Accepted Manuscript

Synthesis and mechanical properties of novel Ti-(SiCf/Al3Ti) ceramic-fiber-reinforced

metal-intermetallic-laminated (CFR-MIL) composites

Chunfa Lin, Yuqiang Han, Chunhuan Guo, Yunpeng Chang, Xiaoxiao Han, Lin Lan,
Fengchun Jiang
PII: S0925-8388(17)32044-3
DOI: 10.1016/j.jallcom.2017.06.057
Reference: JALCOM 42125

To appear in: Journal of Alloys and Compounds

Received Date: 14 March 2017

Revised Date: 31 May 2017
Accepted Date: 5 June 2017

Please cite this article as: C. Lin, Y. Han, C. Guo, Y. Chang, X. Han, L. Lan, F. Jiang, Synthesis and
mechanical properties of novel Ti-(SiCf/Al3Ti) ceramic-fiber-reinforced metal-intermetallic-laminated
(CFR-MIL) composites, Journal of Alloys and Compounds (2017), doi: 10.1016/j.jallcom.2017.06.057.

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 ACCEPTED MANUSCRIPT

Synthesis and mechanical properties of novel Ti-(SiCf/Al3Ti)

ceramic-fiber-reinforced metal-intermetallic-laminated (CFR-MIL)

composites

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Chunfa Lin a, Yuqiang Han a, Chunhuan Guo a,*, Yunpeng Chang a, Xiaoxiao Han a, Lin Lan b,

Fengchun Jiang a,*

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a
Key Laboratory of Superlight Materials & Surface Technology, Ministry of Education,

College of Materials Science and Chemical Engineering, Harbin Engineering University,

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Harbin 150001, PR China
b
College of Materials, Xiamen University, Xiamen 361005, PR China.

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* Corresponding author: fengchunjiang@hrbeu.edu.cn, +86-13946184358
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guochunhuan@hrbeu.edu.cn, +86-18804631852
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Abstract
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The innovative Ti-(SiCf/Al3Ti) ceramic-fiber-reinforced metal-intermetallic-laminated

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(CFR-MIL) composites were successfully fabricated by vacuum hot pressing using titanium foils,

aluminum foils and SiC ceramic fibers. The synthesized Ti-(SiCf/Al3Ti) composite showed a
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unique multilayered microstructure consisting of alternating SiCf/Al3Ti composite layers (SiC

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fiber as reinforcement) and Ti layers. In addition, reaction annealing technique was employed to
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improve the interfacial performance of SiC fiber with Al3Ti matrix. The microstructure evolution

of the laminated composite during hot-pressing and annealing was experimentally characterized

using scanning electron microscopy and energy dispersive spectroscopy. The formation

mechanism of micro-laminated structure was discussed. Furthermore, the mechanical properties of

the Ti-(SiCf/Al3Ti) laminated composite and its components were investigated by tensile and

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nanoindentation tests. The results indicated that Ti-(SiCf/Al3Ti) laminated composite exhibited

superior mechanical properties compared to Ti-Al3Ti, which was likely attributed to the

introduction of SiC fiber. The failure mechanism of CFR-MIL composite was the combined

fracture behaviors of ductile fracture of Ti, brittle fracture of Al3Ti and fiber debonding, pullout

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and breakage of SiC.

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Keywords: SiC ceramic fiber; metal intermetallic laminated composite; reaction annealing;

interfacial performance; failure mechanisms

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1. Introduction

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Recently, inspired from the structure of shell with the interactive brittle inorganic
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compounds layers and ductile organic compounds layers, laminated composites were
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designed and produced to obtain specific layered structures with desirable properties [1-3].

This bionic design is based on energy dissipation principle and the purpose is to minimize the
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effect of raw micro-cracks on the mechanical properties of the materials [4]. The unique
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laminated composites comprised of alternating ductile and brittle layers have received
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considerable attention, owing to their outstanding mechanical properties. Especially, ductile

metal layers were incorporated into the brittle intermetallic compounds to fabricated
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Metal-Intermetallic Laminated (MIL) composites, such as Ti-Al [5-8], Fe-Al [9-11], Ni-Al

[12,13] systems. In MIL composites, the intermetallic compounds provides strength and creep

resistance at elevated temperature and the ductile metal enhances the toughness as a layer

reinforcement [14]. For example, in titanium-titanium tri-aluminide (Ti-Al3Ti)

metal-intermetallic laminated composite, the intermetallic Al3Ti possesses low density, high

specific strength, high specific stiffness, high specific melting point and excellent oxidation
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resistance at elevated temperatures and it is toughened by the layers of ductile metal Ti. It is

such a unique laminated structure that the Ti-Al3Ti system offers an excellent combination of

specific strength, toughness and stiffness for structural applications in aerospace, automotive

and other aspects.

