Samsung Electronics Co., Ltd. v. Demaray LLC
`Samsung Electronic's Exhibit 1042 (Vol 2 of 3)
`
`APPLIED MATERIALS EXHIBIT 1042 (Part 2 of 3)
`
`Page 7 of 8
`Appendix 1029-A
`
`Page 153 of 304
`
`Ex. 1042, Page 153
`
`

`

`Doghecheetal.
`
`1211
`
`method showeda linear electro-optic coefficient r)3 of about
`0.98 pm/V. These results demonstrate the interest of AIN
`thin films to be used in integrated optics applications.
`
`'H. Okano, N. Tanaka, Y. Takahashi, T. Tanaka, K. Shibata, and S. Na-
`kano, Appl. Phys. Lett. 64, 166 (1994).
`2M. A. Khan, J. N. Kuznia, D. T. Olson, J. M. Van Hove, and M.Blasin-
`game, Appl. Phys. Lett. 60, 2917 (1992).
`3§ Nakamura, M. Senoh, S. Nagahama, N. Iwasa, T. Yamada, T. Mata-
`sushita, H. Kiyoku, and Y. Sugimoto,Jpn. J. Appl. Phys., Part 2 35, L74
`(1996).
`+E. Calleja, M. A. Sanchez-Garcia, E. Monroy, F. J. Sanchez, and E. Mu-
`noz, J. Appl. Phys. 82, 4681 (1997).
`5K. Dovidenko, S. Oktyabrsky, J. Narayan, and M. Razeghi, Appl. Phys.
`Lett. 79, 2439 (1996).
`©X. Tang, Y. Yuan, K. Wongchotigul, and M. Spencer, Appl. Phys. Lett.
`70, 3206 (1997).
`7p. K.Tien, R. Ulrich, and J. R. Martin, Appl. Phys. Lett. 14, 291 (1969).
`SF. Flory, G. Albrand, D. Endelma, N. Maythaveekulchai, E. Pelletier, and
`H.Rigneault, Opt. Eng. (Bellingham) 33, 1669 (1994).
`°E. Dogheche, B. Jaber, and D. Rémiens, Appl. Opt. 37, 4245 (1998).
`'g Strike and H. Morkog, J. Vac. Sci. Technol. B 10, 1237 (1992).
`\'L. Roskoveova, J. Pastnak, and R. Babuskova, Phys. Solid State 20, k29
`(1967).
`'2F, Horowitz and S. B. Mendes, Appl. Opt. 33, 2659 (1994).
`13K. §. Chiang, J. Lightwave Technol. LT3, 85 (1985).
`\4,. Boudrioua, E. Dogheche, D. Rémiens, and J. C. Loulergue, J. Appl.
`Phys.85, 1 (1999).
`
`
`
`Ex. 1042, Page 154
`
` Appl. Phys. Lett., Vol. 74, No. 9, 1 March 1999
`
`‘ected inten-
`
`Using TE guided modes, we have investigated the elec-
`trooptic (EO) coefficient using the angular shift technique as
`described by Boudriouaet al.'* The topelectrode consists of
`a semitransparent gold film with a thickness of 10 nm. By
`applying a transverse electric field through the AIN layer, a
`change of the resonant coupling angle (A@) in the guided-
`modes spectrum has been observed. This effect is directly
`correlated to the variation ofthe refractive index (An) due to
`the EO effect. Finally, the linear EO coefficient r)3 obtained
`is evaluated to be 0.98 pm/V.
`In summary, AINthin films have been grown on Si/SiO,
`substrates by radio-frequency magnetron sputtering from an
`aluminum nitride target. The deposition parameters and an-
`nealing process were optimized for the elaboration of highly
`textured AIN thin films. We have investigated the optical
`performances of the films using the prism-coupling tech-
`nique. Refractive indices were therefore determined to be
`no= 2.0058 and n,= 2.0374 at 632.8 nm. From the effective
`guided-modeindices, the analysis of the optical anisotropy
`confirmed the uniaxial nature of the AIN thin film with the
`optical axis likely oriented normalto the surface of the sub-
`strate. The optical
`losses were evaluated to be around 7
`dBcm~!. The EO measurements using the angular shift
`
`tal to the
`‘ected by
`lines the
`g within
`ovides a
`ormal to
`e of our
`: optical
`rate sur-
`
`1 there-
`‘ffective
`inverse
`method
`thin the
`ven by
`\easured
`profiles
`Fig. 4,
`ariation
`y along
`ns con-
`near the
`ot show
`ocess.
`
`|
`
`|j
`|
`
`=1
`
`16
`
`files ob-
`»sited on
`
`~
`
`
`
`Page 8 of 8
`Appendix 1029-A
`
`Page 154 of 304
`
`Page 8 of 8
`Appendix 1029-A
`
`Page 154 of 304
`
`Ex. 1042, Page 154
`
`

