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Original Article
2025
:18;
2762024
doi:
10.25259/AJC_276_2024

Self-propagating high-temperature synthesis of Ti₃SiC₂/diamond composites in a microwave field with the assistance of Ni-Al powders

, , , , , ,
aDepartment of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming University of Science and Technology, Kunming, 650093, Yunnan, China
bState International Joint Research Center of Advanced Technology for Superhard Materials, Kunming University of Science and Technology, Kunming, 650093, China
cState Key Laboratory of Complex Nonferrous Metal Resources Clean Utilization, Kunming University of Science and Technology, Kunming 650093, China

Corresponding authors: Email addresses: stoneye2@163.com (X. Ye); yanglikmust@163.com (L. Yang)

Received: , Accepted: ,
© 2025 Arabian Journal of Chemistry - Published by Scientific Scholar
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Abstract

In this study, a self-propagating high-temperature synthesis (SHS) process was initiated within a microwave field, utilizing the combustion of Ni-Al powders to fabricate Ti3SiC2-based diamond composite materials. To promote the formation of Ti3SiC2, aluminum powders were incorporated into a mixture of elemental Ti, Si, and C powders, along with diamond abrasives, as the raw materials. The effects of aluminum addition and diamond particle size on the phase composition and microstructure of the composites were thoroughly investigated. Under microwave-assisted SHS conditions, the ignition time for the SHS process was significantly reduced to 374 s when the premixed molar ratio of Ti:Si:C:Al was optimized to 3:1:2:0.4, and combined with a diamond particle size of 140/170 mesh. X-ray diffraction (XRD) analysis revealed that the highest conversion rate of Ti3SiC2, reaching 54%, was achieved at a molar ratio of Ti: Si: C: Al = 3:1:2:0.2 and a diamond particle size of 140/170 mesh. Additionally, the maximum wear ratio of 712.85 was observed when the diamond size was 70/80 mesh, with a Ti:Si:C:Al molar ratio of 3:1:2:0.2. Scanning electron microscopy coupled with energy-dispersive spectroscopy (SEM-EDS) revealed that the fracture surface exhibits appropriate interface interactions between the matrix and diamond particles, which supports controlled grain retention and promotes self-sharpening behavior that is critical to diamond grinding wheel performance. The high efficiency of the SHS synthesis process in the microwave field, along with the wear resistance of MAX-phase-bonded diamond composites, provides a promising pathway to reduce manufacturing costs and energy consumption in the production of diamond wheel.

Keywords

Microwave sintering
Ni-Al powders
Self-propagating high-temperature synthesis
Ti3SiC2 bond diamond composite

1. Introduction

The ceramic matrix diamond exhibits remarkable self-sharpening, high grinding efficiency, and exceptional precision [1-6], which has been widely utilized in the processing of materials, geological drilling, precision instrument processing, stone processing, and infrastructure engineering [7-9]. However, the production of ceramic matrix diamond wheels is hindered by challenges such as inadequate bonding between the diamond and ceramic matrix [10], high energy demands, and extended processing times. Therefore, numerous studies have focused on improving the interfacial bonding and manufacturing efficiency of ceramic matrix diamond composites. Consequently, extensive research has been directed toward enhancing interfacial bonding and manufacturing efficiency in ceramic matrix diamond composites. Over the past decade, the ternary layered compound referred to as the Mn+1AXn phase (MAX) have garnered significant attention in various applications, including high-temperature components, foil bearings, burner nozzles, rubber molds, and metal cutting tools [11-14]. This interest stems from their unique combination of properties, such as high elastic modulus, excellent high-temperature resistance, low thermal expansion coefficient, and remarkable oxidation resistance [12,13]. Furthermore, the high thermal conductivity of MAX phase is beneficial in promoting a favorable interfacial bond between the diamond and the binder [15-20].

