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Influence of TiB2 content on the properties of TiC–SiCw composites
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Influence of TiB2 content on the properties of TiC–SiCw composites Mehdi Fattahia, Yaghoub Pazhouhanfarb, Seyed Ali Delbaric, Shahrzad Shaddeld, Abbas Sabahi Naminie,f,∗, Mehdi Shahedi Aslc,∗∗ a
Institute of Research and Development, Duy Tan University, Da Nang, 550000, Viet Nam Aliyazh Sanat Sahand Ipak Company, P.O. Box: 51576-13536, Tabriz, Iran Department of Mechanical Engineering, University of Mohaghegh Ardabili, Ardabil, Iran d Department of Materials Engineering, Sahand University of Technology, Tabriz, Iran e Department of Engineering Sciences, Faculty of Advanced Technologies, University of Mohaghegh Ardabili, Namin, Iran f Department of Engineering Sciences, Faculty of Advanced Technologies, Sabalan University of Advanced Technologies (SUAT), Namin, Iran b c
A R T I C LE I N FO
A B S T R A C T
Keywords: TiC TiB2 SiC SPS Composite
The impact of various volume percentages of TiB2 additive (0, 10, 20, and 30) on the microstructure, relative density (RD), Vickers hardness, flexural strength, and thermal conductivity of as-sintered TiC-10 vol% SiCwbased composite samples were scrutinized. All four samples were sintered using the SPS method under the following circumstances; sintering temperature of 1900 °C, dwell time of 7 min, and external pressure of 40 MPa. The best relative density of 98.73% was achieved for the sample with no TiB2 additive, indicating the negative effect of TiB2 additive on the RD and formation of porosity. The microstructural observations and XRD results confirmed the chemical interaction of TiO2 and B2O3 oxide layers and SiCw and in-situ formation of the TiSi brittle phase and TiC. The most significant values of flexural strength (511 MPa) and hardness (27.67 GPa) were related to TiC-10 vol% SiCw and TiC-10 vol% SiCw-30 vol% TiB2 samples, respectively. On the contrary, the specimens with 30 vol% and 10 vol% TiB2 as additive presented the poorest qualities of flexural strength (234 MPa) and Vickers hardness (22.12 GPa). Finally, the influence of the TiB2 content on the thermal conductivity was evaluated, indicating the positive impact of this secondary phase on this characteristic, so with adding 30 vol% TiB2 to TiC-10 vol% SiCw, a thermal conductivity of 30.7 W/m.K was obtained.
1. Introduction TiC-based materials as the ultra-high-temperature ceramics (UHTCs) have newly found lots of proponents because of the wide range of properties that they provide. Low density, high melting point, acceptable electroconductivity, and thermal conductivity, excellent hardness, high wear resistance, superior chemical and thermal stability, and finally, low thermal expansivity are among the qualifications that make these kinds of materials unique [1–12]. Regarding the mentioned characteristics, TiC-based ceramics take a reliable place in the hightemperature structural applications such as leaning edge parts, rocket nozzle throat liners, hypersonic re-entry vehicles, jet engine components, and high-speed cutting tools [13–25]. Nevertheless, using such substances, especially in the monolithic form, have some limitations due to the poor thermal shock resistance and fracture toughness. These mentioned properties can lead to a failure in abrupt changes in load and temperature during the working [13,21,26,27]. Besides, the sintering of
∗
TiC is difficult too, thanks to its strong covalent bonds and low selfdiffusion coefficient [13,21]. At the same time, utilizing high sintering temperatures to overcome this problem can result in excessive grain growth and consequently, poor mechanical properties [28–37]. To overtake the described limitations, making a composite via adding a suitable sintering aid can be the remedy. During the recent years, quite a few researches have been implemented on the effect of using different metallic additives, such as Ni, Cr, Co, and Mo, and various ceramic sintering aids, including WC, SiC, TiB2, NbC, and TiN, on the mechanical and microstructural qualities of as-sintered TiC-based composite materials [38–48]. On the other hand, the problem of poor sinterability can be solved by using new processes, such as hot isostatic pressing (HIP), spark plasma sintering (SPS), etc., instead of utilizing conventional powder metallurgy technique [47–74]. Among these methods, SPS technique has provided lots of advantages thanks to its low working temperature, short holding time, and also the possibility of applying external pressure. These characteristics make this method an
Corresponding author. Department of Engineering Sciences, Sabalan University of Advanced Technologies (SUAT), Namin, Iran. Corresponding author. Department of Mechanical Engineering, University of Mohaghegh Ardabili, Ardabil, Iran E-mail addresses: [email protected] (A. Sabahi Namini), [email protected] (M. Shahedi Asl).
