Facile Synthesis of Highly Defected Silicon Carbide Sheets for

Jul 25, 2018 - Stacking faults (SFs) within silicon carbide (SiC) are desired because these faults can enhance the electromagnetic (EM) absorption pro...
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Article Cite This: J. Phys. Chem. C 2018, 122, 18537−18544

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Facile Synthesis of Highly Defected Silicon Carbide Sheets for Efficient Absorption of Electromagnetic Waves Xiaolin Lan,† Caiyun Liang,† Maosong Wu,‡ Nan Wu,‡ Liang He,§ Yibin Li,∥ and Zhijiang Wang*,† †

J. Phys. Chem. C 2018.122:18537-18544. Downloaded from pubs.acs.org by UNIV OF SOUTH DAKOTA on 09/01/18. For personal use only.

MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, School of Chemistry and Chemical Engineering, and ∥Center for Composite Materials and Structures, Harbin Institute of Technology, Harbin 150001, China ‡ Science and Technology on Electromagnetic Compatibility Laboratory, China Ship Development and Design Center, Wuhan 430064, China § Shanghai Key Laboratory of Aerospace Intelligence Control Technology, Shanghai 201109, China S Supporting Information *

ABSTRACT: Stacking faults (SFs) within silicon carbide (SiC) are desired because these faults can enhance the electromagnetic (EM) absorption properties of the material. However, most reported SiC materials are prepared using expensive precursors possessing limited SFs. Herein, we report a facile and economical method to fabricate SiC sheets with a record-high SF density of over fourfold enhancement compared with previously reported SiC materials. The use of paper as a carbon source resulted in a 19-fold decrease in fabrication cost. The microstructure, defect structure, and EM wave absorption performance of the synthesized SiC sheets were investigated in detail. Enhancement of the SF content of the SiC sheets enabled significant interfacial dipole polarization, thereby imparting the sheets with superior EM wave absorption. SiC sheets with the maximum SF content obtained in this work revealed a minimum reflection loss of −22 dB and an effective EM wave absorption band (RL < −10 dB) covering the frequency range of 12.8−18 GHz at a thickness of only 2.2 mm. Our research shows that paper-derived SiC can be used as an efficient EM wave absorption material and provides guidelines for synthesizing highly defected SiC sheets.

1. INTRODUCTION Defect control is emerging as a significant approach to regulate the properties of materials for functional applications, including catalysis, sensors, photoactive devices, and energy conversion.1−3 For example, increasing the density of defects on the surface of ZnO nanosheets can enhance their response to acetone-sensing by providing more adsorbed and oxidized reducing gas molecules.4 Installment of surface defects on Au− Fe alloy catalysts has also been shown to significantly improve the catalytic performance of the alloy toward CO2 reduction by decreasing the formation energy of *COOH.5 Crystal structure modification method to fabricated defective FeNb11O29 and nano-TiNb2O7/carbon nanotubes can tackle the issue of poor rate capability for anode material of lithium-ion batteries.6,7 A controllable approach for engineering defects can regulate electronic spins and improve the potential applications of electromagnetic (EM) wave absorbers. The development of EM wave absorbers with excellent performance has become a crucial research topic following the popularization of electronic equipment, including wireless networks, computers, the Internet, mobile phones, and electronic organizers.8 It has been urgently considered that in exceptional cases, EM wave should be absorbed or attenuated to prevent bodies from EM pollution. As a result, © 2018 American Chemical Society