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To thoroughly understand the relationships of processing, structure and property of

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metal-intermetallic laminated composites, the microstructure evolution, damage evolution,

resistance-curve and fracture mechanisms of Ti-Al3Ti MIL composites were systematically

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investigated via quasi-static and dynamic compression tests, tension tests, bending tests and

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ballistics tests as well as experimental-numerical hybrid method [15-19]. The results revealed
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that the fracture toughness of the laminated composite exhibits more than an order of

magnitude improvement compared to that of monolithic Al3Ti (fracture toughness ~2 MPa√m)

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due to the addition of ductile Ti phase in the form of continuous layers. Furthermore, the
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resistance to fatigue crack propagation of the MIL composites increases with increasing
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ductile phase volume fraction. The significant improvement in toughness is attributed

primarily to uncracked ductile Ti layers that bridge the crack wake and shield the crack tip
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from far-field loading. In addition, the MIL composites have excellent damage tolerance due
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to the multiple energy-absorbing mechanism. All the studies mentioned above indicated that
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this kind of laminated composites show excellent mechanical properties for being used in the

aerospace field.

It has been reported that fiber-reinforced intermetallic matrix composites (FR-IMCs)

present superior mechanical properties compared to the monolithic intermetallic compounds

[20-22]. In recent years, combined the aforementioned MIL composites and FR-IMCs, the

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bio-inspired composites were synthesized with distinct performance by manufacturing SiC

fiber reinforced Ti matrix composite and Ti-intermetallic multi-layered composite or Ti-Al

intermetallic compounds as a whole part [23,24]. In these composites, the properties were

found to be superior than that of the Ti-intermetallic multi-layered composite or the SiC

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fiber-reinforced Ti-matrix composite. In addition, another ceramic fibrous-layer reinforced

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MIL composite, Ti-Al3Ti-Al2O3-Al, was fabricated by reactive foil sintering using “metpreg”

tapes (50% Al2O3 fiber volume in Al metal matrix) [25]. In this fibrous-layer reinforced

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laminated composite, the fibers were oriented in 0° and 90° layers with an attempt to enhance

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the toughness of the MIL composite. The results demonstrated that Al2O3 ceramic fiber layer
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arrested cracks formed in the brittle Al3Ti phase and had a considerable toughening effect.

Nevertheless, there is no reported work on introducing SiC fibers into intermetallic layer to
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improve the mechanical properties of metal-intermetallic laminated composite.

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In this paper, a novel metal foil metallurgical method involving hot pressing and reaction
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annealing was adopted to prepare Ti-(SiCf/Al3Ti) ceramic-fiber-reinforced

metal-intermetallic-laminated (CFR-MIL) composites. SiC fibers reinforcement were introduced

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into the laminates with the purpose of improving the comprehensive performances of the
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composite. The microstructure evolution and phase identifications of the as-fabricated

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composites were investigated systematically. This work also aims to evaluate the room

temperature tensile properties of the Ti-(SiCf/Al3Ti) laminated composites.

2. Experimental procedures

2.1 Materials and processing

To prepare Ti-(SiCf/Al3Ti) laminated composite, Ti alloy (Ti-6Al-4V) foils (100 mm ×

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100 mm × 0.5 mm), commercial pure aluminum foils (100 mm × 100 mm × 0.5 mm) and SiC

fibers (fiber diameter 10-15 µm) were used as raw materials in this work. It should be pointed

out the as-received SiC fibers were packed into bunches (every 500 single item) originally.

Before utilization, the fibers had been pretreated at 600 ºC for 0.5 h to remove the colloidal

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materials on the surface, thus the fibers packed together were divided into single ones. Before

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sintering, the foils were polished with silicon carbide papers to remove surface oxide layers.

Then the foils and fibers were cleaned in water bath using ultrasonic cleaning machine for 20

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min, rinsed in alcohol and then dried rapidly. All these procedures were well prepared for

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fabricating the laminated composite.
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Fig. 1 shows the preparation procedure of Ti-(SiCf/Al3Ti) laminated composite. The

metal foils were alternately stacked with SiC fibers arranged in the midst of Ti-6Al-4V and Al
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foils. The top and bottom layers of the stack were both Ti-6Al-4V foils, and hereafter Ti refers
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to Ti alloy (Ti-6Al-4V) throughout this paper. The SiC fiber was fixed on the surface of metal
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foils by the mean of adhering both end of the fiber to the edge of the foils using double

sided sticky tape. The stacked Ti/SiCf/Al foils were sintered in a vacuum hot pressing furnace
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(ZRY-60-30) with a vacuum of ~10-3 Pa to allow them to react with each other under
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appropriate processing parameters that include temperature, pressure, and time. The initial
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pressure applied on the stacked Ti/SiCf/Al foils was 5 MPa that was higher than that normally

used in preparation, such that the metal foils and fibers can compact. The temperature firstly

heated to 600 ℃ and held for 30 min. Then the temperature increased to 630 ℃ at a heating

rate of 1 ℃/min and kept for 10 min, while the pressure reduced to 1.5 MPa in this

temperature level. The temperature was then raised to 660 ℃ and held for 5 h. During this