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https://doi.org/10.1016/j.ceramint.2019.11.236 Received 9 November 2019; Received in revised form 25 November 2019; Accepted 26 November 2019 0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Please cite this article as: Mehdi Fattahi, et al., Ceramics International, https://doi.org/10.1016/j.ceramint.2019.11.236
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specimens was calculated through dividing (the bulk density × 100) by (the theoretical density). The phase analysis was implemented by an XRD machine (Philips, PW3710 X-ray), and an optical microscope (PMG3, Olympus, Japan) and a FESEM (Tescan S8000) equipped with an EDS was used for microstructural evaluation. Moreover, the thermodynamical favorability of possible chemical reactions between different phases was carried out using HSC software. The Vickers hardness tests were carried out through the application of 49 N load on the polished surfaces of TiC-based composite samples. To have an accurate value, six indentations were applied for each specimen. Flexural strength was measured through the three-point bending test by an STM250 universal testing machine. The test samples were standards with the following dimensions; 3 × 4 × 28 mm3 and span length of 15 mm. Ultimately, the thermal conductivity assessment was done by a thermal conductivity meter apparatus (Iran, Sahand Co.) at room temperature.
ideal way to produce high-quality composite materials [3,6,32,51,71,73,75–83]. Some researchers scrutinized on the influence of adding TiB2 and/or SiC as reinforcements on the microstructure and mechanical characteristics of titanium carbide-based composite samples. Mestral et al. did a complete investigation on TiB2-TiC-SiC system. The interfaces of various phases were studied using SEM and TEM to find out about the possible chemical reaction between phases and also diffusion of their elements into each other. Moreover, the hardness of ~26 GPa and the flexural strength of ~360 MPa were obtained for the TiC-based sample codoped with 16.5 vol% TiB2 and 16.5 vol% SiC [84]. The in-situ production of TiC-TiB2 composite samples also carried out using B4C and C as additives by Locci et al. The reactive SPS process was implemented to fabricate the specimens, and XRD and SEM were utilized to investigate on the in-situ produced phases [28,80,85]. Shahedi et al. studied the effect of SiC whiskers as reinforcements on the relative density, Vickers hardness, flexural strength, and thermal conductivity of SPSed TiC-based samples. They reported the relative densities more than 100% by adding 20 vol% and 30 vol% SiCw to the titanium carbide samples. Moreover, the best values of Vickers hardness and thermal conductivity achieved for the sample doped with 30 vol% SiCw, while the most significant flexural strength was related to the TiC20 vol% SiCw specimen [40]. Finally, Babapoor et al. accomplished a thorough investigation on the qualifications and limitations of monolithic TiC ceramics. They reported the sintering temperature of 1900 °C as the optimal temperature, and the following qualities obtained in this temperature: The relative density of 99.4%, Vickers hardness of 25.7 GPa, and thermal conductivity of 17.9 W/mK [48]. Although some valuable research works have been implemented on the in-situ produced TiC-TiB2 and TiC-TiB2-SiC composite samples, there is no available investigation on the influence of adding both exsitu TiB2 and SiC as reinforcements on the microstructure and mechanical properties of TiC-based composite specimens. In this research work, different volume percentages of TiB2 (0, 10, 20, and 30) were added to TiC- 10 vol% SiCw-based composites, and a relatively complete study was fulfilled.
3. Results and discussion 3.1. Consolidation behavior The relative density of SPSed composite samples is presented in Fig. 2. As shown, the most significant relative density of 98.73% was related to the sample with no TiB2 content, indicating the negative effect of this additive on this quality. With adding more TiB2 to TiC10 vol% SiCw system, the RD decreased, as the weakest value of below 93% was obtained for the specimen with 20 vol% TiB2. However, the relative density rose when the amount of titanium diboride increased to 30 vol%, standing at ~94%. The reason for such consolidation behavior can be found in the possible reaction among the initial materials over the sintering process. Shahedi et al. reported the formation of trace content of TiO2 and B2O3 on the surface of similar as-received TiB2 powders [78]. This phase can chemically react with the SiC phase based on Eq. (1), and leads to the in-situ formation of TiC and SiO2 phases. The possibility of this chemical reaction was studied through the HSC software, and, as the ΔG of this reaction is negative all along with the SPS working temperature, this reaction is favorable thermodynamically.
2. Experimental procedure
TiO2 + SiCw = TiC (in-situ) + SiO2
The starting materials were picked out among the available highquality powders. The properties of as-received powders, which all of them were supplied from Xuzhou Hongwu Nanometer Material Co., China, were as follows; TiC: particle size < 12 μm, purity > 99%, SiCw: 5 μm < length < 30 μm, 0.1 μm < diameters < 1 μm, purity > 99%, and TiB2: particle size < 50 μm, purity > 98%. Moreover, SEM images and the corresponding X-ray diffraction patterns of initial powders are presented in Fig. 1. As shown, just peaks of starting materials were detectable, indicating not the availability of unwanted phases. In this research work, four various samples were designed to study the influence of TiB2 reinforcement on the qualities of TiC-10 vol% SiCw composites. Table 1 presents the composition of these mentioned specimens. Initially, based on the information provided in Table 1, all starting materials were weighed. Afterward, the prepared powders were dispersed for 2 h in ethanol by an ultrasonic system. To reach an utterly uniform mixture, and to remove the ethanol, the mixture was heated at 80 °C using a hot plate with a magnetic stirrer. Then, the dried slurries were crushed and passed through a sieve to obtain the homogenous granules and also to minimize the agglomeration. For sintering the final powders, a graphite die lined by two layers of graphite foil was used. The foil was applied to prevent the chemical reaction between the samples and the die during the sintering process. The specimens (30 mm diameter) finally sintered by an SPS machine under the following conditions; sintering temperature: 1900 °C, dwell time: 7 min, and external pressure: 40 MPa. After removing the samples from the die, the graphite foil was eliminated by grinding. The bulk and theoretical density of SPSed samples estimated using the Archimedes principle and the rule of mixtures, respectively. Then the relative density of
(1)
On the other hand, SiO2 can react with TiO2 at temperatures higher than 5205 °C, based on the information provided by HSC software, and results in the TiSi phase and O2 (Eq. (2)). Reaching to this temperature locally at the SPS process is probable thanks to the application of high pressure. Moreover, the probable formation of TiSi also verified by the XRD analysis indicated in Fig. 3. TiO2 + SiO2 = TiSi + 2O2 (g)
(2)
In addition, B2O3 also can react with SiCw based on Eq. (3) at the gaseous form. This oxide layer melts at the temperature of 450 °C and evaporates at 1860 °C and 1 atm. However, applying external pressure can lead to the decrement of evaporation point to the level below 1600 °C [78]. The chemical reaction presented in Eq. (3) is thermodynamically feasible at temperatures more than 1750 °C (based on HSC software data), and boron carbide and two other gaseous phases are the products. Ultimately, the B4C phase can react with the TiC matrix and led to the generation of in-situ formed TiB2 and remained carbon. This equation also checked through the HSC software, and its ΔG was negative all over the sintering temperature range. 4B2O3 (g) + 7SiC = 2B4C + 7SiO (g) + 5CO (g)
(3)
B4C + 2TiC = 2TiB2 + 3C
(4)
As shown in Eqs. (2) and (3), various gaseous phases were produced alongside the TiSi and B4C phases. Forming such phases and trapping them into the matrix can be the main reason why RD dropped when TiB2 added to the composite samples in comparison with the sample 2
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Fig. 1. Scanning electron microscopy images and corresponding XRD patterns of initial powders; (a) TiC, (b) SiCw, and (C) TiB2.