`

`Appendix 1029-B
`Appendix 1029-B
`
`Page 155 of 304
`
`Ex. 1042, Page 155
`
`Page 155 of 304
`
`Ex. 1042, Page 155
`
`

`

`JOURNAL
`Applied physicsletters.
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`Page 1 of 4
`Appendix 1029-B
`
`Page 156 of 304
`
`Ex. 1042, Page 156
`
`Ex. 1042, Page 156
`
`

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`Jetails
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`OCLC : (OCoLC)1580952
`
`Appl. phys. lett.
`Applied physics letters
`Related to : Journal of applied physics
`NewYork etc. AmericanInstitute of Physics.
`v.
`1- Sept. 1962
`962
`
`v. ill. 27. cm.
`
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`Issued as companionto: Journal of applied physics, ISSN 0021-8979.
`General notes
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`Page 2 of 4
`Appendix 1029-B
`
`Page 157 of 304
`
`Ex. 1042, Page 157
`
`

`

`@2287cas a22006011
`
`4500
`
`750829c19629999nyuwrip
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`##$a3 $b3 Sen $18811 $kl $m1
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`$z(OCOLC) 1481730
`$aDLC $cUDI $dCOO $dHUL $dCOO $dDLC SdNSD $dOCL $dYUS $dDLC $dSER $dAIP $dOCL $dNYG $dNST $dOCL $dNST
`
`lett.
`#O0$aApplied physics letters
`@@$aApplied physics letters.
`##$aNew York [etc.] $bAmerican Institute of Physics.
`##$av. Sbill. $c27 cm.
`##$awWeekly, $b1986-
`##$aSemimonthly, $b1963-1985
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`O#$av. 1- Sept. 1962-
`2#$aElectronics and communications abstracts journal (Riverdale) $x@361-3313
`#$aISMEC bulletin $x0306-0039
`2#$aPollution abstracts with indexes $x0032-3624
`2#$aSafety science abstracts journal $x0160-1342
`2#$aInternational aerospace abstracts $x0020-5842
`2#$aGeoRef $x0197-7482
`2#$aMetals abstracts $x@026-0924
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`Page 3 of 4
`Appendix 1029-B
`
`Page 158 of 304
`
`Ex. 1042, Page 158
`
`

`

`APPLIED MATERIALS EXHIBIT 1042 (Part 2 of 3)
`
`Page 4 of 4
`Appendix 1029-B
`
`Page 159 of 304
`
`Ex. 1042, Page 159
`
`

`

`Appendix 1029-C
`Appendix 1029-C
`
`Page 160 of 304
`
`Ex. 1042, Page 160
`
`Page 160 of 304
`
`Ex. 1042, Page 160
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`

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`Page 1 of 1
`
`Page 1 of 1
`Appendix 1029-C
`
`Page 161 of 304
`
`Ex. 1042, Page 161
`
`

`

`Appendix 1029-D
`
`Early Citations to Dogheche
`
`Page 162 of 304
`
`Ex. 1042, Page 162
`
`