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process, in order to avoid the expulsion of molten Al, the pressure nearly dropped to zero

along with the liquid-solid reaction occurred. When the aluminum layers have been

completely consumed, the pressure increased to 3 MPa. Finally, the sample was

furnace-cooled to room temperature while maintaining the pressure of 3 MPa. In addition,

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Ti-Al3Ti laminated composite without fiber reinforcement was also fabricated using the same

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method for making a comparison with Ti-(SiCf/Al3Ti). Both the laminated composites with

and without SiC fiber have the similar titanium volume fraction of ~30%. It should be pointed

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out that it is hard to accurately calculate the volume fraction of SiC fiber ( f SiC ) in the

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CFR-MIL composites owing to the small diameter of SiC fibers. Here, it is estimated
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approximately using the initial diameter and number of SiC fiber and calculated by the

following equation:
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S SiC ⋅ π ⋅ (rSiC ) 2
f SiC = (1)
( STi ⋅ tTi + S FRI ⋅ t FRI ) ⋅ WL
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Where the SSiC, STi and SFRI are the number of SiC fibers, Ti layers and SiCf/Al3Ti
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fiber-reinforced-intermetallic (FRI) composite layers, respectively; the tTi, tFRI, WL and rSiC are
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the thickness of Ti and FRI layer, the width of the laminates and the radius of SiC fiber,

respectively. The volume fraction of SiC fiber in the CFR-MIL composites calculated using
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the above equation is ~1% in the present work.

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Fig. 1 Schematic illustration of fabrication and post-heat treatment process of Ti-(SiCf/Al3Ti)
laminated composite.

The as-fabricated Ti-(SiCf/Al3Ti) laminates prepared in the current study was comprised

of Ti layers and SiC fiber reinforced Al3Ti matrix composite layers (SiCf/Al3Ti). Subsequently,

annealing treatment at 950 ℃ for 3 hours was performed to the as-fabricated laminates. Thus,

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the bonding of SiC fibers with intermetallic Al3Ti matrix could be improved due to the

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metallurgical interfacial reaction occurred in the process of annealing.

2.2 Microstructure characterization

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Metallographic specimens were cut from the as-fabricated and as-annealed

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Ti-(SiCf/Al3Ti) laminates using an electrical discharge machining (EDM). The polished
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surface was perpendicular to the fiber orientation. The cross section was prepared by grinding

step by step with 800, 1000, 1500, 2000, 3000 grit silicon carbide papers in order, polishing
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with abrasive finishing machine. The microstructure of interfacial reaction zone was observed
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by HITACHI SU-70 Scanning Electron Microscope (SEM), and the elements content was
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detected with XFlash Detector 6|60 energy dispersive spectroscopy (EDS). The phases in

laminated composites were identified by X’Pert PRO X-ray diffractometer (XRD). The X-ray
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scanning range (2Theta) was from 20 ° to 90 °.

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2.3 Nanoindentation
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The mechanical properties of the individual phases in Ti-(SiCf/Al3Ti) laminated

composite were characterized via nanoindentation using an MTS Nano Indenter XP

instrument equipped with a Berkovich pyramidal-shaped indenter tip. All nanoindentation

tests were conducted at room temperature. Cross-sectional samples were polished and

prepared for indentation. During the indentation, the various loads were applied to different

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zone for obtaining the limited maximum displacements that 1500 nm for Ti and Al3Ti layers

and 500 nm for SiC fiber, respectively. The hardness and Young’s modulus were determined

from the load-penetration results using Oliver-Pharr analysis. Additionally, Vickers hardness

tests were also performed to the layers and the fibers for evaluating the availability of

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nanohardness.

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2.4 Tensile tests

To analyze the mechanical response of Ti-(SiCf/Al3Ti) laminated composite, tensile tests

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were carried out on Instron 5500R load frame with a constant loading rate of 0.5 mm/min at

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room temperature. The tensile loading was parallel to the SiC fiber orientation for both the
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as-fabricated and the as-annealed Ti-(SiCf/Al3Ti) laminated composite. During the tensile test,

an extensometer was used to monitor the deformation of the sample. Bone-like tensile
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specimens with a gauge of 65 mm (length) × 12.3 mm (width) × 3.6 mm (thickness) were cut
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from the laminated composite plates using electrical discharge machining. Before testing, the
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samples were ground from 600 to 2000 grit, and then carefully polished. The tensile

stress-strain curves were plotted using experimental engineering stress and strain data. The
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tensile strength and elongation at fracture were achieved from the experimental stress-strain
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curves. After tests, the fracture surfaces of tensile specimens were observed by SEM.
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3. Results and discussion

3.1 Microstructure evolution

Fig. 2 shows the microstructures of the Ti-(SiCf/Al3Ti) laminated composite in the

process of hot pressing and reaction annealing. As indicated in Fig. 2a, it can be seen that the

