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Zeli Jia, Xiaomeng Fan, Jiangyi He, Jimei Xue, Fang Ye, and Laifei Cheng, Evolution of microstructure and electromagnetic interference shielding performance during the ZrC precursor thermal decomposition process, Int. J. Miner. Metall. Mater., 30(2023), No. 7, pp.1398-1406. https://dx.doi.org/10.1007/s12613-023-2619-4
Cite this article as: Zeli Jia, Xiaomeng Fan, Jiangyi He, Jimei Xue, Fang Ye, and Laifei Cheng, Evolution of microstructure and electromagnetic interference shielding performance during the ZrC precursor thermal decomposition process, Int. J. Miner. Metall. Mater., 30(2023), No. 7, pp.1398-1406. https://dx.doi.org/10.1007/s12613-023-2619-4
Research Article

Evolution of microstructure and electromagnetic interference shielding performance during the ZrC precursor thermal decomposition process

Author Affilications
  • Corresponding author:

    Xiaomeng Fan      E-mail: fanxiaomeng@nwpu.edu.cn

  • A polymer-derived ZrC ceramic with excellent electromagnetic interference (EMI) shielding performance was developed to meet ultra-high temperature requirements. The thermal decomposition process of ZrC organic precursor was studied to reveal the evolution of phase composition, microstructure, and EMI shielding performance. Furthermore, the carbothermal reduction reaction occurred at 1300°C, and the transition from ZrO2 to ZrC was completed at 1700°C. With the increase in the annealing temperature, the tetragonal zirconia gradually transformed into monoclinic zirconia, and the transition was completed at the annealing temperature of 1500°C due to the consumption of a large amount of the carbon phase. The average total shielding effectiveness values were 11.63, 22.67, 22.91, 22.81, and 34.73 dB when the polymer-derived ZrC was annealed at 900, 1100, 1300, 1500, and 1700°C, respectively. During the thermal decomposition process, the graphitization degree and phase distribution of free carbon played a dominant role in the shielding performance. The typical core–shell structure composed of carbon and ZrC can be formed at the annealing temperature of 1700°C, which results in excellent shielding performance.
  • In recent years, high-temperature electromagnetic interference (EMI) shielding materials have emerged as one of the most promising frontier research areas in the aerospace industry [19]. Polymer-derived ceramics (PDCs) show great potential for applications at high temperature because of their excellent oxidation resistance and high-temperature creep resistance [1013]. The most ceramics prepared by the PDCs method are silicon-based ceramics, such as SiCN, SiC, SiOC, etc. Jia et al. [2] annealed the carbon–silicon carbide (C–SiC) solid solution above 1700°C, and the average total shielding effectiveness (SET) per unit thickness was higher than 20 dB·mm−1. Li et al. [14] fabricated C–SiC nanocomposites with a carbon mass percentage of 7.6wt%, and the EMI shielding effectiveness (SE) was 36.8 dB at room temperature and 33.8 dB at 600°C, respectively, indicating high and stable EMI SE values at room and high temperature in the air. Liu et al. [15] annealed SiC–Si3N4 ceramics from 1100 to 1400°C in an argon (Ar) atmosphere, and the EMI SE was able to reach 35 dB. Si-based ceramics cannot meet the requirement for applications above 1700°C due to active oxidation [1618].

    Ultra-high temperature ceramics can be used above 1700°C to solve the problem of the active oxidation of SiC [3,1921]. Zirconium carbide (ZrC) has attracted considerable attention because of its high melting point (3450°C), high hardness, and good thermal shock resistance [22]. Jia et al. [11] added ZrB2 particles into PDCs–SiOC, and an EMI SE of 72 dB in the Ka-band can be obtained. ZrC can be prepared by the PDC method, which has been employed to improve the ablation resistance. However, the EMI shielding performance of Zr-based ceramics prepared by PDCs is rarely observed.

    During the polymer-to-ZrC ceramic derivation process, a carbothermal reduction reaction occurs to form ZrC, and different product compositions lead to various electromagnetic response characteristics of the as-obtained ceramics, which have rarely been reported in previous studies. Related studies must be carried out to reveal the evolution of the EMI shielding performance in the derivation process. The evolutions of phase composition, microstructure, and EMI shielding properties of PDCs–ZrC ceramics annealed from 900 to 1700°C were explored in this work. Furthermore, the relationship between the microstructure and EMI shielding properties was revealed.

