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Article history: NiCrAlY platelets modified glass matrix composites were prepared. Their microstructures were char-
Received 18 August 2010 acterized, their Young’s modulus, fracture strength in bending, Vickers hardness, and indentation
Received in revised form 8 October 2010 toughness were measured, and their thermal shock resistance was studied using quenching-strength
Accepted 8 October 2010
and indentation-quench methods. With increasing NiCrAlY content, evident enhancements of the Young’s
modulus and indentation toughness were obtained. The NiCrAlY alloy inclusion could exert significant
influences on the retained bending strength of the samples after quench tests, from 9.6 MPa for NiCrAlY-
Keywords:
free glass to 32.0 MPa for 30 wt.% NiCrAlY-containing composites. The indentation-quench tests showed
A. Mechanical characterization
A. Micromechanics
that NiCrAlY alloy inclusion elevated the critical quenching temperatures for propagation of pre-crack,
B. Glass from 150 ◦ C for NiCrAlY-free glass to 225 ◦ C for 30 wt.% NiCrAlY-containing composites. Inclusion debond-
B. Nickel based superalloys ing and intersection, crack deflection and bridging were observed, and are likely the micromechanisms
C. Sintering accounted for the improvement of fracture resistance.
D. Fracture © 2010 Elsevier B.V. All rights reserved.
0921-5093/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2010.10.015
M. Chen et al. / Materials Science and Engineering A 528 (2011) 1360–1366 1361
Table 1
Chemical compositions and physical properties of the composite constituents.
SiO2 Balance
Al2 O3 5.98 Ni Balance
ZnO 9.00
CaO 3.66 Cr 24.73
ZrO2 5.29
TiO2 2.75 Al 4.90
B2 O3 4.66
Na2 O 3.40 Y 0.41
KNO3 7.00
Density, ! (g/cm3 ) 2.68 8.00 a
Fig. 4. DSC curves of the matrix glass powders (heating rate of 20 K/min).
Fig. 3. XRD patterns of the as-sintered E30M composite. (a) #-Ni/#% –Ni3 Al and (b)
NiCr2 O4 .
Table 2
Summary of measured mechanical properties (±std. dev.) of glass-matrix composites containing NiCrAlY platelets inclusions.
√
Weight fraction of NiCrAlY Young’s modulus (GPa) Fracture strength (MPa) Indentation toughness (MPa m) Vickers hardness (HV 0.5) Crack length (!m)
Fig. 6. Back-scattered electron micrographs showing the fracture surfaces of (A) PE, (B) E20M and (C) E30M along with the high magnification (D) of the rectangular zone in
(C).
crystallization (Tc ) from the matrix glass. It is higher than the firing ites agreed with the expected behavior from Hasselman’s model
temperature of the studied glass–NiCrAlY composites. There would [29,30], showing a critical temperature difference ("TC ), where
be crystallites apparently precipitated from the matrix glass only abrupt drop of fracture strength occurred. The curve for all the
after more than 10 h annealing at 850 ◦ C according to our previous tested materials presented the same "TC at about 200 ◦ C, while
woks [12]. the retained strength increased with alloy content: 9.6 MPa for
Combining the EDS line scans at the interface glass/NiCrAlY PE, 20.2 MPa for E10M, 25.1 MPa for E20M and 32.0 MPa for the
and XRD pattern of the composites, we conclude that the included E30M composite. The indentation-induced crack growth after ther-
NiCrAlY alloy was slightly oxidized to form nichromite on its sur- mal shock was presented in Fig. 5B. No obvious crack propagation
faces during sintering. By virtue of the high solubility of most oxides could be detected until the quenching temperatures increased up
in glass, this oxidation product dissolved and diffused in the matrix to a critical value where cracks propagated unstably. Unlike the
glass, markedly altering the glass compositions in front of the inter- results of quenching-strength test, NiCrAlY alloy inclusion elevated
face. the critical temperature differences from 150 ◦ C for NiCrAlY-free
glass to 225 ◦ C for 30 wt.% NiCrAlY-containing composites in the
indentation-quench tests.
3.2. Mechanical and thermal shock properties
Table 2 shows the measured values of the Young’s modulus 3.3. Fracture surface and microcrack–inclusion interactions
(E), fracture strength in bending (#), Vickers hardness (HV 0.5),
indentation toughness (KIC ) and the medial–radial crack length Fig. 6 shows the typical fracture surface of the monolithic glass
(c) of the composite samples. The Young’s modulus and fracture and glass–NiCrAlY composites. With increasing alloy content, the
toughness increased monotonically with alloy content, while Vick- roughness of the fracture surface increased. Few round pores of
ers hardness showed a complex trend: initially increased to an micron sizes, along with the pore-induced striations, could be
extremum (of 20 wt.% NiCrAlY alloy) then decreased slightly. For observed on the relatively flat fracture surface of PE (Fig. 6A), indi-
fracture strength, it followed a sharp drop as the alloy platelet was cating the fracture initiation sites. In cases of glass–NiCrAlY platelet
initially added then a slow increase with the alloy content. composites, ripples featured the fracture surfaces (Fig. 6B and C).