with no TiB2 content. As discussed before, the sample with 30 vol% TiB2 owned higher RD compared with the one with 20 vol% additive. According Eq. (1), SiO2 was one of the byproducts of the reaction between TiO2 and SiCw. Forming such a phase activates the liquid phase sintering mechanism and improves the consolidation behavior [78]. Although this phase is produced in all three samples with TiB2 content, adding more than 20 vol% TiB2 to TiC- 10 vol% SiCw system naturally results in forming more SiO2 phase. In the TiC-10 vol% SiCw-30 vol% TiB2 sample, this phenomenon could finally be more effective in comparison with the negative impact of forming the gaseous phases, and conduct to improve the RD by 1.5%.
Table 1 The list of as-produced composite samples. Sample
TiC (vol%)
SiCw (vol%)
TiB2 (vol%)
1 2 3 4
90 80 70 60
10 10 10 10
0 10 20 30
3.2. Microstructural evaluation Fig. 4 presents the optical microscopy images of SPSed TiC-10 vol% SiCw-based composites. Looking into this Fig., three bold phases are apparent; SiCw dispersed uniformly in the TiC matrix and TiB2 (with an exemption of two-phase sample in Fig. 4a, which indicates TiC-10 vol% SiCw). The form of SiCw changes from whiskers to clusters of intertwined form. It also should be mentioned that the big black holes are not associated with the porosities, but the pull-out grains during the sample preparation (grinding & polishing). The back-scattered SEM images of as-sintered samples are exhibited in Fig. 5. The dark-colored phases are related to SiC whiskers distributed homogeneously in the bright-colored TiC matrix. The greycolored phases also belong to the TiB2 additive. The uniform dispersion of secondary phases is shown in the EDS-mapping of Ti, Si, B, and C elements presented in Fig. 6. This kind of distribution helps secondary phases to play effectively as an inhibitor against the excessive grain growth over the sintering process. As it is clear, adding TiB2 reinforcement conducted to the formation of lots of porosity in the samples that follow the results obtained for the relative density. Fig. 7
Fig. 2. The relative density of SPSed TiC-10 vol% SiCw-(0, 10, 20, and 30 vol%) TiB2 specimens.
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Fig. 3. XRD patterns of SPSed TiC-10 vol% SiCw composite samples with (a) 0 vol% TiB2, and (b) 30 vol% TiB2.
similar. In Fig. 9, which is related to the SPSed TiC-10 vol% SiCw-30 vol % TiB2 specimen, the pores resulted in the incomplete consolidation can be seen obviously. Apparently, the sintering conditions were not appropriate for coalescing these intergranular pores.
indicates a magnified SEM image of SPSed TiC-10 vol% SiCw-20 vol% TiB2 and corresponding EDS point analysis. According to the presented information, points A, B and C are related to TiB2, TiC, and SiC, respectively. Moreover, point D can be possibly associated with the Ti3SiC2 phase, which detected in the XRD pattern (Fig. 3). Also, the high Si content in this EDS can be due to the influence of adjacent SiC particles. The SEM fractographs of SPSed samples are shown in Fig. 8. As it is observable, the intergranular mode was the predominant fracture mode in all four samples. Increasing the porosities in the samples with high TiB2 content is utterly obvious that, as discussed before, is probably because of the formation of some gaseous phases during the sintering process. Even though some large grains can be distinguished in these fractographs, the average grain sizes of all different samples are roughly
3.3. Mechanical properties The values of Vickers hardness of SPSed TiC-10 vol% SiCw-based samples are exhibited in Fig. 10. The Vickers hardness of ~24.5 GPa was obtained for the sample with no TiB2 content. Although titanium carbide presents a high level of hardness thanks to its strong covalent bonds, coexisting with SiCw has been possibly useful in reaching this value of Vickers hardness through the hindering the move of dislocations. Adding TiB2 led to a drop in this quality, as the weakest value of
Fig. 4. Optical microscopy images of SPSed TiC-10 vol% SiCw with different vol% of TiB2: (a) 0, (b) 10, (c) 20, and (d) 30. 4
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Fig. 5. SEM images of SPSed TiC-10 vol% SiCw with different vol% of TiB2: (a) 0, (b) 10, (c) 20, and (d) 30.
