Materials Science and Engineering C 50 (2015) 324–331

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Microstructure and properties of the Ti/Al2O3/NiCr composites fabricated by explosive compaction/cladding Bingfeng Wang a,b,c,⁎, Fangyu Xie a, Bin Wang b, Xiaozhou Luo a a b c

School of Materials Science and Engineering, Central South University, Changsha, Hunan, People's Republic of China Departments of Mechanical and Aerospace Engineering and Nanoengineering, University of California, San Diego, United States Key Lab of Nonferrous Materials, Ministry of Education, Central South University, Changsha, Hunan, People's Republic of China

a r t i c l e

i n f o

Article history: Received 23 October 2014 Received in revised form 25 December 2014 Accepted 9 February 2015 Available online 17 February 2015 Keywords: Explosive cladding Interface Composite Electron microprobe analysis

a b s t r a c t Titanium/aluminum oxide/nickel chromium (Ti/Al2O3/NiCr) composite bar prepared by explosive compaction/ cladding technique represents a new kind of sandwich-structural composites for medical application. Formation of the interfaces of Ti/Al2O3 and Al2O3/NiCr govern the properties of the composite material. The electrical resistivity and microstructure of the intermediate layer and the interfaces of the Ti/Al2O3/NiCr explosive compaction/ cladding bar are investigated by means of four-point probe analysis, optical microscopy, scanning electron microscopy, electron microprobe analysis, and X-ray diffraction. The Ti/Al2O3/NiCr composite bar is characterized by the consolidated ceramic intermediate layer and the metallurgical bonding interfaces. The intermediate ceramic layer plays a role of insulation and thermal conductance in this composite. The average shear strength of the composite bar is about 9.36 MPa. The heat affected zone characterized by relatively larger sizes of grains is distinguished from the other part of the Ti tube. The intermetallics AlTi3 and Al0.9Ni4.22 are generated at the intermediate ceramic layer. Formation mechanism of the interfaces of the explosive compaction/cladding bar are described. © 2015 Elsevier B.V. All rights reserved.

1. Introduction Cervical spondylosis is usually an age-related condition that affects the joints in people's neck. It develops as a result of the wear and tear of the cartilage and bones are of the cervical spine [1]. The biomedical materials for the treatment of the cervical spondylosis require good biocompatibility, special thermal and electrical conductivities. Titanium and titanium alloy are most widely used medical metallic materials for their good biocompatibility [2,3]. Nickel chromium (NiCr) alloy has excellent properties such as high resistance and high strength, and is often used as resistance material [3]. Alumina is a white solid, aluminum oxide and is also a kind of common structural ceramic materials, and it is cheap and easy to obtain. Aluminum oxide (Al2O3) ceramic have excellent high electrical resistance and good thermal conductivity [4]. If the Al2O3 ceramic is used as the intermediate layer between the NiCr alloy bar and pure Ti tube, on the one hand, it can prevent the current pass from the NiCr alloy bar to the Ti tube, and ensures the safety of the composite when current is applied into the NiCr alloy bar. One the other hand, the heat generated by the NiCr alloy can be transferred to pure Ti layer by the Al2 O 3 ceramic intermediate layer. Therefore, a novel Ti/ ⁎ Corresponding author at: University of California, San Diego, 9500 Gilman Drive, La Jolla, CA 92093, United States. E-mail address: [email protected] (B. Wang).

http://dx.doi.org/10.1016/j.msec.2015.02.023 0928-4931/© 2015 Elsevier B.V. All rights reserved.

Al2O3/NiCr sandwich-structured composite is considered to obtain a combination of optimized biocompatibility, high resistance and thermal conductivity, and electric heating functions from titanium, ceramic Al2O 3, and NiCr alloy, respectively. This composite can be used in the medical apparatus and instruments, such as the cervical spondylosis and the muscle pain treatment equipments. The explosive compaction/cladding is a new technique to join a variety of materials for fabricating sandwich-structures [5]. It can be used for consolidating powders and, in the area of superconductors, may lead to high densities and improvement of levitation forces of the bulks obtained [5–7], which can be used in levitating bearings and electrical rotating machines. Here, the explosive compaction/cladding technology is chosen to prepare the Ti/Al2O3/NiCr composite bar for medical applications for the first time. The explosive compaction is a novel material synthesis technology, which uses the energy generated from explosive and acts on the metal or ceramic powders in the form of shock wave to fabricate solid bulk materials [8,9]. An important part of the explosive compaction research has been aimed to achieve fully dense bulk monolithic solids starting with micrometer sized nanostructure powders [9]. Recently, extensive experiments have been carried out to explore the mechanism of explosive compaction [10,11]. Interfaces of the composite play a crucial role in determining the properties and behaviors of the hybrid metal/ceramic system [12]. There is a great effort to explore bonding characteristics and