`

`
`y
`,
`,
`c!2000 The Japan Society of Applied Physics
`
`Deposition of AlN Thin Films with Cubic Crystal Structures on Silicon Substrates
`at Room Temperature
`Zhong-Min REN, Yong-Feng LU, Yeow-Whatt GOH, Tow-Chong CHONG, Mei-Ling NG1, Jian-Ping WANG1,
`Boon-Aik CHEONG1 and Yun-Fook LIEW1
`Laser Microprocessing Laboratory, Department of Electrical Engineering and Data Storage Institute, National University of Singapore,
`10 Kent Ridge Crescent, Singapore 119260
`1Data Storage Institute, 5 Engineering Drive 1, Singapore 117608
`(Received September 20, 1999 accepted for publication March 6, 2000)
`Cubic AlN thin films were deposited at room temperature by nitrogen-ion-assisted pulsed laser ablation of a hexagonal
`AlN target. The full-width at half maximum (FWHM) of the X-ray diffraction peak in the θ ∼ 2θ scan can reach a value of
`0.27 degrees. In the Raman spectroscopy measurement, a new peak at 2333 cm−1 originating from cubic AlN polycrystalline
`was observed. Nitrogen ions not only effectively promote the formation of stable Al–N bonds but also improve the crystal
`properties of the deposited thin films. A nitrogen ion energy of 400 eV is proposed for the thin-film deposition.
`KEYWORDS: AlN pulsed laser deposition thin films cubic crystalline Raman spectroscopy XRD XPS
`
`produced by a 1-cm Kaufman-type ion source irradiated the
`substrate surface to assist the deposition. The ion flux was
`set at 1 mA/cm2. The deposition rate was 0.1 nm/s as mea-
`sured by a microbalance mounted on the substrate. Si(100)
`wafers were used as substrates. The deposited thin films have
`thicknesses of around 200 ∼ 300 nm. After deposition, X-ray
`diffraction (XRD), Raman spectroscopy and X-ray photoelec-
`tron spectroscopy (XPS) measurements were carried out to
`characterize the crystal, chemical binding and compositional
`properties of the deposited thin films.
`Figure 1 shows the XRD θ ∼ 2θ spectrum of an AlN
`thin film deposited by 400 eV nitrogen ion bombardment.
`The measurements were performed on a Philips X’Pert-MRD
`system. Cu Kα irradiation with an average wavelength of
`1.5418 Å was used as an X-ray source in the diffraction mea-
`surements. In the spectrum, besides the Si(200) and Si(400)
`diffraction peaks, there are four distinct peaks at 2θ = 38.5,
`44.7, 65.3 and 78.3, corresponding respectively to orienta-
`tions of (111), (200), (220) and (311) of the cubic AlN crys-
`tal22) although the crystal structure of the target is hexagonal.
`Hexagonal structures are not detected from Fig. 1 when the
`resolution of the MRD system is taken into account. The
`FWHM of the AlN(200) peak is about 0.27 degrees, lower
`than that of films deposited by plasma source molecular beam
`epitaxy.6) The formation of AlN cubic structures on Si(100)
`
`Si(400)
`