EM wave absorber becomes an effective technique to solve the above problems.9 The requirements for EM wave absorbers mainly include strong absorption intensities, broad frequency bandwidth, thinness, and lightness of weight.10,11 To acquire the above requirements of EM wave absorbers, some composites, including graphene−Fe3O4,12 Ni@NG/NC,13 Fe3O4−Fe/graphene,14 NiFe2O4 hollow particle/graphene hybrid,15 Fe3O4−PPy,16 C/SiO2,17 and Ni/C18 have been fabricated. As an excellent dielectric material for potential EM wave absorber, silicon carbide (SiC) possesses low density, good oxidation resistance, hardness, high strength, and endurance against harsh working conditions because of its chemical durability.19,20 As such, considerable effort has been devoted to enhancing the dielectric properties and EM wave absorption abilities of SiC. Doping SiC to obtain materials such as B-doped SiC, N-doped SiC, and Ni-doped SiC shows improved polarization relaxation of the carbide.21,22 Decoration of SiC with magnetic particles, such as SiC−Fe3O4,23 SiC−Co,24 and SiC−Ni,25 has also been attempted. Another approach to improve the properties of SiC is the regulation of Received: June 4, 2018 Revised: July 24, 2018 Published: July 25, 2018 18537

DOI: 10.1021/acs.jpcc.8b05339 J. Phys. Chem. C 2018, 122, 18537−18544

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The Journal of Physical Chemistry C

Figure 1. (a) Schematic of the fabrication of SiC sheets derived from paper. SEM images of (b) raw paper and (c) carbonized paper. Images of SiC sheets synthesized at (d) 1400, (e) 1500, and (f) 1600 °C. (g) XRD characterization of SiC samples synthesized at different temperatures.

2. EXPERIMENTAL SECTION 2.1. Materials. Bleached softwood kraft pulp cellulose was supplied by Hengfeng Paper Co., Ltd. and used as a raw material to prepare the paper sheets. Silicon dioxide and silicon powder were supplied by Sinopharm Chemical Reagent Co. Ltd., China. 2.2. Recycling Cellulose from Paper. The cellulose material was recycled by separation, rinsing, filtration, and drying. First, 2 g of raw materials was cut into debris with a diameter of 5 mm, added to 100 mL of distilled water, and vigorously stirred at 2000 rpm for 5 h. The mixture was then rinsed off its impurities with distilled water. After filtration, the paper sheets were dried at 105 °C in an oven. 2.3. Preparation of the Carbon Template. The temperature of the sintering furnace was ramped to 800 °C at a rate of 5 °C min−1. The paper sheets were pyrolyzed at 800 °C for 2 h under a protective flow of N2 (10 L h−1). 2.4. Fabrication of the SiC Sheets. Si powder and SiO2 particles were mixed at a molar ratio of 1:1 and ground for at least 1 h. The powders and carbon template were placed in a corundum crucible and sintered at 1400, 1500, or 1600 °C in a sintering furnace under a protective flow of argon (10 L h−1) for 3 h. After cooling to room temperature, the samples were heated at 700 °C in air for 8 h to remove the unreacted carbon. 2.5. Characterization. Scanning electron microscopy (SEM) images of the samples were taken by a Helios Nano Lab 600i instrument. X-ray diffraction (XRD) patterns were determined via a Rigaku D/Max-γB diffractometer equipped with a rotating anode and Cu Kα source. Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) images were recorded by an FEI G2 F30 under an accelerating voltage of 300 keV. EM parameters, including complex relative permittivity and permeability, were obtained from a vector network analyzer (Agilent, N5230A). Samples for measurement were prepared by mixing the SiC products with paraffin at a weight ratio of 1:1 and then pressing to obtain a toroidal-shaped composite sample with an inner

its defect structure; this approach has emerged as the most promising among the methods available to date because of its extremely effective improvement and convenient operation. Liu26 found that stacking faults (SFs) in SiC materials can disrupt the balance of electric charge distribution and enhance EM energy dissipation. Zhang27 reported that the strong interfacial dipole polarization caused by a high SF density in the domain of SiC can improve its dielectric permittivity. EM wave attenuation is believed to be strongly affected by the presence of a high SF density in the SiC domain. However, although many studies have focused on the effects of SFs within SiC, the density of SFs in previously reported SiC materials generally falls below 3.21,22,27−35 far lower than the requirements of most applications. Furthermore, because of the use of multiwalled carbon nanotubes as the source material, producing SiC with SFs is expensive, costing about $1000 to obtain a kilogram of the carbide. As such, increasing the density of SFs in SiC via a facile and cost-effective synthesis method is a worthwhile endeavor. Compared to other precursors for carbon such as, PVP,36 hexamethylenetetramine,37 graphene oxide,38 sucrose,39 activated sludge,40 polyacrylonitrile41 and polyvinylidene fluoride,42 cellulose is a promising renewable resource and can offer a new and economical strategy for fabricating high-SF density SiC materials. Herein, we report a facile and economical method for fabricating highly defective SiC sheets with excellent EM wave absorption performance. Common softwood paper is applied as a carbon source material, and conversion is achieved via the reaction of paper, Si powder, and SiO2 particles in an Ar atmosphere without any catalyst at 1600 °C. The EM wave absorption properties of the SiC materials with high SF density were studied over the range of 2−18 GHz, and an EM wave absorption mechanism is proposed according to the microstructural features and EM parameters of the SiC products. 18538