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Table 1 The chemical composition and properties of the materials. Elements (wt.%)

C

Si

N

S

Ti

Cr

Fe

Ni

NiCr CP-Ti

0.08 0.08

1.38 0.02

– 0.03

0.12 –

– 99.57

21.27 –

0.37 0.30

76.78 –

Thermal Modulus of Poisson's Elements Thermal Density Tensile ratio expansion (g/cm3) strength elasticity conductivity (GPa) (kJ/(m∗K∗h)) coefficient (MPa) at 20 °C (10−6/K) NiCr CP-Ti

60.3 58.7

18 8.6

8.4 4.51

850 344

185 105

0.30 0.37

Fig. 3. Schematic of the apparatus for compression-shear experiment.

Fig. 1. X-ray diffraction analysis of the raw Al2O3 nanopowders.

formation mechanism of the interfaces [13–18]. Different studies corresponding to specific metal/ceramic systems arrive at different conclusions due to the facts that bonding characteristics and formation mechanism are highly dependent on the processing methods, such as mechanical joining, direct joining, and indirect bonding [17–19]. However, there are few reports regarding bonding interfaces of metal/ceramic/metal sandwich-structures fabricated by the explosive compaction/cladding. The aims of this paper are (1) to investigate electrical resistivity and bonding strength of Ti/Al2O3/NiCr composite bar; (2) to observe the microstructure and reaction products in the intermediate ceramic layer and the interfaces of Ti/Al2O3/NiCr composite bar; (3) to discuss the formation of the intermediate ceramic layer, and to discuss the formation mechanism of the interfaces of Ti/Al2O3/NiCr composite bar.

Fig. 2. (a) Schematic view of explosive compaction/cladding process. (b) Picture of Ti/Al2O3/NiCr composite bar samples.

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Fig. 4. Schematic of electric resistivity testing. (a) Transverse cross section of Ti/Al2O3/NiCr composite bar, and (b) Transverse cross section of Ti/NiCr explosive cladding bar. Marks “A”, “B”, “C”, and “D” are the testing locations in samples.

2. Method Commercial purity Ti (CP-Ti) grade 2 and NiCr alloy and Al2O3 nanopowders are used in the present work. The chemical composition and properties of the pure Ti and NiCr alloy are given in Table 1. Al2O3 weight content of the Al2O3 nanopowders with an upper size limit of 100 nm is over 90%, and the X-ray diffraction pattern reveals that Al2O3 nanopowders are mixed with about 10% Al(OH)3 shown in Fig. 1. CP-Ti tubes with the dimensions Φ 19.05 (OD) × 1.65 (Wall) × 240 mm were used as the clad material, and NiCr alloy bars with the dimensions Φ 13.75 × 240 mm were used as the base material. The surfaces of the base and clad materials were used as received. Al2O3 nanopowders were filled into the gap between the Ti tube and NiCr alloy bar with packing density of 60–80%. The emulsified explosive with detonation velocity of 3500–4000 m/s and density of 0.8– 1.0 g/cm3 was chosen as explosive material. The cylindrical arrangement was used for experimental set-up for explosive cladding as schematically shown in Fig. 2a. The explosive was uniformly placed around the tube. The detonator was detonated in the center of the top cap. Three Ti/Al2O3/NiCr composite bars were fabricated as shown in Fig. 2b. Due to the inhomogeneous distribution of the explosive, the surfaces of the samples were slight burned. The classical push-out testing were chosen to investigate the shear strengths of the joint interfaces [20]. A mechanical testing machine (Instron 3369) was used to conduct the compression-shear tests

Fig. 5. Electrical resistivity test results of specimens.

(Fig. 3). Specimens with thicknesses of 5 mm were put on a supporting platform, with a centered circular hole about 16.0 mm in diameter. The NiCr insert was pushed by a steel cylinder stub punch, which is concentric with the circular hole about 13.5 mm in diameter. The displacement rate of cross-head was 0.5 mm/min. Shear strength of the interface (τ) was calculated using the following equation: τ¼