    The ZrC ceramic organic precursor (Institute of Process Engineering, Chinese Academy of Sciences, China) was employed in this work. For the preparation of ceramic samples, the as-received liquid-phase ceramic precursor was cross-linked at 200°C for 2 h and then pyrolyzed at 900°C for 2 h under an Ar atmosphere. The as-obtained products were grounded to powder with an average size of ~0.1 mm and then cold-pressed into green bodies with dimensions of 30 mm × 15 mm × 3 mm under a pressure of 20 MPa. Finally, the green bodies were annealed at 1100, 1300, 1500, and 1700°C for 2 h at a heating rate of 5°C·min−1 under Ar atmosphere. For convenience, the samples were designated as S900, S1100, S1300, S1500, and S1700, where the numbers corresponded to the annealing temperature.

    The cross-linked products were characterized by Fourier transform infrared spectroscopy (FT-IR, IRTracer-100, Shimadzu, Japan). The phase composition was analyzed by X-ray diffraction (XRD, X'Pert Pro, Philips, Netherlands). The density and open porosity were measured by the Archimedes method in accordance with the ASTM C-20 standard. The thermal analysis for liquid-phase precursor was carried out on thermal gravimetry (TG)–differential scanning calorimetry equipment (DSC, Netzsch STA 449F3, Germany) under Ar atmosphere at a heating rate of 10°C·min−1. The chemical state was investigated by X-ray photoelectron spectroscopy (XPS, Axis Supra, UK). The state of carbon was investigated by Raman spectroscopy (Alpha300R, WITech, Germany). The proportions of Zr, O, and C atoms were tested by inductively coupled plasma-atomic emission spectroscopy/mass spectrometry (ICP-AES/MS, 7800(MS), Agilent, America), inorganic carbon sulfur test (COREY-200, Instrumentation equipment, China), and inorganic oxygen, nitrogen, and hydrogen tests (TC500, LECO, America). The microstructure was observed by scanning electron microscopy (SEM, Helios G4 CX, FEI, America) and transmission electron microscopy (TEM, Themis Z, FEI, America).

    The scattering parameters (S-parameters) of all batches of samples (dimensions of 22.86 mm × 10.16 mm × 3 mm) in the frequency range of 8.2–12.4 GHz (X-band) were recorded using a vector network analyzer (MS4644A, Anritsu).

    Fig. 1(a) shows the FT-IR spectra of the as-cured product. The stretching vibration band at 2935 cm−1 and the deformation band at 1452 cm−1 were attributed to the C–H group [23]. The C=C vibrational absorption peak at 1594 cm−1 corresponded to the acetylacetonate enol ligand of the conjugated system formed by zirconium atoms. The transmission peak at 1022 cm−1 was generated by the C–O stretching vibration in the Zr–O–C bond [24].

    Fig. 1.  (a) FT-IR spectra of the as-cured product and (b) TG of the as-cured product.

    Fig. 1(b) shows the TG results (from room temperature to 1500°C; heating rate of 10°C·min−1, Ar gas) of the as-cured product. The variation trend of weight loss can be divided into three stages. The first stage was from room temperature to 600°C, in which the breakage and rearrangement of the organic groups of the precursor molecules and the release of small molecular gases resulted in a rapid weight loss of 54.7wt% [24]. The second stage, which occurred from 600 to 1100°C, showed the ease in weight loss resulting from the breakage of small molecules. The third stage occurred from 1100 to 1500°C and involves a weight loss of 10.9wt%, which can be attributed to the carbothermal reduction reaction. When the temperature rises to 1500°C, the yield of the as-cured product is 32wt%.

    Fig. 2 shows the XRD patterns of all the annealed samples. For samples S900 and S1100, two types of ZrO2 phases can be detected, namely, tetragonal ZrO2 (t-ZrO2) and monoclinic ZrO2 (m-ZrO2). For sample S1300, with the exception of t-ZrO2 and m-ZrO2, a small amount of ZrC appearred, indicating the occurrence of a carbothermal reduction reaction. For sample S1500, the diffraction peak intensity of ZrC increased, implying the precipitation of a large amount of ZrC. When the annealing temperature increased to 1700°C, only ZrC was presented, indicating the complete transition from ZrO2 to ZrC.

    Fig. 2.  XRD patterns of all the annealed samples.

    The diameter of ZrO2 nanoparticles can be calculated by the Debye–Scherrer equation:

    D=kλβcosθ
    (1)

    where D is the average crystallite thickness perpendicular to the lattice plane, k is Scherrer’s constant (0.89), β is the angular line width at half maximum intensity in radians, λ is the wavelength of the X-ray (0.154056 nm), and θ is the diffraction angle. The (ˉ111)lattice plane of m-ZrO2 and (111) lattice plane of t-ZrO2 were selected to calculate the size of t-ZrO2 and m-ZrO2 nanocrystals, respectively [25]. When the annealing temperature increased from 900 to 1700°C, the average grain size of m-ZrO2 and t-ZrO2 increased from 5.54 to 8.88 nm and 2.07 to 2.90 nm, respectively, as shown in Table 1.