MAX phases (layered ternary carbides/nitrides with the formula Mₙ₊₁AXₙ), such as Ti3SiC2​, have been extensively studied as ceramic matrix for diamond grinding wheels. For instance, Jaworska et al. prepared Ti3SiC2-based diamond composite by using a high-pressure sintering method at 1400°C, and the composite has been proven to have good bonding properties and excellent wear resistance [21]. Eduardo et al. studied the effects of the content of Ti, SiC, and C, heat treatment temperature, and time on the properties of high-purity Ti3SiC2 [22]. They identified 1300°C as the optimal sintering temperature for achieving the best material performance. Chahhou et al. explored the influence of SiC on the phase composition of Ti3SiC2, composites with up to 50 vol % and 60 vol % of SiC were successfully synthesized at 1500°C [23]. Compared with traditional sintering, self-propagating high-temperature synthesis (SHS) has become increasingly popular in the preparation of Ti3SiC2 matrix composites due to its advantages of low energy consumption and high productivity. Yeh et al. employed the SHS method to produce Ti3SiC2 from elemental powder compact and TiC samples at 1150°C. They achieved an impressive conversion rate of 85% by volume, demonstrating the efficiency and potential of SHS for synthesizing high-quality Ti3SiC2 composites [24]. Moreover, the addition of sintering aids is beneficial to improve the conversion rate and reduce the synthesis temperature​ [25-35]. However, high sintering temperatures and extended sintering times often lead to the graphitization of diamond during sintering [36]. As a result, researchers have focused on developing methods to reduce both the sintering temperature and duration.

Microwave heating involves the use of electromagnetic wave energy to induce heat within a substance through energy absorption. Unlike traditional thermal heating methods, which rely on heat conduction, thermal diffusion, and thermal radiation to elevate temperature, microwave heating offers advantages such as volumetric heating, selective heating, rapid heating rates, and quick start-stop capabilities [37-42]. When applying microwave heating technology to the self-propagating synthesis of Ti3SiC2, the internal heating characteristics of microwaves can significantly enhance the properties of the material. However, initiating the SHS of Ti3SiC2-diamond compacts in a microwave field often necessitates heating the samples to temperatures exceeding 1000°C [36]. Particularly when the thickness of the compact greatly exceeds the penetration depth of microwaves, this can limit the heating rate of the sample [36]. Prolonged high-temperature exposure may lead to thermal damage to the diamond. Therefore, there is a pressing need to explore a more effective novel method.

The M-Al (M = Ti, Ni, Fe, Nb, Cu) system, when mixed in appropriate proportions, generates a significant amount of heat during the sintering process [43]. According to reference studies [43], it has been reported that mixing Ti powder and Al powder in a 1:1 ratio yields a high adiabatic temperature of 1244.85°C. Experimental results indicate that the Ti-Al alloy can induce self-propagating sintering reactions in the samples, but the reproducibility of the experiments is relatively low. Meanwhile, Ni-Al mixed in a 1:1 ratio yields a high adiabatic temperature of 2009.85°C [43]. The high adiabatic temperature ensures that the sample can successfully induce self-propagating sintering reactions in each experiment.

The present study proposes a novel microwave sintering process by introducing high-enthalpy Ni-Al mixed powders as an auxiliary agent into the Ti-Si-C-Al-diamond system to produce Ti3SiC2 bond diamond composites. Utilizing microwave heating in the low-temperature regime, the Ni-Al mixed powders undergo an exothermic alloying reaction, thereby triggering the self-propagating sintering of Ti3SiC2-based diamond composites. The comprehensive performance of Ti3SiC2-based diamond composites was systematically evaluated, considering the impact of sintering methods, raw material compositions, and diamond particle size. This investigation employed X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and grinding tests. This method leads to a decrease in the ignition temperature and duration, ultimately reducing manufacturing costs and energy consumption. This advancement holds considerable potential for the manufacturing of high-performance diamond grinding tools with ceramic binders, enabling a reduction in energy consumption during production.