the amount of TiB2 content played the dominant role in the hardness of these specimens. As discussed before, adding TiB2 up to the level of 20 vol% had a destructive role on RD, so lower hardness values for samples with 10 vol% and 20 vol% TiB2 in comparison with the one with no titanium diboride content makes sense. On the other hand, TiB2
Vickers hardness belongs to the specimen with 10 vol% TiB2, standing at just above 22 GPa. However, with the addition of more titanium diboride to the composite samples, the hardness starts to increase, as the one with 30 vol% TiB2 surpasses the one with no titanium diboride content and reaches to 27.67 GPa. Apparently, the relative density and
Fig. 6. SEM image of SPSed TiC-10 vol% SiCw-30 vol% TiB2 and related EDS elemental maps. 5
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Fig. 7. SEM image of SPSed TiC-10 vol% SiCw-20 vol% TiB2 and the related EDS analysis.
TiB2 presents a higher thermal conductivity at room temperature compared with the TiC-10 vol% SiC samples (96 versus ~20 W/mK, respectively), so the addition of TiB2 additive to the TiC-10 vol% SiC specimen can result in an increment in thermal conductivity [40,86]. However, when a secondary phase is discontinuous in the matrix, the thermal conductivity of a composite is dominantly controlled by the matrix conductivity. Looking into Fig. 12, adding 10 vol% TiB2 resulted in a drop in the thermal conductivity of the samples. According to the formation of porosities and also new grain boundaries, this decrease in the conductivity makes sense. Even though, the addition of more volume percentages of titanium diboride led to an improvement in this characteristic, so the sample with 30 vol% TiB2 reaches to the level of thermal conductivity more than 30 W/m.K. The reason may be due to the much higher thermal conductivity of TiB2 compared with TiC matrix and also the possibility of formation of a continuous network of TiB2 at high volume fractions.
is a harder phase compared with the TiC matrix, so adding such a phase can improve the hardness of the samples. The influence of this issue was so predominant, that TiC-10 vol% SiCw-30 vol% TiB2 sample reached the hardness level of higher than TiC-10vol SiCw, while its RD was lower. The values of the flexural strength of as-sintered specimens are presented in Fig. 11. As shown in this Fig., the most significant flexural strength value of 511 MPa is related to the TiC-10 vol% SiCw sample and adding more TiB2 reinforcement continuously decreases this quality. This effect is so severe that the sample with 30 vol% TiB2 reaches the value of less than half of the value obtained for the specimen without TiB2 content. The main parameters that are effective on flexural strength are RD, grain size, and interfacial bonding between various phases. It seems that the formation of high amounts of porosity is the main reason for obtaining such low flexural strengths for samples with TiB2 reinforcement. As the grain size of samples is approximately the same, this factor cannot be crucial. Furthermore, the interfacial bonding between the TiC matrix, SiCw and TiB2 additive is strong thanks to their clean interfaces and diffusion of the existence phases into each other. However, the formation of the brittle phase of TiSi due to the reaction between TiB2 and SiCw possibly can be another chief factor in dropping the flexural strength to such poor levels.
4. Conclusions The influence of various TiB2 content (0, 10, 20, and 30 vol%) on the microstructure, relative density, hardness, flexural strength, and thermal conductivity of SPSed TiC-10 vol% SiCw-based composites are studied. The conclusions were as follows:
3.4. Thermal conductivity
1 The microstructural evaluation and XRD analysis revealed the formation of the brittle phases of TiSi and Ti3SiC2.
Fig. 12 illustrates the thermal conductivity of SPSed samples with various amounts of TiB2 additive. Firstly, it should be mentioned that 6
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Fig. 8. SEM images of SPSed TiC-10 vol% SiCw with different vol% of TiB2: (a) 0, (b) 10, (c) 20, and (d) 30.
Fig. 9. SEM image of SPSed TiC-10 vol% SiCw-30 vol% TiB2.
2 The best relative density of 98.73% is obtained for the specimen with no TiB2 content, showing the destructive role of TiB2 additive on the RD of TiC-10 vol% SiCw-based samples. 3 The most significant Vickers hardness (27.67 GPa) and flexural strength (511 MPa) of as-sintered composite samples belong to the samples with 30 vol% and 0 vol% TiB2, respectively, while the samples with 10 vol% and 30 vol% TiB2 present the weakest mentioned values. 4 Finally, the thermal conductivity investigation shows that adding more than 20 vol% TiB2 secondary phase played a positive impact on this characteristic, as the thermal conductivity of the TiC-10 vol % SiCw-30 vol% TiB2 sample increases by around 50% in comparison with the one with no TiB2 content.
Fig. 10. Vickers hardness of SPSed TiC-10 vol% SiCw specimens with various content of TiB2.
Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
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Fig. 11. Flexural strength of SPSed TiC-10 vol% SiCw specimens with various content of TiB2. [13]
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Fig. 12. Thermal conductivity of SPSed TiC-10 vol% SiCw specimens with various contents of TiB2.
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Acknowledgments This research work was financially supported by Aliyazh Sanat Sahand Ipak Company, Tabriz, Iran (Grant No. 971210-3), and the authors gratefully appreciate for effective support of Eng. Hamid Sharifiyan and Saeid Sharifiyan (members of the board of directors of Aliyazh Sanat Sahand Ipak Company).
