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Radiation Effects and Defects in Solids

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TiAlN coatings synthesised using a dense plasma focus system and varied focus shots
Tousif Hussain , Riaz Ahmad , Jamil Siddiqui & Nida Khalid
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Department of Physics, Government College University, 54000, Lahore, Pakistan Available online: 31 Oct 2011

To cite this article: Tousif Hussain, Riaz Ahmad, Jamil Siddiqui & Nida Khalid (2011): TiAlN coatings synthesised using a dense plasma focus system and varied focus shots, Radiation Effects and Defects in Solids, 166:11, 873-883 To link to this article: http://dx.doi.org/10.1080/10420150.2011.616957

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Radiation Effects & Defects in Solids Vol. 166, No. 11, November 2011, 873883

TiAlN coatings synthesised using a dense plasma focus system and varied focus shots
Tousif Hussain, Riaz Ahmad*, Jamil Siddiqui and Nida Khalid
Department of Physics, Government College University, 54000 Lahore, Pakistan

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(Received 2 May 2011; nal version received 15 August 2011) TiAlN coatings were synthesised by a 2.3 kJ pulsed plasma focus system. The effect of focus shots on crystallography, microstructure, surface morphology, roughness and hardness was investigated. The coatings crystallography and microstructure were investigated using X-ray diffraction (XRD) characterisation. The XRD data showed that TiAlN coatings were crystallised in the cubic NaCl B1 structure with orientations in the (111), (200), (220) and (311) crystallographic planes. Texture coefcients showed a competition between (111) and (200) planes. The coatings surface morphology and thickness analyses were carried out using scanning electron microscopy (SEM). SEM micrographs showed dense and uniformly spread lm with ne-grained morphology with hardly any pit, hole and crater. The surface roughness and hardness of TiAlN coatings were investigated by atomic force microscopy and Vickers microhardness tester. Grain size and roughness were found to decrease, whereas thickness and hardness were found to increase, with increasing focus shots. Keywords: titanium aluminium nitride; plasma focus system; X-ray diffraction; SEM; AFM

1.

Introduction

Titanium nitride is a member of the refractory transition metal nitrides family showing characteristics of both covalent and metallic compounds (1, 2). For a few decades, TiN coatings have been applied to tools, dies and many mechanical parts to increase their lifetime and performance owing to their excellent mechanical, thermal and electronic properties, such as good thermal stability, high corrosion resistance and low electrical resistivity. Therefore, they have many applications ranging from coatings on cutting tools to diffusion barriers in microelectronic applications. However, TiN coating is degraded by oxidation at high temperature during working. So, it is important to improve its oxidation resistance for successful use. As a possible solution to this problem, aluminium atoms have been added to the TiN material considering that both TiN and TiAlN have the same crystallographic structure (fcc) (3). In high-temperature applications, a dense and strongly adhesive Al2 O3 lm is observed because of diffusion of Al atoms to the surface, which stops further oxidation. TiAlN is expected to be a promising candidate as a hard coating layer because it shows excellent properties, especially for high-temperature use (4, 5).
*Corresponding author. Email: ahriaz@gmail.com

ISSN 1042-0150 print/ISSN 1029-4953 online 2011 Taylor & Francis http://dx.doi.org/10.1080/10420150.2011.616957 http://www.tandfonline.com

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Different TiAlN coatings have been reported and been synthesised by various deposition techniques including cathodic arc ion plating (68), ion beam sputter plating (9), ion mixing and vapour deposition (10) and reactive magnetron sputtering (1115). The dense plasma focus (DPF) (16, 17) technique is one of the prospective hybrid deposition methods for the application of TiAlN coatings. The use of plasma focus for surface modication and thin lm deposition purposes has shown that this pulsed plasma device owns interesting features of high deposition rates and energetic deposition process (1827). It may be signicant to mention that the plasma focus device has not been reported prior to this work for the synthesis of TiAlN coatings to the best of my knowledge. The synthesis of TiAlN coatings using plasma focus deposition system is not only economic, simple, efcient and time-saving, but also provides the high deposition rate having good adhesion between the deposited coatings and the substrate. DPF deposition can produce a denser coated layer in less deposition time. It does not need extra substrate heating during lm deposition because the substrates are heated during ion beam treatment compared with other treatments. In this work, the preparation of TiAlN coatings by varying focus shots by the DPF device is described. The lms were deposited at 9 cm axial position with the anode axis. The effect of varying focus shots on microstructure, surface morphology, surface roughness and hardness of these coatings was studied.

