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Effects of Deep Cryogenic Treatment On The Microstructure and Mechanical Properties of Commercial Pure Zirconium 2015 Journal of Alloys and Compounds
Effects of Deep Cryogenic Treatment On The Microstructure and Mechanical Properties of Commercial Pure Zirconium 2015 Journal of Alloys and Compounds
a r t i c l e i n f o a b s t r a c t
Article history: The effects of deep cryogenic treatment (DCT) on the microstructure and mechanical properties of com-
Received 25 April 2014 mercial pure zirconium were investigated. Experimental results indicated that DCT induced a change in
Received in revised form 3 August 2014 grain orientation and improved internal stress, which in turn increased dislocation density that led to
Accepted 26 August 2014
improved hardness. Hardness in basal planes was found to be signicantly larger than that in prism
Available online 16 September 2014
planes. Moreover, strength was enhanced in DCT-treated zirconium and the ductility was comparable
to that of as-annealed zirconium. This phenomenon was due to the increase in dislocation density and
Keywords:
the good ductility resulting from the motion of pre-existing dislocations and specic dislocation cong-
Metals and alloys
Deep cryogenic treatment
urations. DCT led to the transformation of tensile fracture mode from mixed-rupture characteristics of
Microstructure quasi-cleavage and dimples to quasi-cleavage, thereby increasing compatible deformation capabilities.
Mechanical properties The possible mechanisms underlying microstructural modication, tensile strength, and hardness
Zirconium improvement were discussed.
2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jallcom.2014.08.201
0925-8388/ 2014 Elsevier B.V. All rights reserved.
514 C. Yuan et al. / Journal of Alloys and Compounds 619 (2015) 513519
2. Experimental
The material used in this study was commercial pure Zr plate (chemical
composition summarized in Table 1). The plate was annealed in a vacuum at
1123 K for 4 h to obtain a homogeneous polycrystalline structure. The average grain
size of the as-annealed sample was approximately 3050 lm. The samples cut from
the as-annealed plate were placed in a liquid nitrogen environment at 77 K for 24 h.
Afterwards, the samples were taken out and cooled to room temperature.
X-ray diffraction (XRD) patterns of the as-annealed and DCT-treated samples
were measured using a Rigaku D/max 2500 X-ray diffractometer (18 kW) with Cu
Ka radiation (wavelength k = 1.54 ) in continuous-scanning mode over 2h = 30
80 at a step of 0.02. Differential scanning calorimetry (DSC) was conducted on a
Diamond DSC (PerkinElmer Inc., UK). For dynamic scans, samples were subjected
to temperatures ranging from 20 C to 160 C at a cooling rate of 20 C/min.
Microstructure features before and after DCT were observed by optical microscopy
(OM), electron backscatter diffraction (EBSD), and transmission electron micros-
copy (TEM). EBSD analysis was performed using a HITACHI S-4800 scanning elec-
tron microscopy (SEM) system, whereas TEM observations were carried out with
a JEOL-2010 TEM system at a voltage of 200 kV.
A FM-ARS9000 Vickers microhardness tester was used to measure the hardness
of samples. Indentations were carried out with a given load of 200 g and a dwell
time of 10 s. Hardness distributions over a square area of 4.5 4.5 mm2, with a
space between adjacent indentations of 0.5 mm were obtained. The tensile samples
were machined with a gauge length of 30 mm and a cross-section of 10 1.5 mm2.
Four repeated tensile tests were performed on a MTS test system at a strain rate of
1 104 s1 at room temperature under extensometer-measured strain control.
Fracture surfaces after the tensile test were observed by SEM, and microstructures
near the fracture surfaces were observed by TEM.