    Table  1.  Calculated crystal size and Raman parameters of all samples
    SampleDm-ZrO2 / nmDt-ZrO2 / nmID/IG
    S9005.542.071.73
    S11006.213.151.44
    S13005.813.141.20
    S15008.882.901.43
    S17001.42
     | Show Table
    DownLoad: CSV

    Fig. 3 shows the Raman spectra of all the samples. The appearance of typical D and G peaks indicated the existence of free carbon. The value of ID/IG corresponds to the number of defects and structural ordering in carbon. As listed in Table 1, the ID/IG ratio decreased from 1.73 to 1.20 when the annealing temperature increased from 900 to 1300°C, then, it increased to 1.42 for the sample S1700. For samples S900, S1100, and S1300, the D peak was stronger than the G peak, which indicated the poor graphitization structure of free carbon. According to Ferrari and Robertson’s three-stage model [2627], the graphitization degree increased with the increasing temperature, leading to the decreasing ID/IG ratio. The carbothermal reduction reaction began when the annealing temperature rises beyond 1300°C, the amount of carbon gradually decreases, resulting in inconspicuous D and G peaks. In addition, the increase in the ID/IG ratio indicated that a large number of defects were generated in the carbon during the carbothermal reduction reaction, which is consistent with the reported findings [28].

    Fig. 3.  Raman analysis of all samples.

    Fig. 4 shows the density and open porosity of the as-prepared samples. As the annealing temperature increased, the density decreased from 2.86 to 1.35 g·cm−3, while the open porosity increased from 31vol% to 73vol%. The variation of open porosity can be divided into three stages. The first stage involved the increase in open porosity for samples S900 and S1100 resulting from the phase transition of ZrO2. In the second stage, the carbothermal reduction reaction started as the annealing temperature increased beyond 1300°C, subsequently releasing CO and leading to the increase in open porosity. Finally, as the annealing temperature increased to 1700°C, the density decreased and the open porosity increased, which results in the complete transition from ZrO2 to ZrC.

    Fig. 4.  Density and open porosity of all samples.

    Fig. 5(a) illustrates the XPS spectrum of all samples. The as-obtained ceramics were composed of Zr, C, and O. When the annealing temperature is lower than 1500°C, as the annealing temperature increased, the intensity of the C 1s peaks decreased, indicating the decrease in its relative content. As shown in Fig. 5(b), the two peaks with binding energy of 182.7 and 184.5 eV corresponded to the Zr–O bonds in ZrO2. The intensity of the Zr–O bond decreased and then increased with the increasing annealing temperature. Moreover, the appearance of the Zr–O peak at 180.2 eV indicated the carbon doping of ZrO2, which was marked as Zr(O,C) in Fig. 5(b). As shown in Fig. 5(c), the peak with a binding energy of 284.6 eV corresponded to the C–C bond, while the peaks at 281 eV corresponding to the Zr–C bond [29]. When the annealing temperature is higher than 1300°C, the intensity of the C–C bond peak decreased, and the Zr–C bond peak increased, corresponding to the consumption of the carbon phase and the increase in the ZrC phase by carbothermal reduction reaction.

    Fig. 5.  XPS analysis spectrum of all samples: (a) wide spectrum; (b) Zr 3d, (c) C 1s; (d) element proportion of all the samples measured by ICP-AES, inorganic carbon sulfur, and inorganic oxygen, nitrogen, and hydrogen tests.

    Fig. 5(d) shows the proportion of Zr, O, and C atoms of all the samples (measured by ICP, inorganic carbon sulfur and inorganic oxygen, nitrogen, and hydrogen tests). As the annealing temperature increased, the proportion of the Zr atom increased, and those of the C and O atoms decreased. The variation trend become obvious when the annealing temperature is above 1300°C, resulting from the carbothermal reduction reaction.