2. Materials and Methods

2.1. Experimental materials

The synthesis employed titanium powders titanium powders (purity ≥99.5%, average particle size 74 μm), silicon powders (purity ≥99%, average particle size 45 μm), graphite powders (purity ≥99.95%, average particle size 45 μm), nickel powders (purity ≥99.9%, average particle size 45 μm), and aluminum powders (purity 99.95%, average particle size 1–2 μm). Diamond abrasives with particle sizes of 70/80 mesh (180–212 μm), 140/170 mesh (90–106 μm), and 170/200 mesh (75–90 μm) were also incorporated. All the elemental powders were directly used without further purification.

2.2. Preparation method

The compositions of raw materials have been presented in Table 1, and two pellets were prepared for each experiment. The first pellet was composed of Ti-Si-C-Al powders and diamonds. The mixture of powders of Ti-Si-C-Al was initially subjected to a planetary ball mill for 40 min at a rotary speed of 240 rpm. Subsequently, diamond abrasives with a mass fraction of 10% were added to the mixed powders, and the milling process was continued for another 20 min to ensure thorough mixing. After mixing, 10 grams of the mixture powder were poured into a compression mold with a diameter of 25 mm (GCr25) and cold-pressed into cylindrical preforms at an external pressure of 30 MPa for 5 min to yield cold-pressed pellets. The second pellet was an auxiliary heating pellet, which was prepared by mixing Ni and Al powders in a 1:1 ratio and compacting under the same pressure and time conditions as described above.

Table 1. The molar ratios of raw powders and the quantity of Ni-Al mixed powders.
Nomination Molar ratios Diamond content (wt%) Ni-Al powders (g)
Al Ti:Si:C:Al——3:1:2:0.1 10 5
Ti:Si:C:Al——3:1:2:0.2 10 5
Ti:Si:C:Al——3:1:2:0.3 10 7
Ti:Si:C:Al——3:1:2:0.4 10 7

After the pellet preparation, the first pellet (Ti/Si/C/Al) was placed above the second pellet (Ni-Al), and then both were positioned together on graphite blocks. Subsequently, they were transferred into a microwave tube furnace (HY-ZG3012) under a protective atmosphere of Ar gas at a flow rate of 20 L/h. The microwave frequency was set to 2.45 GHz, with the output power fixed at 3 kW. For each microwave sintering process, the microwave output was maintained for 30 s after the ignition of the self-propagating reaction. After switching off the microwave heating, the sample cooled naturally to 20°C to obtain the Ti3SiC2 bond diamond specimen. In conventional sintering experiments, the cold-pressed Ti/Si/C/Al pellets were sintered in a tubular furnace (YEK60X600/130-YC) under the protection of Ar atmosphere. The power setting was fixed at 3 kW during the entire sintering process. After the sample’s temperature reached 1150°C, the sample was held at 1150°C for 30 s and finally furnace cooling to room temperature. The temperature was measured using an infrared thermometer (SENTEST/NS10PH2CF2). Upon completion of the experiment, Ti3SiC2-based diamond composite materials were produced for subsequent characterizations.

Additionally, as shown in Table 1, when the additive Al ranges from 0.1 to 0.2 mol, 5g of Ni-Al mixed powders was adequate to initiate the SHS reaction. However, when the additive Al ranges from 0.3 to 0.4 mol, 7g of Ni-Al mixed powders was required to initiate the SHS reaction.

2.3. Analytical testing methods

After the SHS reaction, the samples were analyzed for phase composition by using XRD (Cu Kα, X’Pert3MRD). The characterization of the sample’s grinding performance was conducted according to the JB/T 3235—2013 standard using self-developed equipment. As shown in Figure 1, the system consists of a reciprocating worktable (oscillation speed: 19–21 mm/s) and a flat-shaped SiC grinding wheel (ceramic bond, 80-mesh grit) rotating at a linear speed of 25 m/s. During testing, the sample and the SiC grinding wheel are brought into mutual contact under controlled conditions. The wear behavior is evaluated by calculating the wear ratio E, defined as the ratio of the volume loss of the grinding wheel to that of the sample. After the testing of wear performance, the micro-morphological features of the fracture surfaces were observed by using a SEM (Nova NanoSEM 450).

