Cao 2014
Cao 2014
Cao 2014
Liang CAO1, Wen-cai LIU1,2, Zhong-quan LI3, Guo-hua WU1,2, Lü XIAO3, Shao-hua WANG4, Wen-jiang DING1,2
1. National Engineering Research Center of Light Alloy Net Forming,
Shanghai Jiao Tong University, Shanghai 200240, China;
2. Key State Laboratory of Metal Matrix Composite, Shanghai Jiao Tong University, Shanghai 200240, China;
3. Shanghai Aviation Precision Machinery Research Institute, Shanghai 201600, China;
4. Science and Technology on Space Physics Laboratory, Beijing 100076, China
Received 8 April 2013; accepted 5 July 2013
Abstract: The microstructure, mechanical properties and fracture behavior of sand-cast Mg−10Gd−3Y−0.5Zr alloy (mass fraction,
%) under T6 condition (air cooling after solid solution and then aging heat treatment) were investigated. The optimum T6 heat
treatments for sand-cast Mg−10Gd−3Y−0.5Zr alloy are (525 °C, 12 h + 225 °C, 14 h) and (525 °C, 12 h + 250 °C, 12 h) according to
age hardening curve and mechanical properties, respectively. The ultimate tensile strength, yield strength and elongation of the
Mg−10Gd−3Y−0.5Zr alloy treated by the two optimum T6 processes are 339.9 MPa, 251.6 MPa, 1.5% and 359.6 MPa, 247.3 MPa,
2.7%, respectively. The tensile fracture mode of peak-aged Mg−10Gd−3Y−0.5Zr alloy is transgranular quasi-cleavage fracture.
Key words: Mg−10Gd−3Y−0.5Zr; magnesium alloy; heat treatment; fracture; microstructure; mechanical property
Foundation item: Project (51275295) supported by the National Natural Science Foundation of China; Project (USCAST2012-15) supported by the Funded
Projects of SAST-SJTU Joint Research Centre of Advanced Aerospace Technology, China; Project (20120073120011) supported by the
Research Fund for the Doctoral Program of Higher Education of China
Corresponding author: Wen-cai LIU; Tel: +86-21-54742630; E-mail: [email protected]
DOI: 10.1016/S1003-6326(14)63102-2
612 Liang CAO, et al/Trans. Nonferrous Met. Soc. China 24(2014) 611−618
indicates that traditional water cooling process is not
suitable for sand-cast complicated structural components 3 Results and discussion
after heat treatment. Air cooling is verified to be an
effective cooling method to solve the crack problem 3.1 Microstructures
through practice. The microstructures and phase compositions of the
However, few systematical research reports on heat sand-cast and solution heat treated (T4: 525 °C, 12 h)
treatment process of air cooling and subsequent GW103K alloys by OM and XRD analyses are shown in
microstructures, mechanical properties and fracture Figs. 2 and 3, respectively. As shown in Fig. 2(a), the
behavior are found. The present study is aimed to microstructure of the sand-cast GW103K alloy consists
optimize heat treatment process, based on air cooling, of of equiaxed α-Mg matrix and network eutectic
sand-cast Mg−10Gd−3Y−0.5Zr (named as GW103K) compounds which distribute at grain boundaries. The
and investigate its corresponding microstructure, secondary phase is observed and little pseudo eutectic or
mechanical properties at room temperature and fracture dendrite is found in the alloy. The grains’ shapes of the
behavior by various analysis methods.
2 Experimental
Fig. 1 Shape and size of cylindrical tensile specimen (unit: Fig. 3 XRD patterns of sand-cast (a) and T4 treated (b)
mm) GW103K alloy
Liang CAO, et al/Trans. Nonferrous Met. Soc. China 24(2014) 611−618 613
sand-cast alloy is polygons and their boundaries are very sand-cast alloy, which means that the amount of small
clear. The microstructure after solution treatment of cuboid-shaped phase is too little. Therefore, most of
(525 °C, 12 h) is shown in Fig. 2(b). Almost all the small cuboid-shaped phases are produced during solution
eutectic compounds have been dissolved into the matrix. heat treatment.