Fig. 1(a) shows the XRD patterns of as-annealed and DCT- Fig. 1. XRD patterns of as-annealed and DCT-treated samples (a), and the cryogenic
DSC curve of Zr (b).
treated samples. No phase transformation was observed in DCT-
treated Zr compared with as-annealed Zr. However, the intensities
of the diffraction peaks of DCT-treated Zr were slightly enhanced, fraction of HAGBs. No phase transformation and precipitation
which can be attributed to the variation in lattice constants caused occurred during DCT, consistent with the XRD and DSC results.
by DCT. Changes in lattice constants were also observed in DCT- Fig. 2(c) and (d) shows the IPF maps of Zr before and after DCT,
treated Mg [18,19]. To further conrm the microstructure stability respectively. The maximum intensity indicated the number of ran-
of Zr at cryogenic temperature, a cryogenic DSC curve was obtained dom orientations. A strong preference was observed toward the
and is shown in Fig. 1(b). The smooth feature of the DSC curve indi- (0 0 0 1) orientation, which was corroborated by the OIM maps in
cated that no transformation occurred during DCT. Fig. 2(a) and (b). Furthermore, the intensity of prism planes was
lower and the grain orientations were much closer to the (0 0 0 1)
3.2. EBSD analysis basal plane orientation after DCT. This nding can be attributed
to the ordered arrangement of atoms resulting from the small
To gain deep insight into microstructural changes, EBSD analy- changes in lattice constants [18,19]. The misorientation angle dis-
sis was performed. In this analysis, orientation imaging microscopy tributions in Fig. 2(e) and (f) shows that the crystallite boundaries
(OIM) maps, inverse pole gure (IPF) maps, and boundary misori- were mainly high angle in nature. The HAGB fractions of Zr before
entation angle distributions were obtained before and after DCT, and after DCT were about 81.2% and 85.3% of the total grain bound-
as shown in Fig. 2. Fig. 2(a) and (b) shows the OIM maps of Zr ary length, respectively. Thus, DCT improved the formation of
before and after DCT, with high-angle (HAGBs; grain boundary HAGBs. The increase in HAGB fractions may be related to the
misorientations P 15) and low-angle (LAGBs; grain boundary extrinsic dislocations formed during DCT (Fig. 3). The extrinsic dis-
misorientations < 15) grain boundaries depicted by black and locations were probably easier to react with the dislocations in
white lines, respectively. The crystallographic directions corre- LAGBs [20,21]. Therefore, the accumulation and rearrangement of
sponding to various colors can be inferred from the IPF triangle dislocations resulted in the transformation of LAGBs to HAGBs,
shown at the bottom right corner of Fig. 2(a) and (b). The micro- leading to increased HAGB and decreased LAGB fractions.
structure was characterized by equiaxed grains and a higher
Fig. 2. Representative OIM maps of (a) as-annealed and (b) DCT-treated samples. IPF maps of (c) as-annealed and (d) DCT-treated samples. Distribution of boundary
misorientation angle of (e) as-annealed and (f) DCT-treated samples.
temperature, the volume of the material contracted. This volume substantially varied from approximately 140190 Hv, with an average
contraction released great compression deformation energy that value of 159.5 Hv. By contrast, the hardness of DCT-treated Zr gen-
served as the driving force for the formation and movement of dis- erally changed from approximately 160220 Hv, with an average
locations [18]. The improvement in dislocation density played a value of 197.5 Hv. Evidently, the average hardness signicantly
signicant role in enhancing mechanical properties and deforma- increased after DCT. The difference between the two average hard-
tion behavior, as discussed in the following sections. ness values reached 23.8%. Although the spatial distribution of
hardness was not uniform from one area to another, the increase
3.4. Hardness measurements in hardness of the DCT-treated sample was a holistic rather than
localized phenomenon, as can also be conrmed by the hardness
To better understand the variation in hardness of Zr, contour evolution characterized by the color maps in Fig. 4. The inhomoge-
maps of the spatial distribution of the Vickers hardness (Hv) over neity of hardness distribution may be closely related to the grain
a 4.5 4.5 mm2 square area before and after DCT are shown in orientation. An in situ comparison between the OIM map and
Fig. 4(a) and (b), respectively. The hardness of as-annealed Zr OM image of hardness indentation of DCT-treated Zr is presented
516 C. Yuan et al. / Journal of Alloys and Compounds 619 (2015) 513519
M (a) (b)
A
D
B C
B C
D
A M
Fig. 5. (a) OIM map and (b) corresponding OM image of hardness indentation of the DCT-treated Zr.