Fmax πDh

ð1Þ

where Fmax is the maximum load, D is the diameter of NiCr insert, and h is the specimen thickness. In order to test the insulation effect of the intermediate Al2O3 ceramic layer, the resistivity tests were carried out with Four-Point Probe (SDY-4D) on Ti/Al2O3/NiCr composite bar specimens (region “A”, “B”, and “C” in Fig. 4a). For comparison, resistivity test was also carried out with the Ti/NiCr explosive cladding bar [3] (region “D” in Fig. 4b). Samples for optical microscope observations were cut in the crosssection of the cladding bar and normal to the plane of the cladding interface. The chemical attack for CP-Ti is the solution made by 4 ml HNO3 + 6 ml HCl + 5 ml HF + 100 ml H2O, and the NiCr alloy side is not etched. Investigations of optical microscopy were performed with POLYVAR-MET. Scanned electron microscopy (SEM) observations were carried out in FEI Quanta-200, operated at 20 kV. The electron probe microanalysis (EPMA) with wavelength-dispersive X-ray spectrometry (WDS-20 kV) was used to analyze the distribution of chemical

Fig. 6. Optical micrographs of transverse cross section of the composite bar.

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(a)

327

(b)

(c) Fig. 7. SEM images of transverse cross section of the Ti/Al2O3/NiCr composite bar. (a) The intermediate layer, (b) The interface of Ti/NiCr, and (c) The interface of Ti/Al2O3. The boundaries of NiCr/ Al2O3 and Al2O3/Ti are indicated as “1” and “2” in (a), respectively. Consolidated and embedded Al2O3 particles are marked as “a” and “b” in (b) with red and black arrows, respectively.

elements in the interfaces. Reaction products were detected by X-ray diffraction (XRD), using a Cu target at an operating voltage of 40 kV and current 250 mA. Scanning span was 5–80° with speed of 8°/min.

metals and ceramics inducing very high stresses on the interface during the process, in particular during the cooling stage after joining.

3.2. Microstructure of the composite bar's interfaces 3. Results and discussion 3.1. Electrical resistivity and bonding strength of the cladding bar Fig. 5 shows the electrical resistivity of the Ti/Al2O3/NiCr composite bar and the Ti/NiCr explosive cladding bar. It can be seen that the resistivity of the Ti/NiCr explosive cladding bar is nearly similar to the resistivity of CP-Ti tube, however, the values of resistivity test in the region across the intermediate Al2O3 ceramic layer are too large to measure. Therefore, NiCr bar can be isolated from Ti layer by the intermediate layer, and the current can only come through the NiCr alloy bar. After the current comes through, the heat generated in the NiCr bar via the intermediate ceramic layer can be conducted to the outside of the Ti layer. The compression-shear experiment is an important way of measuring bonding strength of explosive cladding bar. The mechanical results show that the average shear strengths of composite bar is about 9.36 MPa, which indicates that CP-Ti tube, Al2O3 nanopowders, and NiCr bar are bonded together by explosive compaction/cladding. The relative low value of bonding strength is caused by the brittle intermetallics and the differences of thermal expansion coefficients between

Fig. 6 shows an optical micrograph of Ti/Al2O3/NiCr composite interface. It can be seen that bonding of Ti/Al2O3/NiCr is achieved by explosive compaction/cladding, and shape of the boundaries of Ti/Al2O3 and Al2O3/NiCr are approximately an irregular wave curve caused by the excess of the explosive. The irregular wave curve of the boundaries make the CP-Ti tube and the Al2O3 ceramic and the NiCr alloy bar bonding well. The heat affected zone near the intermediate ceramic layer in the Ti tube is distinguished from the other part of the Ti tube, where the sizes of grains are much larger than those in the other part of Ti tube. It can be also seen that some molten metallic particles were inserted into the intermediate ceramic layer under the condition of high-velocity collision and high temperature. The interfaces and cross-sectional morphologies of the as-prepared Ti/Al2O3/NiCr composite bar are shown in Fig. 7. It is worth noticing that undergone explosive compaction, Al2O3 nanopowders are consolidated together and achieve a dense structure, as shown in Fig. 7a. It also can be seen that high quality bonding interfaces of Ti/Al2O3 and Al2O3/ NiCr are obtained, and Al2O3 particles are covered by metal at the interfaces. Some bright and nearly-round Al2O3 particles with sizes of 0.5–

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Fig. 9. X-ray diffraction analysis of the cladding interface. Fig. 10. The cooling rate (V) versus time (t) curves obtained within the melting zone.

