<?xml version="1.0" encoding="UTF-8"?><!DOCTYPE article  PUBLIC "-//NLM//DTD Journal Publishing DTD v3.0 20080202//EN" "http://dtd.nlm.nih.gov/publishing/3.0/journalpublishing3.dtd"><article xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" dtd-version="3.0" xml:lang="en" article-type="research article"><front><journal-meta><journal-id journal-id-type="publisher-id">AMPC</journal-id><journal-title-group><journal-title>Advances in Materials Physics and Chemistry</journal-title></journal-title-group><issn pub-type="epub">2162-531X</issn><publisher><publisher-name>Scientific Research Publishing</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.4236/ampc.2013.31A012</article-id><article-id pub-id-type="publisher-id">AMPC-30386</article-id><article-categories><subj-group subj-group-type="heading"><subject>Articles</subject></subj-group><subj-group subj-group-type="Discipline-v2"><subject>Chemistry&amp;Materials Science</subject><subject> Physics&amp;Mathematics</subject></subj-group></article-categories><title-group><article-title>
 
 
  XRD Characterization of AlN Thin Films Prepared by Reactive RF-Sputter Deposition
 
</article-title></title-group><contrib-group><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>.</surname><given-names>Matsunami</given-names></name><xref ref-type="aff" rid="aff1"><sup>1</sup></xref><xref ref-type="corresp" rid="cor1"><sup>*</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>H.</surname><given-names>Kakiuchida</given-names></name><xref ref-type="aff" rid="aff2"><sup>2</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>M.</surname><given-names>Sataka</given-names></name><xref ref-type="aff" rid="aff3"><sup>3</sup></xref></contrib><contrib contrib-type="author" xlink:type="simple"><name name-style="western"><surname>S.</surname><given-names>Okayasu</given-names></name><xref ref-type="aff" rid="aff3"><sup>3</sup></xref></contrib></contrib-group><aff id="aff2"><addr-line>National Institute of Advanced Industrial Science and Technology (AIST), Nagoya, Japan</addr-line></aff><aff id="aff1"><addr-line>Energy Science Division, EcoTopia Science Institute, Nagoya University, Nagoya, Japan</addr-line></aff><aff id="aff3"><addr-line>Japan Atomic Energy Agency (JAEA), Tokai, Japan</addr-line></aff><author-notes><corresp id="cor1">* E-mail:<email>n-matsunami@nucl.nagoya-u.ac.jp(.M)</email>;</corresp></author-notes><pub-date pub-type="epub"><day>26</day><month>04</month><year>2013</year></pub-date><volume>03</volume><issue>01</issue><fpage>101</fpage><lpage>107</lpage><history><date date-type="received"><day>January</day>	<month>22,</month>	<year>2013</year></date><date date-type="rev-recd"><day>March</day>	<month>10,</month>	<year>2013</year>	</date><date date-type="accepted"><day>April</day>	<month>18,</month>	<year>2013</year></date></history><permissions><copyright-statement>&#169; Copyright  2014 by authors and Scientific Research Publishing Inc. </copyright-statement><copyright-year>2014</copyright-year><license><license-p>This work is licensed under the Creative Commons Attribution International License (CC BY). http://creativecommons.org/licenses/by/4.0/</license-p></license></permissions><abstract><p>
 
 
      
   AlN thin films have been grown on R((1-12) surface-cut)-Al<sub>2</sub>O<sub>3</sub>, SiO<sub>2</sub>-glass and C((001) surface-cut)-Al<sub>2</sub>O<sub>3</sub> substrates, by using a reactive-RF-sputter-deposition method. X-ray diffraction (XRD) shows that AlN film has (110) orientation of wurtzite crystal structure for R-Al<sub>2</sub>O<sub>3</sub> and (001) orientation for SiO<sub>2</sub>-glass and C-Al<sub>2</sub>O<sub>3</sub> substrates. The film thickness was analyzed by Rutherford backscattering spectroscopy (RBS) and it appears that XRD intensity does not show a linear increase with the film thickness but a correlation with the stress, i.e., deviation of the lattice parameter of the film from that of bulk. The film composition and impurities have been analyzed by ion beam techniques. Effects of high-energy ion beams are briefly presented on atomic structure (whether stress relaxation occurs or not), surface morphology and optical properties.  
   
