
==== Front
Heliyon
Heliyon
Heliyon
2405-8440
Elsevier

S2405-8440(24)13153-2
10.1016/j.heliyon.2024.e37122
e37122
Research Article
Microstructure, mechanical properties and strengthening mechanism of in-situ synthesized TiC/6061 nanocomposites
Zhuang Weibin zhuangweibin@lntu.edu.cn
⁎
Li Jinghui
Cao Qing
Qin Longjian
Jia Jing
Liu Jingfu
School of Materials Science and Engineering, Liaoning Technical University, Fuxin, 123000, China
⁎ Corresponding author. zhuangweibin@lntu.edu.cn
29 8 2024
15 9 2024
29 8 2024
10 17 e3712225 5 2024
11 8 2024
28 8 2024
© 2024 The Authors. Published by Elsevier Ltd.
2024

https://creativecommons.org/licenses/by-nc/4.0/ This is an open access article under the CC BY-NC license (http://creativecommons.org/licenses/by-nc/4.0/).
In-situ synthesized 1 wt%, 3 wt% and 5 wt%TiC/6061 nanocomposites were prepared by the reaction using Al-K2TiF6-C as starting materials. Microstructure, mechanical properties and strengthening mechanism of the nanocomposites were investigated. SEM observation illustrates the in-situ synthesized ceramic TiC particles show shape of a polygon and its average size is 60 nm. TEM results show that the interface between the Al matrix and TiC reinforcement is clear and no reaction products can be found. Grain refining can be observed in the composites, as the TiC content increased from 0 wt% to 3 wt%. However, grain coarsening appears in the 5 wt%TiC/6061 composites. As increasing the TiC content from 0 wt% to 5 wt%, the mechanical properties of the composites increase firstly and then decreases. The Vickers hardness, yield strength, tensile strength and elongation of the as-cast 3 wt%TiC/6061 composites achieve the maximum value of 80.7 HV, 135 MPa, 202 MPa and 15.3 %, respectively. Strengthening mechanisms of the TiC/6061 nanocomposites is the micromechanical strengthening mechanisms. As the TiC content increasing, CTE strengthening plays an important role.

Keywords

Aluminum matrix composites
In-situ synthesized
TiC particles
Mechanical properties
Strengthening mechanism
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pmc1 Introduction

Ceramic particles reinforced aluminum matrix composites (AMCs) can achieve outstanding properties in certain aspects, such as high specific strength, wear resistance, corrosion resistance, and thermal conductivity [1,2]. The manufacture methods of ceramic particles reinforced AMCs mainly include the ex-situ and in-situ methods. The in-situ synthesized nano ceramic particle reinforced AMCs have attracted extensive attention due to their advantages of fine particle size, uniform particle distribution, good interface bonding and stable thermodynamic state of reinforcement [[3], [4], [5], [6], [7]]. Contact Reaction Synthesis (also known as Direct Reaction Synthesis) is the most widely used to in-situ synthesize ceramic particle reinforced aluminum matrix composites among all kinds of methods [[8], [9], [10], [11]].

In-situ synthesized TiC/Al nanocomposites were prepared by reaction system of Al-Ti-C [[12], [13], [14], [15], [16]], Al-Ti-B4C [[17], [18], [19]], Al-K2TiF6-C [[20], [21], [22]]. Samal et al. fabricated the in-situ synthesized TiC/AA5052 composites using titanium and graphite powders as raw materials [12]. With the synergistic reinforcement of carbon nanotubes, the highest ultimate tensile strength and yield strength of the in-situ synthesized TiC/AA5052 were achieved to 206.44 MPa and 136.15 MPa, respectively. Yang et al. fabricated the Al-14TiC master alloy by pure Al, pure Ti and graphite [13]. The TiC size ranged from about 30 to 90 nm and the interface between the TiC and α-Al is clean and well-bonded. Ma et al. proposed a novel method of direct reaction synthesis (DRS) for hybrid-sized in situ TiC–TiB2 reinforced Al-Cu composites [17]. The strengthening mechanism of the composites was discussed. Liu et al. used Al-K2TiF6-C system to synthesize TiC particles in purity Al at a low temperature of 800 °C [20].

Compared with other systems, the Al-K2TiF6-C system can dissolve the aluminum oxide film and provide a clean liquid aluminum-molten salt interface. Moreover, the wettability between the particles and the aluminum matrix can be improved [21,23,24]. In the present work, in-situ synthesized nano TiC reinforced 6061 aluminum matrix composites were manufactured by Al-K2TiF6-C system by Contact Reaction. The effect of TiC content on the microstructure and mechanical properties of the as-cast composites was studied. Strengthening mechanism of the in-situ synthesized TiC/6061 nanocomposites was also discussed.