2 μm (denoted as “a” in Fig. 7b and c) locate on the polished surface of Al2O3 substrate and some particles are bonded together with each other, and a few Al2O3 particles (denoted as “b” in Fig. 7b) are embedded into the CP-Ti and the NiCr alloy substrate due to high-speed collision. In order to determine the distribution of elements across the bonding interfaces, map and line scanning of elements Ti, Ni, Cr, and Al are taken from 215 μm across the interface along line “ ”, as shown in Fig. 8. It can be seen that the element contents of Ti and Ni and Cr and Al are all experience fast declined at boundaries of CP-Ti and the intermediate ceramic layer and the NiCr alloy bar shown in Fig. 8b. Melting zone “1” with thickness about 18 μm mixing with elements Ti and Al is in the boundary between the intermediate Al2O3 layer and the Ti tube, and melting zone “2” with thickness about 38 μm mixing with elements Ni, Cr, and Al is in the boundary between the intermediate Al2O3 layer and the NiCr bar. Elements are randomly distributed in the melting zones, and the element diffusions during explosive cladding process do not occur (Fig. 8c). The X-ray diffraction result reveals that two kinds of the intermetallics AlTi3 and Al0.9Ni4.22 are detected from the interfacial reactions during the explosive cladding process (Fig. 9). It should be noted that no intermetallics with elements Ti and Ni are generated in the cross section of the composite bar due to the CP-Ti tube is isolated from the NiCr alloy bar. Therefore, the Ti/Al2O3/NiCr composite bar is characterized by the consolidated ceramic intermediate layer and the metallurgical bonding interfaces. The intermetallics AlTi3 and Al0.9Ni4.22 are generated in the bonding interfaces. 3.3. Formation mechanism of the interface of the composite bar The formation of bonding interface of Ti/Al2O3/NiCr composite bar plays a crucial role in deciding the properties of the composite. In this work, intermetallics AlTi3 and Al0.9Ni4.22 are produced by interfacial reactions of molten Al2O3 and molten metals indicating that the temperature during explosive cladding process reaches up to the melting point of Al2O3 (2323 K). Many parameters may control the formation of the interfaces, and cooling rate is one of the key factors to decide the quality of interfaces. The temperature field of the explosive cladding interface can be illustrated as follows [21]. rffiffiffiffi tr T ð0; t Þ ¼ T m  ðt≻t r Þ ð2Þ t

∂T Tm pffiffiffiffi 1  t r  pffiffiffiffiffi ¼− 2 ∂t t3

ðt≻t r Þ

ð3Þ

where tr is the time of detonation wave back to explosive cladding interface, and T, Tm and t are the temperature, the melting point of Al2O3 and time, respectively. The parameter tr is defined as follows.

tr ¼

2H C0

ð4Þ

where H is the thickness of clad material, C0 is the speed of volume wave. The physical parameters of the Ti/Al2O3/NiCr composite bar are the follows. H, Tm, and C0 are 2 mm, 2323 K (2050 °C), and 4695 m/s, respectively. Then, the tr is 0.852 microseconds (μs), and the solidification rate is shown as follow, T ð0; t Þ ¼ 1:792  t

−12

∂T −3 ¼ −0:896  t 2 : ∂t

ðt≻0:852 μsÞ

ð5Þ ð6Þ

When the time t is larger than 0.852 μs, the relation between time (t) and the cooling rate (V) in the melting zone is shown in Fig. 10. At the beginning, the cooling rate reaches up to 1.14 × 109 K/s (1.14 × 109 °C/s). And the cooling rate declines fast with increasing the time. Therefore, the intermetallics AlTi3 and Al0.9Ni4.22 produced by interfacial reactions of molten Al2O3 and molten metals can be reserved and no mass diffusion occurs during the cooling. From the above results and analysis, three main stages proceeding during the formation process of the tri-layered Ti/Al2O3/NiCr composite bar are proposed, as shown in Fig. 11. They include the explosive compaction of Al2O3 nanopowders, the collision with NiCr alloy bar and the formation of the interface of NiCr/Al2O3, and the collision with Ti tube and the formation of the interface of Ti/Al2O3. In the first stage (Fig. 11a), dramatic deformation and surface melting of the Al2O3 particles are considered as the main mechanism which contribute to good bonding of ceramic powders. Energy of heat induced by adiabatic friction allows deposition of powders on the surface, which cannot transmit into the inner of powders in extremely short time, and the dramatic adiabatic temperature rise lead to formation of molten surface [10,11]. Shang and Meyers had also observed molten areas and

Fig. 8. Distribution of chemical elements Ti, Al, Ni, Cr by electron probe analysis. (a) Scanned micrograph of the interface, (b) Line scan of elements in the interface, and (c) Map scan of elements in the interface.