    
 
</p></abstract><kwd-group><kwd>Aluminum Nitride Film; Composition; Impurities; Atomic Structure; Surface Morphology; Optical  Properties</kwd></kwd-group></article-meta></front><body><sec id="s1"><title>1. Introduction</title><p>It has been known that aluminum nitride (AlN) has a wide direct-bandgap (6.2 - 5.8 eV) [1,2] with hexagonalwurtzite crystal structure [<xref ref-type="bibr" rid="scirp.30386-ref3">3</xref>] and unique properties: good thermal conductivity (~3 W/cmK at 300 K) [<xref ref-type="bibr" rid="scirp.30386-ref4">4</xref>], good insulator (&gt;10<sup>11</sup> Ω∙cm) [<xref ref-type="bibr" rid="scirp.30386-ref5">5</xref>], high dielectric constant [<xref ref-type="bibr" rid="scirp.30386-ref6">6</xref>], relatively small linear-expansion coefficients (5.3 and 4.2 &#215; 10<sup>−6</sup> K<sup>−1</sup> along aand c-axis) [<xref ref-type="bibr" rid="scirp.30386-ref7">7</xref>], high sound velocity (6 km/s) [<xref ref-type="bibr" rid="scirp.30386-ref8">8</xref>] and large hardness [<xref ref-type="bibr" rid="scirp.30386-ref9">9</xref>]. Owing to these properties, AlN films have potential applications to electronic devices [<xref ref-type="bibr" rid="scirp.30386-ref10">10</xref>], surface acoustic wave (SAW) devices [<xref ref-type="bibr" rid="scirp.30386-ref11">11</xref>], actuator [<xref ref-type="bibr" rid="scirp.30386-ref12">12</xref>], transparent hard coatings and AlN composites to light-emitting devices [<xref ref-type="bibr" rid="scirp.30386-ref13">13</xref>]. Also, AlN films have been used as buffer layer for GaN [<xref ref-type="bibr" rid="scirp.30386-ref14">14</xref>] and ZnO [<xref ref-type="bibr" rid="scirp.30386-ref15">15</xref>] film growth. For these applications, X-ray diffraction (XRD) technique have been extensively employed to evaluate the crystalline quality and growth orientation of AlN films which have been grown by various techniques, chemical-vapor atomic-layer deposition (a special type of CVD) [<xref ref-type="bibr" rid="scirp.30386-ref2">2</xref>], metal organic CVD [<xref ref-type="bibr" rid="scirp.30386-ref16">16</xref>], molecular beam epitaxy [<xref ref-type="bibr" rid="scirp.30386-ref17">17</xref>], ion beam enhanced deposition (electron beam evaporation of Al combined with N ion bombardment) [<xref ref-type="bibr" rid="scirp.30386-ref5">5</xref>], reactive radio-frequency (RF) magnetron sputtering deposition [6,10,18], pulsed laser deposition (PLD) [<xref ref-type="bibr" rid="scirp.30386-ref19">19</xref>] on various substrates, sapphire [2,19], Si [5,14-16,18], SiC [<xref ref-type="bibr" rid="scirp.30386-ref17">17</xref>], Al [<xref ref-type="bibr" rid="scirp.30386-ref6">6</xref>], Mo [<xref ref-type="bibr" rid="scirp.30386-ref12">12</xref>] etc. For AlN films grown on Si(111), the authors have shown that oxygen impurities near the substrate surface affect the growth orientation and suggest that the XRD intensity decreases with increasing the stress and nearly diminishes when the stress exceeds 2%, irrespective of the film thickness (27 - 470 nm) [<xref ref-type="bibr" rid="scirp.30386-ref20">20</xref>]. Here, the stress is defined as the difference of the lattice parameters between film and bulk. Use of the stress can be justified based on the fact that c-axis length increases with the residual-stress [<xref ref-type="bibr" rid="scirp.30386-ref18">18</xref>] and temperature dependence of the lattice parameter is similar to that of the residual-stress in terms of pressure [<xref ref-type="bibr" rid="scirp.30386-ref19">19</xref>]. The result does not agree with the lattice relaxation around 50 nm of AlN on SiC [<xref ref-type="bibr" rid="scirp.30386-ref17">17</xref>] and favors the constant stress throughout the AlN film on Si(111) [<xref ref-type="bibr" rid="scirp.30386-ref16">16</xref>]. It is of interest to study whether the suggested stress is useful for the quality evaluation of AlN film grown on different substrates other than Si(111).