Adjustable Thermal Expansion Properties in Zr2MoP2O12/ZrO2 Ceramic Composites

Zr₂MoP₂O₁₂/ZrO₂ composites were successfully synthesized by the solid state method in attempt to fabricate the near-zero thermal expansion ceramics. The phase composition, micromorphology and thermal expansion behavior of the Zr₂MoP₂O₁₂/ZrO₂ composites with different mass ratios were investigated using X-ray diffraction, scanning electron microscopy and thermal mechanical analysis. Results indicate that Zr₂MoP₂O₁₂/ZrO₂ composites can be prepared by pre-sintering at 500°C for 3 h and then sintering at 1050°C for 6 h. The resulting Zr₂MoP₂O₁₂/ZrO₂ composites consisted of orthorhombic Zr₂MoP₂O₁₂ and monoclinic ZrO₂. With increasing content of Zr₂MoP₂O₁₂, the Zr₂MoP₂O₁₂/ZrO₂ ceramics became more compact and the coefficient of thermal expansion decreased gradually. Zr₂MoP₂O₁₂/ZrO₂ composites show an adjustable coefficient of thermal expansion (CTE) from 5.57 × 10⁻⁶ K⁻¹ to −5.73 × 10⁻⁶ K⁻¹ by changing the mass ratio of Zr₂MoP₂O₁₂ and ZrO₂. The Zr₂MoP₂O₁₂/ZrO₂ composite with a mass ratio of 2:1 showed near zero thermal expansion, and the average linear thermal expansion coefficient is measured to be 0.0065 × 10⁻⁶ K⁻¹ in the temperature range from 25 to 700°C.

Introduction

It is well known that the vast majority of materials expand on heating. However, some materials shrink as the temperature rises and display negative thermal expansion (NTE). NTE materials have attracted considerable attention due to the anomalous phenomenon and their potential application in controlled thermal expansion composites and other areas (Chen et al., 2015). Control of thermal expansion is crucial to many applications. Mismatch of thermal expansion in component materials of high-precision device may result in serious problems, such as mechanical destruction and positional deviation. An easy method to prepare the material with near-zero or low thermal expansion is combining NTE materials with positive thermal expansion materials (Liu et al.2012; 2012a; Gao et al., 2016; Zhang et al., 2017). Materials displaying zero or low thermal expansion are both dimensionally stable and highly resistant to thermal shock.

The longtime leading NTE exemplar was ZrW₂O₈. Cubic ZrW₂O₈ exhibits strong isotropic NTE over a wide temperature range (Mary et al., 1996; Nishiiyama et al., 2006; Kanamori et al., 2008; Banek et al., 2010; Liu et al., 2011, 2012b). With the goal of thermal expansion control, several studies of the composites containing ZrW₂O₈ have been reported, such as ZrW₂O₈/ZrO₂ (Lommens et al., 2005; Yang et al., 2007), ZrW₂O₈/Cu (Yilmaz, 2002), ZrW₂O₈/Al (Wu et al., 2013), ZrW₂O₈/cement (Kofteros et al., 2001), ZrW₂O₈/PI, and ZrW₂O₈/epoxy (Sullivan and Lukehart, 2005; Yang et al., 2010). The thermal expansion coefficient of composites can be effectively controlled by using ZrW₂O₈ as NTE filler, however, the cubic ZrW₂O₈ is metastable at room temperature and needs to be quenched after sintering at 1200°C. Meanwhile, ZrW₂O₈ undergoes a structural phase transition from α -ZrW₂O₈ to β -ZrW₂O₈ at around 160°C and the coefficient of thermal expansion will decrease from about −8.8 × 10⁻⁶ K⁻¹ to −4.9 × 10⁻⁶ K⁻¹. In addition, when ZrW₂O₈ was heated to about 740°C in air, it will decompose into ZrO₂ and WO₃ (Mary et al., 1996; Nishiiyama et al., 2006; Kanamori et al., 2008; Banek et al., 2010; Liu et al., 2011, 2012b). Quenching, thermal decomposition and the abrupt change of thermal expansion are disadvantageous for composite design.