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Fig. 11. Schematic of formation process of interfaces of Ti/Al2O3/NiCr composite bar. (a) Consolidation of the Al2O3 nanopowders, (b) Formation of the interface of Al2O3/NiCr, and (c) Formation of the interface of Al2O3/Ti.

heavy deformation of ceramic powders in the research of explosive compaction [22]. In fact, consolidation is achieved as a shock-wave passes through a porous medium and is related to the following sequences, which include high-velocity collision, plastic deformation, fracture of particles, filling the interstices, interparticle friction, cleaning of surfaces, preferential heating of particle surfaces leading to partial melting, and subsequent bonding. Macrocracks and remaining pores are the two major problems in the dynamic consolidation of ceramic powders [11]. Because the Ti tube reduces the direct impact of the explosive in the present work, macro crack is rare observed in samples, and some Al 2O 3 particles are bonded together via molten surface, as marked by arrows “a” in Fig. 7b and c. Therefore, the Al2O3 nanopowders are excellently bonded under explosive processing conditions. As for the second and the third stage (Fig. 11b and c, respectively), wetting of Al2O3 powders by molten metals and rapid cooling rate of the products are considered as key factors to explain the formation of hetero interfaces. The Al2O3 powders with high packing density are pushed forward by Ti tube and violently crash into the NiCr bar with high-speed, and the temperature rise in the NiCr alloy caused by the collision is over 2300 K which is able to melt the surface of Al2O3 and produce the jets of the NiCr alloy (Fig. 11b); Reflected wave inducing by the collision of Al2O3/NiCr acted on the Ti tube and resulted in dramatic temperature rise at the interface of Ti/Al2O3 which accounts for the formation of the jets of the CP-Ti. The Al2O3 particles are covered by the jets with high temperature. The Al2O3 powders at the interfaces of Ti/Al2O3 and Al2O3/NiCr are covered by molten metals and achieve intimate contact marked by arrows “b” (Fig. 7b). The active elements Ti and Ni interact with Al2O3 and produce intermetallics AlTi3 and Al0.9Ni4.22 (Fig. 9), which are good for promoting wetting of Al2O3 by the molten metal. Adhesion can be improved by interfacial reaction between a liquid metal and ceramic [23–25]. Subsequently, they cool

down at a high cooling rate up to 1.14 × 109 K/s at the beginning (Fig. 10). There is no time for the element diffusions during explosive cladding process. The average thickness of the melting zone in the interface of Al2O3/NiCr is about 38 μm, while the average thickness of the melting zone in the interface of Ti/Al2O3 is about 18 μm, as shown in Fig. 8. The melting zone of the NiCr/Al2O3 alloy is relatively much thicker than that of the Al2O3/Ti due to melting point of NiCr alloy is lower than that of CP-Ti. Therefore, the good quality interfaces of the Ti/Al2O3/NiCr composite bar in this study are owing to that the molten surfaces of Al2O3 particles which are surrounded by molten metal and achieve metallurgical bonding at the interfaces. At the same time, occurrence of intermetallics through interfacial reaction is beneficial for formation of interfaces of the Ti/Al2O3/NiCr composite bar.

4. Conclusion The CP-Ti tube, the Al2O3 nanopowders, the NiCr alloy bar are bonded through explosive compaction/cladding process. The Ti/Al2O3/NiCr composite bar is characterized by the consolidated ceramic intermediate layer and the metallurgical bonding interfaces. The intermediate ceramic layer with fully consolidated Al2O3 nanopowders plays a role of insulation and thermal conductance in the Ti/Al2O3/NiCr composite bar. This composite bar can meet specific demands of medical apparatus and instruments, such as biocompatibility and electric heating function and at the same time ensuring safety in use. The melting zone and the heat affected zone are generated at the cladding interfaces. The average shear strength of the composite bar is about 9.36 MPa. The intermetallics AlTi3 and Al0.9Ni4.22 are generated in the bonding interfaces. The process of the formation of the trilayered Ti/Al2O3/NiCr cladding bar includes the explosive compaction of the Al2O3 nanopowders, the collision with the NiCr alloy bar and

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the formation of the interface of NiCr/Al2O3, and the collision with the CP-Ti tube and the formation of the interface of Ti/Al2O3. Acknowledgments This work was financial supported by the Hunan Provincial Natural Science Foundation of China (No. 12JJ2028), and by a scholarship from the China Scholarship Council (No. 201308430093). The authors would like to express their sincere thanks to Professor Marc. A. Meyers at university of California, San Diego for good suggestions and experimental conditions.

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Titanium/aluminum oxide/nickel chromium (Ti/Al2O3/NiCr) composite bar prepared by explosive compaction/cladding technique represents a new kind of san...
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