J. Cent. South Univ. (2021) 28: 648-656

DOI: https://doi.org/10.1007/s11771-021-4634-9

Influence of B₄C particle size on microstructure and damping capacities of (B₄C+Ti)/Mg composites

YAO Yan-tao(姚彦桃)¹, CHEN Li-qing(陈礼清)², WANG Wen-guang(王文广)³

1. School of Environmental and Safety Engineering, Liaoning Petrochemical University,Fushun 113001, China;

2. State Key Laboratory of Rolling and Automation, Northeastern University, Shenyang 110819, China;

3. School of Mechanical Engineering, Liaoning Petrochemical University, Fushun 113001, China

Central South University Press and Springer-Verlag GmbH Germany, part of Springer Nature 2021

Abstract: To study the influence of B₄C particle size on the microstructure and damping capacities of (B₄C+Ti)/Mg composites, in situ reactive infiltration technique was utilized to prepare Mg-matrix composites. The microstructure, produced phases and damping capacities of the composites prepared with different particle size of B₄C were characterized and analyzed. The results show that the reaction between B₄C and Ti tends to be more complete when finer B₄C particle was used to prepare the composites. But the microstructure of the as-prepared composites is more homogenous when B₄C and Ti have similar particle size. The strain-dependent damping capacities of (B₄C+Ti)/Mg composites improve gradually with the increase of strain amplitude, and composites prepared with coarser B₄C particles tend to have higher damping capacities. The temperature-dependent damping capacities improve with increasing the measuring temperatures, and the kind of damping capacities of the composites prepared with 5 mm B₄C are inferior to those of coarser particles. The dominant damping mechanism for the strain-damping capacity is dislocation damping and plastic zone damping, while that for the temperature-damping capacity is interface damping or grain boundary damping.

Key words: Mg-matrix composites; in situ reactive infiltration; particle size; microstructure; damping capacity; mechanism

Cite this article as: YAO Yan-tao, CHEN Li-qing, WANG Wen-guang. Influence of B₄C particle size on microstructure and damping capacities of (B₄C+Ti)/Mg composites [J]. Journal of Central South University, 2021, 28(3): 648-656. DOI: https://doi.org/10.1007/s11771-021-4634-9.

1 Introduction

Damping capacity refers to the ability of a material to convert mechanical vibration energy to thermal energy [1]. High damping materials can mitigate or eliminate the damage caused by mechanical vibration or noise, and this is of great significance in automotive, architectural industry, and aerospace areas [2-5]. Experimental investigation shows that the damping capacity of Mg is 10 times as high as that of Al, and 100 times that of 316 stainless steel [6]. Mg-matrix composites reinforced by suitable ceramic particulates, which can exhibit excellent damping capacities and mechanical properties simultaneously, have been a hot issue [7, 8].

So far, several kinds of conventional preparation methods have been developed for synthesizing Mg-matrix composite, such as stir casting [9, 10], powder metallurgy [11-14], and infiltration [15, 16]. In recent years, researchers have placed a emphasis on in situ reactive infiltration technique, and by using this method, the reinforcement can be in situ synthesized and simultaneously Mg melt infiltrates the preform [17]. Many researchers have utilized this method to prepare Mg-matrix composite [18-20] and the as-prepared composites have lots of advantages. Firstly, fine reinforcing phases with thermal stability and uniform distribution can be in situ formed, which contributes to a substantial increase of the mechanical performance of the composites. Moreover, owing to the generation of clean interface between the reinforcing phases and Mg matrix, the bonding strength of the composite is greatly improved. Finally, by tailoring the density of preform, a near-net-shape composite reinforced by ceramic particles with a high volume fraction can be obtained in an easy and cost-effective manner.

