Low-Temperature Spark Plasma Sintering of ZrW2−xMoxO8 Exhibiting Controllable Negative Thermal Expansion
Abstract
:1. Introduction
2. Materials and Methods
3. Results and Discussion
3.1. Fabrication of Dense ZrW2−xMoxO8 Sintered Bodies
3.2. Evaluation of Thermal Expansion Properties of ZrW2−xMoxO8 Sintered Bodies
3.3. Rietveld Structure Refinement of ZrW2−xMoxO8 Compounds
4. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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Compound | x = 0.0 | x = 0.2 | x = 0.5 | x = 0.6 | x = 0.7 | x = 1.0 |
---|---|---|---|---|---|---|
Sintering temperature (°C) | 600 | 600 | 550 | 550 | 550 | 500 |
Density (g/cm3) | 4.6271 | 4.6832 | 4.4217 | 4.4855 | 4.2760 | 4.1689 |
Theoretical density (g/cm3) | 5.08 | 4.93 | 4.71 | 4.63 | 4.56 | 4.33 |
Relative density (%) | 91.0846 | 94.9939 | 93.8790 | 96.8790 | 93.7719 | 96.2794 |
Coefficient of Thermal Expansion (×10–6 °C−1) | Phase Transition Temperature (°C) | ||
---|---|---|---|
Compound | α Phase | β Phase | |
x = 0.0 | −7.85 (50–130 °C) | −3.22 (200–400 °C) | 170 |
x = 0.2 | −11.79 (50–130 °C) | −4.17 (200–400 °C) | 145 |
x = 0.5 | −15.34 (50–70 °C) | −3.16 (200–400 °C) | 78 |
x = 0.6 | −9.01 (50–70 °C) | −3.21 (200–400 °C) | 60 |
x = 0.7 | - | −2.91 (200–400 °C) | - |
x = 1.0 | - | −2.50 (200–400 °C) | - |
Temperature | Room Temperature | 300 °C | ||||
---|---|---|---|---|---|---|
Compound | ZrW2O8 | ZrW1.8Mo0.2O8 | ZrW1.5Mo0.5O8 | ZrW2O8 | ZrW1.8Mo0.2O8 | ZrW1.5Mo0.5O8 |
Goodness-of-fit (x2) | 1.776 | 6.993 | 3.983 | 1.375 | 2.928 | 3.194 |
Space Group | P 21 3 | P 21 3 | P 21 3 | P a | P a | P a |
Atom | Zr | Zr | Zr | Zr | Zr | Zr |
x = y = z | 0.000319 | 0.004534 | 0.002891 | 0.000000 | 0.000000 | 0.000000 |
Occupancy | 1 | 1 | 1 | 1 | 1 | 1 |
Atom | W1 | W(Mo)1 | W(Mo)1 | W1 | W(Mo)1 | W(Mo)1 |
x = y = z | 0.342614 | 0.343947 | 0.351651 | 0.340273 | 0.339711 | 0.338886 |
Occupancy | 1 | W1:0.9, Mo1:0.1 | W1:0.75, Mo1:0.25 | 0.5 | W1:0.45, Mo1:0.05 | W1:0.375, Mo1:0.125 |
Atom | W2 | W(Mo)2 | W(Mo)2 | W2 | W(Mo)2 | W(Mo)2 |
x = y = z | 0.601688 | 0.603332 | 0.608726 | 0.603304 | 0.605205 | 0.606212 |
Occupancy | 1 | W2:0.9, Mo2:0.1 | W2:0.75, Mo2:0.25 | 0.5 | W2:0.45, Mo2:0.05 | W2:0.375, Mo2:0.125 |
Atom | O1 | O1 | O1 | O1 | O1 | O1 |
x | 0.042345 | 0.021103 | 0.008577 | 0.050445 | 0.055887 | 0.05519 |
y | −0.19759 | −0.179137 | −0.183323 | −0.205553 | −0.201601 | −0.202851 |
z | −0.058376 | −0.066893 | −0.057469 | −0.069239 | −0.073105 | −0.0735229 |
Occupancy | 1 | 1 | 1 | 1 | 1 | 1 |
Atom | O2 | O2 | O2 | - | - | - |
x | 0.078837 | 0.094246 | 0.121337 | - | - | - |
y | −0.057928 | −0.071485 | −0.094012 | - | - | - |
z | 0.211437 | 0.221976 | 0.205825 | - | - | - |
Occupancy | 1 | 1 | 1 | - | - | - |
Atom | O3 | O3 | O3 | O3 | O3 | O3 |
x = y = z | 0.486051 | 0.479937 | 0.469176 | 0.509573 | 0.510211 | 0.512884 |
Occupancy | 1 | 1 | 1 | 0.5 | 0.5 | 0.5 |
Atom | O4 | O4 | O4 | O4 | O4 | O4 |
x = y = z | 0.250373 | 0.262464 | 0.262221 | 0.231004 | 0.228680 | 0.231430 |
Occupancy | 1 | 1 | 1 | 0.5 | 0.5 | 0.5 |
Compound | Calculated Coefficient of Thermal Expansion by Lattice Parameter (×10−6 °C−1) | |
---|---|---|
α Phase | β Phase | |
ZrW2O8 | −9.88 | −5.35 |
ZrW1.8Mo0.2O8 | −7.4 | −4.72 |
ZrW1.5Mo0.5O8 | - | −3.95 |
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Wei, H.; Hasegawa, M.; Mizutani, S.; Aimi, A.; Fujimoto, K.; Nishio, K. Low-Temperature Spark Plasma Sintering of ZrW2−xMoxO8 Exhibiting Controllable Negative Thermal Expansion. Materials 2018, 11, 1582. https://doi.org/10.3390/ma11091582
Wei H, Hasegawa M, Mizutani S, Aimi A, Fujimoto K, Nishio K. Low-Temperature Spark Plasma Sintering of ZrW2−xMoxO8 Exhibiting Controllable Negative Thermal Expansion. Materials. 2018; 11(9):1582. https://doi.org/10.3390/ma11091582
Chicago/Turabian StyleWei, Hui, Marin Hasegawa, Shunsuke Mizutani, Akihisa Aimi, Kenjiro Fujimoto, and Keishi Nishio. 2018. "Low-Temperature Spark Plasma Sintering of ZrW2−xMoxO8 Exhibiting Controllable Negative Thermal Expansion" Materials 11, no. 9: 1582. https://doi.org/10.3390/ma11091582