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2 Thin Solid Films 515 (7) Thermal oxidation properties of titanium nitride and titanium aluminum nitride materials A perspective for high temperature air-stable solar selective absorber applications Abstract Y. Yin a,, L. Hang a,b, S. Zhang c, X.L. Bui c a Applied and Plasma Physics, Physics School, University of Sydney, NSW 6, Australia b Optical Thin Films Lab, Xian Institute of Technology, China c School of Mechanical and Aerospace Engineering, Nanyang Technological University, Singapore Received 6 July 5; received in revised form 12 January 6; accepted 22 March 6 Available online 15 May 6 Air-stable high temperature solar selective surfaces have the advantages of simplifying the design, and reducing the cost of solar thermal energy conversion systems. Previous studies on the properties of titanium nitride (TiN) or titanium aluminum nitride (TiAlN) films suggested that these materials could be a candidate for solar energy applications. In this paper, we report that oxidation occurs at 45 C, and an oxide layer of about 3 nm was formed after only a few minutes of heat treatment with oxygen. The thickness of the oxide layer is comparable to the thickness of the absorbing layer of the solar thermal selective absorbers, which can affect significantly the solar thermal performance. TiN produced at higher nitrogen pressure (2.1 Pa with 4% nitrogen in argon) could absorb oxygen more easily into bulk and was less oxidation resistant during the heat treatment than that produced at.4 Pa of 4% nitrogen in argon. The hardness after the oxidation treatment was slightly increased by approximately 1%, consistent with reported oxidation resistant properties of this material for mechanical protection applications. As a result of this study, TiN or TiAlN as an element may not be suitable candidates for use as solar selective absorbers in air-stable high temperature applications. 6 Elsevier B.V. All rights reserved. PACS: i; Bz; 89.3.Cc Keywords: Solar thermal energy conversion; Solar thermal selective surface; Titanium nitride 1. Introduction Titanium nitride (TiN) was first proposed for use as an element in high temperature air-stable solar selective absorbers in 1984 [1]. TiAlN was also recently suggested for applications in solar selective absorbers and solar control windows [2]. However, no experimental results were reported showing reasonable high temperature air-stable solar thermal performance of such solar selective absorbers using TiN or TiAlN materials. Another related material, titanium nitride oxide (TiN x O y ), was commercially developed successfully as a solar absorbing material for increased operation temperature applications in air [3], which now has a sizable market fraction in flat panel solar hot water systems. Similar to solar selective absorbers using metal/dielectric cermet materials [4], solar Corresponding author. address: (Y. Yin). absorption of TiN x O y results from the compositional mixture of metallic element and dielectric material. In this case, TiN x behaves as metallic element and TiO y as dielectric material. During the deposition of the films for such solar selective surfaces applications in conventional large scale deposition systems, oxygen is easily incorporated into TiN or TiAlN thin films unless costly equipment and procedures are used. High temperature air-stable solar selective absorbers are required to operate in air at temperatures of over 4 C for cost reduction and efficiency improvement in solar thermal power plant and solar cooling applications [5]. Unfortunately, air-stable solar thermal selective surfaces are not available at this stage for such a high temperature. Various literatures reported that TiN and TiAlN coatings for wear resistant applications were good candidates for oxidation resistance (45 C for TiN and over 6 C for TiAlN [6,7]). These temperatures are much higher than that for TiN x O y. However, for wear resistant applications, thick coatings (up to 4-69/$ - see front matter 6 Elsevier B.V. All rights reserved. doi:1.116/j.tsf

