J. Cent. South Univ. (2020) 27: 2557-2566

DOI: https://doi.org/10.1007/s11771-020-4481-0

Particle erosion of C/C-SiC composites with different Al addition in reactive melt infiltrated Si

LIU Lei(刘磊)¹, FENG Wei(冯薇)¹, LI Bo-yan(李博岩)¹, LI Jian-ping(李建平)¹, ZHANG Lei-lei(张磊磊)², GUO Yong-chun(郭永春)¹, HE Zi-bo(何子博)¹, CAO Yi(曹毅)², BAO Ai-lin(包艾琳)¹

1. School of Materials and Chemical Engineering, Xi’an Technological University, Xi’an 710021, China;

2． State Key Laboratory of Solidification Processing, Northwestern Polytechnical University,Xi’an 710072, China

Central South University Press and Springer-Verlag GmbH Germany, part of Springer Nature 2020

Abstract: Particle erosion of C/C-SiC composites prepared by reactive melt infiltration with different Al addition was studied by gas-entrained solid particle impingement test. SEM, EDS and XRD were performed to analyze the composites before and after erosion. The results indicate that a U shape relationship curve presents between the erosion rates and Al content, and the lowest erosion rate occurs at 40 wt% Al. Except for the important influence of compactness, the increasing soft Al mixed with reactive SiC, namely the mixture located between carbon and residual Si also, plays a key role in the erosion of the C/C-SiC composites through crack deflection, plastic deformation and bonding cracked Si.

Key words: C/C-SiC; Al addition; reactive melt infiltration; solid particle erosion

Cite this article as: LIU Lei, FENG Wei, LI Bo-yan, LI Jian-ping, ZHANG Lei-lei, GUO Yong-chun, HE Zi-bo, CAO Yi, BAO Ai-lin. Particle erosion of C/C-SiC composites with different Al addition in reactive melt infiltrated Si [J]. Journal of Central South University, 2020, 27(9): 2557-2566. DOI: https://doi.org/10.1007/s11771-020-4481-0.

1 Introduction

C/C-SiC composites have great potential in many fields due to their low density, high strength, good wear resistance and outstanding thermal stability [1-5]. They can be used as housings and structural elements for optical systems [6], throat insert or nozzle [7], turbine engine blade [8], piston of internal combustion engine [9], brake disc of high speed or heavy vehicles [10], armor [11] and so on. In service, they will be damaged by space debris, un-burnt particles, fine sand, fragments and other solid particles. In other word, the strength and lifespan of corresponding structural component would be weakened drastically by the particle flow. For example, the life of helicopter rotor blade decreased to 1/8 designed by solid particle erosion [12] and ablation rate of the composites in particle erosion environment was much higher than that without particle erosion [13, 14].

Up to now, particle erosion of polymer matrix composites [15], metal [16] and ceramic [17] has been greatly studied. However, to our best knowledge, few papers can be found on the erosion of the C/C-SiC composites induced by particle flow. It has been found that both more SiC and fewer pores are beneficial for the anti-erosion of C/C composites [18-21]. And the interface composition is important to the erosion resistance of SiC_f/SiC composites [22]. To make C/C-SiC composites more competent for application, there has been strong interest in optimizing their ingredients and microstructures to develop the erosion resistance [23].

Ductile Al modified C/C-SiC composites have lower preparation temperature [24], reduced manufacturing time and cost [25], higher bending strength and fracture toughness [26], and better oxidation [27] and ablation resistance [28]. Besides, based on our previous work that adding different Al in infiltrated Si could change the mechanical properties of C/C-SiC composites [24], and referencing the outstanding erosion resistance of ER7 and black gold coatings [12] which came from the optimization of soft and hard element, it can be inferred that certain amount of Al addition might improve anti-erosion ability of C/C-SiC composites.

To understand how Al addition works on the erosion, C/C-SiC composites were prepared by reactive melt infiltration and evaluated by gas- entrained solid particle impingement test. Evolutions of microstructure, morphology and element/phase distribution before and after erosion were mainly investigated to reveal the mechanism.

