of indenter.Lucas and Oliver[20]differentiated and simplified the Eqs.(1)and(2),and obtained the expression of indentation strain rate as follows

2.2.Hardness and SRS exponents

Nanoindentation tests are commonly applied to measure hardness and modulus of thin film and bulk materials based on the load-displacement curves.The value of hardness of an individual grain can be calculated from unloading portion of the curve using the method developed by Oliver and Pharr[19]as following expression

where P denotes the applied load and A denotes the projected contact area that can be calculated by

Then,nanoindentation tests under constant strain rate were applied to the sample using a standard continuous stiffness measurement(CSM)method for determining the SRS properties.The rate sensitivity of two selected grains with different orientations was measured through indentations made for three targeted indentation strain rate,varying between 0.2,0.05,and 0.01 s-1.For each grain and strain rate,four repeated indents were made.The peak load was set as 10 mN and the preload P0 set as 500 μN,which were the same for all tests.The preload setting aimed to avoid the useless vibration of indenter in contact with the surface of sample.The surface topography around indents was measured by Bruker Dimensions Icon AFM,and the data analyzed by NanoScope Analysis software.The nanoindentation tests were performed at room temperature.

which indicates that the indentation strain rate can keep constant as long as the ratio of loading rate(P˙)to load(P)remains a constant value.For SRS measurements,Mayo and Nix[21]purposed that the indentation rate could be derived from the concept of true strain,and defined the SRS exponent,m,using a constant loading rate by

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2.3.Crystal plasticity framework

In present work,the crystal plasticity constitutive model is employed based on the work of Peirce et al.[22].The crystal orientation and activated slip systems are taken into account.The total deformation gradient F of finite strain can be decomposed into elastic part Fe and plastic part Fp according to following equation

The nanoindentation simulation and experiments focused on the mesoscopic mechanical behavior of β phase in titanium.A new type of near β titanium alloy Ti-7333 (Ti-7Mo-3Nb-3Cr-3Al) designed by Northwestern Polytechnical University(NPU)was subjected as the experiment material.The β transus temperature of Ti-7333 alloy was approximately 850 ℃measured by metallographic method.Forged bar of Ti-7333 alloy was solution-treated at the temperature of 900 ℃for 30 min followed by water quenching in order to obtain the single β phase. The samples were from the bar with a dimension of 10 mm×7 mm×5 mm.The specimens were ground with sand papers and polished with OP-S diluted H2O2(with a ratio 1:9 of H2O2:OP-S)by Struers Metallographic Polisher,obtaining high-quality surface required for nanoindentation test and EBSD measurement.The microhardness tester was used to mark a target region with a half of rectangular frame.

where Fe is derived from the elastic stretching and rigid body rotation,and Fp is derived from dislocation slip.Dislocation slip is assumed to the sole mechanism for plastic deformation,and therefore,the evolution of velocity gradient Lp can be given by

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where and mα are plastic shear strain rate,slip direction vector and normal vector to slip plane on the α-th slip system,respectively.The shear rate on each slip system depends on resolved shear τα and slip system resistance gα by a rate-dependent power law as following

Simulated pileup profiles of indented surfaces along AC and BD directions of each grain are assembled in Fig.5.From the curves of different grains,it can be seen that the maximum height of pileup ranged from only 5–10 nm due to the good capability of plastic deformation for BCC crystal.Combined the results of Fig.4 and Fig.5,the width of pileup and the maximum value of height differs among those grains with different orientations,indicating that the morphology of pileup in β phase of Ti-7333 alloy is related to the orientation of indented grains.

The crystal plasticity constitutive model incorporated into the finite element code using user material subroutine.For single crystal model,the current strengths,shear strains,resolved shear stresses,slip directions and normals to slip plane are considered as solution dependent state variables[23].The subroutine automatically updates the solution dependent state variables at the end of each increment step.The values of the material Jacobian matrix∂ Δσ∂ /Δε can also calculate in the subroutine.

The SRS properties were evaluated from the curves of hardness versus displacement of indenter obtained by nanoindentation tests under constant strain rate in Fig.6.The initial measured hardness is inaccurate due to the preloading at early stage of deformation.In order to avoid the error resulting from the instability,the initial part of the curves was neglected.In Fig.6(b),the average values of hardness obtained at the depth of 300 nm assembled to fit the SRS exponent,m.It should be mentioned that these grains numbered 1 and 2 are not the same as the ones in Fig.2.

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where h0 is the initial hardening modulus,τ0 and τ0 are initial value and saturation value of the yield strength,respectively.And γ is the Taylor cumulative shear strain on all activated slip systems.The latent hardening modulus can be described as whereq is a constant.

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Fig.1.Three-dimensional finite element model of nanoindentation:modeled and meshed.(color is required only for online version).