Orthorhombic Zr₂MoP₂O₁₂, a member of A₂M₃O₁₂ family, has received widespread attention in recent years. It shows stable NTE and its average linear expansion coefficient is −4.5 × 10⁻⁶ K⁻¹ over a broad temperature range from −264 to 1050°C. What's more, it overcomes all the limitations of ZrW₂O₈ discussed above, suggesting its potential use for fabricating near-zero or low thermal expansion materials (Cetinkol et al., 2009; Isobe et al., 2016). ZrO₂ ceramics has been widely used in optical, electrical and high temperature fields. The average linear thermal expansion coefficient of ZrO₂ is about 10 × 10⁻⁶ K⁻¹(Lommens et al., 2005; Yang et al., 2007). The absolute values of thermal expansion coefficient of ZrO₂ and Zr₂MoP₂O₁₂ are thus similar but have opposite signs, suggesting that these materials are good candidates for the preparation of ceramic composites with tunable CTEs. In this work, a new series of Zr₂MoP₂O₁₂/ZrO₂ composites were synthesized by solid state method with the goal of tailoring the thermal expansion. The effects of mass ratio between Zr₂MoP₂O₁₂ and ZrO₂ on the phase composition, microstructure, and thermal expansion coefficient of the Zr₂MoP₂O₁₂/ZrO₂ ceramic composites were also investigated.

Experimental

Sample Preparation

Zr₂MoP₂O₁₂, ZrO₂, and Zr₂MoP₂O₁₂/ZrO₂ composites (mass ratios: 1:2, 1:1, 2:1) were prepared using stoichiometric amounts of ZrO₂ (purity ≥99.95%, metals basis), MoO₃ (purity ≥99.99%, metals basis), and NH₄H₂PO₄ (purity ≥99.5%, metals basis). A summary of samples prepared can be found in Table 1. The starting compounds were mixed in ethanol using ball milling for 6 h to form a uniform mixture and dried at 80°C, then the mixtures were pre-heated at 500°C for 3 h. The mixtures, under 50 MPa, were cold pressed into pellets which were 7 mm in diameter and about 2 mm in thickness. Finally, the pellets were calcined at 1050°C in air for 6 h and cooled down in the furnace. In the solid-state synthesis, the following reactions may take place:

$\begin{array}{cc}\begin{array}{l}{\text{ZrO}}_2+{\text{MoO}}_3+{\text{2NH}}_4{\text{H}}_2{\text{PO}}_4\to {\text{ZrP}}_2{\text{O}}_7+{\text{2NH}}_3\uparrow \\ +{\text{3H}}_2\text{O}+{\text{MoO}}_3({500}^{°}\text{C})\end{array}& (1)\end{array}$

$\begin{array}{cc}{\text{ZrO}}_2+{\text{MoO}}_3+{\text{ZrP}}_2{\text{O}}_7\to {\text{Zr}}_2{\text{MoP}}_2{\text{O}}_{12}({1050}^{°}\text{C})& (2)\end{array}$

$\begin{array}{cc}\begin{array}{l}\text{Or}:(1+\text{x}){\text{ZrO}}_2+{\text{MoO}}_3+{\text{ZrP}}_2{\text{O}}_7\to {\text{Zr}}_2{\text{MoP}}_2{O}_{12}\\ +{\text{xZrO}}_2({1050}^{°}\text{C})\end{array}& (3)\end{array}$

TABLE 1

Table 1. Synthesis conditions for ZrO₂, Zr₂MoP₂O₁₂, and Zr₂MoP₂O₁₂/ZrO₂ ceramics.

In this work, the 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite was also prepared using the pure Zr₂MoP₂O₁₂ and ZrO₂ as raw materials, and the synthetic process is the same as that of the above process.

Experimental Techniques

Identification of the different phases presented in the samples was performed using powder X-ray diffraction (PXRD) on a Shimadzu XRD 7000 with Cu Ka radiation. Data were collected at 40 kV and 35 mA, with a scanning speed of 5°/min over an angular range of 10–60°. The micromorphologies of the samples were observed using a scanning electron microscopy (SEM, TESCAN VEGA3). The elemental composition of the samples were analyzed using energy-dispersive X-ray spectrometry (EDX, Bruker XFlash 6160) as well.The CTEs of the samples were measured by thermal mechanical analyzer (TMA/SS, Seiko 6300) using a heating rate of 5°C/min from room temperature to 700°C in air.