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Ti-(SiCf/Al3Ti) composite consists of alternating Ti metal layer and SiCf/Al3Ti

fiber-reinforced-intermetallic (FRI) composite layer. The SiC fibers distribute along the

central section of the SiCf/Al3Ti composite layers. Pure Al foils were completely consumed

and transformed into Al3Ti phases, which was determined by the result of XRD (see Fig. 3a),

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in which no residual Al phase was detected by XRD patterns. When Al was exhausted, the

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residual aluminum oxide connected together at the center of the SiCf/Al3Ti composite layer

and the micro-pores appeared. Thus, discontinuous “center line” formed within the composite

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layer, which was similar to Ti-Al3Ti laminated composite [26]. Whereas, a portion of Ti was

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remained after hot pressing. In addition, it is clear that the interface between SiCf/Al3Ti
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composite layer and Ti layer is rather compact and well-bonded, and none of other

intermetallic compounds form (see Fig. 2b). The characteristics of interfacial zone between
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fiber reinforcement and intermetallic matrix are shown in Fig. 2c. The interfacial reaction
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products are presumed to be TiC and TiSi2, which is in accordance with the result of XRD
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shown in Fig. 3a. It is also noted that the circle interface around SiC fiber is not intact. There

are interstices and gaps in some region of the interface. Therefore, the experimental facts
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indicate that the bonding between fiber and intermetallic is the mixture of the metallurgical
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reaction and mechanical joint.

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Fig. 2 Representative SEM images of microstructure of Ti-(SiCf/Al3Ti) composites: (a), (b) and (c)
show the layered structure, the interlamination interface and the fiber/matrix interface of the
as-fabricated composite, respectively; (d), (e) and (f) show the SiCf/Al3Ti composite layer, the
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metallurgical bonding of SiC fiber with Al3Ti and the interaction product layer between Ti layer
and Al3Ti layer in as-annealed laminates. The schematic diagram for EDS point scanning around
the interfacial zone was indicated in (e) and (f).
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Subsequently, the following annealing at 950 ℃ for 3 hours with no pressure was carried
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out in heat treatment furnace with the purpose of improving the bonding strength of

SiCf/Al3Ti interface. The microstructure of the as-annealed laminated composite is presented

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in Figs. 2d-2f. The corresponding chemical composition of elements detected by EDS point
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scan are given in Table 1. Conspicuously, interfacial reaction occurred between SiC fiber and
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Al3Ti matrix, and thus the fiber is well-bonded metallurgically with the matrix, as is shown in

Fig. 2e. In addition, a reaction product layer with the average thickness of ~1 µm forms

surrounding the SiC fiber. The reaction product layer is comprised of dark gray phases with

the respective chemical compositions of 11.4 at. % Si-31.0 at. % C-45.4 at. % Al-12.2 at. %

Ti according to EDS point scan, corresponding to the complex compounds, including TiC,

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TiSi2, Ti2AlC and Al4SiC4 phases). XRD patterns also give evidence for the results, as

indicated in Fig. 3b. Moreover, interfacial product layer (~8 µm) between SiCf/Al3Ti

composite layer and Ti layer is obviously observed, which contains two different phase: white

phases and light gray phases (see Fig. 2f) with the respective compositions of 61.1 at. %

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Al-34.0 at. % Ti-4.9 at. % V and 47.5 at. % Al-49.9 at. % Ti-2.6 at. % V based on EDS point

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scan, which corresponds to TiAl2 phases and TiAl phases. This is in consistence with the

results of XRD. Consequently, Ti-(SiCf/Al3Ti) laminated composite with good interfacial

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bonding are achieved through hot pressing and reaction annealing.

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Fig. 3 X-ray patterns of the Ti-(SiCf/Al3Ti) composites (a) without and (b) with annealing
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treatment.
Table 1 Typical chemical compositions of each layer and phase detected by EDS
Composition (at. %)
Number Possible phases
C

Si C Al Ti V
Spectrum 1 47.6 51.8 0.4 0.2 0 SiC
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Spectrum 2 8.0 37.2 42.1 12.7 0 TiC, TiSi2,

Spectrum 3 11.4 31.0 45.4 12.2 0 Ti2AlC, Al4SiC4
Spectrum 4 0.9 4.2 72.0 22.8 0.1 Al3Ti, Al4SiC4
Spectrum 5 0 0 72.2 24.7 3.1 Al3Ti, Al3Ti0.2V0.8
Spectrum 6 0 0 61.1 34.0 4.9 Al2Ti
Spectrum 7 0 0 47.5 49.9 2.6 TiAl
Spectrum 8 0 0 10.2 82.3 7.5 Ti-6Al-4V

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3.2 Formation mechanism of Metal/FRI laminated structure

The formation of Ti-(SiCf/Al3Ti) laminated composite was actually associated with a

series of reaction-diffusion process during fabrication and heat treatment. After vacuum hot

pressing, the Metal/FRI (M/FRI) laminated structure formed containing alternating metal

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layers and fiber-reinforced intermetallic compounds layer. The formation mechanism of this

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unique laminated microstructure is similar with that of Ti-Al3Ti metal-intermetallic laminated

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(MIL) composite [27]. Then, owing to the reaction annealing, further interfacial reactions

occurred between Al3Ti and Ti, as well as Al3Ti and SiC. This interaction is a diffusion

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behavior accompanied by the formation and transformation of a series of Titanium-Aluminum
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intermetallic compounds and some other binary or ternary compounds [28-30]. Fig. 4 shows
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the schematics of the synthesis mechanism of Ti-(SiCf/Al3Ti) laminated composite.