DOI: 10.1021/acs.jpcc.8b05339 J. Phys. Chem. C 2018, 122, 18537−18544

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Figure 2. TEM images of the SiC sheet synthesized at 1600 °C. (a) Representative morphology, (b) typical HRTEM image, and (c) SAED pattern.

obtained.32,43 The XRD patterns of defect-free SiC are shown in Figure S1. The SF peaks of the defect-free SiC exhibit an inexistent peak. Most of the reported SiC materials with high SF density show a nanowire morphology and SF density below 3.21.22,27−35 Surprisingly, the SiC sheets derived from paper, in this work, contain an extremely high density of SFs. The SF densities of the SiC sheets at 1400, 1500, and 1600 °C are 3.87, 6.05, and 12.55, respectively, and the SiC sheet produced at 1600 °C demonstrates over fourfold enhancements in SF content compared with previously reported SiC materials. Further investigations on microstructure were carried out by TEM. Figure 2 shows representative TEM images of the SiC sheets synthesized at 1600 °C. The lattice boundary between the grains in the SiC crystal structure is clearly visible in Figure 2a. Moreover, black lines and shaded regions, which are attributed to the high SF density of the sheets, appear in the SiC domains. The HRTEM image in Figure 2b confirms the extremely high density of SFs in the paper-derived SiC sheets; these faults induce strong spots and streaks in the selected area electron diffraction (SAED) pattern (Figure 2c) in a Bragg diffraction condition. The TEM images obtained are in agreement with the above XRD analysis, thus confirming the high density of SFs in the paper-derived SiC sheets. On the basis of the SEM, XRD, and TEM analyses above, as well as the materials’ intrinsic properties, the reactions for paper-derived SiC formation may be considered to consist of a solid-phase reaction and a vapor−solid reaction. Referring to previous reports,43,44 the proposed reactions for the present SiC materials are as follows, Solid-phase reactions

diameter of 3 mm, an outer diameter of 7 mm, and a height of 3 mm. The test data of 20, 30, 40, and 60% SiC filler loading in paraffin were supplied in the Supporting Information. According to transmission−reflection line theory,43 EM wave absorption properties may be calculated following 2-1 and 2-2. Zin = Z0(μr /εr)1/2 tanh[j(2πfd /c)(μr /εr)1/2 ] RL = 20 log10

Zin − Z0 Zin + Z0

(2-1)

(2-2)

where d is the thickness of the absorber; f is the frequency of the EM waves; μr and εr are the relative complex permeability and permittivity of the absorber, respectively; c is the velocity of light; Z0 is the impedance of free space; and Zin is the input impedance of the absorber.