Results and Discussion

XRD Analysis

Figure 1 shows typical XRD patterns of the Zr₂MoP₂O₁₂/ZrO₂ (mass ratios 1:2, 1:1, and 2:1) composites in addition to those of the pure Zr₂MoP₂O₁₂ and ZrO₂ ceramics obtained under the same preparation condition. Figure 1a shows typical powder XRD pattern of pure ZrO₂ ceramics sintered at 1050°C for 6 h, all the observed reflections could be well indexed and attributed to monoclinic ZrO₂ in agreement with JCPDS card number 65–1,023. The typical powder XRD pattern of pure Zr₂MoP₂O₁₂ specimen sintered at 1050°C for 6 h is shown in Figure 1e, all diffraction peaks match those expected for orthorhombic Zr₂MoP₂O₁₂, which agrees with literature reports (Cetinkol et al., 2009; Isobe et al., 2016). No impurity phases were detected, confirming the purity of the two products. The PXRD patterns of the Zr₂MoP₂O₁₂/ZrO₂ (mass ratio: 1:2, 1:1, and 2:1) composites were shown in Figures 1b–d, it can be seen that all the diffraction peaks of the specimens could be indexed as both monoclinic ZrO₂ and orthorhombic Zr₂MoP₂O₁₂. With increasing mass ratio of Zr₂MoP₂O₁₂, the intensity of diffraction peaks of Zr₂MoP₂O₁₂ become much stronger. The diffraction peaks of both ZrO₂ and Zr₂MoP₂O₁₂ were sharp and intense, indicating their highly crystalline nature.

FIGURE 1

Figure 1. XRD patterns of the obtained ZrO₂ ceramics, Zr₂MoP₂O₁₂ ceramics and Zr₂MoP₂O₁₂/ZrO₂ composites with different mass ratios sintered at 1050°C for 6 h.

To investigate whether a chemical reaction occurred between ZrO₂ and Zr₂MoP₂O₁₂ during sintering at 1050°C. The 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite was also prepared using the pure Zr₂MoP₂O₁₂ and ZrO₂ as raw materials. The Zr₂MoP₂O₁₂ was mixed with ZrO₂ at a mass ratio of 2:1 and finally calcined at 1050°C in air for 6 h. The XRD patterns of the ZrO₂, Zr₂MoP₂O₁₂, and 2:1 Zr₂MoP₂O₁₂/ZrO₂ were shown in Figure 2. Except for monoclinic ZrO₂ and orthorhombic Zr₂MoP₂O₁₂, no new peaks were detected, confirming that no chemical reaction occurred between ZrO₂ and Zr₂MoP₂O₁₂ during sintering at 1050°C.

FIGURE 2

Figure 2. XRD patterns of the obtained 2:1 Zr₂MoP₂O₁₂/ZrO₂ composites sintered at 1050°C for 6 h using the Zr₂MoP₂O₁₂ and ZrO₂ as raw materials, and the XRD patterns of pure Zr₂MoP₂O₁₂ and ZrO₂ were also given for reference.

SEM Images and Density Analysis

Further study was carried out by the SEM analysis to identify microstructures of as-prepared Zr₂MoP₂O₁₂, ZrO₂, and Zr₂MoP₂O₁₂/ZrO₂ composites. Figure 3 shows SEM images of fracture surfaces of the pure ZrO₂, pure Zr₂MoP₂O₁₂ sintered bodies, and the Zr₂MoP₂O₁₂/ZrO₂ composites fabricated with different mass ratio of 1:2, 1:1, and 2:1. As shown in Figure 3a, as-prepared ZrO₂ ceramics sintered at 1050°C is not compact and the ZrO₂ grain growth is not observed obviously due to the insufficient sintering. The SEM images of the Zr₂MoP₂O₁₂/ZrO₂ composites fabricated at different mass ratio of 1:2, 1:1, and 2:1 are shown in Figures 3b–d. It can be seen that the Zr₂MoP₂O₁₂/ZrO₂ composites show nearly the same SEM images of fracture surfaces, which consist of irregular grains and some pores. With increasing content of Zr₂MoP₂O₁₂, Zr₂MoP₂O₁₂/ZrO₂ ceramics became denser and displayed larger particle sizes and less porosity, suggesting that the increase of Zr₂MoP₂O₁₂ slightly promoted the particle growth and increased the density of the Zr₂MoP₂O₁₂/ZrO₂ ceramics. Figure 3e shows the SEM images of fracture surfaces of the obtained pure Zr₂MoP₂O₁₂ ceramics. The Zr₂MoP₂O₁₂ sintered body was denser compared with the ZrO₂ ceramics fabricated at same sintering temperature. It is compact, which is in agreement with the results reported earlier (Cetinkol et al., 2009; Isobe et al., 2016). The elemental composition and distribution of 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite was also investigated using the EDX. The distribution of zirconium, oxygen, phosphorus, molybdenum is shown in Figures 3f–j.