Gd and Y atoms dissolved into the magnesium matrix Figure 4 shows the microstructures of sand-cast T6
and formed supersaturated solid solution. Compared with treated (solution: 525 °C, 12 h) GW103K alloy. As seen
WANG’s result [12] of the T4 treated GW103K alloy from Figs. 4(a)−(c), no significant change in morphology
which was carried out water cooling after solution heat is observed in terms of grain size after aging heat
treatment, the microstructure in this work which used air treatment. Small granular black dots dispersively
cooling after solution appears to be more homogeneous distributed both in grains and at grain boundaries after
and there is less secondary phase retained. Moreover, aging 225 °C while they mostly segregated at grain
some unevenly distributed small granular black dots are boundaries after aging at 250 °C. Besides, some Zr cores
observed along grain boundaries and inside the grains. are also observed inner the grain of alloys aged at 250 °C.
These dots are cluster remnant secondary phase and The corresponding XRD analysis towards the T6 treated
small cuboid-shaped phase (γ phase). Based on the GW103K alloy is presented in Fig. 5. It can be seen that
results by WANG [12] and HE [14], small cuboid-shaped β′′ and β′ phases are detected. With the increase of aging
phase is a compound with high contents of rare earth time from under-aging to peak-aging period, the peaks of
elements and its size is 2−5 μm. It has face-centered β′′ phase gradually disappear and the peaks of β′ phase
cubic structure and the lattice constant is 5.6 Å. The appear. The precipitation sequence of GW103K is: α-Mg
corresponding XRD analysis results of the sand-cast and supersaturated solid solution (S.S.S.S.)→ metastable β"
solution treated GW103K alloy are shown in Fig. 3. It (D019)→metastable β' (cbco)→metastable β1 (fcc)→
can be seen that the sand-cast GW103K alloy contains stable β (fcc). The metastable β′ phase is regarded as the
two different phases: α-Mg phase and the eutectic phase main strengthening phase in Mg–Gd alloys [14]. The
consisting of Mg24(Gd,Y)5. Compared with the sand-cast diffraction peaks of small cuboid-shaped phase are
alloy, the peak of eutectic phase Mg24(Gd,Y)5 almost detected at the range of 28°−30° and 47°−49°, which are
disappears in the solution treated alloy. Meanwhile, the also detected in the XRD patterns of solution treated
peak of γ phase appears. According to XRD results, the GW103K alloy. This indicates that aging heat treatment
main composition of T4 treated GW103K alloy is α-Mg cannot eliminate the γ phase produced in the
and γ phase. There is no diffraction peak of γ phase in solution heat treatment, which accords with the results of
Fig. 4 Microstructures of T6 treated GW103K alloy under different aging conditions with various amplifications: (a, b) 225 °C, 14 h;
(c, d) 250 °C, 12 h
614 Liang CAO, et al/Trans. Nonferrous Met. Soc. China 24(2014) 611−618
hardness test results. Compared with the hardness of
as-cast GW103K alloy (HV85.4), the peak hardnesses at
two aging treatment temperatures increase by 41.6% and
29.9%, respectively, showing obvious aging hardening
behavior.