Many researchers have done profound studies about the damping capacities of Mg-matrix composite. LI et al [21] found that the damping capacity of 304/Mg composite can be increased by using infiltration casting. BABAK et al [22] found that the damping capabilities of the as-prepared composites may be adversely affected by the decrease of the particle size of the reinforcement or using Mg alloys instead of pure Mg. YU et al [23] found that Ti₂AlC, which is superior to SiC or graphite, remarkably helps the damping capacity of Ti₂AlC/AZ91D composites. DENG et al [24] found that the measuring temperature largely determined the damping capacity of AZ91 alloy and its composites. Generally speaking, the effect of the reinforcement, amplitude, frequency, temperature and alloy composition on the damping capacity of the composites and the corresponding mechanism have always been the key issue of the research.

In our previous studies [20, 25], the influence of holding time and preparation temperature on the microstructure, wear resistance and damping capacities of the as-prepared composites has been reported. The present research focuses on the effect of the particle size of B₄C on the microstructure, reinforcing phases and damping capacity of the as-prepared composites at different temperatures.

2 Experimental methods

The starting raw materials for preparing (B₄C+Ti)/Mg composites were B₄C, Ti powder and pure Mg ingot, and their detailed information was listed in Table 1. In order to study the particle size of B₄C on the in situ reactive infiltration, B₄C particle has an average size of 28, 10 and 5 mm, respectively, while Ti has a mean size of 10 mm. Pure Mg ingot was utilized as the infiltration metal.

Table 1 Starting raw materials used for preparing (B₄C+Ti)/Mg composites

As shown in Figure 1, there mainly contain two steps for preparing (B₄C+Ti)/Mg composites by this technique. The first step is the preparation of (B₄C+Ti) preform and the second is the in situ reactive infiltration. The details of the preparation can refer to Ref.[25]. It should be noted that the infiltration system was heated up to 1173 K for 90 min and the heating rate was 5 K/min.

DMA Q800 was used to test the damping capacity of pure Mg and the as-prepared composites. The specimens have dimensions of 35 mm×8 mm×1 mm. To measure the strain-dependent damping capacity at room temperature, the strain amplitude and the vibration frequency was set as 1×10^-6-1.2×10^-3 and 1 Hz, respectively. The temperature-dependent damping capacities were tested with the strain amplitude of 4×10^-4and vibration frequency of 1 Hz from room temperature to 573 K at a rate of 5 K/min.

Figure 1 Process flow diagram of in situ reactive infiltration technique for preparing (B₄C+Ti)/Mg composites

Scanning electron microscope (SEM, FEI Quanta 600) equipped with energy dispersive spectroscopy (EDS) and transmission electron microscope (TEM, Tecnai G² F20) were used to characterize the microstructure and morphology of the bending fracture surfaces of (B₄C+Ti)/Mg composites, and phase composition of the as-prepared composites was detected by X-ray diffractometer (XRD, X’Pert Pro).

3 Results and discussion

3.1 Microstructure and phase analysis

SEM micrographs of (B₄C+Ti)/Mg composites prepared with different particle size of B₄C at 1173 K for 90 min are displayed in Figures 2(a)- (c). From Figures 2(a) and (b), it can be seen that B₄C particulates in black and Ti particulates in grey with irregular shapes have a relatively uniform distribution within the matrix. There almost has no segregation or agglomeration of reinforcing particulates, or apparent pores or voids within the matrix, which means that magnesium matrix composites with nearly full densification could be obtained by using this method. Besides, we may notice that some white phases were produced around the reinforcing particulates, and they were confirmed to be titanium boride or titanium carbide by EDS (Figure 2(d)).

Figure 2 also shows that Ti in (B₄C+Ti)/Mg composites tends to be finer with the decrease of the particle size of B₄C, and when its particle size decreased to 5 μm (Figure 2(c)), Ti particulates could hardly be observed. Besides, B₄C particulates were all surrounded by thick white phases, and all of these indicate that the reaction between the starting materials tends to be more complete. Figure 2(c) also indicates that there exists obvious particulate segregation and apparent pores or voids within the composites, which means that too fine B₄C particulates may adversely affect their microstructure. When B₄C and Ti have similar particle size (Figure 2(b)), the as-prepared composites tend to have the most homogeneous microstructure.