    ZrO2 has three crystal forms, including monoclinic (m-ZrO2), tetragonal (t-ZrO2), and cubic (c-ZrO2), and their transition temperature are 1000 and 2370°C, respectively. Usually, only m-ZrO2 can be found at room temperature, whereas t-ZrO2 is still present at room temperature in this work. The retainment of t-ZrO2 at room temperature can be explained by various models, size effect mechanisms, and doping mechanisms [30]. According to thermodynamic calculations, crystal size of less than 30 nm resulted in the stabilization of t-ZrO2 [31]. As listed in Table 1, the average crystal size of t-ZrO2 was ~3 nm, which can play the stabilization role. Moreover, amorphous carbon can play the doping effect to stabilize the t-ZrO2 crystal [30,32]. Thus, amorphous carbon inhibits the phase transition from t-ZrO2 to m-ZrO2 in the cooling process.

    As shown in Fig. 6(a–b), S900 and S1100 showed the typical agglomerated morphology, which was formed by stacking powder. Further increase in the annealing temperature led to the formation of particles with sharp edges, corresponding to the precipitation of ZrC (Fig. 6(c)). With the precipitation of a large amount of ZrC, two types of particles can be observed (Fig. 6(d)). According to energy dispersive spectroscopy (EDS), the spherical particles were ZrO2, and the conical ones were ZrC, as shown in Table 2. When the annealing temperature increased to 1700°C, the skeletal structure composed of ZrC can be observed (Fig. 6(e)).

    Fig. 6.  SEM images of all samples: (a) S900; (b) S1100; (c) S1300; (d) S1500; (e) S1700.
    Table  2.  EDS analysis of sample S1500 wt%
    Position in Fig. 6(d)ZrOC
    Point 176.375.0518.58
    Point 276.729.1114.17
    Point 368.8710.7921.35
     | Show Table
    DownLoad: CSV

    As shown in Fig. 7(a), two types of ZrO2 crystal and amorphous carbon can be observed. However, the increasing annealing temperature led to a rapid decline in the amorphous phase (Fig. 7(b)). The boundary of ZrO2 was very clear, and the two phases of ZrO2 showed staggered and adjacent morphology, and amorphous carbon was distributed around the ZrO2 particles in a slice-like structure (Fig. 7(a–d)). For sample S1300, a small amount of ZrC phase appeared and mainly distributed in the middle of the ZrO2 and amorphous carbon phase, as shown in Fig. 7(d). As presented in Fig 7(e), the lattice stripe spacing corresponded sufficiently to the m-ZrO2 and ZrC plane for sample S1500. As the reaction proceeds, ZrO2 was eventually transformed into ZrC completely. As shown in Fig 7(f), only ZrC and amorphous carbon can be found in sample S1700.

    Fig. 7.  TEM images of all samples: (a) S900; (b–c) S1100; (d) S1300; (e) S1500; (f) S1700.

    As the annealing temperature increased, the state and distribution of free carbon change. The carbon phase was amorphous for S900 and S1100. As the annealing temperature reached 1300°C, turbotrain carbon appeared, indicating the increase in the graphitization degree of carbon. The turbotrain carbon had a short length and intertwines with amorphous carbon. Carbon and oxygen atoms reacted with each other, and the amorphous carbon content surrounding the particles was enriched. A typical core–shell structure can be formed in S1500 and S1700. When the annealing temperature was 1500°C, the turbostratic carbon formed the sandwich structure with the amorphous carbon, and it became longer and wraps around the ZrC and ZrO2 grains. When the annealing temperature was 1700°C, the turbostratic carbon was completely consumed, leaving the amorphous carbon and corresponding Raman results.

    The SET can be calculated using S-parameters (S11 and S21), in accordance with the following formulas [2,33]:

    SET=SEA+SER
    (2)
    R=|S11|2=|S22|2
    (3)
    T=|S21|2=|S12|2
    (4)
    R+T+A=1
    (5)
    SER=10lg(1R)
    (6)
    SEA=10lg[T/(1R)]
    (7)

    where SET, SEA, and SER denote the total shielding effectiveness, absorption shielding effectiveness, and reflection shielding effectiveness, respectively; R, A, and T represent the reflectance, absorbance, and transmission, respectively; S11, S12, S21, and S22 are scattering parameter.

    Fig. 8(a) shows the average SET, SEA, and SER of S900 were 11.63, 9.00, and 2.63 dB, respectively. When the annealing temperature increased to 1100, 1300, 1500, and 1700°C, the average SET were 22.67, 22.81, 22.91, and 34.73 dB, respectively, revealing the increasing tendency with the annealing temperature. As shown in Fig. 8(b–c), the SEA accounted for the main part of shielding efficiency compared with the SER for all the samples.

    Fig. 8.  EMI SE of all the samples: (a) SET; (b) SEA; (c) SER.