3. RESULTS AND DISCUSSION 3.1. Microstructural Analysis. The schematic for the fabrication of SiC sheets derived from paper is illustrated in Figure 1a. Typically, a piece of paper is pyrolyzed under a N2 atmosphere at 800 °C, followed by sintering with Si and SiO2. During carbonization, the volume of the paper contracts and the sheet turns black. After sintering, the SiC sheet obtained shows no apparent difference from the carbonized sheet, except that the color of the sintered sheet turns from black to gray-blue. The micro- and crystalline structures of the products were determined by SEM and XRD analysis, and SEM images of the raw paper, carbonized paper, and as-synthesized SiC sheets are shown in Figure 1b−f. The paper comprises lamellar cellulose fibers with a mean thickness of 10 μm. The SEM images clearly reveal that the stacked-layer morphology of the paper template is basically maintained after carbonization and sintering. The SiC sheet fabricated at 1400 °C has nearly the same morphology as the raw paper. When the sintering temperature is increased from 1400 to 1600 °C, some free-standing SiC nanowires are formed on the surface of the SiC sheets. The density and length of these nanowires increase with increasing sintering temperature. Figure 1g illustrates the XRD patterns of the SiC sheets synthesized at 1400−1600 °C. The diffraction peaks at 35.7°, 41.4°, 60.0°, 71.8°, and 75.4° are, respectively, aligned with the (111), (200), (220), (311), and (222) planes of the crystalline cubic zincblende form of β-SiC (JCPDS card 75-0254). No impurity peaks are found, thus indicating that the paper had been completely converted into SiC materials via our developed method. The diffraction peak of 33.6° in the XRD patterns is assigned to the feature peak of SFs.29,32 The intensity ratio of the diffraction peaks of 33.6°−41.4° (I33.6°/ I41.4°) confirms the presence of SFs within the SiC materials

C(s) + Si(s) = SiC(s)

(3-1)

SiO(g) + 2C(s) = SiC(s) + CO(g)

(3-2)

Vapor-solid reactions SiO2 (s) + Si(s) = 2SiO(g)

(3-3)

SiO2 (s) + C(s) = SiO(g) + CO(g)

(3-4)

C(s) + CO2 (g) = 2CO(g)

(3-5)

SiO(g) + 3CO(g) = SiC(s) + 2CO2 (g)

(3-6)

The solid-phase and vapor−solid reactions are believed to take place simultaneously, resulting in a complex morphology of SiC sheets and nanowires. The SiC sheets appear to be generated mainly via solid-phase reactions because the parental sheet morphology is well-inherited. SiC grown in situ by solidphase reactions are processed as presented in 3-1 and 3-2, thus implying the construction of SiC sheets. Free-standing SiC nanowire growth then occurs via vapor−solid reactions, which are shown in 3-3 to 3-6. After the reaction of gaseous SiO and 18539

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between the reactants in the generated SiC crystals markedly differ, and atoms cannot be stacked regularly because assigning a location for the newly added SiC before the next atom enters the crystal lattice is difficult. Thus, a defect-free ordered structure cannot be achieved in the solid-state reactions. High temperatures are beneficial for the emergence of intrinsic disorders, leading to the formation of vacancies and SFs.27,29,30,45 In our developed approach, high SF densities are achieved in the paper-derived SiC sheets, and SF content is increased by increasing the sintering temperature. 3.2. EM Absorption Analysis. In general, the relative complex permittivity (δe = ε′ − jε″) determines the EM wave absorption property of dielectric materials. As illustrated in Figure 5, the ε′ of the three samples exhibits a similar declining tendency versus frequency. Moreover, all of the ε″ of sample curves go up along with the frequency. When SiC sheets are synthesized at a temperature of 1400 °C (SiC-1400), ε′ is in the range of 4.9−6.3 and ε″ is in the range of 0.9−1.5. The SiC sheets obtained at 1600 °C (SiC-1600) show lower ε′ in the range of 4.8−7.5 and ε″ in the range of 0.8−2.7. The ε′ of the SiC sheets produced at 1500 °C (SiC-1500) is in the range of 4.0−5.6 and their ε″ is in the range of 0.9−2.0. SiC-1500 shows spectral features that differ from those of SiC-1600 and SiC-1400, which may be because of its transition state. The same phenomenon has been observed for SiC nanowires.27 SiC nanowires with SFs usually have one dielectric resonance peak.27 However, the SiC sheets derived from paper in this work reveal five obvious dielectric resonance peaks in the ε″ curve, likely because ε′ and ε″ are strongly affected by the SF content of the sheets. SFs within the SiC crystal structure can disrupt the balance of the electric charge distribution.46,47 Charges accumulated in the SF/SiC interfaces create a large number of interfacial dipoles that oppose the applied EM field and then induce dipole polarization losses and energy dissipation.48 Thus, a high density of SFs in the SiC sheets can trigger interfacial polarization and dipole polarization, which plays an important role in enhancing their dielectric permittivity.49 The SiC-1600 with the highest density SFs shows larger permittivity level than that of other samples. In according with the Debye theory, when the dielectric polarization relaxation exists, ε′ and ε″ will meet the following relationship:50