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Influence of TiB2 content on the properties of TiC–SiCw composites Mehdi Fattahia, Yaghoub Pazhouhanfarb, Seyed Ali Delbaric, Shahrzad Shaddeld, Abbas Sabahi Naminie,f,∗, Mehdi Shahedi Aslc,∗∗ a
Institute of Research and Development, Duy Tan University, Da Nang, 550000, Viet Nam Aliyazh Sanat Sahand Ipak Company, P.O. Box: 51576-13536, Tabriz, Iran Department of Mechanical Engineering, University of Mohaghegh Ardabili, Ardabil, Iran d Department of Materials Engineering, Sahand University of Technology, Tabriz, Iran e Department of Engineering Sciences, Faculty of Advanced Technologies, University of Mohaghegh Ardabili, Namin, Iran f Department of Engineering Sciences, Faculty of Advanced Technologies, Sabalan University of Advanced Technologies (SUAT), Namin, Iran b c
A R T I C LE I N FO
A B S T R A C T
Keywords: TiC TiB2 SiC SPS Composite
The impact of various volume percentages of TiB2 additive (0, 10, 20, and 30) on the microstructure, relative density (RD), Vickers hardness, flexural strength, and thermal conductivity of as-sintered TiC-10 vol% SiCwbased composite samples were scrutinized. All four samples were sintered using the SPS method under the following circumstances; sintering temperature of 1900 °C, dwell time of 7 min, and external pressure of 40 MPa. The best relative density of 98.73% was achieved for the sample with no TiB2 additive, indicating the negative effect of TiB2 additive on the RD and formation of porosity. The microstructural observations and XRD results confirmed the chemical interaction of TiO2 and B2O3 oxide layers and SiCw and in-situ formation of the TiSi brittle phase and TiC. The most significant values of flexural strength (511 MPa) and hardness (27.67 GPa) were related to TiC-10 vol% SiCw and TiC-10 vol% SiCw-30 vol% TiB2 samples, respectively. On the contrary, the specimens with 30 vol% and 10 vol% TiB2 as additive presented the poorest qualities of flexural strength (234 MPa) and Vickers hardness (22.12 GPa). Finally, the influence of the TiB2 content on the thermal conductivity was evaluated, indicating the positive impact of this secondary phase on this characteristic, so with adding 30 vol% TiB2 to TiC-10 vol% SiCw, a thermal conductivity of 30.7 W/m.K was obtained.
1. Introduction TiC-based materials as the ultra-high-temperature ceramics (UHTCs) have newly found lots of proponents because of the wide range of properties that they provide. Low density, high melting point, acceptable electroconductivity, and thermal conductivity, excellent hardness, high wear resistance, superior chemical and thermal stability, and finally, low thermal expansivity are among the qualifications that make these kinds of materials unique [1–12]. Regarding the mentioned characteristics, TiC-based ceramics take a reliable place in the hightemperature structural applications such as leaning edge parts, rocket nozzle throat liners, hypersonic re-entry vehicles, jet engine components, and high-speed cutting tools [13–25]. Nevertheless, using such substances, especially in the monolithic form, have some limitations due to the poor thermal shock resistance and fracture toughness. These mentioned properties can lead to a failure in abrupt changes in load and temperature during the working [13,21,26,27]. Besides, the sintering of
∗
TiC is difficult too, thanks to its strong covalent bonds and low selfdiffusion coefficient [13,21]. At the same time, utilizing high sintering temperatures to overcome this problem can result in excessive grain growth and consequently, poor mechanical properties [28–37]. To overtake the described limitations, making a composite via adding a suitable sintering aid can be the remedy. During the recent years, quite a few researches have been implemented on the effect of using different metallic additives, such as Ni, Cr, Co, and Mo, and various ceramic sintering aids, including WC, SiC, TiB2, NbC, and TiN, on the mechanical and microstructural qualities of as-sintered TiC-based composite materials [38–48]. On the other hand, the problem of poor sinterability can be solved by using new processes, such as hot isostatic pressing (HIP), spark plasma sintering (SPS), etc., instead of utilizing conventional powder metallurgy technique [47–74]. Among these methods, SPS technique has provided lots of advantages thanks to its low working temperature, short holding time, and also the possibility of applying external pressure. These characteristics make this method an
Corresponding author. Department of Engineering Sciences, Sabalan University of Advanced Technologies (SUAT), Namin, Iran. Corresponding author. Department of Mechanical Engineering, University of Mohaghegh Ardabili, Ardabil, Iran E-mail addresses: [email protected] (A. Sabahi Namini), [email protected] (M. Shahedi Asl).
∗∗
https://doi.org/10.1016/j.ceramint.2019.11.236 Received 9 November 2019; Received in revised form 25 November 2019; Accepted 26 November 2019 0272-8842/ © 2019 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Please cite this article as: Mehdi Fattahi, et al., Ceramics International, https://doi.org/10.1016/j.ceramint.2019.11.236
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specimens was calculated through dividing (the bulk density × 100) by (the theoretical density). The phase analysis was implemented by an XRD machine (Philips, PW3710 X-ray), and an optical microscope (PMG3, Olympus, Japan) and a FESEM (Tescan S8000) equipped with an EDS was used for microstructural evaluation. Moreover, the thermodynamical favorability of possible chemical reactions between different phases was carried out using HSC software. The Vickers hardness tests were carried out through the application of 49 N load on the polished surfaces of TiC-based composite samples. To have an accurate value, six indentations were applied for each specimen. Flexural strength was measured through the three-point bending test by an STM250 universal testing machine. The test samples were standards with the following dimensions; 3 × 4 × 28 mm3 and span length of 15 mm. Ultimately, the thermal conductivity assessment was done by a thermal conductivity meter apparatus (Iran, Sahand Co.) at room temperature.