2 Experimental procedure

2.1 Composites preparation

Porous skeletons with size of 12 mm×12 mm× 12 mm were cut from a bulk C/C composite which was thermal gradient chemical vapor infiltrated 2.5D needle punched fabric. Densities of the fabric before and after infiltration of pyrocarbon were 0.45 and 0.95 g/cm³, respectively. The cut skeletons were cleaned in distilled water for 0.5 h by ultrasonic wave, and then dried at 100 °C for 24 h. Meanwhile, mixed powders of Si and Al with different ratios were prepared by ball milling for 1-2 h. The Si powder was 45-55 μm and the Al powder was 80-120 μm. Then the C/C skeletons were embedded into the powder mixtures in a graphite crucible and heat treated at 1100-1200 °C for 1-3 h in 10-2 Pa vacuum. After furnace cooling, the Si-Al infiltrated C/C composites were taken out from the crucible and hand-abraded with 80 and 400 grit SiC papers to remove the surface adhered powders and reacted phases. Finally, samples with dimensions of 11 mm×11 mm×11 mm were hand- polished by 400 grit SiC papers for test.

2.2 Tests and characterization

The density of the prepared composite was determined by drainage according to Archimedean principle. The erosion test was performed at room temperature in a gas-blast device which was manufactured according to ASTM G76-2007. The main parameters are listed in Table 1 and the test is illustrated in Figure 1. Compressed air-entrained 50-115 μm angular Al₂O₃+5 wt% iron-oxide particles were accelerated in an alundum nozzle tube and then sprayed from the end of the nozzle and impinged vertically to the sample surface for 20 s from 10 mm distance. The impinging stream was parallel to the web and non woven layer, as shown in Figure 1. Inner diameter and length of the nozzle tube were 3 and 100 mm, respectively. Pressure of the air was 0.4 MPa and the particle feed rate was 600 mg/s. The particle impact velocity was 70 m/s which was measured by the rotating double-disk method. The linear and mass erosion rates were calculated according to Eqs. (1) and (2).

                                 (1)

                                (2)

where R_l is linear erosion rates; Δd is the change of the sample’s thickness at centre region before and after erosion; R_m is the mass erosion rate; Δm is the change of the mass before and after erosion; t is erosion time. The samples were measured and weighed at the accuracies of 1 μm and 0.1 mg, respectively.

The phase analyses of the prepared composite were conducted by X-ray diffraction (XRD, X’Pert Pro MPD). Morphology and chemical composition were investigated by scanning electron microscopy (SEM, JSM6460) combined with energy dispersive spectroscopy (EDS).

Table 1 Key parameters of erosion test

Figure 1 Schematic of erosion test method (a) and morphology and XRD pattern of impacted solid particles (b)

3 Results and discussion

3.1 Microstructure of C/C-SiC composites

Representative cross-section morphologies of the prepared C/C-SiC composites with different Al content are shown in Figure 2. To make the following discussion convenient, the C/C-SiC composites prepared with Si powder containing 0, 10%, 20%, 30%, 40% and 50% (wt) Al were labeled as C/C-SiC-0Al, C/C-SiC-10Al, C/C-SiC- 20Al, C/C-SiC-30Al, C/C-SiC-40Al and C/C-SiC- 50Al, respectively. The densities of C/C-SiC-0Al and C/C-SiC-10Al were similar (0.95 g/cm³), while these of C/C-SiC-20Al, C/C-SiC-30Al and C/C- SiC-40Al were about 2.00 g/cm³. When the Al content increased to 50 wt%, the density of composites was 1.15 g/cm³. Obviously, C/C-SiC- 20Al, C/C-SiC-30Al and C/C-SiC-40Al got better infiltration than others, which was in accordance with the morphology in Figure 2. Some white phases located at the porous black skeleton of C/C-SiC-0Al and C/C-SiC-50Al, while C/C-SiC- 20Al and C/C-SiC-40Al were compact and composed of white, grey and black phases. Moreover, the content of grey phase in C/C-SiC- 40Al was more than that in C/C-SiC-20Al. EDS analysis indicated that the white phase was Si and the black phase was carbon. Besides, structures of all the composites were overlapped layers of non-woven layer X, web and non-woven layer Y, which were determined by the needle punched fibers fabric.