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Fig. 4 Schematics of the synthesis mechanism of Ti-(SiCf/Al3Ti) laminated composite: (a) First
stage, showing the interdiffusion of layers during fabrication; (b) Second stage, indicating the
formation of M/FRI laminated structure consisting of newly-formed SiCf /Al3Ti composite layer
and remained Ti layer; (c) Third stage, displaying the interaction between individual layer or SiC
and Al3Ti during anneal; (d) Fourth stage, exhibiting the final microstructure of Ti-(SiCf /Al3Ti)
laminated composite with good interfacial bonding after heat treating process.

First, during hot pressing, the interdiffusion of Ti and Al in solid Ti layer and the mixture

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layer (including liquid Al, SiC fiber and aluminum oxides) occurred and thus Al3Ti layer

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formed at the interface between the solid Ti layer and the liquid Al layer. In the composite, the

intermetallic Al3Ti was the solely newly-formed intermetallic compound because Al3Ti was

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thermodynamically and kinetically favored over the formation of other titanium aluminides

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due to this low synthesis temperature (660 ℃) [27]. It is noteworthy that as the hot pressing
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time increased, the thickness of remnant mixture layer became thinner due to the outward

diffusion of Al atoms within the mixture layer and the compressive stress originated from the
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thickening of Al3Ti layer. Thereby, SiC fiber and aluminum oxides began to concentrate
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towards the center of mixture layer. Additionally, Al3Ti layer grew much faster towards the Al
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layer than that towards the Ti layer because of the higher diffusion of Al in Al3Ti than that of

Ti (the Kirkendall effect [31]). Thus, the as-fabricated laminates were composed of alternating
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remained Ti layers and SiCf/Al3Ti composite layers. The fiber distributed along the “center
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line”, which formed as a result of aluminum oxides and voids. Furthermore, the results of
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EDS line scan are shown in Figs. 5a and 5b. The content fluctuation trends of reaction

elements across the interface between Ti layer and SiCf/Al3Ti composite layer reflect the

characteristics of element diffusion. A trace amount of TiC and TiSi2 formed between SiC

fiber and Al3Ti matrix, which was demonstrated by the results of XRD (Fig. 3a). Nevertheless,

vacancies formed at the interface between SiC and Al3Ti because of the diverse diffusion rates

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of Si, C, Al and Ti atoms [31].

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Fig. 5 SEM images (a) and (c) of the metal/intermetallic interfacial zones in the as-fabricated and
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as-annealed Ti-(SiCf/Al3Ti) composite, respectively and the corresponding EDS line scan results (b)
and (d) obtained along the red arrow.

As the anneal treatment proceeded, the Al atoms in SiCf /Al3Ti composite layer and Ti
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atoms in Ti layer continued to diffuse, leading to the formation of TiAl intermetallic layer at

the Ti/Al3Ti interface, as shown in Fig. 5c. Subsequently, ascribing to the decomposition of
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TiAl, island-like Al2Ti phase nucleated within TiAl phase (see details in Fig. 5c). Fig. 5d

shows the identical result with the content fluctuation trends of Ti and Al across the interfacial
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reaction product layer between Ti and Al3Ti in the as-annealed laminates. Meanwhile, more

reaction products (Ti2AlC and Al4SiC4) formed at the interfacial zone surrounding SiC fiber

and good interfacial bonding of the fiber with the matrix was achieved. The EDS line analysis

results of the interfacial zone between SiC fiber and Al3Ti matrix are presented in Figs. 6b and

6d. The content fluctuation of reactive elements reflect the characteristics of downhill

diffusion at the interfacial reaction product layer. The element C was not detected accurately
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by EDS line analysis, which was consistent with the literature [32]. The results of EDS point

scan analysis (as shown in Table 1) indicate that C atoms diffused authentically from SiC

fiber to Al3Ti matrix.

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Fig. 6 SEM images (a) and (c) of the fiber/intermetallic interfacial zones in the as-annealed
Ti-(SiCf/Al3Ti) composite and the corresponding EDS line scan results (b) and (d) obtained along
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the red arrow.