Schematic diagram of grinding performance characterization equipment.
Figure 1.
Schematic diagram of grinding performance characterization equipment.

Based on the XRD data, the content of Ti3SiC2, TiC, and Ti5Si3 phases in the samples were calculated by using the semi-quantitative Eqs. (1-3) [26].

(1)
ω T S C = I T S C I T S C + 4.519 I T S + 0.818 I T C

(2)
ω T S = I T S I T S + 0.240 I T S C + 0.197 I T C

(3)
ω T C = I T C I T C + 1.222 I T S C + 5.084 I T S

where, ωTSC, ωTS, and ωTC represent the material mass fraction of Ti3SiC2, TiC, and Ti5Si3, respectively. Moreover, ITSC, ITS, and ITC denote the integrated peak intensities of the Ti3SiC2 (104), TiC (111), and Ti5Si3 (102) diffraction peaks, respectively.

3. Results and Discussion

3.1. Effects of various sintering processes on heating characteristics

The temperature curves of cold-pressed pellets during various heating processes have been shown in Figures 2-3, including the traditional oven heating, microwave heating, and microwave heating assisted by Ni-Al powders. As illustrated in Figure 2, the microwave heating process consists of two distinct stages. In the initial stage, the sample temperature soars from room temperature to 1030°C within 15 min, corresponding to a heating rate of 66°C/min. The second stage starts at 1030°C and ceases at 1150°C, with a decreased heating rate of 4°C/min. The decreased heating rate could be attributed to the increased heat loss at high temperatures. The overall heating rate of the microwave heating process was 28.6°C/min, significantly surpassing the traditional oven heating rate of 9°C/min.

Heating curve of Ti-Si-C system under Ar atmosphere: microwave heating and conventional heating without Ni-Al mixed powders.
Figure 2.
Heating curve of Ti-Si-C system under Ar atmosphere: microwave heating and conventional heating without Ni-Al mixed powders.
Heating curve of Ti-Si-C system under Ar atmosphere: microwave heating with Ni-Al mixed powders.
Figure 3.
Heating curve of Ti-Si-C system under Ar atmosphere: microwave heating with Ni-Al mixed powders.

It could be observed from Figure 3 that the combustion of the Ni-Al mixture triggered a self-propagating reaction in the Ti-Si-C-diamond system, as evidenced by a rapid temperature increase from 572.4°C to 1300°C within 10 s. The incorporation of Ni-Al powder cold pellets can significantly improve the sintering efficiency.

Figure 4 depicts the heating curves for microwave sintering processes assisted by Ni-Al powders with different diamond particle sizes. By utilizing Ni-Al mixed powders to assist in microwave-induced reactions, the Ti-Si-C-diamond systems with varying ratios successfully induce thermal explosion reactions within the ignition temperature range from 568.4°C to 750.7°C and ignition time ranges from 334 s to 622 s. The ignition temperature was lower than the diamond graphitization temperature (900°C) [44], and the overall sintering time was less than 622 s. Compared with the conventional thermal sintering process, the overall sintering time can be reduced from 8000 s to 600 s, which significantly improves the sintering efficiency. Moreover, the ignition temperature of self-propagating combustion decreases with increasing Al content. This is because the molten Al at high temperature can fill the gap between particles and provide a bridging effect [28]. Meanwhile, Al addition enhances the diffusion of Ti and Si, thereby reducing the ignition temperature [28]. However, increasing the diamond particle size will reduce the interfacial contact among various phases, forming a high kinetic barrier during the reaction, which slows down propagation and prolongs the reaction time [45]. Therefore, under the same ratio, the ignition times of self-propagating combustion occur earlier when the diamond size is 140/170 and 170/200 than that of 70/80 mesh.