FIGURE 3

Figure 3. SEM images of the obtained ZrO₂ ceramics, Zr₂MoP₂O₁₂ ceramics and Zr₂MoP₂O₁₂/ZrO₂ composites with different mass ratios sintered at 1050°C for 6 h. (a) ZrO₂ (b) Zr₂MoP₂O₁₂:ZrO₂ = 1:2 (c) Zr₂MoP₂O₁₂:ZrO₂ = 1:1 (d) Zr₂MoP₂O₁₂:ZrO₂ = 2:1 (e) Zr₂MoP₂O₁₂ (f) overlaid with elemental analysis results of 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite using EDX (g–j) distribution of zirconium, oxygen, phosphorus, molybdenum elements in the selected area.

Thermal Expansion Properties

For a better analysis of the thermal expansion behaviors of the composites, Figure 4A shows the thermal expansion curves of the Zr₂MoP₂O₁₂/ZrO₂ composites with different mass ratio calcined at 1050°C for 6 h. The thermal expansion curves of the pure Zr₂MoP₂O₁₂ and pure ZrO₂ ceramics are also given for reference. As shown in Figures 4A–a, Pure ZrO₂ specimen shows positive thermal expansion in the testing temperature from 25 to 700°C with an average linear thermal expansion coefficient of 5.57 × 10⁻⁶ K⁻¹, which agrees with literature reports (Lommens et al., 2005; Yang et al., 2007). In Figures 4A-e, it can be seen that pure Zr₂MoP₂O₁₂ ceramics showed strong negative thermal expansion. Its average linear thermal expansion coefficient was measured to be −5.73 × 10⁻⁶ K⁻¹ in the testing temperature range of 25–700°C. It can be found that the thermal expansion curves of the obtained samples except pure Zr₂MoP₂O₁₂ ceramics overlap below 200°C, this abnormal behavior in the beginning of thermal expansion curves may be caused by the instrument. Above 200°C, all the samples show stable and almost linear change in the curves of thermal expansion with the increased temperature. Based on the above SEM analysis, the compact microstructure of the composites will promotes the stability of thermal expansion performance. Average linear thermal expansion coefficients of the obtained pure ZrO₂, pure Zr₂MoP₂O₁₂, and Zr₂MoP₂O₁₂/ZrO₂ composites with different mass ratios are summarized in Table 2. With increasing content of Zr₂MoP₂O₁₂, the thermal expansion coefficient of Zr₂MoP₂O₁₂/ZrO₂ composite decreased gradually. The 1:2 Zr₂MoP₂O₁₂/ZrO₂ composite showed positive thermal expansion with a thermal expansion coefficient of 2.30 × 10⁻⁶ K⁻¹. When the mass ratio of Zr₂MoP₂O₁₂/ZrO₂ decreased to 1:1, the composite also exhibited positive thermal expansion, but the CTE value decreased to 1.14 × 10⁻⁶ K⁻¹. The 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite showed very low thermal expansion with an average linear thermal expansion coefficient of 0.0082 × 10⁻⁶ K⁻¹ in the temperature range of 25–700°C. Figure 4B shows the cyclic thermal expansion curves of the Zr₂MoP₂O₁₂/ZrO₂ composites. The two thermal expansion curves are almost the same, and the second average linear thermal expansion coefficient was test to be 0.0049 × 10⁻⁶ K⁻¹ in the same temperature range, indicating the 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite shows a stable thermal expansion property and the mass ratio of 2:1 (Zr₂MoP₂O₁₂/ZrO₂) is appropriate one. With the increase of the temperature, the volume shrinkage of the NTE Zr₂MoP₂O₁₂ just can accommodate the volume expansion of ZrO₂, which will keep a little change of the volume value of the 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite. This near-zero expansion ceramic composite can withstand thermal stresses arising during sintering and subsequent quenching, which is an important criterion for a number of potential application in many fields. The results suggest that the thermal expansion coefficients of Zr₂MoP₂O₁₂/ZrO₂ composites can be tailored from 5.57 × 10⁻⁶ K⁻¹ to −5.73 × 10⁻⁶ K⁻¹ by adjusting the weight fraction of Zr₂MoP₂O₁₂. Figure 5 shows the relation between coefficients of thermal expansion and the mass ratio of the Zr₂MoP₂O₁₂/ZrO₂ composites sintered at 1050°C for 6 h. The points is the data measured in the work. There is no linear relationship between the coefficients of thermal expansion and the mass ratio of the Zr₂MoP₂O₁₂/ZrO₂ composites. The red line is the best-fit line. According to the fitting equation, when the mass ration of Zr₂MoP₂O₁₂/ZrO₂ is 0.57, the Zr₂MoP₂O₁₂/ZrO₂ composite show zero thermal expansion. This fitting result deviates from the data obtained in the experiment. When the mass ration of Zr₂MoP₂O₁₂/ZrO₂ is 0.67, the near-zero thermal expansion Zr₂MoP₂O₁₂/ZrO₂ composite was obtained. This deviation mainly caused by the defects in the composites, such as pores and microcracks.