Fig. 9 Typical SEM images showing fracture surfaces of specimens under different conditions: (a) Peak-aging at 225 °C;
(b) Magnified view of central region in (a); (c) Peak-aging at 250 °C; (d) Magnified view of central region in (c)
Fig. 10 Typical SEM images showing fracture surfaces under different conditions: (a) Under-aging at 225 °C; (b) Peak-aging at
225 °C
comparatively and some dimples in the fracture of conditions. The specimens show the secondary crack
peak-aged alloy show that the fracture mode is morphologies. Apparent transgranular secondary cracks
transgranular quasi-cleavage fracture. This indicates that from both microstructures of alloys aged at 225 °C and
the toughness of sand-cast GW103K alloy improves with 250 °C are observed, which indicates that fracture mode
the progress of aging heat treatment, which is consistent of T6 treated GW103K alloy is mainly transgranular
with results in Refs. [12,14,20]. fracture. Inside some grains, a large number of fine twins
Figure 11 shows the microstructures of fracture are observed. Twinning is an especially important
surface of GW103K alloy under different aging deformation mechanism for HCP magnesium alloys, in
Liang CAO, et al/Trans. Nonferrous Met. Soc. China 24(2014) 611−618 617
Fig. 11 Optical micrographs showing fracture surface of age-treated GW103K alloy under different aging conditions: (a) Peak-aging
at 225 °C; (b) Magnified view of boxed region in (a); (c) Peak-aging at 250 °C; (d) Magnified view of boxed region in (c)
4 Conclusions References
1) The microstructure of the sand-cast [1] LIU Wen-cai, DONG Jie, SONG Xu, BELNOUE J P, HOFMANN F,
Mg−10Gd−3Y−0.5Zr alloy mainly consists of α-Mg and DING Wen-jiang, KORSUNSKY A M. Effect of microstructures and
eutectic compound Mg24(Gd,Y)5. After solution texture development on tensile properties of Mg−10Gd−3Y alloy [J].
Materials Science and Engineering A, 2011, 528(6): 2250−2258.
treatment, the main composition is α-Mg and γ phase. β′
[2] POLMEAR I J. Magnesium alloys and applications [J]. Mater Sci
phase gradually precipitates with the progress of aging.
Technology, 1994, 10(1): 1−16.
2) Considerable precipitation hardening is
[3] GAO Xiang, HE Shang-ming, ZENG Xiao-qin, PENG Li-ming,
exhibited by aging treatment. The Mg−10Gd−3Y−0.5Zr DING Wen-jiang, NIE Jian-feng. Microstructure evolution in a
alloy solution treated at 525 °C for 12 h reaches the peak Mg−15Gd−0.5Zr (wt.%) alloy during isothermal aging at 250 °C [J].
hardness of HV120.9 and HV110.9 aged at 225 °C for 14 Material Science and Engineering A, 2006, 431(1−2): 322−327.
h and 250 °C for 12 h respectively. The yield strength, [4] NIE Jian-feng, GAO Xiang, ZHU Su-ming. Enhanced age hardening
ultimate tensile strength and elongation reach 251.6 MPa, response and creep resistance of Mg−Gd alloys containing Zn [J].
339.9 MPa, 1.5% and 247.3 MPa, 359.6 MPa, 2.7% at Scripta Materialia, 2005, 53(9): 1049−1053.
aging conditions of (225 °C, 14 h) and (250 °C, 12 h), [5] GAO Xiang, NIE Jian-feng. Enhanced precipitation–hardening in
Mg−Gd alloys containing Ag and Zn [J]. Scripta Materialia, 2008,
respectively. With regards to hardness and tensile
58(8): 619−622.
properties, the processes of (525 °C, 12 h + 225 °C, 14 h)
[6] ZHENG Kai-yun, DONG Jie, ZENG Xiao-qin, DING Wen-jiang.
and (525 °C, 12 h + 250 °C, 12 h) are selected as the
Precipitation and its effect on the mechanical properties of a cast
optimized heat treatment conditions, respectively. Mg–Gd–Nd–Zr alloy [J]. Material Science and Engineering A, 2008,
3) Based on air cooling after heat treatment, the 489(1−2): 44−54.
Mg−10Gd−3Y−0.5Zr alloy shows superior function of [7] LIANG Shu-quan, GUAN Di-kai, CHEN Liang, GAO Zhao-he,
elongation than the alloy is water cooled after heat TANG Hui-xiang, TONG Xu-ting, XIAO Rui. Precipitation and its
618 Liang CAO, et al/Trans. Nonferrous Met. Soc. China 24(2014) 611−618
effect on age-hardening behavior of sand-cast Mg−Gd−Y alloy [J]. Shanghai Jiao Tong University, 2007. (in Chinese)
Materials and Design, 2011, 32(1): 361−364. [15] DRITS M E, ROKHLIN L L, NIKITINA N I. State diagram of the
[8] LIU Wen-cai, DONG Jie, ZHANG Ping, KORSUNSKY A M, SONG Mg−Y−Gd system in the range rich in magnesium [J]. Izvestiya
Xu, DING Wen-jiang. Improvement of fatigue properties by shot Akademii Nauk SSSR Metally, 1983, 5: 215−219.