</p><p>In this paper, we have grown AlN on R-plane cut sapphire (R-Al<sub>2</sub>O<sub>3</sub>), SiO<sub>2</sub>-glass and C-plane cut sapphire (C-Al<sub>2</sub>O<sub>3</sub>) substrates by a reactive RF-sputter deposition method. We have measured XRD, the composition, thickness and impurities, and examined use of the stress for the film quality evaluation. We also have measured surface morphology (grain size, shape and surface smoothness), which may affect the crystalline quality, since films are polycrystalline, and optical absorption. These properties might be important for applications mentioned above. For AlN on R-Al<sub>2</sub>O<sub>3</sub>, irradiation with high-energy (90 MeV Ni) ions was performed in order to study whether stress relaxation, surface smoothing and bandgap modification occur or not by ion irradiation.</p></sec><sec id="s2"><title>2. Experimental</title><p>AlN films were grown on R-Al<sub>2</sub>O<sub>3</sub>, SiO<sub>2</sub>-glass and CAl<sub>2</sub>O<sub>3</sub> substrates by using a reactive-RF-sputter-deposition method with Al target (purity of 99.999%) in pure N<sub>2</sub> gas of ~0.3 Pa with a method described in [20,21]. A reason for usage of pure N<sub>2</sub> gas is to avoid Ar inclusion into films, considering that conventionally Ar and N<sub>2</sub> mixture gas has been employed. The substrates were subjected to ultrasonic rinse in ethanol prior to the film deposition. XRD with Cu-kα radiation was performed to examine crystalline quality and orientation. The thickness, composition and impurities of films were analyzed by RBS. The growth rate was obtained to be approximately 3 nm/min for AlN on three substrates used in this study. Light impurities such as carbon and oxygen near the film surface were analyzed by using nuclear reaction analysis (NRA), <sup>12</sup>C(d, p)<sup>13</sup>C and <sup>16</sup>O(d, α)<sup>14</sup>N with 1.2 MeV d at the reaction angle of 160˚ [<xref ref-type="bibr" rid="scirp.30386-ref20">20</xref>]. In RBS and NRA, stopping powers are taken after [<xref ref-type="bibr" rid="scirp.30386-ref22">22</xref>] with the AlN density of 3.26 g∙cm<sup>−3</sup> (4.8 &#215; 10<sup>22</sup> Al cm<sup>−3</sup>). Surface morphology was observed by atomic force microscopy (AFM) and optical absorption was measured by using a conventional spectrometer. Irradiation with 90 MeV Ni ions was performed by using a TANDEM accelerator at Japan Atomic Energy Agency at Tokai.</p></sec><sec id="s3"><title>3. Results and Discussion</title><sec id="s3_1"><title>3.1. Characterization</title><p><xref ref-type="fig" rid="fig1">Figure 1</xref> shows XRD patterns and rocking curves of AlN film on R-Al<sub>2</sub>O<sub>3</sub>, SiO<sub>2</sub> and C-Al<sub>2</sub>O<sub>3</sub> substrate. The substrate temperature T<sub>s</sub> was optimized, 150˚C, 200˚C and 200˚C for these substrates, respectively so that the XRD peak intensity is maximized and the full-width at halfmaximum (FWHM) of XRD rocking curve is minimized. It is found that AlN film has exceptionally a-axis, i.e., (110) orientation on R-Al<sub>2</sub>O<sub>3</sub> (diffraction angle 2θ ≈ 59˚), in contrast to c-axis (2θ ≈ 36˚), i.e., (001) orientation grown on other substrates, Si, SiO<sub>2</sub>, C-Al<sub>2</sub>O<sub>3</sub> etc. FWHM of the rocking curve of as-deposited film on R-Al<sub>2</sub>O<sub>3</sub> is order of 2˚ (<xref ref-type="fig" rid="fig1">Figure 1</xref>(a) and <xref ref-type="table" rid="table1">Table 1</xref>). AlN on SiO<sub>2</sub> glass-substrates has (001) orientation and FWHM is much larger (~10˚) (<xref ref-type="fig" rid="fig1">Figure 1</xref>(b) and <xref ref-type="table" rid="table2">Table 2</xref>). FWHM</p></sec></sec></body><back><ref-list><title>References</title><ref id="scirp.30386-ref1"><label>1</label><mixed-citation publication-type="other" xlink:type="simple">W. M. Yim, E. J. Stofko, P. J. Zanzucchi, J. I. Pankove, M. Ettenberg and S. L. Gilbert, “Epitaxially Grown AlN and Its Optical Band Gap,” Journal of Applied Physics, Vol. 44, No. 1, 1973, pp. 292-296.  
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