2 Experimental details

The 6061 aluminum alloy was selected as the composites matrix. Commercial K2TiF6 powders and carbon powders (both with a purity of 98 %) are chosen as the raw materials to synthesize ceramic TiC particles. Molar ratio of Ti: C was 1:1, according to that K2TiF6 powder and carbon powder were calculated and weighed to manufacture 1 wt%, 3 wt% and 5 wt%TiC/6061 composites. After ball milling 4 h (ball-to-powder ratio of 5:1, ball milling speed of 200 r/min), the mixture powder was pressed to many preforms. The matrix was melted in an atmosphere protection resistance furnace [25] with an accurate ±2 °C. The preforms were pressed into the liquid aluminum at 900 °C and hold temperature for 1 h. In order to obtain a good distribution of in-situ synthesized TiC, a mechanical stirring with a speed of 200 rpm/min was carried out to the melted metal. After slag removing at 720 °C, the molten were poured into a pre-heated (300 °C) graphite mold. The as-cast samples can be obtained.

The XRD test was conducted by the Shimadzu XRD-6100 with Cu Kα radiation. The Olympus OLS4000 laser scanning, JSM-7500F SEM and JEM-2100F TEM were used to observe the microstructure of the samples. Vickers hardness of the samples were tested by the HV-1000Z. The room temperature tensile tests were conducted by an electronic tensile test equipment (WDW-100E). The cross head speed was 0.5 mm/min. The plate tensile samples have a gauge length of 12 mm and a thickness of 2 mm.

3 Results and discussions

3.1 Thermodynamic analysis

In the present paper, the Al-K2TiF6-C reaction system can be described as Al-Ti-C system [15,[26], [27], [28]], chemical reactions happen as follows. The standard Gibbs free energy calculation of Al-Ti-C system is illustrated in Fig. 1.(1) [Ti]+3Al→Al3Ti

(2) 3C+4Al→Al4C3

(3) [Ti]+C→TiC

(4) 3Al3Ti + Al4C3→3TiC+13Al

(5) Al3Ti + C→TiC+3Al

Fig. 1 Standard Gibbs free energy calculation of Al-Ti-C system.

Fig. 1

It can be seen in Fig. 1 that the only stable phase is TiC, and all other phases are transformed to TiC as the reactions temperature higher than 1173 K. C will firstly react with [Ti] to produce TiC (Eq. (5)), and if there is residual C, it will react with Al to produce Al4C3 (Eq. (4)). After Eq. (5) and Eq. (4) finishing, it is almost impossible to have residual C to happen Eq. (2). Significantly Eq. (2) is impossible to occur according to the principle of Spontaneous reaction determined by Gibbs free energy. Experiments in Ref 27 also proved this results.

3.2 Phase analysis

X-ray diffraction patterns of the samples are shown in Fig. 2. Obviously, Al phase and TiC phase can be found in the in-situ synthesized TiC/6061 composites, while the Al3Ti and Al4C3 are not found. The experiment results coincide with the standard Gibbs free energy calculation in Fig. 1. This illustrates that the in-situ synthesized TiC/6061 composites are successfully prepared.Fig. 2 X-ray diffraction patterns of the samples.

Fig. 2

3.3 Microstructure observation

Fig. 3 is the optical microstructure of the samples. It is illustrated in Fig. 3(a) and (b) that the average grain size of the in-situ synthesized 1 wt% TiC/6061 composites is reduced to 115.5 μm, compared with the 6061 aluminum matrix (158.1 μm). As the TiC content increased to 3 wt%, the grain size was further refined to 60.3 μm, as shown in Fig. 3(c). However, as the TiC particle content increased to 5 wt%, the grain size increases to 129.1 μm (Fig. 3(d)). Attributing to the TiC particles provide heterogeneous nucleation for the solidification, which blocks the migration of grain boundaries, the grains fining happens in the 1 wt% TiC/6061 and 3 wt% TiC/6061 composites. Grain coarsing in the 5 wt% TiC/6061 composites may be caused by the serious aggregation of the reinforcement [29].Fig. 3 Optical microstructure of the samples (a) 6061; (b) 1 wt% TiC/6061; (c) 3 wt% TiC/6061; (d) 5 wt% TiC/6061.