Figure 2 SEM micrographs of (B₄C+Ti)/Mg composites prepared with different particle size of B₄C:

Figure 3 shows the XRD spectra of (B₄C+Ti)/Mg composites that correspond to Figure 2, and there mainly contain five phases, i.e., B₁₃C₂, Mg, Ti, TiB and TiC, in (B₄C+Ti)/Mg composites when B₄C is 28 μm. TiB and TiC were in situ formed in infiltration process due to preliminary chemical reaction between the starting materials. As B₄C particle size was decreased to 10 μm (Figure 3), Ti, Mg, TiB, TiC and Ti₃B₄ phases were produced within (B₄C+Ti)/Mg composites. And there mainly exist Mg, TiB, TiC, Ti₃B₄ and TiB₂ in the composites prepared with B₄C particle size decreasing to 5 μm (Figure 3). According to SHAMEKH et al [19], the final equilibrium phases of Mg-Ti-B₄C system are TiB₂, TiC and Mg. By comparing the produced phases in different conditions, it can be deduced that with decreasing B₄C particle size, the reaction between Ti and B₄C tend to be more complete. The main reason may be the much greater contacting area between the starting materials.

Figure 3 XRD spectra of (B₄C+Ti)/Mg composites prepared with different particle size of B₄C

3.2 Damping characterization

3.2.1 Strain-dependent damping capacity

The damping capacities of Mg and the as-prepared composites reinforced with B₄C of different particle size are shown in Figure 4. It is obvious that the damping capacity of the as-prepared composites is better than that of pure Mg, and the main reason may be the increase of dislocation densities within the composites. According to SIVA et al [26], the coefficient of thermal expansions (CTE) between the reinforcing phases and the metal matrix have relatively large difference, leading to a high-volume fraction of dislocation in the composites. In Figure 4, it is obvious that the strain amplitude dependent damping capacities of Mg and the composites can fall into two regions, and thus the damping Q^-1 (tand) consists of two parts [27]:

                          (1)

where Q^-1, ,mean the total damping, strain amplitude independent damping and dependent damping, respectively.

Figure 4 Strain-dependent damping capacities of (B₄C+Ti)/Mg composites prepared with different particle size of B₄C

In region 1, the damping has little to do with the strain amplitude. In region 2, at higher strain amplitude, the damping increases sharply with the strain. According to Granato-Lücke theory, the strain-dependent component directly depends on the dislocation density and follows the formula [28]:

                       (2)

                             (3)

                               (4)

where e means the strain amplitude; C₁ and C₂ are physical constants; F_B is the binding force between dislocations and weak pinning points; E is the elastic modulus; L_c and L_N are average dislocation distance between weak pinning points and strong pinning points, respectively; K is constant; b is the Burgers vector; r is the dislocation density and h is the size ratio of solvent to solute atoms.

Figure 5 Dislocation arrangement in (B₄C+Ti)/Mg composite prepared with B₄C of 28 μm

Based on Granato-Lücke mechanism [29], dislocation is pinned by strong pinning points (reinforcing particles, grain boundaries, etc.) and weak pinning points (solution atoms, vacancies, etc.) within the metal matrix. The dislocation arrangement in the composite prepared with B₄C of 28 μm is shown in Figure 5, in which dislocations were pinned by the produced phase TiC, which belongs to strong pinning points. At lower strain amplitude, dislocation strings vibrate to dissipate energy, and in this region, the damping capacity of the composites has little to do with the strain amplitude. Their damping capacities slowly improve with increasing the strain amplitude, and the unpinning of the dislocations from the weak pinning points may be the main reason for it. Above a certain strain, the dislocation unpinning between the weak pinning points occurs in a snow slide-like mode. And the dislocation strings between the strong pinning points become long and move free to dissipate energy, therefore the damping capacities of (B₄C+Ti)/Mg composites and Mg improve significantly.