2.

Experimental setup and method

Synthesis of the TiAlN thin lms was done using polished 10 10 5 mm3 aluminium substrates and a titanium target tted at the top of the anode. The substrates and target were cleaned by rinsing in an ultrasonic bath of water. The deposition was performed in a Mather-type DPF device powered by a single 32 F, 15 kV capacitor. Details of the plasma focus device are given in earlier works (16, 17, 27). The schematic diagram of the system is shown in Figure 1. For the deposition of TiAlN coatings, a copper anode with a titanium target tted at top was used. Nitrogen was used as a working gas. The chamber was evacuated up to 1 102 mbar by a rotary vane pump and lled with high-purity nitrogen gas at optimum pressure of 1.25 mbar before plasma focus operation. The substrates are mounted, at the anode axis, at a xed distance of 9 cm from the top of the anode using a substrate holder behind a movable metallic shutter. It always takes several focus shots to get strong focusing after each fresh loading of gas for lm deposition. A metallic shutter in between the anode and the substrate was used to prevent the exposure of substrate to these early weak focusing shots as shown in Figure 1. The shutter is removed after two or three focus shots, after getting good focusing. The focusing action was recorded using a simple resistive voltage probe and Rogowski coil. The dip in the Rogowski coil signal and spike in the voltage probe signal help in ascertaining good focusing action in the plasma focus (PF) discharge. The focus shot at which a maximum dip in the Rogowski coil signal/maximum spike in the voltage probe signal takes place is termed as the stronger focus, and it is a very common experience that focusing action becomes stronger and stronger as focus gets stabilised after ring a few focus shots resulting in the generation of higher energy, higher ux ions. The focus shots are red at a frequency of one-shot at a time long enough to ensure thermal relaxation of specimen after being heated by the preceding ion beam. The coatings were synthesised, at room temperature substrates, with 10, 20, 40 and 50 focus shots. The qualitative understanding of thin lm deposition process, in a DPF device, is as follows: DPF transfers the electrical energy stored in the capacitor to the chamber by a spark gap switch. The dielectric breakdown of gas occurs along the insulator surface between an anode and a cathode and an axisymmetric current sheath forms around the insulator. This current sheath moves towards the open end of electrode assembly under J B force. When this current sheath reaches the

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Wilson seal

Vaccum chamber Sample holder

Shutter

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Sample

Insert Electrode assembly

C S Trigger
Figure 1. Schematic diagram of the DPF system.

HV

top of electrode assembly, it collapses radially inward during the nal focus phase. This is the instant where microinstabilities, mainly m = 0 instabilities, start to grow and in turn strengthen the induced electric eld locally. This enhanced electric eld, coupled with magnetic eld, breaks the focused plasma column by accelerating ions towards the top of chamber and electrons towards the positively charged anode. After this, disruption of the plasma column starts, and it breaks up completely to form hot (12 keV) and dense (102526 m3 ) plasma. The TiAlN coatings were characterised for their structure, surface morphology, roughness and hardness by a variety of techniques. The crystalline structure of the lms was characterised by X-ray diffraction (XRD) using an XPert PRO MPD X-ray diffractometer. A HITACHI S-3400 N scanning electron microscope (SEM) was used to study surface morphology of the lms and to nd thickness using a cross-sectional view. The surface roughness was measured using a Pico instrument atomic force microscope (AFM) (Molecular Imaging Inc.). The hardness measurement was taken using a Wilson Wolpert 401 MVA Vickers microhardness tester.

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3.