Fig. 7. Normalized strain hardening rate (H) against the true strain of as-annealed
and DCT-treated samples.
Fig. 8. TEM images of (a) as-annealed and (b) DCT-treated samples after tensile tests.
(a) (b)
500 m 500 m
(c) (d)
500 m 500 m
Fig. 9. SEM images showing the fracture surfaces of as-annealed and DCT-treated Zr tensile samples. (a) and (b) are the edge and middle region of as-annealed Zr sample; (c)
and (d) are the edge and middle region of DCT-treated Zr sample.
localization during tensile test. For comparison, the fracture characteristics in the edge and middle region exhibited by as-
surfaces of DCT-treated Zr in the same regions are presented in annealed Zr. By contrast, the motion of pre-existing dislocations
Fig. 9(c) and (d), respectively. The fracture characteristics of two and specic dislocation congurations effectively enhanced the
regions were mainly consisted of quasi-cleavage facets. No obvious compatible deformation capability, resulting in the same fracture
necking was observed in the edge and middle regions of the characteristics in both regions of the DCT-treated sample.
fracture surfaces.
The above ndings indicated that DCT restricted strain localiza- 4. Conclusion
tion occurring in the edge regions of tensile samples. For as-
annealed Zr, plastic instability (i.e., necking) occurred in the edge Based on the above-described investigations, the following con-
region of tensile samples before ultimate fracture. Moreover, clusions were drawn.
Fig. 2(e) and (f) shows that the fraction of LAGBs before DCT was
slightly larger than that after DCT. LAGBs are reportedly associated (1) The grain orientations were much closer to the (0 0 0 1) basal
with the early onset of plastic instability during tensile testing plane orientation after DCT. DCT increased HAGB fractions
[3335]. The plastic instability accounted for the different fracture and dislocation density.
C. Yuan et al. / Journal of Alloys and Compounds 619 (2015) 513519 519
(2) Hardness was closely related to grain orientations and dislo- [8] R. Thornton, T. Slatter, A.H. Jones, R. Lewis, Wear 271 (2011) 23862395.
[9] T. Slatter, R. Lewis, A.H. Jones, Wear 271 (2011) 14811489.
cation density. The hardness in basal planes was much
[10] P.J. Singh, S.L. Mannan, T. Jayakumar, D.R.G. Achar, Eng. Fail. Anal. 12 (2005)
higher than that in prism planes. After DCT, dislocation den- 263271.
sity increased the resistance of dislocation motion, thereby [11] S. Zhirafar, A. Rezaeian, M. Pugha, J. Mater. Process. Technol. 186 (2007) 298
improving hardness. 303.
[12] V. Leskovek, B. Podgornik, Mater. Sci. Eng., A 531 (2012) 119129.
(3) Strength levels were high and good ductility could still be [13] H.H. Liu, J. Wang, B.L. Shen, H.S. Yang, S.J. Gao, S.J. Huang, Mater. Des. 28 (2007)
achieved after DCT. The enhancement in strength was due 10591064.
to the increase in dislocation density, and the maintenance [14] P.F. Stratton, Mater. Sci. Eng., A 449 (2007) 809812.
[15] A. Bensely, S. Venkatesh, D. Mohan Lal, G. Nagarajan, A. Rajadurai, Krzysztof
of good ductility resulted from the motion of pre-existing Junik, Mater. Sci. Eng., A 479 (2008) 229235.
dislocations and specic dislocation congurations. [16] X.Q. Jiang, N. Li, H. He, X.J. Zhang, C.C. Li, H. Yang, Mater. Sci. Forum 546549
(4) The fracture surfaces exhibited mixed features with quasi- (2007) 845848.