Temperature curves of samples with different ratios and different diamond grain sizes.
Figure 4.
Temperature curves of samples with different ratios and different diamond grain sizes.

3.2. Phase analysis

The XRD patterns and phase contents of samples prepared by using various methods have been shown in the Figures 5-7. XRD analyses confirmed that Ti3SiC2 bond diamond composites were successfully synthesized by using SHS with the assistance of the combustion of Ni-Al. Moreover, XRD patterns revealed the combination of phases including Ti3SiC2, TiC, Ti5Si3, and C (diamond), which aligns with other reports [46,47]. XRD analysis revealed the presence of Ti3SiC2 (peaks at 2θ = 39.7°, 40.9°, and 42.6°), TiC (peaks at 2θ = 35.9°, 41.7°, and 60.4°), and Ti5Si3 (peaks at 2θ = 36.8°, 37.6°, and 66.5°) phases in the sintered composites. Additionally, peaks at 2θ = 43.9° and 75.3° were associated with C (diamond). The synthesis of Ti3SiC2 involves a series of complex chemical reactions. At the lower temperature stage, in a Ti-rich environment, Ti, Si, and C initially reacted to form TiC and Ti5Si3CX. As the temperature increases, Ti reacts with C to form TiC, and then Ti reacts with Si to form Ti5Si3, accompanied by some side reactions. Subsequently, TiC, Ti, and Si reacted to produce Ti3SiC2. Finally, Ti5Si3 reacted with TiC and additional C, further promoting the formation of Ti3SiC2 [48,49]. The significant Eqs (4)-(7) relevant to this study are as follows [34,47]:

(4)
T i + C = T i C

(5)
5 T i + 3 S i = T i 5 S i 3

(6)
2 T i C + T i + S i = T i 3 S i C 2

(7)
T i 5 S i 3 + 4 T i C + 2 C = 3 T i 3 S i C 2

XRD analyses for the samples containing 70/80 mesh: (a) XRD patterns of the Ti–Si–C samples after Ni/Al assisted microwave sintering; (b)Identify phase mass fraction diagrams.
Figure 5.
XRD analyses for the samples containing 70/80 mesh: (a) XRD patterns of the Ti–Si–C samples after Ni/Al assisted microwave sintering; (b)Identify phase mass fraction diagrams.
XRD analyses for the samples containing 140/170 mesh: (a) XRD patterns of the Ti–Si–C samples after Ni/Al assisted microwave sintering; (b)Identify phase mass fraction diagrams.
Figure 6.
XRD analyses for the samples containing 140/170 mesh: (a) XRD patterns of the Ti–Si–C samples after Ni/Al assisted microwave sintering; (b)Identify phase mass fraction diagrams.
XRD analyses for the samples containing 170/200 mesh: (a) XRD patterns of the Ti–Si–C samples after Ni/Al assisted microwave sintering; (b)Identify phase mass fraction diagrams.
Figure 7.
XRD analyses for the samples containing 170/200 mesh: (a) XRD patterns of the Ti–Si–C samples after Ni/Al assisted microwave sintering; (b)Identify phase mass fraction diagrams.

As depicted in Figure 5, increasing the Al additive ratio from 0.1 to 0.4 led to a progressive increase in the Ti3SiC2 diffraction peak intensity in the XRD pattern for diamond particles of 70/80 mesh. XRD-based phase content calculations indicated that the Ti3SiC2 phase exhibits a minimum mass fraction of 32.75% at an Al ratio of 0.1, and reaches a maximum mass fraction of 48.89% at an Al ratio of 0.3. As the amount of Al added increases, the content of Ti3SiC2 in the product significantly rose. Correspondingly, the contents of Ti5Si3 and TiC decreased significantly. This is consistent with Eqs. (4)-(7) that Ti5Si3 and TiC were intermediate products and they were continuously consumed during the formation of Ti3SiC2, and were continuously synthesized by the raw materials, and the remaining portions eventually form a thermodynamically stable phase with Ti3SiC2. According to the XRD results, the addition of an appropriate amount of Al can eliminate silicates and significantly promote the synthesis of Ti3SiC2.