Therefore, interfacial behavior of the layers involved three steps: 1) formation of Al3Ti
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phase at the interface between Ti and Al; 2) generation of intermetallic TiAl phase; 3)
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nucleation of island-like Al2Ti phase within TiAl layer. The following reactions may occur
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during hot pressing and reaction annealing:

Ti + 3 Al → Al3Ti (2)

2Ti + Al3Ti → 3TiAl (3)

2TiAl → Ti + Al2Ti (4)

Fiber/matrix interfacial behavior involved two steps: 1) formation of TiC and TiSi2 phases

during fabrication; 2) formation of Ti2AlC and Al4SiC4 phases during reaction annealing.
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According to the above results and analysis, the following reactions may occur between SiC

and Ti or Al3Ti:

SiC → Si + C (5)

Ti + C → TiC (6)

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Ti + Si → TiSi2 (7)

Al3Ti + Si + C → Ti2 AlC + Al4 SiC4 (8)

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3.3 Nanoindentation studies

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Fig. 7 shows the typical load-penetration curves and the derived nanohardness and

Young’ modulus for different phases (Ti, Al3Ti and SiC) of Ti-(SiCf/Al3Ti) laminated

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composite. The results obtained from nanoindentation and traditional Vickers hardness tests in

the present work are summarized in Table 2. It is noted that the dimensionless microhardness
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values (HV) were switched to the unit of GPa according to Eq. (9) [33]:

H GPa = H V × 0.009807 / 0.93

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(9)
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Where, HGPa and HV are the transferred hardness value and traditional Vickers hardness value,

respectively. It is evident that the nanohardness of Ti (Ti-6Al-4V, ~4.2 GPa), Al3Ti (~7.5 GPa)
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and SiC (~28 GPa) phases is close to those obtained from the Vickers method. It is also noted
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that the nanohardness values show good consistency with other published works [34-36], as
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can be seen in Table 2. Additionally, the fiber (SiC) and the layers (Ti and Al3Ti) exhibit the

approximate elastic modulus values compared to the results of the previously reported works

[35,36]. Based on the aforementioned discussion, it is indicated that the properties

(nanohardness and elastic modulus) derived from nanoindentation tests are characterized

properly and accurately. Moreover, the results shows that SiC fiber has higher elastic modulus

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and hardness than Ti and Al3Ti. Besides, the density of SiC fiber is lower than that of the

matrix. Therefore, Ti-(SiCf/Al3Ti) CFR-MIL composite shows a good combination of lower

density and higher modulus in comparison with Ti-Al3Ti MIL composites without fiber

reinforcement. These experimental facts reveals that SiC fiber is an appropriate reinforcement

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for designing intermetallic matrix composites to improve their mechanical and physical

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properties.

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Fig. 7 (a) Schematic of load-penetration depth curves and (b) average Young’s modulus and
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hardness of SiC fiber, intermetallic Al3Ti and metal Ti.

Table 2 Comparison of mechanical properties of metal Ti, intermetallic Al3Ti and ceramic SiC
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obtained by nanoindentation and conventional method. H indicates nanohardness, HV is Vickers

hardness and E denotes the Young’s modulus
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Phases/Materials H (GPa) HV (GPa) E (GPa) References

Ti (Ti-6Al-4V) layer 4.2 ± 0.1 3.2 ± 0.2 128 ± 1 This work
Al3Ti layer 7.5 ± 0.2 6.3 ± 0.2 203 ± 2 This work
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SiC fiber (in laminates) 28.4 ± 0.4 25.6 ± 5.3 225 ± 4 This work
SiC fiber (as-received state) - - 236 This work
Ti-6Al-4V - 3.7 - [34]
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CP-Ti - 3.0 116 [35]

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Al3Ti+0.3%Al - 6.0 -
[36]
Al3Ti - - 216

3.4 Tensile properties

Fig. 8a shows the representative tensile stress-strain curves of the as-fabricated and

as-annealed Ti-(SiCf/Al3Ti) CFR-MIL composites, as well as Ti-Al3Ti MIL composite. It can

be seen that all the laminated composites show a two-stage tensile characteristics consisting

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of an initial linear region, followed by a non-linear yield stage up to the ultimate tensile

strength (σUTS), and then an obvious plastic deformation region before fracture. While the

as-fabricated CFR-MIL composite exhibits a sudden light drop of stress at the end of yield

stage, as indicated in Fig. 8a. This is credited to the debonding behavior between SiC fiber

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and Al3Ti matrix due to the relatively poor bond of the fiber with the matrix. It is noteworthy

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that the stress of the as-fabricated CFR-MIL composite for the plastic deformation region is

higher than the corresponding one of Ti-Al3Ti MIL composite. This deformation region before

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failure is mainly attributed to the elongated ductile Ti layers and the incompletely ruptured

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SiCf/Al3Ti composite layers that possess numerous micro-cracks.
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Fig. 8 (a) Tensile stress-strain curves of Ti-(SiCf/Al3Ti) CFR-MIL and Ti-Al3Ti MIL composite; (b)
showing the tensile properties of the laminated composites.