CO, SiC nanowires are successfully incorporated into the SiC sheets with a random distribution. To confirm the reason of the proposed reaction equations, the intermediates are detected. In situ detection of CO is processed by directly venting the gas outlet of sintering furnace into the sampling loop of a gas chromatograph (Agilent 7890A). Figure 3 shows the characteristic peaks of the outlet

Figure 3. Gas chromatogram chart of outlet gas in the sintering furnace.

gas. The peak corresponding to CO is obviously present, which indicates that CO gas was truly produced during the reaction. The SiO gas is quite difficult to be in situ detected because of its metastable property, which is easily decomposed into Si and SiO2 when the temperature was below 1440 °C. Correspondingly, we indeed found that solid powder was piled up in the outlet of the furnace at end of each preparation. The collected powders were analyzed by XRD. Figure 4 shows the XRD

2 ε + ε∞ yz2 ij i ε − ε∞ yz jjε′ − s zz + (ε″)2 = jjj s zz 2 { k k 2 {

Figure 4. XRD characterization of the powder at the outlet in the sintering furnace.

(3-7)

where εs is the static permittivity and ε∞ is the relative complex permittivity under the limit of the high frequency. That is to say, the curve of ε″ versus ε′ will show a semicircle, which is called the Cole−Cole semicircle. Figure 6 is the curves of ε″ versus ε′ of the SiC sheets at different temperatures. Two obvious Cole−Cole semicircles can be seen for the SiC-1400, with each semicircle corresponding to a Debye relaxation process. For SiC-1500 and SiC-1600, the ε′ and ε″ curve has three and five Cole−Cole semicircles, respectively. The phenomenon is due to the existence of more SF/SiC interfaces with the higher density SFs, which gives rise to interfacial polarization and dipole polarization.51,52 To evaluate the EM wave absorption performance of the SiC sheets, the reflection losses (RL) of the absorbers were systemically calculated according to transmission−reflection line theory. A suitable EM wave absorber should have an RL lower than −10 dB, representing 90% attenuation of EM

pattern of these powders. The diffraction peaks are aligned with the (101), (111), (102), and (200) planes of SiO2 (JCPDS no. 39-1425) and the (201) and (211) planes of Si (JCPDS no. 40-0932), respectively. The presence of Si and SiO2 in the outlet of the furnace verifies the intermediate of SiO formed during the reaction. SFs are disturbances in the sequence of atomic stacking that occur during SiC growth. The inserted SFs can promote β-SiC formation with decreased energy requirements. Our previous study demonstrated that SiC nanowires with an SF density of only 1.8227 can be formed during vapor−solid reaction. In this report, the paper-derived SiC sheets demonstrate much higher SF densities than previous SiC materials, which could be because of the solid-phase reaction controlled by atomic diffusion at elevated temperatures. The diffusion coefficients 18540

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Figure 5. Complex permittivity characterization of SiC samples in the 2−18 GHz range. (a) Real part of permittivity and (b) imaginary part of permittivity.