As depicted in Figure 6, for a diamond size of 140/170 mesh, the intensity of the Ti3SiC2 diffraction peak was the highest when the addition of Al powder reached 0.3 mol, indicating the highest content of the Ti3SiC2 phase among the four samples. Upon further increasing the Al powder addition to 0.4 mol, the intensity of the Ti3SiC2 diffraction peak exhibited a decreasing trend, accompanied by a reduction in the content of the Ti3SiC2 phase, while the content of TiC and Ti5Si3 phases relatively increased. It could be deduced that a moderate addition of Al powder as an additive can facilitate the synthesis of the Ti3SiC2 phase. Calculations reveal that when the molar ratio of Al powder was 0.3, the content of the Ti3SiC2, TiC, and Ti5Si3 phases in the product was 52.61%, 25.92%, and 21.46%, respectively. At 1000°C, Al formed a liquid Al-Si alloy within the Ti-Si-C-Al mixture, thereby converting the original solid-solid reactions into liquid-solid reactions. This transformation facilitated the diffusion of Ti and Si, thereby promoting the synthesis of Ti3SiC2 [25]. A small amount of Al evaporated from the grain boundaries rather than forming a solid solution within Ti3SiC2 [50]. However, an excessive addition of the additive inhibited this effect, resulting in a reduced formation of the Ti3SiC2 phase [25].

As depicted in Figure 7, for a diamond size of 170/200 mesh, the intensity of the Ti3SiC2 diffraction peak progressively increases with the rising ratio of additive Al. Additionally, the TiC content in the system was higher when the diamond size was 170/200 than that of 70/80 and 140/170 mesh. This is because the addition of small-sized diamond particles in composite materials leads to a reduction in thermal conductivity [51,52], the barrier of atomic diffusion between materials is also reduced, which leads to the improvement of solid phase reaction. Smaller diamond size is linked to a larger specific surface area, leading to increased TiC formation on the graphitized diamond. [53,54].

3.3. Wear ratio analysis

Figure 8 summarizes the wear ratio data of Ti3SiC2/diamond composites prepared by various microwave SHS processes with the assistance of Ni-Al powders. It was observed that the highest wear ratio of 712.85 occurred with 70/80 mesh diamond particles and a Ti:Si:C:Al molar ratio of 3:1:2:0.2, while the lowest wear ratio of 28.66 was recorded with 140/170 mesh diamond particles and a Ti:Si:C:Al molar ratio of 3:1:2:0.4. The incorporation of Al formed an Al-C-Si-Ti liquid phase, which facilitated the diffusion of Ti and Si, thereby accelerating the reaction and sintering processes. Furthermore, the addition of Al reduced the twin interface energy of TiC, promoted more TiC to form Ti3SiC2, and reduced the content of TiC in the product [25,50].

Friction and wear test diagram of Ti3SiC2/diamond composites prepared by Ni-Al assisted microwave induced SHS.
Figure 8.
Friction and wear test diagram of Ti3SiC2/diamond composites prepared by Ni-Al assisted microwave induced SHS.

Phase analysis reveals that the wear ratio is closely linked to the composition of the matrix, especially for systems with the same diamond particle size. Taking the system with the highest wear ratio as an example, with 70/80 mesh diamond and an increase in the Al ratio from 0.2 to 0.3, the Ti3SiC2 content rose from 42% to 49%, while the TiC content dropped from 31% to 26%. Concurrently, the system’s wear ratio significantly decreased from 712.85 to 356.59. This suggests that TiC significantly contributes to the wear ratio in the matrix, likely due to its high strength, hardness, and wear resistance. Furthermore, TiC’s thermal expansion coefficient, similar to that of diamond, may further improve the system’s mechanical properties [55]. In contrast, in the system with the lowest wear ratio, both Ti3SiC2 and TiC contents are relatively low, underscoring the significant impact of matrix composition on the wear ratio.