ideal way to produce high-quality composite materials [3,6,32,51,71,73,75–83]. Some researchers scrutinized on the influence of adding TiB2 and/or SiC as reinforcements on the microstructure and mechanical characteristics of titanium carbide-based composite samples. Mestral et al. did a complete investigation on TiB2-TiC-SiC system. The interfaces of various phases were studied using SEM and TEM to find out about the possible chemical reaction between phases and also diffusion of their elements into each other. Moreover, the hardness of ~26 GPa and the flexural strength of ~360 MPa were obtained for the TiC-based sample codoped with 16.5 vol% TiB2 and 16.5 vol% SiC [84]. The in-situ production of TiC-TiB2 composite samples also carried out using B4C and C as additives by Locci et al. The reactive SPS process was implemented to fabricate the specimens, and XRD and SEM were utilized to investigate on the in-situ produced phases [28,80,85]. Shahedi et al. studied the effect of SiC whiskers as reinforcements on the relative density, Vickers hardness, flexural strength, and thermal conductivity of SPSed TiC-based samples. They reported the relative densities more than 100% by adding 20 vol% and 30 vol% SiCw to the titanium carbide samples. Moreover, the best values of Vickers hardness and thermal conductivity achieved for the sample doped with 30 vol% SiCw, while the most significant flexural strength was related to the TiC20 vol% SiCw specimen [40]. Finally, Babapoor et al. accomplished a thorough investigation on the qualifications and limitations of monolithic TiC ceramics. They reported the sintering temperature of 1900 °C as the optimal temperature, and the following qualities obtained in this temperature: The relative density of 99.4%, Vickers hardness of 25.7 GPa, and thermal conductivity of 17.9 W/mK [48]. Although some valuable research works have been implemented on the in-situ produced TiC-TiB2 and TiC-TiB2-SiC composite samples, there is no available investigation on the influence of adding both exsitu TiB2 and SiC as reinforcements on the microstructure and mechanical properties of TiC-based composite specimens. In this research work, different volume percentages of TiB2 (0, 10, 20, and 30) were added to TiC- 10 vol% SiCw-based composites, and a relatively complete study was fulfilled.
3. Results and discussion 3.1. Consolidation behavior The relative density of SPSed composite samples is presented in Fig. 2. As shown, the most significant relative density of 98.73% was related to the sample with no TiB2 content, indicating the negative effect of this additive on this quality. With adding more TiB2 to TiC10 vol% SiCw system, the RD decreased, as the weakest value of below 93% was obtained for the specimen with 20 vol% TiB2. However, the relative density rose when the amount of titanium diboride increased to 30 vol%, standing at ~94%. The reason for such consolidation behavior can be found in the possible reaction among the initial materials over the sintering process. Shahedi et al. reported the formation of trace content of TiO2 and B2O3 on the surface of similar as-received TiB2 powders [78]. This phase can chemically react with the SiC phase based on Eq. (1), and leads to the in-situ formation of TiC and SiO2 phases. The possibility of this chemical reaction was studied through the HSC software, and, as the ΔG of this reaction is negative all along with the SPS working temperature, this reaction is favorable thermodynamically.
2. Experimental procedure
TiO2 + SiCw = TiC (in-situ) + SiO2
The starting materials were picked out among the available highquality powders. The properties of as-received powders, which all of them were supplied from Xuzhou Hongwu Nanometer Material Co., China, were as follows; TiC: particle size < 12 μm, purity > 99%, SiCw: 5 μm < length < 30 μm, 0.1 μm < diameters < 1 μm, purity > 99%, and TiB2: particle size < 50 μm, purity > 98%. Moreover, SEM images and the corresponding X-ray diffraction patterns of initial powders are presented in Fig. 1. As shown, just peaks of starting materials were detectable, indicating not the availability of unwanted phases. In this research work, four various samples were designed to study the influence of TiB2 reinforcement on the qualities of TiC-10 vol% SiCw composites. Table 1 presents the composition of these mentioned specimens. Initially, based on the information provided in Table 1, all starting materials were weighed. Afterward, the prepared powders were dispersed for 2 h in ethanol by an ultrasonic system. To reach an utterly uniform mixture, and to remove the ethanol, the mixture was heated at 80 °C using a hot plate with a magnetic stirrer. Then, the dried slurries were crushed and passed through a sieve to obtain the homogenous granules and also to minimize the agglomeration. For sintering the final powders, a graphite die lined by two layers of graphite foil was used. The foil was applied to prevent the chemical reaction between the samples and the die during the sintering process. The specimens (30 mm diameter) finally sintered by an SPS machine under the following conditions; sintering temperature: 1900 °C, dwell time: 7 min, and external pressure: 40 MPa. After removing the samples from the die, the graphite foil was eliminated by grinding. The bulk and theoretical density of SPSed samples estimated using the Archimedes principle and the rule of mixtures, respectively. Then the relative density of
(1)
On the other hand, SiO2 can react with TiO2 at temperatures higher than 5205 °C, based on the information provided by HSC software, and results in the TiSi phase and O2 (Eq. (2)). Reaching to this temperature locally at the SPS process is probable thanks to the application of high pressure. Moreover, the probable formation of TiSi also verified by the XRD analysis indicated in Fig. 3. TiO2 + SiO2 = TiSi + 2O2 (g)
(2)
In addition, B2O3 also can react with SiCw based on Eq. (3) at the gaseous form. This oxide layer melts at the temperature of 450 °C and evaporates at 1860 °C and 1 atm. However, applying external pressure can lead to the decrement of evaporation point to the level below 1600 °C [78]. The chemical reaction presented in Eq. (3) is thermodynamically feasible at temperatures more than 1750 °C (based on HSC software data), and boron carbide and two other gaseous phases are the products. Ultimately, the B4C phase can react with the TiC matrix and led to the generation of in-situ formed TiB2 and remained carbon. This equation also checked through the HSC software, and its ΔG was negative all over the sintering temperature range. 4B2O3 (g) + 7SiC = 2B4C + 7SiO (g) + 5CO (g)
(3)
B4C + 2TiC = 2TiB2 + 3C
(4)
As shown in Eqs. (2) and (3), various gaseous phases were produced alongside the TiSi and B4C phases. Forming such phases and trapping them into the matrix can be the main reason why RD dropped when TiB2 added to the composite samples in comparison with the sample 2
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Fig. 1. Scanning electron microscopy images and corresponding XRD patterns of initial powders; (a) TiC, (b) SiCw, and (C) TiB2.