Figure 6. Cole−Cole curves of the SiC sheets (a) 1400, (b) 1500, and (c) 1600 °C.

during which extensive induced interfacial dipole polarization converts the EM energy into thermal energy. Table 1 summarizes the EM wave absorption performance of some reported SiC materials. Compared to previously reported SiC materials, the SiC sheets derived from paper in this work demonstrate wider effective absorption coverage with decreased thickness. Besides their high strength, good resistance to oxidation and corrosion, and low cost, the SiC sheets developed from paper reveal promising EM wave absorption properties for practical applications.

waves. Three-dimensional (3D) map of the EM wave absorption of defect-free SiC is depicted in Figure S2. The defect-free SiC has a much smaller RL value of −8 dB, which is defined as not valid absorption. Figure 7 shows the EM wave absorption characteristics of the synthesized SiC sheets. As the minimum RL of the SiC-1400 sample is −9 dB, this sheet is considered the poorest EM wave absorber among the three samples obtained. The minimum RL of SiC-1500 is −18 dB, and its effective absorption band covers the frequency range of 15.0−18.0 GHz at a thickness of 2.2 mm. The minimum RL of the SiC-1600 sample is −22 dB, and its effective absorption band covers 5.2 GHz (12.8−18 GHz) at a thickness of 2.2 mm. Thus, the EM wave absorption properties of the three samples can be ranked as follows: SiC-1600 > SiC-1500 > SiC-1400. Figure 7d presents the structure−property relationships of the paper-derived SiC sheets. The EM wave absorption of the SiC sheets demonstrates a dependence on their SF content. The SiC-1600 sample, which contains the most SFs among the samples fabricated, exhibits the best EM wave absorption,

4. CONCLUSIONS In summary, SiC sheets with high SF density were successfully synthesized using paper sheets as a raw material via a combined process of solid-phase and vapor−solid reactions. The sheets were controllably synthesized by tuning the sintering temperature. SFs generated extensive interfacial dipole polarization, thereby endowing the resulting SiC sheets with high-performance EM wave absorption abilities. Among the samples fabricated, the SiC sheets with the most SFs 18541

DOI: 10.1021/acs.jpcc.8b05339 J. Phys. Chem. C 2018, 122, 18537−18544

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Figure 7. 3D maps of the EM wave absorption of SiC sheets obtained at (a) 1400, (b) 1500, and (c) 1600 °C. (d) Relationship between SF content and minimum RL.

Table 1. EM Wave Absorption Properties of Some Representative SiC Materials absorption bandwidth (RL < −10 dB) samples SiC SiC SiC SiC SiC SiC SiC

minimum RL (−dB)

frequency range (GHz)

frequency coverage (GHz)

thickness (mm)

refs

30.0 31 20 21.5 19.9 16 22

6.0−9.7 8.2−12.4 13.6−18 6.0−8.4 9.2−11.7 8.6−11.2 12.8−18

3.7 4.2 4.4 2.4 2.5 2.6 5.2

4.6 3.3 2.2 2 2 3.2 2.2

27 53 54 55 56 57 this work

NWs 1 NWs 3 NWs 3 NWs 2 nanofibers fiber sheet-1600

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ACKNOWLEDGMENTS The authors acknowledge financial support from the National Natural Science Foundation of China (no. 51572062), Natural Science Foundation of Heilongjiang Province (no. B2015002), Heilongjiang Postdoctoral Scientific Research Developmental Fund (no. LBH-Q16079), and Hubei Provincial Natural Science Foundation of China (no. 2017CFB292).

exhibited the best EM wave-attenuation performance. Under optimal conditions, 2.2 mm thick SiC sheets can achieve an effective EM wave absorption band (RL < −10 dB) covering the frequency range of 12.8−18 GHz. Hence, fabrication of high-SF density SiC sheets provides a facile approach to enhancing wave EM absorption.

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ASSOCIATED CONTENT

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* Supporting Information S

The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.jpcc.8b05339.

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XRD pattern and 3D map of the EM wave absorption of defect-free SiC; complex permittivity; and 3D maps of the EM wave absorption for 20, 30, 40, and 60% SiC filler loading in paraffin (PDF)

AUTHOR INFORMATION

Corresponding Author

*E-mail: [email protected]. Phone/Fax: +86 451 86418409. ORCID

Yibin Li: 0000-0003-4228-1528 Zhijiang Wang: 0000-0001-9314-7922 Notes

The authors declare no competing financial interest. 18542

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DOI: 10.1021/acs.jpcc.8b05339 J. Phys. Chem. C 2018, 122, 18537−18544