`AlN(311)
`
`AlN(220)
`
`AlN(111)
`
`AlN(200)
`
`Si(200)
`
`20
`
`Intensity(arb.unit)
`
`40
`
`60
`
`80
`
`2
`Fig. 1. XRD θ ∼ 2θ spectrum of a AlN thin film deposited by KrF laser
`l
`400 V
`T
`
`
`
`Recently there has been tremendous interest in the synthe-
`sis of AlN thin film due to its wide band gap and other desir-
`able properties of thermal conductivity, electrical resistivity
`(dielectric constant) and acoustic properties.1–3) Many exper-
`imental methods have been used to deposit AlN thin films, in-
`cluding metalorganic chemical vapor deposition (MOCVD),4)
`plasma-assisted molecular beam epitaxy (PAMBE),5–7) RF re-
`active magnetron sputtering,8–11) ion-assisted chemical vapor
`deposition12) and pulsed laser deposition (PLD).13–19) A num-
`ber of new theoretical works have also been published re-
`cently.20 21) Almost all the deposition methods require high
`substrate temperatures (normally above 600◦C) although the
`defects both inside the thin films and at the interface between
`the substrate and the thin film cannot be avoided.6) To date, all
`the deposited AlN thin films have hexagonal structures with a
`highly textured orientation of (0001) on sapphire, silicon and
`glass substrates.3 6 7 9 10 18 19)
`In our study, we attempted to use pulsed laser ablation to
`deposit AlN thin films on silicon substrates at room tempera-
`ture. PLD has been proven to be suitable to fabricate AlN thin
`films on silicon and sapphire substrates. Compared with other
`methods, PLD has two main aspects of advantages. First, it
`can faithfully transfer the target material to the substrate sur-
`face without an obvious change in the compositional ratios of
`compound materials. Second, the energetic radicals in the ab-
`lated plume are beneficial to the formation of ideal crystalline
`structures in the deposited thin films. In our experiments, the
`ion-assisted PLD combines the advantages of ion bombard-
`ment and laser ablation. With this approach, we can indepen-
`dently control the energies of the AlN radicals in the ablated
`plasma and the nitrogen ions in the ion beam to improve the
`quality of the deposited thin films. Moreover, the nitrogen
`ions can also compensate for the loss of nitrogen species in
`the ablation process.
`In the experiment, we used a KrF excimer laser at a wave-
`length of 248 nm to ablate an AlN target. The deposition was
`carried out in a PLD system with a background vacuum of
`1×10−6 Torr. An AlN target with a standard hexagonal crys-
`tal structure and a purity of 99.995% was mounted on a target
`holder that was rotated by an external motor. The target was
`placed 2 cm away from the substrate surface. The laser pulse
`duration was 30 ns The laser fluence was set at 2 J cm−2 with
`
`Page 163 of 304
`
`Ex. 1042, Page 163
`
`