3.Results and discussion

3.1.Three-dimensional finite element model

As shown in Fig.1,a three-dimensional finite element model generated with a dimension of 5.12µm×2.56µm×5.12µm.The whole model includes a cube representing the single crystal and a Berkovich indenter located on the surface of cube.We assumed that there is no Friction between the indenter and materials.

Since the Young's modulus of diamond is much larger than titanium alloy,deformation of the indenter was neglected by assuming that it is a rigid body.And the cubic was set as deformable part consisting of 14,520 eight-node brick elements and 16,236 nodes with reduced integration(C3D8R).The maximum number of elements already verified to guarantee a satisfying compromise between the accuracy and computational costs.Given the real constraint conditions of samples during indentation process,the bottom surface and four surrounding surfaces of the cubic were constrained.

由图2可知,电压互感器1、2、3、4、5、6、7、8、9和11号A相的量测数据序列之间的平均欧氏距离均小于阈值,而电压互感器10的量测数据序列与上述电压互感的量测数据序列的平均欧氏距离大于阈值,由此可以判定电压互感器10,也就是宾叙一线A相的电压互感器发生故障。

The parameters of crystal plasticity constitutive model for β phase of Ti-7333 alloy are assembled in Table 1.It should be mentioned that twelve slip systemsof β phase are considered in the model.

3.2.Effect of orientations on nanoindentation results

From a microscopic point of view,it is essential to investigate the effect of grain orientations on mechanical response in meso-scale.Plastic deformation of crystal inherently derives from the dislocation slipping on slip plane.Therefore,the change of grain orientation determines different loading direction during indentation process,which also leads to the change of activated slip systems.

The HKL channel 5 software is used to analyze the EBSD results in specific region previously marked (Fig. 2(a)), especially for theorientation information.The orientation mapping inserts in the rectangle of Fig.2(a).Fig.2(b)exhibits the inverse pole figure of different orientation.These grains conducted nanoindentation test are numbered and marked in Fig.2(b).

Table 1 The crystal plasticity constitutive parameters of β phase in Ti-7333 alloy.

γ0˙ /s- 1 n h0 /M Paτ0/ M Pa [24] τs /M Pa [24]0.001 15 1500 300 353

Fig.3 integrates the load-displacement curves of six selected grains obtained by their nanoindentation tests.From Fig.3,it can be seen that there are divergence existing in the maximum indent depth,and the slope of unloading part determines hardness of indented materials.Meanwhile,Table 2 lists measured hardness with different orientations varying from 3.78 to 4.27 GPa with an average value of 4.06 GPa.According to the curves in Fig.4 and the data in Table 2,the hardness shows a certain orientation-dependent characteristics.

However,due to its body-centered crystal structure,β phase of Ti-7333 alloy includes up to 48 slip systems,which might activates during plastic deformation.The change of loading direction has little effect on the number of activated slip systems.Thus,grain orientation has slight effect on the load-displacement curves of nanoindentation.

The displacement-controlling loading mode was used to simulate the movement process of indenter,and displacement-time data from experiments were used as input amplitude.The simulated values of hardness calculated by the Oliver-Pharr method using the simulated load-displacement curves are listed in Table 2,existing an acceptable error with 12.89%.The crystal plasticity constitutive parameters in Table 1 show a reasonable accuracy.

Under experimental conditions,the tip of Berkovich indenter was inevitably worn in contrast to the perfectly sharp indenter used in simulation.Even though the maximum indented depth in experiments and simulation were identical,plastic deformation took up a greater proportion during simulation process resulting in a lager residual indented depth.Therefore,the experimental results show better elastic resilience and higher hardness than the simulated results.

3.3.Pileup patterns

The top views of simulated surface morphology for corresponding grains after unloading are shown in Fig.4.It can be clearly observed that a similar distribution of three pileup areas occurs evenly along three sides of Berkovich indents boundaries,reflecting a character of symmetrical plastic deformation mechanism in β phase of Ti-7333 alloy.

Qualitatively,in each case,the height of the pileup was not the same along the three sides.There was a major pileup that was larger than the other two pileup hillocks with the exception of grains numbered 4 and 5.The three-dimensional view of grain 1 in Fig.5(a)is cut along two directions in AC(through one pileup)and BD(through the others pileup).The materials below indented surface had positive displacements,indicating that pileup comes from the internal material plastic accumulation.

Fig.2.(a)SEM image of target area and inserted EBSD orientation map,(b)inverse pole figure showing the orientation of grain with indentations.(color is required only for online version).

Fig.3.Load-displacement curves for nanoindentation of 6 grains numbered in Fig.2.(color is required only for online version).

Table 2 Hardness of 6 grains calculated from experiments and simulation.