Fig. 8b illustrates the histograms of ultimate tensile strength (σUTS) and elongation at
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fracture of the MIL and the CFR-MIL composites in the present work. The mechanical

properties of both the MIL and the CFR-MIL composites obtained from room temperature tensile

tests are also summarized in Table 3. Besides, some reported results of Ti-intermetallic layered

composites elsewhere [23,24,37,38] are also listed in Table 3. It is noted that the ceramic or

metal fiber-reinforced multilayered composites exhibit superior mechanical properties

(strength and ductility) than those of the Ti-intermetallic laminates, including strength and
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ductility. In addition, it can be clearly seen that compared to Ti-Al3Ti laminated composite

without fiber reinforcement, the σUTS and the elongation of the as-fabricated Ti-(SiCf/Al3Ti)

laminated composite have increased by 22% and 7%, respectively. The increase is ascribed to

the debonding, pullout and fracture of SiC fiber during the deformation process of CFR-MIL

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samples. The results indicate that the strength of the CFR-MIL composite is significantly

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enhanced while improving the ductility because of the added fiber reinforcement. In light of

this, strategy of the CFR-MIL composite could provide a feasible approach for solving the

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inversion problem of strength and ductility, which was also investigated elsewhere [38,39].

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Moreover, the as-annealed Ti-(SiCf/Al3Ti) laminated composites exhibit slight enhancement
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of strength and ductility in comparison with the as-fabricated composite. It is believed that

owing to the good interfacial bond between the fiber and the matrix, the load was effectively
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transferred from the matrix to the fiber that possessed high tensile strength. Hence, more
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energy was necessary to cause the rupture of the fiber reinforced composite, and then strength
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and elongation of the as-fabricated Ti-(SiCf/Al3Ti) CFR-MIL composite were further

improved.
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Table 3 Tensile properties of the MIL and the CFR-MIL composites

Laminated composites Processes σUTS (MPa) Elongation (%) References
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Ti-Al3Ti 379 ± 4 4.2 ± 0.2 This work

Hot pressed (HP)
460 ± 12 4.5 ± 0.2 This work
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Ti-(SiCf/Al3Ti)
HP + Reaction annealed 471 ± 13 4.6 ± 0.3 This work
(SiCf/Ti)-intermetallic 610 4.2 [23]
Ti-intermetallic 404 4.3 [24]
HP
Ti-Al3Ti 327 3.6
394 4.3 [37]
Ti-(Al2O3f/Al3Ti)
HP + Hot isostatic pressed 434 4.8
Ti-(NiTif/Al3Ti) HP 613 4.6 [38]

In order to reveal the fracture mechanisms of Ti-(SiCf/Al3Ti) laminated composites, the

fracture surfaces of the tested samples were observed via scanning electron microscope (SEM)
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in SE mode for both the as-fabricated and the as-annealed CFR-MIL composites. The typical

fracture characteristics observed from the overall fractured sample surface are shown in Figs.

9a and 10a. It can be seen that the fracture surfaces of the laminates are rather rough,

implying tortuous crack propagation paths. The fracture are obviously divided into two

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individual layers: rough Ti layer and fragmented SiCf/Al3Ti composite layer. When

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macro-strain reached the maximum tolerance, micro-cracks would be formed in the brittle

SiCf/Al3Ti composite layer and propagated to the interfaces between SiCf/Al3Ti composite

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layer and Ti layer. Afterward, the debonding or delamination between Ti layer and the

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fiber-reinforced Al3Ti layer occurred due to the effect of the ductile Ti layer [18,19]. This
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crack deflection and blunting could delay the premature fracture of the SiCf/Al3Ti composite

layer, effectively improving the elongation of SiCf/Al3Ti composite layer. Ultimately, the
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brittle cracks were mainly distributed in the brittle composite layer, which revealed an
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effective route to absorb the energy during the fracture procedure.

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Figs. 9b and 9c show the fracture surface morphologies of the fractured Ti layer and

intermetallic Al3Ti of the as-fabricated Ti-(SiCf/Al3Ti) laminated composite. It is noted in

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Fig.9b that the surface of fractured Ti exhibits obvious plastic deformation with numerous
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dimples, which contains the formation, growth and coalescence of micro-voids in the process
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of deformation and fracture, namely micro-void coalescence fracture mode. Further fracture

observations of Ti in the as-annealed CFR-MIL composite present the similar ductile fracture

(Fig. 10b). The plastic deformation plays an important role in the tensile behavior of

Ti-(SiCf/Al3Ti) laminated composite with and without annealing treatment. Whereas, the

intermetallic Al3Ti of the hot-pressed and reaction-annealed CFR-MIL composites exhibit

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brittle fracture with different fracture modes. As shown in Fig. 9b, the near-interfacial

cracking is observed in the brittle phase, which is similar with the previous work [18]. As can

be seen in Fig. 9c, in terms of the as-fabricated composite, the major fracture mode of the

intermetallic is intergranular fracture. Transgranular fracture is also found in the intermetallic,

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but it only take a relatively small portion compared to the intergranular. Adharapurapu et al.