Fig. 5 shows the thermal shock behaviors of PE, compos- The retained alloy platelets, dispersed with various angles to the
ites E10M, E20M and E30M by using the quenching-strength fracture surface, demonstrated a firm bonding to the glass matrix
and indentation-quench tests. As shown in Fig. 5A, the strength and a complex inclusion–microcrack interaction mechanism. Two
responses of the monolithic glass and glass–NiCrAlY compos- ways of cracks propagation were observed. One was to deflect and
1364 M. Chen et al. / Materials Science and Engineering A 528 (2011) 1360–1366
Fig. 7. Back-scattered electron micrographs showing microcrack–inclusion interactions. Crack propagation direction was from left to right: (A) crack bridging and partially
debonding; (B) crack deflection and bridging; (C) fully debonding; (D) inclusion sectioned with limited plastic deformation.
pass through the glass matrix on intercepting a platelet vertical to aluminum and copper, the inherent ductility of which had been
the crack plane, as indicated by arrows in Fig. 6B, where crack front successfully exploited in glass matrix composites by plastic defor-
moved from bottom toward top. Another way was to run along mation, NiCrAlY alloy was of higher hardness (HV 387) and fracture
the interface and thus resulted in debonding of the platelet paral- strength values (550 MPa) [31], suggested more difficulty in defor-
lel to the crack plane, as indicated by arrows indicated in Fig. 6C. mation, therefore, less effect in toughening of brittle glasses. Big
Fig. 6D illustrates the detached interface at higher magnification. mismatches of CTE (coefficient of thermal expansion) and elastic
Some glass flakes could be observed still bonded on the platelet modulus between glass matrix and NiCrAlY inclusions (as shown
surfaces. No plastic deformation of platelet was found. in Table 1) would produce large internal stresses which steered
Fig. 7 shows four modes of crack–inclusion interactions behind the propagating cracks around the inclusions and again avoided
the crack tip after Vickers indenting. The first mode is bridging utilization of the inclusion ductility. Fig. 8 shows the circumfer-
of the propagating crack and partially debonding of the metallic ential cracks formed around platelet in the composite E30M after
inclusion, as indicated by arrow in Fig. 7A where the initial crack thermal shocked ("T = 300 ◦ C). Therefore, crack deflection, created
tip moved through the parent glass with a contact angle of about new crack surface as progressing, still not contributed substantially
61◦ to the elongated alloy platelet. Fig. 7B shows the second mode to the composites toughness. According to the theory proposed by
where the crack tip deflected in front of the inclusion and then cut Faber et al. [32], which demonstrated toughening by random spac-
through it. The third one is that cracks extended along the inter- ing platelet inclusions due to crack deflection, a maximal increase
face of glass/NiCrAlY and led to detachment of the NiCrAlY platelet in toughness of 80% is predicted for a 13 vol.% (here 30 wt.%) com-
from the glass matrix, as shown in Fig. 7C where the crack tip moved posite over that of the unreinforced matrix. The actual increase in
almost parallel to the interface. The fourth mode is the perfect inter- toughness found for this composite was 113%, larger than expected.
section of the NiCrAlY platelet, as shown in Fig. 7D where crack run This higher value, coupled with the more rapid increase in tough-
vertically to the platelet (especially of small particle size). ness over that of the modulus, indicated that additional toughening
mechanisms were involved, especially at higher alloy contents.
4. Discussion In fact, the composites were fired in a process that the tem-
peratures were elevated slowly from room temperature to the
Dense bulk composites of glass/NiCrAlY alloy platelet were designed firing point in air. The alloy platelet was initially oxidized
prepared by using pressureless sintering. Experimental results and nichromite was produced at the surface before the glass soft
revealed the benefits on composites fracture toughness with point. After that, glass melted and wetted the platelet followed by
increasing alloy content. Theoretically, compared to metals nickel, the dissolution and diffusion of nichromite into glass (as shown
M. Chen et al. / Materials Science and Engineering A 528 (2011) 1360–1366 1365
Table 3
Thermal shock resistance parameters of glass–NiCrAlY composites.
Quenching-strength Indentation-quench
the two parts combined: the thermal stress due to the sharp drop monotonically increased from 9.6 for PE to 32.0 MPa for E30M
of temperature and the following exterior stress due to the three- composite.
point bending. At "T < "TC , the thermal stress was not big enough
to initiate cracks, and the exterior stress causes the crack initiation Acknowledgements
and propagation to fracture. The increased temperature differ-
ences only decreased a little of the fracture strength. However at This project is financially supported by the Knowledge Inno-
"T ≥ "TC , the thermal stresses have been increased and become vation Program of the Chinese Academy of Sciences, grant no.
big enough for the initiation of cracks. So a much lower value of YYYJ-0912, and by National Natural Science Foundation of China,
exterior stress (here corresponded to the retained strength) could grant no. 50774074.
cause the already produced cracks to propagate unstably. By using
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