FIGURE 4

Figure 4. (A)Thermal expansion curves of the obtained ZrO₂ ceramics, Zr₂MoP₂O₁₂ ceramics and Zr₂MoP₂O₁₂/ZrO₂ composites with different mass rati006Fs sintered at 1050°C for 6 h. (a) ZrO₂ (b) Zr₂MoP₂O₁₂:ZrO₂ = 1:2 (c) Zr₂MoP₂O₁₂:ZrO₂ = 1:1 (d) Zr₂MoP₂O₁₂:ZrO₂ = 2:1 (e) Zr₂MoP₂O₁₂. (B) Cyclic thermal expansion curves of the 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite.

TABLE 2

Table 2. Average linear thermal expansion coefficients of ZrO₂ ceramics, Zr₂MoP₂O₁₂ ceramics, and Zr₂MoP₂O₁₂/ZrO₂ composites with different mass ratios in corresponding testing temperature range from 25 to 700°C.

FIGURE 5

Figure 5. Relation between coefficients of thermal expansion and the mass ratio of the Zr₂MoP₂O₁₂/ZrO₂ composites sintered at 1050°C for 6 h.

Conclusions

With the goal of thermal expansion control, NTE Zr₂MoP₂O₁₂ was combined with the positive thermal expansion ZrO₂ to fabricate the composites with a tailorable thermal expansion. The obtained Zr₂MoP₂O₁₂/ZrO₂ composites synthesized at 1050°C for 6 h were composed of orthorhombic Zr₂MoP₂O₁₂ and monoclinic ZrO₂, no intermediate phase was observed. With increasing content of Zr₂MoP₂O₁₂, the thermal expansion coefficient of Zr₂MoP₂O₁₂/ZrO₂ composite decreased while the density of the composite increased gradually. The thermal expansion coefficients of the Zr₂MoP₂O₁₂/ZrO₂ composites can be tailored from 5.57 × 10⁻⁶ K⁻¹ to −5.73 × 10⁻⁶ K⁻¹ by changing the weight fraction of Zr₂MoP₂O₁₂. In addition, the 2:1 Zr₂MoP₂O₁₂/ZrO₂ composite displayed near-zero thermal expansion with an average linear thermal expansion coefficient of 0.0065 × 10⁻⁶ K⁻¹ in the testing temperature range of 25–700°C. This near-zero thermal expansion material will have a number of potential application in many fields due to its dimensional stability and high resistance to thermal shock.

Author Contributions

HL and ZZ designed experiments. WS, XX, and LY carried out experiments. HL, ZZ, XZ, MZ, and XC analyzed experimental results. HL and ZZ wrote the manuscript.

Conflict of Interest Statement

The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Acknowledgments

The authors thank the National Natural Science Foundation of China (No.51602280 and No.51102207), Qing Lan Project of Jiangsu Province, Guangling College of Yangzhou University Natural Science Research Foundation (ZKZD17001). Yangzhou University Science and Technique Innovation Foundation (No.2015CJX007).

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