peening for Mg−10Gd−3Y alloy under different conditions [J]. [16] GAO Lei, CHEN Rong-shi, HAN En-hou. Microstructures and
Materials Science and Engineering A, 2011, 528(18): 5935−5944. strengthening mechanisms of a cast Mg−1.48Gd−1.13Y−0.16Zr
[9] DONG Jie, LIU Wen-cai, SONG Xu, ZHANG Ping, DING (at. %) alloy [J]. Journal of Material Science, 2009, 44(16):
Wen-jiang, KORSUNSKY A M. Influence of heat treatment on 4443−4454.
fatigue behavior of high-strength Mg−10Gd−3Y alloy [J]. Materials [17] HONMA T, OHKUBO T, HONO K, KAMADO S. Chemistry of
Science and Engineering A, 2010, 527(21−22): 6053−6063. nanoscale precipitates in Mg−2.1Gd−0.6Y−0.2Zr (at.%) alloy
[10] LIU Wen-cai, WU Guo-hua, ZHAI Chun-quan, DING Wen-jiang, investigated by the atom probe technique [J]. Materials Science and
KORSUNSKY A M. Grain refinement and fatigue strengthening Engineering A, 2005, 395(1−2): 301−306.
mechanisms in as-extruded Mg−6Zn−0.5Zr and Mg−10Gd−3Y− [18] GAO Lei, CHEN Rong-shi, HAN En-hou. Fracture behavior of high
0.5Zr magnesium alloys by shot peening [J]. International Journal of strength Mg−Gd−Y−Zr magnesium alloy [J]. Transactions of
Plasticity, 2013, 49: 16−35. Nonferrous Metals Society of China, 2010, 20(7): 1217−1221.
[11] ANYANWU I A, KAMADO S, KOJIMA Y. Creep properties of [19] PENG Qiu-ming, HOU Xiu-li, WANG Li-dong, WU Yao-ming,
Mg−Gd−Y−Zr alloys [J]. Material Transactions, 2001, 42(7): CAO Zhan-yi, WANG Li-min. Microstructure and mechanical
1212−1218. properties of high performance Mg−Gd based alloys [J]. Materials
[12] WANG Qi-long. Study on the microstructure and mechanical and Design, 2009, 30(2): 292−296.
properties of sand mould cast Mg−10Gd–3Y–Zr alloy [D]. Shanghai: [20] GAO Lei, CHEN Rong-shi, HAN En-hou. Effects of rare-earth
Shanghai Jiao Tong University, 2010. (in Chinese) elements Gd and Y on the solid solution strengthening of Mg alloys
[13] HE Shang-ming, ZENG Xiao-qin, PENG Li-ming, GAO Xiao-qin, [J]. Journal of Alloys and Compounds, 2009, 481(1−2): 379−384.
NIE Jian-feng, DING Wen-jiang. Precipitation in a Mg−10Gd−3Y− [21] LIU Zhi-jie, WU Guo-hua, LIU Wen-cai, PANG Song, DING
0.4Zr (wt. %) alloy during isothermal aging at 250 °C [J]. Journal of Wen-jiang. Effect of heat treatment on microstructures and
Alloys and Compounds, 2006, 421(1−2): 309−313. mechanical properties of sand-casting Mg−4Y−2Nd−1Gd−0.4Zr
[14] HE Shang-ming. Study on the microstructural evolution, properties magnesium alloy [J]. Transactions of Nonferrous Metals Society of
and fracture behavior of Mg−Gd−Y−Zr(−Ca) alloys [D]. Shanghai: China, 2012, 22(7): 1540−1548.