3 283 Y. Yin et al. / Thin Solid Films 515 (7) Table 1 RBS oxygen content for different TiN samples before and after heat treatment at 45 C Sample Top layer Bulk layer D-TiN 1 nm thick, TiO 1.3 TiN 1.2 O (b.1) C-TiN 1 nm thick, TiO 1.3 TiN 1.2 O (b.1) P-TiN 1 nm thick, TiO 1.3 TiN 1. O.2 Heated D-TiN nm thick, TiO 1.3 TiN 1.2 O (b.1) Heated C-TiN 25 nm thick, TiO 1.3 TiN 1.2 O (b.1) Heated P-TiN nm thick, TiO 1.3 TiN.9 O.3 1 μm) are often required. This thickness is much higher than that for the solar thermal selective absorbing layer, typically less than.2 μm [4,8]. Also, as mechanical hard coatings, the optical properties are not critical and the required high temperature working life may be in the order of hours or days. However, the working life of solar selective absorbers should be in the order of years. With these doubts in mind, this work set out to find out whether TiN and TiAlN can indeed be good candidates for solar selective absorbers as reported. 2. Experimental details TiN and TiAlN thin films were deposited using direct current magnetron sputtering. Four different batches of samples were deposited: 1) TiN deposited at.4 Pa pressure of 4% nitrogen in argon at deposition rate of about 1 nm/min (denoted as D- TiN); 2) TiN deposited at 2.1 Pa pressure of 4% nitrogen in argon with a deposition rate of about 1 nm/min (denoted as P- TiN); 3) TiN deposited at.4 Pa pressure of 4% nitrogen in argon with a collimated device to provide direct beam deposition at deposition rate of about 5 nm/min (denoted as C-TiN). The TiN samples were deposited using a commercial sputtering system (Applied Materials P55) with a base pressure of Pa. The substrates used were (1) silicon wafers; the thickness of the films was about 1 nm; 4) TiAlN was deposited by co-sputtering of Ti and Al targets on glass slides at process pressure of.4 Pa (the gas flow rate of Ar and N 2 was 5 and 5 sccm respectively). The power density applied on the Ti target was 2.5 W/cm 2 and that on the Al target was 1.2 W/cm 2, which resulted in an Al:Ti atomic ratio of 1:3. Oxidation treatment was undertaken at various temperatures and durations in air. Energy dispersive X-ray (EDX) method was used to analyse the oxygen contents for these films. The oxygen incorporation was quantified using Rutherford backscattering spectrometry (RBS) with 2 MeV alpha particles. The hardness was assessed using an UMIS- nano-indentor. A 1. μm diameter spherical indentor was used and the maximum penetration depth was about one third of the total TiN thickness. The contact pressure (or Meyers hardness, which is initially elastic) and modulus were calculated from the load-penetration data by using the analysis procedure developed by Field and Swain [9]. AVarian Cary 5 optical spectrometer and a Shimadzu infrared spectrometer were used for optical analyses in the wavelength range between 3 nm and 25 μm. EDX analysis was performed at Philips SEM 55 with accelerating voltage of kv. 3. Results and discussion The first set of thermal oxidation tests was to oxidise the TiN samples at 45 C in air by transferring samples into an opendoor furnace and idled at 45 C, then closing the door and flushing dry nitrogen (3 l per min) for 1 h to cooling down the furnace to 3 C before taking the sample out. We estimated the oxidation time in this process was about 5 1 min (noted as 5 min below). Humidity of the air was about 42%. RBS measurement indicated that a 25 nm thick layer at the top of the treated samples was converted into titanium oxide with an oxygen to titanium atomic ratio of about 1.3. Table 1 shows the oxygen content in the films before and after heat treatment in air obtained from RBS for the top layer and bulk respectively. In all cases, we found that the heat treated TiN films all had significantly different colour from that of the as-deposited. The heat treatment resulted in a 25 nm thick surface layer for all samples with similar oxygen content. However, the TiN deposited at higher nitrogen pressures had higher oxygen content in the bulk layer after the treatment. It is known that [1] the TiN x O y resistivity increases with an increase of oxygen content. Fig. 1 shows the typical data of sheet resistivity as a function of time for the as-deposited TiN films. The resistivity of the P-TiN sample was much higher than that of D-TiN sample. This is due to the much higher nitrogen deposition pressure for P-TiN films. Both the as-deposited D- TiN and C-TiN films had a golden colour, but the P-TiN films were brown. The sheet resistivity of the as-deposited TiN films increased in air at room temperature, and the rate of the increase depended on deposition conditions. The sheet resistivity of the D-TiN changed about 8% within about two weeks while that of P-TiN was 4% during the same period. This can be interpreted as oxygen incorporation into the films through grain boundaries. As shown in Table 1, the oxygen content in the bulk asdeposited P-TiN films was high, whilst the oxygen content in the bulk as-deposited C-TiN and D-TiN films was not detectable. This indicates that at the room temperature the golden coloured C-TiN and D-TiN films were resistant to oxygen diffusion but not the P-TiN films. In other words, the Sheet Resistivity (Ohm-cm) 6 4 D-TiN P-TiN Time (hrs) Fig. 1. Sheet resistivity of TiN samples as a function of time in air at room temperature.