3.4. Microscopic morphology analysis

Figure 9 depicts SEM images of the grinding surface of Ti3SiC2-based diamond composites synthesized by SHS with Ni-Al powders in a microwave field. The EDS point scanning results of points a and b in Figure 9 were summarized in Table 2. According to Figure 9 and Table 2, the elemental compositions of spherical particles of point a were C, Si, and Ti, with mass fractions of 17.13%, 0.71%, and 77.84%, respectively. It was evident that the molar ratio of Ti: C is approximately 1:1, while the mass fraction of Si was negligible. Combined with XRD analysis, the spherical particle could be identified as TiC. This is attributed to graphite’s higher affinity for Ti compared to Si, and at elevated temperatures, graphitization would inevitably occur on the surface of the diamond abrasives [36]. Consequently, graphite reacts with Ti to form TiC, which then diffuses into the Ti-Si system, promoting the synthesis of Ti3SiC2.

SEM of grinding surface of Ti3SiC2/diamond composites prepared by Ni-Al assisted microwave induced SHS: (a) Low-magnification; (b) High-magnification (red box marks a representative pore).
Figure 9.
SEM of grinding surface of Ti3SiC2/diamond composites prepared by Ni-Al assisted microwave induced SHS: (a) Low-magnification; (b) High-magnification (red box marks a representative pore).
Table 2. EDS point scanning results (point a and b in Figure 9).
Position Element C Si Ti
a wt% 17.13 0.71 77.84
At% 44.06 0.78 50.21
b wt% 10.23 19.39 69.28
At% 28.11 22.79 47.71

Alternatively, the elemental compositions of point b were C, Si, and Ti, with mass fractions of 10.23%, 19.39%, and 69.25%, respectively. The ratio of Ti: Si: C was approximately 3:1:2, which is consistent with the atomic composition of the Ti3SiC2. Furthermore, the presence of pores in the Ti3SiC2 layer in Figure 9(b) was primarily attributed to the intense exothermic sintering reaction, resulting in the rapid generation of a large amount of heat. Moreover, during the reaction, there was a significant difference in the solubility of liquid and solid substances. When the liquid substance condensed rapidly, the gas within the liquid substance could not escape, resulting in the formation of gas pores [56,57].

SEM images of the cross-section of Ti3SiC2/diamond composite materials after friction and wear tests are presented in Figure 10. Figures 10(a) and (b) depict the microstructure of the grinding surface of a material with the highest wear ratio of 712.85. The sample featured relatively small and evenly distributed pores, which enhanced the grip for the diamond abrasive. Figures 10(c) and (d) display the grinding surface of a material with a wear ratio of 28.66. Morphological observations show that the sample’s grinding surface was much rougher compared to Figure 10(a), with uneven pore sizes that reduced its grip on the diamond. Figure 10(d) further demonstrated the bond between the matrix and the diamond, but irregular pits around the diamond resulted in insufficient wrapping of the diamond by the matrix. In areas with larger pores, the surrounding matrix was relatively thin, increasing the likelihood of fracture and compromising the sample’s overall grinding performance.

Ti3SiC2/diamond composite friction and wear test section SEM: (a) high wear ratio low magnification diagram (70/80 mesh, Ti:Si:C:Al = 3:1:2:0.2); (b) High wear ratio high magnification diagram(70/80 mesh, Ti:Si:C:Al = 3:1:2:0.2; (c) Low wear ratio low rate diagram(140/170 mesh, Ti:Si:C:Al = 3:1:2:0.4); (d) Low wear ratio high rate diagram(140/170 mesh, Ti:Si:C:Al = 3:1:2:0.4).
Figure 10.
Ti3SiC2/diamond composite friction and wear test section SEM: (a) high wear ratio low magnification diagram (70/80 mesh, Ti:Si:C:Al = 3:1:2:0.2); (b) High wear ratio high magnification diagram(70/80 mesh, Ti:Si:C:Al = 3:1:2:0.2; (c) Low wear ratio low rate diagram(140/170 mesh, Ti:Si:C:Al = 3:1:2:0.4); (d) Low wear ratio high rate diagram(140/170 mesh, Ti:Si:C:Al = 3:1:2:0.4).