Grain Hardness/Gpa Experimental Simulated 1 3.78 3.49 2 4.27 3.72 3 4.19 3.74 4 3.95 3.33 5 4.13 3.52 6 4.02 3.42 Average 4.06 3.54

where denotes the reference value of the slip rate,n represents the reciprocal of SRS exponent.As dislocations accumulating during shear,the materials is work hardened through both self and latent hardening mechanisms,and the rate of change of slip resistance can be given by

3.4.Relationship between orientations and SRS exponents

where hαβ is the hardening modulus.The PAN hardening model is used in this work,and the self-hardening modulus can be given by

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The results show that β grains exhibit different hardness under each constant strain rate,and the higher strain rate it applies,the larger hardness it obtains.In Fig.6(a),the hardness has slightly decline under a rate of 0.2 and 0.05 s-1,in comparison to the obvious decline at a rate of 0.01 s-1 in Fig.6(b).The decrease occurs mainly in the initial stage,and the hardness tends to be stable as the depth of indentation increases.

The m values were evaluated from the plots of hardness against strain rate in log-log form,showing in Fig.6(c)-(d).The hardness rises continuously with increasing strain rate,from about 3.3–4.0.The AFM images of two grains with the strain rate of 0.05 s-1 were added in Fig.6,showing pile-up distribution surrounding the indents.It is noteworthy that there was one prominent pileup in each grain,which is consistent with simulated results shown in Fig.4.Thus,the reliability of CPFE model established in this paper is verified.

Compared between two grains,there is no obvious difference in hardness under the same strain rate,showing that the strain rate has more significant influence than grain orientations on the value of hardness in β phase of Ti-7333 alloy.With similar m value(0.056 and 0.064)for two orientations,the rate sensitivity is independent of grain orientation in terms of β phase.In early researches,the SRS exponent has a strong dependence on the orientation in nano-twin copper[25],which is much higher in the hard loading direction(vertical to twin boundaries).The SRS exponent of dual phase titanium Ti-6242 and Ti-6246[8]exhibits differences in the degree of orientation dependence,which is attributed to the volume fraction and thickness of β lath combined with the ability for dislocation to easily slip across complex microstructures. However, there are no precipitation or twinning structure found in the solution-treated Ti-7333 alloy of single β phase.Besides,the BCC structure of β phase owns greater capability of plastic deformation, in comparison to the HCP structure of α phase determining the soft and hard orientation during slip.Therefore,the grain orientation has nearly no effect on the SRS exponent in β phase of Ti-7333 alloy.Still,the relationship between the m value obtained through nanoindentation tests and the rate sensitive measurement of macrodeformation still needs further investigation.

4.Conclusions

By the combination of instrumented nanoindentation,EBSD and AFM experimental measurements,and CPFE modeling,the deformation process of nanoindentation in near β Ti-7333 titanium alloy is assessed.The crystal orientation dependency of the alloy is characterized by analyzing the pileup topography distribution around indentations,and the rate sensitivity properties investigated with a nanoindentation CSM method using multiple indentations at different constant strain rate.

Fig.4.Simulated pileup morphology of 6 grains from Fig.2(color is required only for online version).

Fig.5.Simulated pileup pattern in(a)3D view and sections in(b)AC and(c)BD paths and simulated pileup profiles of indented surfaces along(d)AC and(e)BD directions.(color is required only for online version).

Fig.6.Individual hardness vs.displacement curves and the hardness vs.strain rate(log-log form)for(a,c)grain 1 and(b,d)grain 2 under different strain rate.(color is required only for online version).

The typical nanoindentation tests have been used to discuss the relationship between hardness and grain orientations in β phase of Ti-7333 alloy.Nanohardness and load-displacement curves of six grains with different orientations show a character of orientation dependence.Based on the results of CPFE simulation for single crystal nanoindentation process,pileup pattern of β phase appears symmetrical distribution because of its body-centered cubic microstructure,while the width and height of pileup relates to grain orientations.Most of grains own one major pileup and two relatively smaller pileup hillocks.Moreover,under a constant strain rate,the value of hardness shows decreasing tendency as the indentation depth increasing,and the SRS exponents m exhibit independence of grain orientation in the β phase.

Acknowledgements

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The authors gratefully acknowledge the National key Research and Development Program of China(2016YFB0701303)and the“111”Project(No.B08040)for financial support.

Research data

The raw data of individual nanoindentation associated with section 4.3 can be found in the online version at http://dx.doi.org/10.17632/ddxtvjjfdk.4.

Declarations of interest

None.

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Mengqi Zhang,Jinshan Li,Bin Tang,Hongchao Kou,Jiangkun Fan
《Progress in Natural Science:Materials International》2018年第6期文献

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