4 Y. Yin et al. / Thin Solid Films 515 (7) Oxygen atomic ratio (arb. units) Heat Treated C-TiN D-TiN P-TiN Fig. 2. EDX oxygen content of the TiN samples before and after being heated in air for 5 min at 45 C. Fig. 4. Optical micrograph of TiAlN after heat treatment at 5 C for 1 h. TiN deposited at higher nitrogen pressure is less dense, so that the oxygen content in the bulk layer increases with time to the level as shown in Table 1. The RBS data in Table 1 was taken two weeks after the deposition. The resistivity was not reversible by placing the samples in vacuum, indicating that the absorbed oxygen was chemically bonded into the films. The uncertainty of the oxygen content from RBS analysis was about 1%. The oxygen content detected from the EDX analysis provided estimation for the oxygen ratio for these films in the whole TiN layer, which was used as estimation in this work because all films had the same thickness and substrate. Fig. 2 shows a comparison of the oxygen content determined by EDX before and after thermal treatment. Approximately, the total oxygen content was almost doubled after thermal treatment for all samples. Combining with the RBS data that a 25 nm thick TiO 1.3 layer was formed after thermal treatment, we estimated that the oxygen content in as-deposited bulk TiN (D- TiN and C-TiN) was about 1%. The P-TiN deposited under high pressure had higher bulk oxygen content due to a lower density. This is consistent with the data in Fig. 1. The results on oxidation tests indicated that TiN did not have ideal oxidation properties for applications as high temperature solar thermal selective surfaces. Hardness (GPa) Heat Treated The hardness of the TiN films before and after the heat treatment was shown in Fig. 3. The hardness of the TiN films after the heat treatment did not reduce, but actually increased. This can be interpreted as an effect resulting from an incorporation of oxygen atoms into the films, which increased the density of the films. The densification effect of the oxidation treatment of the TiN and TiAlN films was also confirmed when the adhesion failure due to the oxidation treatment was observed. Fig. 4 shows an example of a 1 μm thick TiAlN film buckling up from the substrate due to high intrinsic stress built up in the film. The TiAlN sample was heated in air at 5 C for 6 min. The dimension of the worm-like feature is about 3.5 μm (both its width and height). It is possible to improve the adhesion by inserting an adhesion layer or using different substrates such as for surface protection applications. In solar thermal selective absorbing applications, however, adhesion layer, even as thin as a few nanometres, can alter significantly the optical performance. As solar thermal selective absorbers require much longer working lifetime (in years), such mechanical stress induced by oxidation is not desirable. The optical properties of TiN and TiAlN films were found to depend on thermal treatment history, which was expected Reflectance (%) o C 5 o C Wavelength (nm) Fig. 3. Mechanical hardness of the TiN samples before and after being heated in air for 5 min at 45 C. Fig. 5. Reflectance spectra of TiAlN after being heated at different temperatures for 1 h.