Fig. 3

Fig. 4 shows the SEM micrographs of the in-situ synthesized 5 wt% TiC/6061. A lot of second phases are enriched at grain boundaries, as is shown in Fig. 4(a). The EDS analysis in Fig. 4(d) confirms that the enriched second phases are TiC particles. Fig. 4(b) is a magnification of Fig. 4(a). The shape of TiC particles shows as polygon (Fig. 4(b)). The average size of TiC particles is 60 nm (Fig. 4(c)).Fig. 4 SEM micrographs of the in-situ synthesized 5 wt% TiC/6061 (a) SEM micrograph; (b) Magnification of (a); (c) TiC particles size distribution; (d) EDS of (a).

Fig. 4

Fig. 5 is the TEM micrographs of the in-situ synthesized TiC/6061. Combining the EDS analysis and selected area electron diffraction spectrum, the Al matrix, Si particles, and TiC particles can be clearly distinguished (Fig. 5(a)). From the TEM bright field image, it can be seen that there are no reaction products at the interface between the Al matrix and TiC reinforcement. The SAED pattern as shown in Fig. 5(b) also confirms that the particles are TiC particles.Fig. 5 TEM micrographs of the in-situ synthesized TiC/6061 (a) Bright field and EDS analysis (b) SAED pattern of A.

Fig. 5

3.4 Hardness and tensile properties

Fig. 6 illustrates the Vickers hardness of the in-situ synthesized TiC/6061. The Vickers hardness of the as-cast 6061 Al matrix is 65 HV. As the TiC particles content increasing from 1 wt% to 5 wt%, Vickers hardness of the TiC/6061 composites initially rises before declining. It can be seen that Vickers hardness of the 3 wt%TiC/6061 composites reaches a peak value (80.7 HV), which is 24 % greater than that of the 6061 Al matrix.Fig. 6 Vickers hardness of the in-situ synthesized TiC/6061.

Fig. 6

Fig. 7 is the typical stress-strain curves of the as-cast in-situ synthesized TiC/6061. Fig. 8 is the effect of TiC particles content on tensile properties of the as-cast in-situ synthesized TiC/6061. It is clearly that the tensile properties of the in-situ synthesized TiC/6061 composites are higher than the 6061 Al matrix. As the TiC content increasing from 1 wt% to 5 wt%, yield strength, tensile strength, and elongation of the in-situ synthesized TiC/6061 composites first increase and then decrease. As the TiC content is 3 wt%, these properties achieve the highest value of 135 MPa, 202 MPa, 15.3 %, which increase 39.2 %, 74.1 %, 115 % than that of the 6061 Al matrix. These properties are higher than the same materials reported in literature [30].Fig. 7 Typical stress-strain curves of the as-cast in-situ synthesized TiC/6061.

Fig. 7

Fig. 8 Effect of TiC particles content on tensile properties of as-cast the in-situ synthesized TiC/6061.

Fig. 8

Fig. 9 is the tensile fracture of the as-cast in-situ synthesized TiC/6061. The fracture surface of the 6061 Al matrix showed numerous deep equiaxed dimples and torn edges (Fig. 9(a)), indicating a typical ductile failure. As the TiC content increasing, the dimples of the composites became larger and more profound (Fig. 9(b)∼(d)). This suggests that the composites have a higher ductility than the matrix. This result agrees well with the elongation results in Fig. 8.Fig. 9 Tensile fracture of the as-cast in-situ synthesized TiC/6061 (a) 6061; (b) 1 wt% TiC/6061; (c) 3 wt% TiC/6061; (d) 5 wt% TiC/6061.

Fig. 9

3.5 Strengthening mechanisms discussion

The yield strength strengthening mechanisms of the in-situ synthesized particulate reinforced Al composites mainly include load transfer strengthening and micromechanical strengthening [14,25]. Moreover, the micromechanical strengthening mechanism include CTE strengthening, grain refinement strengthening and Orowan strengthening [[30], [31], [32], [33], [34], [35], [36]]. As the volume content of particles is small (fv <5 %), the effect of load transfer strengthening will be much smaller than that of micromechanical strengthening [25,31,32]. The TiC volume content of the 1 wt% TiC/6061, 3 wt% TiC/6061 and 5 wt% TiC/6061 are 0.004 %, 0.015 % and 0.021 %. The reinforcement volume content is less than 5 %. The load transfer strengthening will not be discussed. The following discusses the quantitative contributions of micromechanical strengthening mechanisms to yield strength of the in-situ synthesized TiC/6061.(1) CTE strengthening. The coefficient thermal expansion (CTE) between the in-situ synthesized TiC particles and the Al matrix can increase the dislocation density of the composites. The CTE contributes to the yield strength increasement can be calculated using the following formula [25]:

(6) ΔσCTE=Gb12ΔαΔTVpbd(1−Vp)

where, △α is the CTE difference of the Al matrix (23.6 × 10−6 K−1) and TiC particles (7.6 × 10−6 K−1), △T is the difference of the processing temperature (900 °C) and test temperature (300 °C).(2) Grain refinement strengthening. Grain boundaries can block the dislocation slip and make the dislocations pile up, which generates the stress strengthening [25,37]. The grain refinement strengthening model is mainly derived based on the Hall-Petch relationship (Eq. (7)) combined with actual experimental conditions.

(7) Δσgrain=Δσ0+kH−PD−1/2

where, Δσgrain is the strengthen caused by grain refinement, Δσ0 is the strengthening effect caused by lattice friction stress, kH−P is the Hall-Petch parameter, and the value is 0.1 MPa M1/2, D is the average grain size of the composites. For Δσ0, as the lattice friction stress is the inherent blocking stress of periodically arranged lattices on slip dislocations in the material, Δσ0 is usually ignored when comparing and calculating the fine grain strengthening effects of matrix metals and composites.(3) Orowan strengthening. The Orowan strengthening is based on the dislocation bypass mechanism [38]. Young's modulus of the TiC is 450 GPa, which is big enough to make the dislocations in the Al matrix loop around them. This will make the composites difficult to generate plastic deformation. The strengthening model of Orowan can be expressed by Eq. 8 [25]:

(8) ΔσOR=2Gbd(π6Vp)1/3

where, G (26 GPa) and b (0.286 nm) are the shear modulus and Burgers vector of the matrix aluminum, d is the TiC average diameter and Vp is TiC volume content.

The micromechanical strengthening can be summarized by Ref. [25]:(9) ΔσTotal=Δσgrain+ΔσOR2+ΔσCTE22

The contribution calculation of micromechanical strengthening mechanisms is given in Table 1. It can be seen that calculated results (ΔσTotal) are similar to the experimental results (ΔσExperiment). It is also noteworthy that as the TiC content increasing, CTE strengthening plays an important role for the composites.Table 1 The contribution calculation of micromechanical strengthening mechanisms (unit, MPa).

Table 1Materials	ΔσGR	ΔσOR	ΔσCTE	ΔσTotal	ΔσExperiment	
1 wt% TiC/6061	9.3	2.9	9.4	19.1	19	
3 wt% TiC/6061	12.8	4.6	18.4	35.2	38	
5 wt% TiC/6061	8.8	5.1	21.8	31.2	30	

4 Conclusions

(1) In-situ synthesized TiC/6061 nanocomposites were successfully manufactured by the Al-K2TiF6-C reaction. The in-situ synthesized ceramic TiC particles show shape of a polygon and its average size is 60 nm.

(2) As the TiC content increased from 0 wt% to 3 wt%, the grain refining can be observed obviously in the composites. However, owing to the TiC aggregation, grain coarsening happens in the 5 wt%/6061 composites.

(3) As increasing the TiC content from 0 wt% to 5 wt%, the mechanical properties of the composites increase firstly and then decreases. The Vickers hardness, yield strength, tensile strength and elongation of the 3 wt%TiC/6061 composites achieve the maximum value of 80.7 HV, 135 MPa, 202 MPa, 15.3 %, respectively.

(4) Strengthening mechanisms of the TiC/6061 nanocomposites is the micromechanical strengthening mechanisms. As the TiC content increasing, CTE strengthening plays an important role.

Statements and Declarations

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.

CRediT authorship contribution statement

Weibin Zhuang: Writing – review & editing, Supervision, Funding acquisition, Conceptualization. Jinghui Li: Writing – original draft, Investigation, Data curation. Qing Cao: Software, Methodology, Investigation, Formal analysis. Longjian Qin: Software, Data curation. Jing Jia: Software, Investigation. Jingfu Liu: Writing – review & editing, Validation.

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.

Acknowledgments

This work was financial supported by Scientific Research Foundation of 10.13039/501100007620 Educational Department of Liaoning Province for Basic Research (CN) (No. LJKMZ20220670 and JYTMS20230806).
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