To better understand the microstructure of the prepared composites, highly magnified webs of C/C-SiC-0Al, C/C-SiC-20Al, C/C-SiC-40Al and C/C-SiC-50Al are shown in Figure 3. It was clear that there were some pores and holes in C/C-SiC-0Al and C/C-SiC-50Al, whereas the interspaces in C/C skeletons of C/C-SiC-20Al and C/C-SiC-40Al were filled completely by grey and white phases. Moreover, some white particles located at the cavity of C/C-SiC-0Al, while thin integrated white shell coated on the pyrocarbon which enwrapped carbon fiber in C/C-SiC-50Al. EDS analysis indicated that the white particle in C/C-SiC-0Al was a compound of C and Si and the shell around carbon in C/C-SiC-50Al was composed of C, Si and Al. In C/C-SiC-20Al and C/C-SiC-40Al, the white phase was Si and the grey phase was a mixture of C, Si and Al. The grey phase layer between black carbon and white Si in C/C-SiC-40Al was thicker than that in C/C-SiC- 20Al, and contained more Al. Besides, a few cracks could be found in C/C-SiC-20Al and they located at interface of carbon and grey layer (marked as Crack I). Nevertheless, a number of cracks distributed in C/C-SiC-40Al. Not only more Cracks I but also a great deal of micro-cracks in the thicker grey layer (marked as Crack II) were found in C/C-SiC-40Al.

Figure 4 shows the XRD patterns of the prepared composites. The results indicate that C/C-SiC-0Al consists of carbon and SiC, and C/C-SiC-20Al and C/C-SiC-40Al are composed of carbon, SiC, Al and Si, while C/C-SiC-50Al is composed of carbon, SiC and Al₄C₃. It is obvious that C/C-SiC-40Al has more Al than others according to the relative intensities of Al diffraction peaks at 38.47°, 44.74°, 65.13° and 78.23°. In another words, the Al content of composites increased with the rising ratio of Al in infiltrated Si and up to the maximum at 40 wt%. And then Al₄C₃ appeared at 50 wt% Al. This implies that the Al in Si powder should not exceed 40 wt% since the Al₄C₃ is an unstable phase which is always avoided during composites fabrication. Moreover, no oxides are found in the XRD analysis, which seems to be inconsistent with the EDS analysis in Figure 3. This should result from the low content of oxygen which might solute in Al. Besides, in combination with analysis of Figure 3, the grey layers in C/C-SiC- 20Al and C/C-SiC-40Al should be a mixture of SiC and Al.

Figure 2 Backscattered electron morphology of prepared C/C-SiC composites:

3.2 Erosion property of C/C-SiC composites

The erosion rates of the prepared composites are shown in Figure 5. The linear and mass erosion rates presented good consistency and the relationship between the erosion rates and Al content was a U shape curve. The sudden decline and rise of erosion rates happened at 10%-20% and 40%-50% Al (mass fraction), which were adversely proportional to the densities of composites. Besides, C/C-SiC-20Al, C/C-SiC-30Al and C/C-SiC-40Al had similar densities but different erosion rates. The better erosion resistance of C/C-SiC-40Al should come from their diverse microstructures and phase compositions.

Figure 6 shows the eroded morphology of the C/C-SiC composites corresponding to Figure 2. The web layer at surface of C/C-SiC-0Al was depleted by solid particles. Differently, non-woven layers of C/C-SiC-20Al and C/C-SiC-40Al were destructed more seriously than the web, while the different layers in C/C-SiC-50Al possessed near anti-erosion ability. Obviously, the web layer was strengthened by infiltrated Si, Al and the product of SiC. Moreover, the survived web layers of C/C-SiC-20Al and C/C-SiC-40Al were also different although they had similar high densities. The residual phases of web layer at the surface of C/C-SiC-40Al were segregated by each other but flat on the whole. Nevertheless, block white phases in the eroded web of C/C-SiC-20Al were separated. Thus, it can be inferred that the erosion mechanism varied with the density and Al content of the prepared C/C-SiC composites.