    Two factors influence the EMI shielding properties: open porosity and phase composition. The open porosity of as-fabricated samples increased from 31vol% to 73vol% as the annealing temperature increased from 900 to 1700°C. It is a porous structure, and a better impedance match can be achieved, leading to the reflection of fewer electromagnetic (EM) waves [3438]. When the electromagnetic wave entered the ceramic interior, internal reflection occurred, leading to the dissipation of electromagnetic waves and contributing to the absorption-dominated EMI shielding performance [3942]. Thus, the average absorption shielding performance increased from 9 to 21.67 dB when the annealing temperature increased from 900 to 1700°C. In general, the increase in open porosity will reduce the shielding performance [40,4344]. However, in this work, as the annealing temperature increased, the open porosity rose rapidly with the shielding performance. Thus, open porosity is not the main factor, phase composition plays the dominant role.

    The S1100, S1300, and S1500 sample demonstrated similar shielding performances. S1100 and S1300 had a higher carbon content, which increased the SET. Although sample S1500 had a low carbon content, ZrO2 was converted to ZrC with a higher electrical conductivity. When the annealing temperature was 1700°C, the ZrO2 transformed into ZrC completely, and a trace amount of carbon remained. The typical core–shell structure, composed of carbon and ZrC, can be observed, which led to excellent shielding performance and high porosity.

    Fig. 9 illustrates the power balance of all the samples. With the increase of annealing temperature, the percentage of reflected power increases from 45% to 89%, while the absorbed power decreases from 47% to 9.2%. As shown in Fig. 9, the dominant shielding mechanism is reflection loss. However, it is not the main mechanism for SET. The appropriate method for assessing the reflective capacity is to calculate the ratio of the reflected power to the incident power, and the method for the assessment of absorption capacity is the calculation of the ratio of absorbed power and power penetrating the material [33]. The higher absorption capacity symbolizes the superior capabilities of SEA over SER. Therefore, the dominant SE of the samples is SEA. The percentage of transmitted power can be ignored compared with the reflected and absorbed powers. Therefore, hardly any electromagnetic waves passed through the material, indicating excellent shielding properties.

    Fig. 9.  Power balance of all samples.

    The EMI shielding mechanism of samples was proposed (Fig. 10). When waves reached the surface of samples, reflection, absorption, and transmission occurred simultaneously [45]. For the ZrC ceramic, EM wave absorption played the dominating role. When EM waves penetrated the interior of the samples, the porous structure allowed the EM waves to be reflected in multiple ways inside the samples, thereby consuming EM waves and resulting in an absorption-dominated shielding performance.

    Fig. 10.  Schematic of EMI shielding mechanisms of samples.

    Table 3 compares the shielding properties of ZrC with other relevant materials [2,46–48]. The listed materials have similar electromagnetic shielding properties at different annealing temperatures. Compared with the reported Si-based ceramics, ZrC ceramics prepared by PDCs contain a substantial ultra-high temperature phase, which reveals great application potential in harsh environment.

    Table  3.  Comparison of EMI shielding properties of ultra-high temperature ceramics [2,4648]
    MaterialsProcessFabrication temperature / °CFrequency / GHzSET / dBRef.
    SiC–CPDC17008.2–12.429.14[2]
    SiC/CPDC12508.2–12.436.60[46]
    SiC–Si3N4PDC14008.2–12.435.00[47]
    SiC/HfCxN1−x/CSPS6008.2–12.4>40.00[48]
    ZrCPDC17008.2–12.434.73This work
    Notes: PDC represents polymer-derived ceramic; SPS represents spark plasma sintering.
     | Show Table
    DownLoad: CSV

    In this work, ZrC ceramics were successfully fabricated by pyrolysis of an organic polymeric precursor of ZrC, which was annealed at temperature ranging from 1100 to 1700°C. The carbothermal reduction reaction between t-ZrO2 and amorphous carbon started at 1300°C. With the increase in the annealing temperature, typical core–shell structures can be formed by surrounding carbon with ZrO2 and ZrC, which resulted in a high electromagnetic shielding performance. When the annealing temperature reached 1700°C, ZrO2 was completely converted to ZrC, and the SET and SEA of as-obtained porous ZrC ceramics reached 34.73 and 21.67 dB, respectively, which indicated an excellent electromagnetic shielding performance.

    This work was supported by the National Natural Science Foundation of China (No. 52072303) and the National Science and Technology Major Project (No. J2019-VI-0014-0129).

    All authors certify that they have no affiliations with or involvement in any organization or entity with any financial interest or non-financial interest in the subject matter or materials discussed in this manuscript.

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