with no TiB2 content. As discussed before, the sample with 30 vol% TiB2 owned higher RD compared with the one with 20 vol% additive. According Eq. (1), SiO2 was one of the byproducts of the reaction between TiO2 and SiCw. Forming such a phase activates the liquid phase sintering mechanism and improves the consolidation behavior [78]. Although this phase is produced in all three samples with TiB2 content, adding more than 20 vol% TiB2 to TiC- 10 vol% SiCw system naturally results in forming more SiO2 phase. In the TiC-10 vol% SiCw-30 vol% TiB2 sample, this phenomenon could finally be more effective in comparison with the negative impact of forming the gaseous phases, and conduct to improve the RD by 1.5%.
Table 1 The list of as-produced composite samples. Sample
TiC (vol%)
SiCw (vol%)
TiB2 (vol%)
1 2 3 4
90 80 70 60
10 10 10 10
0 10 20 30
3.2. Microstructural evaluation Fig. 4 presents the optical microscopy images of SPSed TiC-10 vol% SiCw-based composites. Looking into this Fig., three bold phases are apparent; SiCw dispersed uniformly in the TiC matrix and TiB2 (with an exemption of two-phase sample in Fig. 4a, which indicates TiC-10 vol% SiCw). The form of SiCw changes from whiskers to clusters of intertwined form. It also should be mentioned that the big black holes are not associated with the porosities, but the pull-out grains during the sample preparation (grinding & polishing). The back-scattered SEM images of as-sintered samples are exhibited in Fig. 5. The dark-colored phases are related to SiC whiskers distributed homogeneously in the bright-colored TiC matrix. The greycolored phases also belong to the TiB2 additive. The uniform dispersion of secondary phases is shown in the EDS-mapping of Ti, Si, B, and C elements presented in Fig. 6. This kind of distribution helps secondary phases to play effectively as an inhibitor against the excessive grain growth over the sintering process. As it is clear, adding TiB2 reinforcement conducted to the formation of lots of porosity in the samples that follow the results obtained for the relative density. Fig. 7
Fig. 2. The relative density of SPSed TiC-10 vol% SiCw-(0, 10, 20, and 30 vol%) TiB2 specimens.
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Fig. 3. XRD patterns of SPSed TiC-10 vol% SiCw composite samples with (a) 0 vol% TiB2, and (b) 30 vol% TiB2.
similar. In Fig. 9, which is related to the SPSed TiC-10 vol% SiCw-30 vol % TiB2 specimen, the pores resulted in the incomplete consolidation can be seen obviously. Apparently, the sintering conditions were not appropriate for coalescing these intergranular pores.
indicates a magnified SEM image of SPSed TiC-10 vol% SiCw-20 vol% TiB2 and corresponding EDS point analysis. According to the presented information, points A, B and C are related to TiB2, TiC, and SiC, respectively. Moreover, point D can be possibly associated with the Ti3SiC2 phase, which detected in the XRD pattern (Fig. 3). Also, the high Si content in this EDS can be due to the influence of adjacent SiC particles. The SEM fractographs of SPSed samples are shown in Fig. 8. As it is observable, the intergranular mode was the predominant fracture mode in all four samples. Increasing the porosities in the samples with high TiB2 content is utterly obvious that, as discussed before, is probably because of the formation of some gaseous phases during the sintering process. Even though some large grains can be distinguished in these fractographs, the average grain sizes of all different samples are roughly
3.3. Mechanical properties The values of Vickers hardness of SPSed TiC-10 vol% SiCw-based samples are exhibited in Fig. 10. The Vickers hardness of ~24.5 GPa was obtained for the sample with no TiB2 content. Although titanium carbide presents a high level of hardness thanks to its strong covalent bonds, coexisting with SiCw has been possibly useful in reaching this value of Vickers hardness through the hindering the move of dislocations. Adding TiB2 led to a drop in this quality, as the weakest value of
Fig. 4. Optical microscopy images of SPSed TiC-10 vol% SiCw with different vol% of TiB2: (a) 0, (b) 10, (c) 20, and (d) 30. 4
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Fig. 5. SEM images of SPSed TiC-10 vol% SiCw with different vol% of TiB2: (a) 0, (b) 10, (c) 20, and (d) 30.