`

`L 424
`
`Jpn. J. Appl. Phys. Vol. 39 (2000) Pt. 2, No. 5A
`
`Z.-M. REN et al.
`
`For the thin films deposited without nitrogen ions, no obvi-
`ous Raman peak can be observed, implying that the nitrogen
`ions can effectively improve the crystal property of the thin
`film. Although it induces defects, ion implantation can possi-
`bly benefit the growth of the crystal grains. The energetic ni-
`trogen ions can enhance the chemical combinations between
`Al and N atoms and thus lead to more and larger AlN crystal
`grains.
`The chemical binding and compositional properties of
`the AlN thin films were analyzed by XPS measurements.
`Figure 3 shows the XPS Al 2p spectra for three AlN thin films
`deposited with different ion energies. The binding energy of
`the Al 2p electron increases slightly with increasing nitrogen
`ion energy from 100 to 400 eV, due to the fact that the ener-
`getic nitrogen ions can effectively react with Al atoms to form
`AlN compounds. The binding energy of the Al 2p electron in
`the AlN compound is higher than that in atomic Al due to the
`weak shielding effect. Higher ion energy can lead to the for-
`
`Al 2p
`100 eV
`
`200 eV
`
`400 eV
`
`Intensity(arb.unit)
`
`Intensity(arb.unit)
`
`Intensity(arb.unit)
`
`70
`
`82
`
`80
`78
`76
`74
`72
`Binding Energy (eV)
`Fig. 3. XPS Al 2p spectra for AlN thin films deposited under different ni-
`trogen ion energies of 100, 200, and 400 eV. The laser fluence is 2 J/cm2.
`The ion flux is 1 mA/cm2.
`
`(a)
`
`400 eV N+
`
`N-Al
`
`N 1s
`
`N-N
`
`398
`
`(b)
`
`398
`
`406
`404
`402
`400
`Binding Energy (eV)
`N2 atmosphere
`N-N
`
`408
`
`N 1s
`
`N-Al
`
`406
`404
`402
`400
`Binding Energy (eV)
`f AlN
`fil
`
`408
`
`400 V N+
`
`F
`
`4 XPS N
`
`
`
`substrates is different from most other research results in
`which hexagonal AlN structures are formed.15 18 19) In the
`detailed studies6 7) of the microstructures and initial stages
`of thin-film deposition, AlN films have an initial amorphous
`region at the interface between the substrate and the thin
`film, followed by c-axis-oriented columnar grains. Substrate
`temperatures higher than 600◦C can significantly reduce the
`amorphous regions at the interface and promote to grow AlN
`with hexagonal (0001) orientation. However, in our deposi-
`tion, since substrate temperature is low, the c-axis-orientated
`growth of hexagonal AlN is not preferred. Instead, another
`metastable state of the crystal AlN with a cubic structure was
`obtained from our deposition, although the hexagonal AlN is
`possibly in a much stable state. The PLD at room temperature
`with the assistance of ion-beam coprocessing leads to mainly
`(111)-oriented c-AlN thin films.
`We also deposited AlN thin films without nitrogen ion
`bombardment. These deposited thin films exhibit no XRD
`peaks, indicating only amorphous structures. The result re-
`veals the important role of nitrogen ions in the synthesis of
`AlN thin films with cubic crystal structures. Moreover, ni-
`trogen ion energy lower than 400 eV leads to weaker and
`broader XRD peaks. Therefore, nitrogen ions with an en-
`ergy of 400 eV can effectively assist in the formation of cu-
`bic crystalline structures in the deposited thin films. When
`the nitrogen ion energy exceeds 400 eV, the deposition will
`be impeded due to the resputtering effect caused by the ion
`bombardment.
`Figure 2 shows the Raman spectra of the AlN thin films de-
`posited under the different nitrogen ion energies of 100, 200,
`and 400 eV. Similar to most other research findings,19 23 24)
`the Raman peaks of the AlN thin films are weak. The peaks at
`618, 670 and 826 cm−1 reflect the phonon modes of E1(TO),
`A1(LO) and E1(LO), respectively,23 24) indicating the crystal
`structures of the deposited thin films. The intensities of these
`Raman peaks increase with increasing nitrogen ion energy
`from 100 to 400 eV, implying that the nitrogen ion energy of
`400 eV is optimal for the deposition of crystal AlN thin films,
`in agreement with the XRD analysis result. Besides these
`peaks, there is a sharp and strong peak at 2333 cm−1 which is
`observed for the first time. The intensity of this peak also in-
`creases with the nitrogen ion energy and reaches a maximum
`when the ion energy increases to 400 eV. Therefore, this peak
`must originate from the cubic structure of AlN.
`
`Intensity(arb.unit)
`
`400 eV
`
`200 eV
`
`2333
`
`826
`670
`618
`
`Si
`
`100 eV
`2700
`
`Si
`1800
`900
`Raman Shift (cm-1)
`Fig. 2. Raman spectra of AlN thin films deposited under different nitrogen
`f 00 200
`400 V T l
`fl
`2 J/
`2 T
`
`Page 164 of 304
`
`Ex. 1042, Page 164
`
`