As shown in Figure 11(a), further examination of the interface between the diamond and Ti3SiC2 revealed that the fracture surface shows an appropriate interfacial interaction between the matrix and diamond particles, which supports controlled grain retention and facilitates the self-sharpening behavior critical to the performance of diamond grinding wheels. EDS analysis confirmed the presence of Ti, Si, and C elements, with no detectable Ni or Al, as shown in Figure 11(b). This indicated that the combustion of Ni-Al powders would not contaminate the sample. Furthermore, the clear stratification of the C element with Ti and Si elements at the diamond position further confirms the integrity of the diamond, as widespread graphitization, which would provide a source of C for reactions with Ti and Si elements, has not occurred.

Microstructure of Ti₃SiC₂/diamond composite transition layer: (a) SEM morphology; (b) Corresponding elemental mapping (Ti, C, Si distributions).
Figure 11.
Microstructure of Ti₃SiC₂/diamond composite transition layer: (a) SEM morphology; (b) Corresponding elemental mapping (Ti, C, Si distributions).

4. Conclusions

Ti3SiC2-based diamond composites were successfully prepared using Ni-Al powders in a microwave-assisted self-propagating high-temperature process. The Ti3SiC2 bond diamond could be prepared within 660 s, and the addition of Al powders in raw materials could promote the formation of the Ti3SiC2 phase. Specifically, with the incorporation of 0.3 mol of Al powder, the resulting product contains 52.61% Ti3SiC2, 25.92% TiC, and 21.46% Ti5Si3. Furthermore, the addition of 0.2 mol of Al additive not only promotes the synthesis of the Ti3SiC2 phase but also enables the Ti3SiC2/diamond composite material to achieve optimal grinding performance, with the highest wear ratio reaching 712.85. In this case, with a diamond size of 70/80 mesh and a Ti: Si: C: Al molar ratio of 3: 1: 2: 0.2. The SEM images reveal the good grip of diamond abrasives from Ti3SiC2 matrix, and EDS analysis indicates that the Ni-Al combustion would not contaminate the Ti3SiC2 bond diamond composite. The Ni-Al powder-assisted microwave sintering method effectively minimizes thermal damage to the diamond, reduces energy consumption, and significantly improves the grinding performance of the composites.

Acknowledgment

This work was supported by National Natural Science Foundation of China (No. 52364051, No. 52374389) and Caiyun Postdoctoral Program in Yunnan Province of China (No. CG24056E003A, No. CG24056E014A). The authors (Shenghui Guo, Yunling Scholar; Li Yang, Industrial Innovation Scholar) would like to acknowledge Yunnan Province Xingdian Talent Support Plan Project.

CRediT authorship contribution statement

Yuanjia Lu: Writing – original draft, Validation, Software, Formal analysis, Data curation. Shuhao Shi: Writing – review & editing, Supervision, Resources. Kaihua Chen: Writing – review & editing, Supervision, Resources, Project administration. Xiaolei Ye: Writing – review & editing, Methodology, Investigation, Formal analysis. Li Yang: Validation, Supervision, Funding acquisition. Ming Hou: Validation, Methodology. Shenghui Guo: Validation, Investigation, Funding acquisition.

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.

Declaration of generative AI and AI-assisted technologies in the writing process

The authors confirm that there was no use of artificial intelligence (AI)-assisted technology for assisting in the writing or editing of the manuscript and no images were manipulated using AI.

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