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[19] also showed the similar results in the fatigue fracture surfaces of Ti-Al3Ti MIL

composites. Nevertheless, cleavage steps are conspicuously observed in Al3Ti of the

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as-annealed composite, indicating the typical transgranular cleavage fracture mode, as

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indicated in Fig. 10c. This is because the crack preferred to propagate within Al3Ti grains due
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to the stress concentration at grain boundaries. Therefore, transgranular cleavage fracture is

the major failure mode, which is consistent with intermetallic Ti3Al reported in the previous
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literature [40,41].
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As shown in Fig. 9d, debonding, pullout and breakage behavior of SiC fibers are found
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in the as-fabricated composite, which can improve the properties of the fiber reinforced

composite by increasing the resistance to crack propagation and constraining microcrack

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extension. However, fiber fracture is the main failure mechanism in the as-annealed
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composite and the form of fiber pullout is not found (see details in Fig. 10d). This implies that
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the excessive interface bonding strength of the fiber with the matrix may limit the

enhancement effect of the fiber reinforcement, which is in accordance with that reported in

literature [42]. The fiber reinforcement plays a key role in increasing the ductility and strength

of the Ti-(SiCf/Al3Ti) laminated composites. Thus, more annealing process should be

investigated in the following works.

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Fig. 9 The typical fracture characteristics observed from the fractured specimen surface of the
as-fabricated Ti-(SiCf/Al3Ti) laminated composite: (a) the overall fracture morphology; (b) Ti
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layers; (c) intermetallic Al3Ti; (d) indicating the fracture feature of SiCf/Al3Ti composite.
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Fig. 10 The typical fracture characteristics of the as-annealed Ti-(SiCf/Al3Ti) laminated composite:
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(a) the overall fracture morphology; (b) Ti layers and Al3Ti layers; (c) intermetallic Al3Ti; (d)
SiCf/Al3Ti composite.

Consequently, Ti-(SiCf/Al3Ti) laminated composites possess a good combination of

tensile strength and ductility, which is attributed to: (i) The intrinsic high tensile strength and

superior ductility of Ti layer have a significant effect on the improvement of the ductility and

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strength for the laminated composite; (ii) SiC fiber can increase the resistance to crack

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propagation by fiber pullout and breakage, which improves the tensile strength effectively; (iii)

Ti-(SiCf/Al3Ti) laminated composites show the multi-layered structure, which can effectively

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redistribute stress and inhibit strain localization by load transferring to adjacent layers. Thus,

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the formation of micro-cracks will be postponed and the extra deformation capacity is
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imparted by the laminated structure, as reported in the references [43-45]. Therefore, both the

laminated structure and the fiber reinforcement have considerable contribution to the ductility
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enhancement of Ti-(SiCf/Al3Ti) CFR-MIL composite.

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4. Conclusions
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A novel class of Ti-(SiCf/Al3Ti) ceramic-fiber-reinforced metal-intermetallic-laminated

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(CFR-MIL) composite was successfully fabricated using vacuum hot pressing and heat treated
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through reaction annealing. The microstructure evolution, phase identifications, mechanical

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properties and fracture behavior of the CFR-MIL composite were investigated systematically.

The principal conclusions drawn from the current work are summarized as the following:

(1) The feasible approach has been successfully explored to fabricate Ti-(SiCf/Al3Ti)

laminated composite, which showed a unique Metal/FRI laminated structure composed of

alternating Ti layers and SiCf/Al3Ti composite layers.

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(2) Interaction between SiC fiber and Al3Ti matrix occurred during annealing treatment

and good interfacial bonding was achieved between the fiber and the Al3Ti. Thus the

performance of the fiber/matrix interface was remarkably improved. Meanwhile, new

intermetallic layer formed between Ti layer and SiCf/Al3Ti composite layer.

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(3) Ti-(SiCf/Al3Ti) CFR-MIL composite showed a good combination of low density and

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high modulus, which indicated that SiC fiber was a candidate of reinforcement for Al3Ti

intermetallic compounds to synthesize ceramic-fiber-reinforced metal-intermetallic-laminated

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composites having enhanced mechanical properties.

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(4) The Ti-(SiCf/Al3Ti) laminated composite exhibited superior ductility and strength
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compared to Ti-Al3Ti MIL composite, showing a significantly toughening and strengthening

effect of SiC fiber on the CFR-MIL composite. This was because the fiber debonding, pullout
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and breakage absorbed fracture energy and delayed the premature fracture of Al3Ti matrix.
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Acknowledgements
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The authors gratefully acknowledge the financial supports of this study by the National
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Natural Science Foundation of China (No.51671065), Key Program of Natural Science

Foundation of Heilongjiang Province (ZD2015012), Shanghai Aerospace Science and

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Technology Innovation Fund Project (SAST2016052) and the Fundamental Research funds
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for the Central Universities (HEUCFD15010).

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Highlights:

(1) A feasible method for fabricating Ti-(SiCf/Al3Ti) laminated composite is exploited.

(2) Formation mechanism of unique metal/(fiber-reinforced-intermetallic) laminated structure of

the composite is discussed.

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(3) The composite shows good comprehensive mechanical properties.

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(4) The effect of reaction annealing on the microstructure and mechanical properties of the

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composite are investigated.

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