The highly magnified webs of the eroded C/C-SiC composites are shown in Figure 7. Compared with Figure 3(a), cracked carbon matrix and broken fiber in Figure 7(a) indicate that both carbon fiber and matrix are brittle. The debonding of fiber and matrix implies that more energy was consumed during the damage of the C/C skeleton. To the compact C/C-SiC-20Al and C/C-SiC-40Al, the eroded morphologies are also distinct. At surface of C/C-SiC-20Al, eroded carbon fiber, carbon matrix and other matrix phases kept good adherence to each other and there were no cracks among them. Only some cracked Si (indicated by arrow) distributed on the Si block. However, the Si (indicated by arrow) in C/C-SiC-40Al cracked completely but most of them adhered to the surface. Moreover, the fiber and matrix debonded (indicated by circle) and some fiber were peeled off (marked by ellipse). Thus, it could be concluded that the more Al and micro-cracks not only changed the failure mode of matrix, but also affected the breakage of pyrocarbon surrounded fiber. At the damaged surface of C/C-SiC-50Al, there were broken matrix, debonded fiber and matrix sheaths which came from removed fibers. The eroded characteristics of C/C-SiC-50Al were similar to C/C-SiC-40Al except for the adhered Si particles, which should be caused by the different densities.

Figure 3 Backscattered electron morphology of prepared C/C-SiC composites at high magnification and relative EDS analysis:

Figure 4 XRD patterns of prepared C/C-SiC composites

Figure 5 Erosion rates of C/C-SiC composites as function of Al content

To further clarify the erosion mechanism of the compact C/C-SiC composites, the eroded morphologies of non-woven layer and representative matrix in web of C/C-SiC-20Al and C/C-SiC-40Al are shown in Figure 8. Obviously, non-woven layer of C/C-SiC-20Al was flat and few pull-out fibers can be found, which indicates that the fracture of fiber and matrix were synchronous. However, the non-woven layer of C/C-SiC-40Al was ladder-shaped, which resulted from the detached and removed fibers (indicated by arrow). This was in accordance with the eroded characteristic in Figures 7(b) and (c). From Figures 8(c) and (d), it could be found that some scuffs (indicated by arrow) were at surface of both composites, and the scuffs in C/C-SiC-40Al were shallower and shorter. Thus, it can be inferred that the damage of C/C-SiC-20Al induced by impacted particles was more serious. Moreover, some craters and platelets (indicated by ellipse) induced by scraping and extrusion located at the surface of C/C-SiC-40Al, which was the representative feature of ductile materials.

3.3 Erosion mechanism of C/C-SiC composite

To the C/C-SiC composites in this study, there were several key constituents including carbon fiber, carbon matrix, Si matrix, a mixture matrix of SiC and Al, some pores and micro-cracks. The all constituents were smaller than the impacted Al₂O₃ particles. During normal impact of particles, brittle materials tend to crack while erosion of ductile materials involves scraping and extrusion of material to form ridges that are vulnerable to be attacked by other particles [29]. Thus the erosion of the C/C-SiC composites should involve gouging by sharp corner and strike by blunt edge of the impacted particles. Meanwhile, the impact of particles would induce crack of carbon fiber, pyrocarbon matrix and Si matrix, plastic deformation of the SiC and Al mixture, and debonding of different constituents. The schematic diagram of particle erosion of prepared C/C-SiC composites with different Al content in infiltrated Si is shown in Figure 9.

Figure 6 Eroded morphology of prepared C/C-SiC composites:

Figure 7 Morphology of eroded web of C/C-SiC composites:

For C/C-SiC-0Al, as shown in Figure 9(a), crack expansion followed fracture of pyrocarbon matrix, then fiber broken and finally damage of C/C skeleton happened, which was similar to the erosion of C/C composites [20]. The high porosity in web reduced the bearing components and accelerated the crack propagation, which resulted in the severe erosion.

To the compact C/C-SiC-20Al and C/C-SiC- 40Al, the infiltrated Si, Al and formed SiC improved the erosion resistance greatly. Their different erosion rates mainly came from the influence of Al contents in infiltrated Si. High Al content in the composites not only resulted in thicker SiC+Al layer but also induced more micro-cracks (Figure 3). The SiC+Al layer could deform under impact of particle while micro-cracks would prolong the expending path of crack (Figures 9(b) and (c)). In other words, more Al in the matrix could absorb more impact energy through plastic deformation and crack deflection, which could weaken the fragmentation of nearby brittle Si. And the Al also bonded the cracked Si and protected them from removal (Figure 7(c)). The residual cracked Si in turn prevented the binder Al from plowing, cutting and gouging. Thus both C/C-SiC-20Al and C/C-SiC-40Al were well infiltrated, but C/C-SiC-40Al presented better particle erosion resistance.