5 2832 Y. Yin et al. / Thin Solid Films 515 (7) according to the above oxidation result. Fig. 5 shows the reflectance spectra of the TiAlN after being heated at various temperatures in air for 1 h. The wavelength range between 3 nm and 2 μm is correspondent to solar absorption and the wavelength beyond 2 μm is relevant to the energy loss through thermal radiation from solar thermal selective surfaces. Though solar thermal performance of solar selective surfaces depends on the combined optical effect of multi sublayers, stable optical properties of each sublayer are necessary, in particular, for the air-stable high temperature applications. The reflectance (for the sample being heated at 4 C in air for 1 h) changed about 1% in the main solar radiation range, which suggests an unacceptable surface degradation occurred for applications as a solar thermal selective absorber. Further heating the sample in air (5 C in air for 1 h) the reflectance spectrum was changed significantly in both the solar spectrum range and infrared long wavelength range. This indicates a catastrophic degradation for its solar thermal applications. The thermal oxidation process does not necessarily produce an optical homogeneous material as indicated by the RBS analysis. From the morphology analysis, we can conclude that changes of optical performance for samples heat treated at temperatures up to 4 C were originated from the changes of optical constants and that the changes for samples heat treated at 5 C were resulted from a combination of the effects from both optical constants and surface morphology or roughness. 4. Conclusions TiN and TiAlN were found in this study not suitable as elements in use for the air-stable high temperature solar selective absorbers application as previously expected. Heat treatment in air at 45 C for a few minutes resulted in a replacement of nitrogen with oxygen, predominately in a thin sublayer on the top of the surface. The thin oxide layer, about 25 nm, is very thin for mechanical protection applications, but quite thick compared to the total thickness of the absorbing layer of solar thermal selective surfaces. Such change due to oxidation can result in a significant degradation of the optical performance of the surface. When metallic material is incorporated into dielectric substance to form a cermet-type solar absorption layer, the metallic layer or particles should have dimensions in the range of about 1 nm, too small to allow such an oxidation layer to be formed. The less dense TiN absorbed oxygen more easily at room temperature and had a higher oxidation rate or less resistance to oxidation in the heat treatment. This explains that conventional TiN x O y solar selective surfaces are not resistant to oxidation or not suitable to operate at temperatures above 25 C. The hardness of the films after heat treatment did not reduce compared to that of asdeposited ones, consistent with the observation that TiN and TiAlN films are good candidates for wear resistance applications at high temperatures. This study suggested that TiN or TiAlN as an element may not be suitable candidates for use as solar selective absorbers in air-stable high temperature applications. Acknowledgements This work is supported by USSS Pty Ltd through the University of Sydney, and LH acknowledges support from the Chinese National Scholar Foundation. References [1] P.J. Martin, R.P. Netterfield, W.G. Sainty, C.G. Pacey, J. Vac. Sci. Technol., A 2 (1984) 341. [2] A. Schuler, V. Tommen, P. Reimann, P. Oelhafen, J. Vac. Sci. Technol., A 19 (1991) 922. [3] C. Lampert, Proc. SPIE 3138 (1997) 134. [4] Y. Yin, R.E. Collins, J. Appl. Phys. 77 (1995) [5] D. Mills, G. Morrison, Sol. Energy 68 (1999) 263. [6] L. Rebouta, F. Vaz, M. Andritschky, M. DaSilva, Surf. Coat. Technol (1995) 7. [7] P. Panjan, B. Navinsek, M. Cekada, A. Zalar, Vacuum 53 (1999) 127. [8] Q. Zhang, Y. Yin, D.R. Mills, Sol. Cells Mater. 4 (1996) 43. [9] J. Field, M. Swain, J. Mater. Res. 1 (1995) 11. [1] E. Alves, A. Ramos, N. Barradas, F. Vas, P. Cerquerira, L. Rebouta, U. Kreissig, Surf. Coat. Technol (4) 372.

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