Results and discussion

3.1. Phase identication Figure 2 shows the XRD peak patterns, ranging from 30 to 85 , of four coatings for various focus shots. XRD patterns showed the development of two phases: one with fcc NaCl B1 structure similar to TiN structure and the other with AlN (fcc phase). Differentiation of the TiN and TiAlN phases using the diffraction method is impossible because of their isomorphous nature, as TiAlN is, in fact, the secondary solid solution based on titanium nitride. The diffraction patterns exhibit a pattern of crystalline TiAlN with orientations of (111), (200), (220) and (311) and AlN with orientations of (111), (200) and (220). Native oxide of aluminium, which was presented in a substrate surface, is removed gradually with the increase in the number of focus shots (28, 29). The observed intensity of the TiAlN planes for TiAlN coatings showed an increasing trend when focus shots increased (Figure 3). Taking into account that the intensity of diffraction peaks is related to the quantity of planes that generate diffraction (30), an increase in intensity shows greater compaction in the coatings with the increase in focus shots. The possible explanation of increasing intensity for higher focus shots is that the intensity of diffraction of the peaks is dependent on the energy and ux of ions that are impinging on the lm surface. As more focus shots are red, the focus becomes more stable and has stronger focusing action, resulting in the generation of high-energy and high-ux ions (31). 3.2. Lattice constant

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In order to further investigate the microstructural changes of plasma focus deposited TiAlN coatings, the lattice constants were calculated. The peak position revealed a nonlinear variation of the lattice parameter (Figure 4), which is considered to result from the composite nature of the ternary nitrides and the substrate high heating effect during deposition. The reported lattice parameter of TiN (32) is 0.424 nm. It is clear from Figure 4 that the lattice parameter of (111) and (200) planes are less than the reported lattice parameter of TiN. The smaller lattice parameter was related to the formation of a solid

Figure 2. XRD patterns obtained for TiAlN coatings deposited at a distance of 9 cm at zero angular positions for various number of focus shots.

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Figure 3.

Intensity as a function of the number of focus shots.

Figure 4.

Lattice constant with varying number of focus shots.

solution structure where Al atoms substitute Ti atoms in the TiN cubic lattice (remaining still a fcc structure), since the aluminiums atomic radius (0.143 nm) is smaller than that of Ti (0.146 nm). This leads to shrinkage in the lattice parameter and hence a shift in 2 value in the XRD. 3.3. Grain size

Using the broadening of the peaks, it is possible to determine the grain size from the Scherrer formula (33). The grain size (D) of the thin lms was estimated from the following equation: D= 0.9 , cos (1)

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Figure 5.

Grain size as a function of the number of focus shots.

where is the full width at half maximum (FWHM) of the diffraction peak, is the wavelength of the incident Cu K X-ray (1.514 ) and is the diffraction angle. The grain size curve (Figure 5) is inuenced by the number of focus shots, when increasing the focus shots, the grain size was found to decrease linearly. With the reduction in the grain size, the dislocation activity is restricted and crack propagation along grain boundaries is prevented. 3.4. Texture coefcient

The XRD spectra consist of primarily (111) and (200) reection. The texture coefcients of the TiAlN coatings as a function of focus deposition shots were calculated from their respective XRD peaks using the following formula: Texture coefcient (Tc ) = I(hk1) , I(111) + I(200) (2)

where hkl represents the (111) and (200) orientations. The Tc value for a particular set of (hkl) planes is proportional to the number of grains that are oriented with the plane parallel to the surface of sample (34). The texture coefcients of the (111) and (200) orientation are high compared with other orientations in the plasma focus deposited TiAlN thin coatings (Figure 6). The presence of mixed (111) and (200) texture for deposited lms is due to the competitive growth between the surface and strain energy. Random orientations might be due to higher aluminium contents in coatings. 3.5. Surface morphology

The surface morphological studies of the plasma focus deposited TiAlN coatings that exhibit good crystallinity were observed by SEM as shown in Figure 7. The sample exposed to 10 focus shots showed dense and ne-grained morphology with few pit holes and crater present throughout the TiAlN coating. It is noticeable that there is no trace of columnar growth in all synthesised TiAlN coatings. The columnar growth results from

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Figure 6. Texture coefcient with varying number of focus shots.