`

`Jpn. J. Appl. Phys. Vol. 39 (2000) Pt. 2, No. 5A
`
`Z-M.RENetal.
`
`L425
`
`mation of more Al—N bonds and therefore an increase in the
`bic AIN crystal. An ion energy of 400 eV was determined to
`Al 2p binding energy.
`be appropriate for the deposition process.
`Figure 4 shows two XPSNIs spectra for AIN thin films
`Acknowledgements
`deposited with and without the assistance of nitrogen ions,
`The authors would like to thank Miss. H. L. Koh for her
`respectively. It is evident that, in the thin films, there are two
`technical assistance in this research.
`nitrogen statuses related to N-N and N—AI bonds. Thediffer-
`ence between these two spectra in Fig. 4 is quite obvious. The
`thin film deposited in the N> atmosphere has a very strong N—
`N peak whereas that deposited with 400 eV N* implantation
`has a strong N—Al peak. The nitrogen ions in the deposition
`promote the formation of Al-N bondsand reducethe density
`of N-N bonds. Therefore, nitrogen ions with an energy of
`about 400 eV are beneficial to the synthesis of AIN thin films,
`in agreement with the above XRD and Raman results.
`The N/AI atomicratio of the deposited thin films is in the
`range of 0.90 to 1.12. The N/Al atomic ratio is evaluated us-
`ing N : Al = An/Sy : Aai/Sai. where Ay and Ag) are the
`areas under the Nls and Al2p peaks, and the constants Sy
`and Sq) are the sensitivity factors of nitrogen and aluminum,
`respectively. The ratio is slightly lower than 1.0 when the
`ion energy is 400 eV, due to the resputtering effect. Depo-
`sition with ion-beam bombardmentis a nonequilibrium pro-
`cess. The low substrate temperature does not provide any en-
`ergy for the equilibrium growth of an AIN crystal. The de-
`position is accomplished by energetic ions with energies of
`about 400eV. Therefore, the crystalline growth mechanism
`is quite different from other deposition methods where high
`substrate temperatures and low ion energies are employed.
`Hexagonal AIN thin films were deposited by PLD at substrate
`temperatures above 675°C)>-!®) and by RF magnetic sputter-
`ing and molecular beam epitaxy with substrate temperatures
`higher than 400°C,°-9:!0!9even onsilicon®?:!®) and glass!
`substrates. However, in our deposition, the c-axis-oriented
`growth which leads to the hexagonal structure is not possible
`due to the low substrate temperature. In contrast, the ener-
`getic ions promote the formation of another metastable state
`of crystal AIN with a cubic structure. Therefore, the use of
`nitrogen ions with the energy of about 400 eV plays an im-
`portantrole in the formation of a cubic AIN crystal.
`In summary, AIN thin films were deposited at room tem-
`perature on Si(100) substrates by nitrogen-ion-assisted pulsed
`laser ablation of a hexagonal AIN target. The thin films
`have cubic crystal structures with orientations of (111), (200),
`(220) and (311), different from most other research results in
`which hexagonal AIN was obtained. Energetic nitrogen ion
`implantation plays an importantrole in the formation of a cu-
`
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`Page 165 of 304
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`Ex. 1042, Page 165
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`Ex. 1042, Page 165
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`

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`Ex. 1042, Page 166
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`

`

`JOURNAL OF APPLIED PHYSICS
`VOLUME 88, NUMBER 12
`15 DECEMBER 2000
`Room temperature synthesis of c-AlN thin films by nitrogen-ion-assisted
`pulsed laser deposition
`Z. M. Ren, Y. F. Lu,a) and H. Q. Ni
`Laser Microprocessing Laboratory, Department of Electrical Engineering and Data Storage Institute,
`National University of Singapore, 10 Kent Ridge Crescent, 119260 Singapore
`T. Y. F. Liew, B. A. Cheong, S. K. Chow, M. L. Ng, and J. P. Wang
`Data Storage Institute, 5 Engineering Drive 1, 117608 Singapore
`共Received 10 April 2000; accepted for publication 28 August 2000兲
`Cubic aluminum nitride (c-AlN) thin films have been deposited at room temperature on silicon
`substrates by nitrogen-ion-assisted pulsed laser ablation of a hexagonal AlN target. The deposited
`thin films exhibit good crystal properties with sharp x-ray diffraction peaks. The influences of the
`nitrogen ion energy on the morphological, compositional, and electronic properties of the AlN thin
`films have been studied. The nitrogen ions can effectively promote the formation of Al–N bonds
`and improve the crystal properties of the deposited thin films. A nitrogen ion energy of 400 eV is
`proposed to deposit high quality c-AlN thin films. © 2000 American Institute of Physics.
`关S0021-8979共00兲03623-9兴
`
`I. INTRODUCTION
`Aluminum nitride is increasingly receiving high interest
`from the material research community due to its wide band
`gap, high thermal conductivity, high electrical resistivity 共di-
`electric constant兲, and good acoustic properties.1–3 Many re-
`search groups are exploring the synthesis of high quality
`AlN. Some experimental methods have been used to deposit
`AlN thin films,
`including metalorganic chemical vapor
`deposition,4 plasma-assisted molecular beam epitaxy,5–7 rf
`reactive magnetron sputtering,8–11 ion-assisted chemical va-
`por deposition12 and pulsed laser deposition 共PLD兲.13–19
`Most of the deposition methods require high substrate tem-
`peratures 共normally above 800 C兲 although the defects, both
`in the thin films and at the interface between the substrate
`and the thin film, cannot be avoided.6 Such a high substrate
`temperature is undesira