the amount of TiB2 content played the dominant role in the hardness of these specimens. As discussed before, adding TiB2 up to the level of 20 vol% had a destructive role on RD, so lower hardness values for samples with 10 vol% and 20 vol% TiB2 in comparison with the one with no titanium diboride content makes sense. On the other hand, TiB2
Vickers hardness belongs to the specimen with 10 vol% TiB2, standing at just above 22 GPa. However, with the addition of more titanium diboride to the composite samples, the hardness starts to increase, as the one with 30 vol% TiB2 surpasses the one with no titanium diboride content and reaches to 27.67 GPa. Apparently, the relative density and
Fig. 6. SEM image of SPSed TiC-10 vol% SiCw-30 vol% TiB2 and related EDS elemental maps. 5
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Fig. 7. SEM image of SPSed TiC-10 vol% SiCw-20 vol% TiB2 and the related EDS analysis.
TiB2 presents a higher thermal conductivity at room temperature compared with the TiC-10 vol% SiC samples (96 versus ~20 W/mK, respectively), so the addition of TiB2 additive to the TiC-10 vol% SiC specimen can result in an increment in thermal conductivity [40,86]. However, when a secondary phase is discontinuous in the matrix, the thermal conductivity of a composite is dominantly controlled by the matrix conductivity. Looking into Fig. 12, adding 10 vol% TiB2 resulted in a drop in the thermal conductivity of the samples. According to the formation of porosities and also new grain boundaries, this decrease in the conductivity makes sense. Even though, the addition of more volume percentages of titanium diboride led to an improvement in this characteristic, so the sample with 30 vol% TiB2 reaches to the level of thermal conductivity more than 30 W/m.K. The reason may be due to the much higher thermal conductivity of TiB2 compared with TiC matrix and also the possibility of formation of a continuous network of TiB2 at high volume fractions.
is a harder phase compared with the TiC matrix, so adding such a phase can improve the hardness of the samples. The influence of this issue was so predominant, that TiC-10 vol% SiCw-30 vol% TiB2 sample reached the hardness level of higher than TiC-10vol SiCw, while its RD was lower. The values of the flexural strength of as-sintered specimens are presented in Fig. 11. As shown in this Fig., the most significant flexural strength value of 511 MPa is related to the TiC-10 vol% SiCw sample and adding more TiB2 reinforcement continuously decreases this quality. This effect is so severe that the sample with 30 vol% TiB2 reaches the value of less than half of the value obtained for the specimen without TiB2 content. The main parameters that are effective on flexural strength are RD, grain size, and interfacial bonding between various phases. It seems that the formation of high amounts of porosity is the main reason for obtaining such low flexural strengths for samples with TiB2 reinforcement. As the grain size of samples is approximately the same, this factor cannot be crucial. Furthermore, the interfacial bonding between the TiC matrix, SiCw and TiB2 additive is strong thanks to their clean interfaces and diffusion of the existence phases into each other. However, the formation of the brittle phase of TiSi due to the reaction between TiB2 and SiCw possibly can be another chief factor in dropping the flexural strength to such poor levels.
4. Conclusions The influence of various TiB2 content (0, 10, 20, and 30 vol%) on the microstructure, relative density, hardness, flexural strength, and thermal conductivity of SPSed TiC-10 vol% SiCw-based composites are studied. The conclusions were as follows:
3.4. Thermal conductivity
1 The microstructural evaluation and XRD analysis revealed the formation of the brittle phases of TiSi and Ti3SiC2.
Fig. 12 illustrates the thermal conductivity of SPSed samples with various amounts of TiB2 additive. Firstly, it should be mentioned that 6
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Fig. 8. SEM images of SPSed TiC-10 vol% SiCw with different vol% of TiB2: (a) 0, (b) 10, (c) 20, and (d) 30.
Fig. 9. SEM image of SPSed TiC-10 vol% SiCw-30 vol% TiB2.
2 The best relative density of 98.73% is obtained for the specimen with no TiB2 content, showing the destructive role of TiB2 additive on the RD of TiC-10 vol% SiCw-based samples. 3 The most significant Vickers hardness (27.67 GPa) and flexural strength (511 MPa) of as-sintered composite samples belong to the samples with 30 vol% and 0 vol% TiB2, respectively, while the samples with 10 vol% and 30 vol% TiB2 present the weakest mentioned values. 4 Finally, the thermal conductivity investigation shows that adding more than 20 vol% TiB2 secondary phase played a positive impact on this characteristic, as the thermal conductivity of the TiC-10 vol % SiCw-30 vol% TiB2 sample increases by around 50% in comparison with the one with no TiB2 content.
Fig. 10. Vickers hardness of SPSed TiC-10 vol% SiCw specimens with various content of TiB2.
Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
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Fig. 11. Flexural strength of SPSed TiC-10 vol% SiCw specimens with various content of TiB2. [13]
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Fig. 12. Thermal conductivity of SPSed TiC-10 vol% SiCw specimens with various contents of TiB2.
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Acknowledgments This research work was financially supported by Aliyazh Sanat Sahand Ipak Company, Tabriz, Iran (Grant No. 971210-3), and the authors gratefully appreciate for effective support of Eng. Hamid Sharifiyan and Saeid Sharifiyan (members of the board of directors of Aliyazh Sanat Sahand Ipak Company).
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