Figure 7. SEMs of the TiAlN coatings synthesised at (a) 10 focus shots; (b) 20 focus shots; (c) 40 focus shots and (d) 50 focus shots.

self-shadowing during deposition process and is the characteristic feature for evaporation and sputter deposition (3537). For sufciently high energies, the impacting cluster compresses and anneals the area directly, hindering the columnar growth. The energetic cluster also leads to a self-smoothing of surface (38, 39). The average thicknesses of the samples synthesised using various focus shots can be measured from the corresponding cross-sectional SEM images as shown in Figure 8. The results showed that the deposition thickness of the TiAlN coatings in a plasma focus system is in some way

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Figure 8. Thickness as a function of the number of focus shots (inset: cross-sectional SEM of TiAlN coating synthesised with 40 focus shots).

linear with the typical deposition rate of about 276 50 nm per shot at focus bank storage of 2.3 kJ energy. It may be noted that the deposition rate achieved in plasma focus is high compared with the deposition rates obtained in other devices. It may also be noted that energetic ions also sputtered the substrate. 3.6. Roughness measurement The coating morphology was also analysed using AFM. Figure 9(ac) and (d) presents the 3D surface topography and root mean square (RMS) roughness of the TiAlN coatings synthesised with varying number of focus shots, respectively. All the AFM images were obtained in a scanning area of 5 m 5 m. The values of RMS roughness were derived from AFM images, which were obtained from the average of the values measured in four random areas. Roughness decreases up to 40 number of focus shots as thickness increases (Figure 8) and again increases slightly for 50 number of focus shots. The lm roughness is found to decrease with the increase in the focus shots except for thin lms deposited for 50 focus shots which is consistent with SEM results. Bertalot et al. (40) commented that the ions emitted in plasma focus have a wide energy range in a fountain-like geometry with anisotropy in their angular distribution. Most of the ions are emitted in a small solid angle along the anode axis and their ux decreases with the increase in the angle. This also infers that roughness would be different at different areas of samples, which is consistent with our results as shown in Figure 9. 3.7. Microhardness

The Vickers microhardness (HV) as a function of imposed load for plasma focus deposited TiAlN coatings is shown in Figure 10. Four hardness measurements at 25, 50, 100 and 200 gf loads, applied for dwell time of 5 s, for each sample were used for microhardness prole. The hardness of untreated aluminium sample is also presented for comparison. The hardness was observed to increase with the increase in focus shots except for 50 focus shots. A steep fall of the microhardness values in the near-surface region of the samples exposed to focus shots suggests a concentration

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Figure 9. Atomic force micrographs of the TiAlN coatings synthesised at (a) 10 focus shots; (b) 20 focus shots; (c) 40 focus shots and (d) graph of RMS roughness with varying focus shots.

Figure 10.

Microhardness as a function of the applied load and the number of focus shots.

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gradient towards the bulk. The morphology of the material, that is, microstructure-related effects, severely affects the hardness of the material (41). The increase in the microhardness values may be credited to increase in ion ux and incorporation of titanium and nitrogen ions into the deposited TiAlN coatings (42). There are many factors that may affect the measured hardness of TiAlN coatings, including the grain size, residual stresses and densication of coatings. A hardening (H) because of a decrease in the average grain size (d) according to the HallPatch relationship H1/d 1/2 might also be included in the present case. This can be deduced from the observation that hardness increases as the grain size decreases from about 49 to 29 nm (Figure 4). 4. Conclusions

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TiAlN coatings were grown by the DPF system with varying focus shots. The inuence of focus shots on crystallography, microstructure, surface morphology, roughness and hardness was studied. According to the XRD analysis, crystallographic orientation in (111), (200), (220) and (311) planes was found, presenting a competition between (111) and (200) planes. On the other hand, a decrease in the grain size is observed with increase in focus shots. SEM micrographs showed a dense and uniformly spread lm with ne-grained morphology. Hardness is found to follow the HallPatch relationship. The observed variation in XRD, SEM and hardness results is explained based on the ion emission characteristics of the plasma focus system. The results showed that 40 focus shots are acceptable for the synthesis of dense, smoother and harder coatings of TiAlN at room temperature using the plasma focus system. Acknowledgements
One of the authors, Tousif Hussain, would like to thank HEC, in Pakistan, for their nancial support. Dr Shahzad Naseem (Center for Solid-State Physics, University of the Punjab, Lahore, Pakistan), Dr M. Zakkaullah (Physics Department, Quaid-i-Azam University, Islamabad, Pakistan) and R. Sammynaiken (Saskatchewan Structural Sciences Centre, University of Saskatchewan, Saskatoon, Canada) are also acknowledged for their technical support in the SEM, hardness and AFM analyses, respectively.

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