When the Al content in infiltrated Si increased to 50 wt%, the excessive reaction between Al and carbon inhibited the infiltration of molten Al-Si, which led to the low density of C/C-SiC-50Al. Although the SiC and Al₄C₃ around pyrocarbon matrix modified the anti-erosion ability of web (Figure 9(d)), the massive pores resulted in the high erosion rates.

Figure 8 Eroded morphology of C/C-SiC composites:

Figure 9 Schematic diagram of particle erosion of prepared C/C-SiC composites with different Al content in infiltrated Si:

In summary, the increasing Al in infiltrated Si powder caused different densities and microstructures of prepared C/C-SiC composites. The density was a key factor for erosion resistance. Besides, to the compact C/C-SiC, the Al content and micro-cracks in composites were important to the consumption of impact energy of particles.

4 Conclusions

C/C-SiC composites are prepared by reactive melt infiltration with different Al additions. Gas-entrained solid particle impingement test reveals a U shape relationship curve between the erosion rates and Al content, with the lowest linear and mass erosion rates occurring at 40 wt% Al. Eroded morphology suggests that a high compactness of the composites could improve the erosion resistance effectively and the increasing soft Al could further strengthen the anti-erosion ability. Besides fracture, crack deflection, Al plastic deformation and peeling off of cracked Si from Al substrate also play key roles in the consumption of impact energy during erosion.

Contributors

LIU Lei provided the concept, composite preparing technique and test method, and wrote the original draft. FENG Wei conducted the literature review, data curation and original draft review. LI Bo-yan and ZHANG lei-lei prepared the composite and performed the erosion test. LI Jian-ping and GUO Yong-chun analyzed the erosion data. HE Zi-bo, CAO Yi and BAO Ai-lin edited the draft of manuscript. All authors replied to reviewer's comments and revised the final version.

Conflict of interest

LIU Lei, FENG Wei, LI Bo-yan, LI Jian-ping, ZHANG Lei-lei, GUO Yong-chun, HE Zi-bo, CAO Yi, and BAO Ai-lin declare that they have no conflict of interest.

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(Edited by FANG Jing-hua)

中文导读

Al添加量对反应熔渗C/C-SiC复合材料粒子冲蚀特性的影响

摘要：本文基于气固两相流冲击测试方法，对反应熔渗中添加不同Al含量的C/C-SiC粒子的冲蚀特性进行了研究。采用SEM、EDS以及XRD对材料冲蚀前后的形态、微结构、物相等进行了分析，结果表明，冲蚀率和Al添加量之间呈U型曲线关系，除材料致密度对其抗冲蚀性有重要影响外，分布在碳和残余Si之间的混合物，即SiC混杂塑性Al，通过塑性变形、诱导裂纹偏转、粘连碎裂Si等耗能方式也对材料的冲蚀行为和耐冲蚀能力起重要作用。

关键词：C/C-SiC；添加Al；反应熔渗；固态粒子冲蚀

Foundation item: Project(51902239) supported by the National Natural Science Foundation of China; Project(2020JQ-808) supported by the Science and Technology Fund of Shaanxi Province, China; Projects(19JK0400, 19JK0402) supported by the Education Fund of Shaanxi Province, China; Project(SKLSP201752) supported by the State Key Laboratory of Solidification Processing in Northwestern Poly Technical University, China; Project(XAGDXJJ17008) supported by the Principal Fund of Xi’an Technological University, China; Project supported by the Youth Innovation Team of Shaanxi Universities, China

Received date: 2020-01-18; Accepted date: 2020-06-19

Corresponding author: LIU Lei, PhD, Lecturer; Tel: +86-29-83208080; E-mail: liuleiNIN@126.com; ORCID: https://orcid.org/0000- 0003-3168-7303; FENG Wei, PhD, Lecturer; Tel: +86-29-83208080; E-mail: cindybear@126.com; ORCID: https://orcid.org/0000-0003-4013-0603