Equation (2) can be alternated as Eq. (5):

                      (5)

Equation (5) reveals thatand e^-1 follow linear functional relationship, and the intercept and slope in this equation are lnC₁ and -C₂, respectively. The G-L plots of the as-prepared composites and Mg based on this equation can be obtained as Figure 6 shows. But it is apparent that the G-L plots just satisfy liner functional in very limited strain amplitude range, which means that there must exist other damping mechanisms, such as plastic zone, interface, or grain boundary damping.

Figure 6 G-L plots for (B₄C+Ti)/Mg composites prepared with different particle size of B₄C

As shown in Figure 4, the particle size of B₄C has influences on the damping capacities of (B₄C+Ti)/Mg composites. Higher tand value can be achieved by reinforcing the composite with B₄C of 28 μm, followed by that of 10 μm, and finally 5 μm. Besides the dislocation damping mentioned above, plastic zone appeared around the reinforcing particles owing to their addition within the matrix, and this also played an important role in the energy dissipation. According to CARRENO-MORELLI et al [30], the plastic zone damping can be determined according to the following equation:

                        (6)

where f_zp represents the plastic zone volume fraction; G is the shear modulus; d is the smallest dimension of the particle; s₀ is the alternating shear stress amplitude; s and e are the corresponding stress and strain acting on the specimen, respectively. The plastic zone damping is proportional to the plastic zone volume fraction and improves with the increase of it. SIVA et al [26] proposed that the plastic zone size C_s can be determined by the following equation:

                        (7)

where △a is the difference in CTEs; △T is the temperature difference; E and n are the matrix elastic modulus and Poisson ratio; s_y is the matrix yield stress and r_s is the particulate radius. Equation (7) shows that the plastic zone size is proportional to the particulate radius. Therefore, it can be deduced that the improvement of plastic zone damping of the as-prepared composites can be attributed to the increases of B₄C particle size.

3.2.2 Temperature-dependent damping characteriza-tion

The temperature-dependent damping capacities of (B₄C+Ti)/Mg composites prepared with different particle size of B₄C are shown in Figure 7. It is obvious that pure Mg always exhibits excellent damping capacity as being above 0.02 in the whole range of temperature. It can be also observed that at lower temperatures, the damping capacities of pure Mg and the as-prepared composites changed a little. Besides, the damping capacities of the as-prepared composites improved gradually with increasing the temperature as T>343 K, while that of pure Mg decreased slowly and then increased with the temperature increment, which means that their high temperature damping capacities closely related to the measuring temperature. GU et al [31] proposed that at low temperatures the intrinsic damping of constituents and dislocation damping are responsible for the damping capacity, while the primary mechanisms acting at higher temperatures are grain boundary sliding or interface sliding. At lower temperatures, the interfacial bonding strength of the composites is strong enough to restrain the occurrence of the interface damping.

Figure 8 shows the typical TEM photographs of the interface region between the reinforcing particles and Mg, and prismatic compounds are clearly seen. The grain boundaries or interface between the reinforcements and matrix are clean, which indicates good interfacial bonding. When the temperature increases, the matrix becomes soft in the first place and the interface bonding gradually becomes weak. When the friction resistance at the interface is lower than the shear stress, interface sliding will occur inevitably to dissipate energy. LEDERMAN [32] proposed a formula to describe the increase of the interface damping:

                    (8)

where m is the coefficient of friction between the ceramic particulate and metal matrix; s_r is the radial stress at the interface under the applied stress amplitude s₀; e₀ is the strain amplitude corresponding to s₀; e_crit is the critical interface strain corresponding to the critical interface shear stress t_crit at which the friction energy dissipation begins. According to Eq. (8), above certain temperature, as the interface shear stress is big enough to overcome the friction resistance (t>t_crit), the friction loss caused by the interfacial slip is the main reason of interface damping increasing with the temperature increment.