[17] D.F. Guo, M. Li, Y.D. Shi, T.Y. Ma, Z.B. Zhang, T.S. Wang, X.Y. Zhang, Mater. Sci.
cleavage facets and dimples for as-annealed Zr and quasi- Eng., A 581 (2013) 133139.
cleavage facets for DCT-treated Zr. The grains were divided [18] J.W. Liu, G.F. Li, D. Chen, Z.H. Chen, Chin. J. Aeronaut. 25 (2012) 931936.
into smaller blocks because of the interaction of dislocations [19] X.F. Zhang, G.H. Wu, W.C. Liu, W.J. Ding, Trans. Nonferrous Met. Soc. China 22
(2012) 28832890.
during the tensile process of DCT-treated Zr. Consequently, [20] P. Xue, B.L. Xiao, Z.Y. Ma, Mater. Sci. Eng., A 532 (2012) 106110.
the compatible deformation capability of materials was [21] Y.H. Zhao, J.F. Bingert, Y.T. Zhu, X.Z. Liao, R.Z. Valiev, Z. Horita, T.G. Langdon,
enhanced and good ductility could still be achieved. Y.Z. Zhou, E.J. Lavernia, Appl. Phys. Lett. 92 (2008) 081903.
[22] D.N. French, D.A. Thomas, Trans. AIME 233 (1965) 950952.
[23] T. Takahashi, E.J. Freise, Philos. Mag. 12 (1964) 18.
[24] B. Roebuck, P. Klose, K.P. Mingard, Acta Mater. 60 (2012) 61316143.
Acknowledgment [25] L. Zhang, Y. Han, J. Lu, Nanotechnology 19 (2008) 165706.
[26] G.E. Dieter, Mech. Metall., third ed., McGraw-Hill, London, 1988.
[27] D.F. Guo, M. Li, Y.D. Shi, Z.B. Zhang, T.Y. Ma, H.T. Zhang, X.Y. Zhang, Mater. Sci.
Financial support from the National Basic Research Program of Eng., A 558 (2012) 611615.
China (Grant No. 2010CB731606) is greatly acknowledged. [28] D.F. Guo, M. Li, Y.D. Shi, Z.B. Zhang, H.T. Zhang, X.M. Liu, X.Y. Zhang, Mater.
Lett. 66 (2012) 305307.
[29] X.X. Huang, Scr. Mater. 60 (2009) 10781082.
References [30] L. Lu, X. Chen, X. Huang, K. Lu, Science 323 (2009) 607610.
[31] X.X. Huang, N. Hansen, N. Tsuji, Science 312 (2006) 249251.
[1] R.F. Barron, Cryogenics 22 (1982) 409414. [32] Z.W. Shan, Raja K. Mishra, S.A. Syed Asif, Oden L. Warren, Andrew M. Minor,
[2] K.M. Asl, A. Tari, F. Khomamizadeh, Mater. Sci. Eng., A 523 (2009) 2731. Nat. Mater. 7 (2008) 115119.
[3] M. Koneshlou, K.M. Asl, F. Khomamizadeh, Cryogenics 51 (2011) 5561. [33] R. Kapoor, N. Kumar, R.S. Mishra, C.S. Huskamp, K.K. Sankaran, Mater. Sci. Eng.,
[4] A. Molinari, M. Pellizzari, S. Gialanella, G. Straffelini, K.H. Stiasny, J. Mater. A 527 (2010) 52465254.
Process. Technol. 118 (2001) 350355. [34] P.L. Sun, C.Y. Yu, P.W. Kao, C.P. Chang, Scr. Mater. 52 (2005) 265269.
[5] P. Baldissera, Mater. Des. 31 (2010) 47254730. [35] N. Kumar, R.S. Mishra, C.S. Huskamp, K.K. Sankaran, Mater. Sci. Eng., A 528
[6] P. Baldissera, C. Delprete, Open Mech. Eng. J. 2 (2008) 111. (2011) 58835887.
[7] B. Podgornik, F. Majdic, V. Leskovsek, J. Vizintin, Wear 288 (2012) 8893.