Figure 7 reveals that the damping capacity of (B₄C+Ti)/Mg composite prepared with B₄C of 28 μm is similar to that of 10 μm, and their damping capacities are obviously better than that of 5 μm. As is mentioned above, when finer B₄C particles were used to prepare composites, there exist much more contacting area between the starting materials, and thus the chemical reactions between B₄C and Ti tend to be more complete. There exists more in situ formed reinforcement and the interfacial bonding is stronger, and thus the interface microslip is unlikely to occur. Therefore, the increase of interfacial bonding played a part in the decrease of high temperature damping capacity, and this is consistent with the study of GU et al [31].

As shown in Figure 9, the improved interface bonding in the as-prepared composites can be further evidenced by their bending fracture surfaces. It is obvious that there exist lots of pulling out or debonding of reinforcing particles on the fracture surface of the composite prepared with B₄C particles of 28 μm, while there is no apparent something similar in Figures 9(b) and(c), especially in Figure 9(c), which indicates stronger interfacial bonding with decreasing B₄C particle size.

4 Conclusions

1) For preparing (B₄C+Ti)/Mg composites by in situ reactive infiltration, B₄C particle size has an important effect on the in situ reaction process. The chemical reaction between B₄C and Ti tends to be more complete when the composites prepared with finer B₄C particle size, and the microstructure of the as-prepared composites tends to be more homogeneous when B₄C has similar particle size with Ti.

2) (B₄C+Ti)/Mg composites prepared with coarser B₄C particles have higher damping capacity at room temperature, and all excel that of pure Mg. For (B₄C+Ti)/Mg composites, the dominant damping mechanisms at room temperature are dislocation damping and plastic zone damping.

3) The particle size of B₄C plays a positive role in the temperature-dependent damping capacity of (B₄C+Ti)/Mg composite at higher temperatures and the interface or grain boundaries sliding is responsible for the temperature damping.

Figure 9 SEM micrographs of bending fracture surfaces of composites prepared with different particle size of B₄C:

Contributors

YAO Yan-tao conducted the literature review and wrote the first draft of the manuscript. YAO Yan-tao and CHEN Li-qing provided the concept and edited the draft of manuscript. WANG Wen-guang edited the draft of manuscript.

Conflict of interest

YAO Yan-tao, CHEN Li-qing and WANG Wen-guang declare that they have no conflict of interest.

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(Edited by HE Yun-bin)

中文导读

B₄C颗粒尺寸对(B₄C+Ti)/Mg复合材料组织和阻尼性能的影响

摘要：由于镁或镁合金的化学活性比较高，利用常规方法制备镁基复合材料时具有一定的困难。本研究提出一种新的制备金属基复合材料的方法―原位反应浸渗技术，该方法综合了原位合成法和无压浸渗法的优势，可以低成本、简洁高效地制备出界面清洁，且增强体与基体结合良好的金属基复合材料。针对原位反应浸渗法制备的(B₄C+Ti)/Mg复合材料，研究了B₄C颗粒尺寸对其微观组织、生成物相及阻尼行为的影响规律。结果表明，B₄C颗粒尺寸越小越利于原位反应的进行，而当B₄C和Ti颗粒尺寸相近时，复合材料的组织最为均匀；该复合材料的室温阻尼性能随着振幅的增加而提高，其主要机制为位错阻尼和塑性区阻尼，高温阻尼性能随着测试温度的升高而提高，其主要机制为界面阻尼或晶界阻尼。

关键词：镁基复合材料；原位反应浸渗；颗粒尺寸；组织；阻尼性能

Foundation item: Project(51901095) supported by the National Natural Science Foundation of China

Received date: 2020-05-30; Accepted date: 2020-11-16

Corresponding author: YAO Yan-tao, PhD, Lecturer; E-mail: yaoyantao@lnpu.edu.cn; ORCID: https://orcid.org/0000-0002-8585-3197