Applied Surace Science 216 (2014) 612-648 ® SERGE scene Contents lists available at ScienceDirect Applied Surface Science journal homepage: www.clsevier.com/locatelapsuse XPS, UV-vis spectroscopy and AFM studies on removal mechanisms of Si-face SiC wafer chemical mechanical polishing (CMP) Creare Yan Zhou*”, Guoshun Pan*', Hua Gong®, Guihai Luo" Xiaolei Shi”, Li Xu*?, Chunli Zou*”, tte Key taboratery of Tibeloy, ings Univers Beng 100084, Cina * Shnahen ey aboratery of MrafNane Manfoctuing esearch init of Tinga Universit in hence, Shenzhen $1057, hina ARTICLE INFO ABSTRACT ‘ester Received 14 Api 2014 Received in revised fern 22 uly 2014 Accepted 3 August 2074 Avalabe online August 204 ‘Chemical mechanical polishing (CMP) removal mechanisms of on-axis St face SiC wafer have been inves. Ligated through X-ray photoelectron spectroscopy (XPS), UV-visible (UV-vis) spectroscopy and atomic force microscopy (AFM), XPS seats indicate that silicon oxide is formed on Stace surface polished by the slury including oxidant H,0,, but not that alter srsmersing in #0, solution. UV-vis spectroscopy curves prove that «OH hydrexyi radical coulé be generated only under CMP plishingby the surry includ ing H.0, and abrasive 3038 to promote oxidation of Siface to realize the effective removal; meanwhile. alkali KOH during CMP could induce the production af more radicals to smprove the cemeval On the Sion ari ther side. ultra-smooth polished surface wih atomic step structure morphology and extremely low Ra femoal of about 0.06:um (through AFM) is obtained using the developed slurry with silica nanoparticle abrasive xis ‘Tarough investigating the variations ofthe atomic step morphology on the surface polished by diferent Uveme slurtes, is reveals that CMP removal mechanism involves a simultaneous process of surface chemical Revwores Sion carbide (3 feaction and nanoparticle atomic scale abrasion, (© 2014 Elsevier BV. Allrghts reserved. 1, Introduction Chemical mechanical polishing (CMP) has been the most effi- cient method to obtain total planarization with ultra-smooth susfacein ultra large scale integration (ULSI) fabrication (1-3). With the urgency of energy conservation and light emitting diode (LED) technology rapid development, CMP has also been applied in manu- facturing LED chip substrate [411] The CMP removal mechanisms for semiconductor fabrication materials, such as Cu, Si, Al, W, have ‘been widely studied {12.13]. However. there is few research to dis- ‘cuss CMP removal mechanism of LED substrates. Recently, sapphire ‘wafer substrate is widely applied in LED chip production. On the other side, due to it better performance, SiC has attracted much attention and will become the widest applied Il-V compotind key material for LED substrate in the future [14.15]. Any micro-defects such as pt, scratch on the substrate surface could influence GaN epilayer growth quality, thus planarization of substrate wafer is very crucial for high performance LED devices. © Corresponding author a Stte Key Laboratory of Tbolgy, partment of Mechaniealenginecne Bling 903, Tsinghoa Unversity, Being 100084 China Tels wb 75526957301: fe =96 755 26957008, hpdedolori10r0t6japsusc201408011 (0160-43210 20:4 Hseier RV Al ihts reserved However, SiC single crystalline is almost incapable of reacting, ‘with any substances at room temperature, except for hot HF solu- tion or phosphoric acid above 200°C [16]. Therefore, super high ‘mechanical hardness and super strong chemical inertness make SiC ‘wafer quite difficult to realize deal planarization with high removal and good surface 8,17).As the literatures indicated [18,19], Si-face (0001) of Sic wafer is more difficult to be removed than C-face (0001). Otherwise, compared with C-face, Si-face is considered to be more useful for epitaxial film growth, Therefore, itis very nportant to investigate CMP removal mechanism of Si-face SiC water. ‘CMP process is considered to realize effective removal and good surface quality though synergetic effect between the mechanical abrading and chemical reaction. The basic components in CMP involve wafer, slurry and pag [20-22]. The major composition of the slurry generally includes abrasive particle, oxidant, corrosive and chelating agent (23-25), The slury is very critical to influence SiC wafer substrate surface quality and removal rate. The effects of the indigents in the slurry on the removal mechanism of SiC waer hnave been explored and are presented in the paper. X-ray photoelectron spectroscopy (XPS) has been extensively used to study the surface chemistry of metals, alloys and oxides relative to oxidation, corrosion reaction [26-28], Different surface chemical states are of potential considerable value in understand- ing and controlling chemical reaction, But few literatures areou ¥ Mow eta. Appie Suse Scence 216 (2014) 62-648 reported to be applied to study the CMP processing of SIC wafer via XPS. UV-vis spectrophotometry is applied widely to characterize ‘chemical ingredients using an appropriate chromogenic indicator [29-31], Otherwise, few literatures are demonstrated to be used for the investigation of CMP removal mechanism through UV-vis spectrophotometry. Here, UV-vis spectroscopy is used to detect OH hydroxyl generated in polishing process of SiC wafer, which ‘may be helpful to improve the removal of SiC wafer. AFM is gener- ally applied to measure the surface roughness. Nerveless, the study ‘on the variation of atomic step morphology on the ultra-smooth surface through AFM is seldom reported. The relative experim tal analysis and removal mechanism exploration would be useful to design CMP system, develop slurries, and improve the removal and surface quality of SiC water, as well as other CMP materials. 2. Experimental 2in/370 am on-axis Si-face 4H-SiC wafers were carried out pla- narization through CETR CP-4 bench-top polishing tester. Before (CMP processing, the wafers were polished by silica abrasive slurry from the ground wafers by diamond abrasive slurry, and the initial surface Ra of the wafers was below O.1nm by atomic force microscopy (AFM) measurement. Every CMP process was performed for 1h with a polyurethane polishing pad. The down- ‘ward pressure was 0.04MPa, slurry supplying rate was 70 ml/min, and work piece rotating speed was 120rpm, and down plate rotating speed was 160rpm. The procedure was carried out by slurry recycling flow. 0-5 wt oxidant hydrogen peroxide (H202), (0-06 wt% alkali potassium hydroxide (KOH), and 0-25 wi cot loidal silica abrasive with average particle size of 100nm were ‘chosen fo add into the slurry. Deionized water was used as dis- persed medium in the slurry. After the polishing process, the wafers ‘were cleaned by detergent and deionized water, and then dried off for measurements. The surface topography and roughness Ra were ‘observed by AFM (Braker Dimension Icon), Material removal rate (MRR) of SIC is thro follows: calculation as Am. sic Ams the removal weight of SiC wafer by professional electronic balance (OHAUS DISCOVERY), whose resolution is 0.00001 g, psc is 3.2 glen, ris the radium of SiC wafer, and ts polishing time. XPS analysis has been performed with the spectrometer (MICROLAB 350, Thermo Fisher) with Alka X-ray {hv= 1486.6 €V) to detect the surface of the processed waters, In order to investigate SiC removal mechanism and active substance of the slurry, we used ultraviolet-vsible (UV-vis) spec- trophotometry that involves using 0.04 wt%2-hydroxy benzoic acid to detect «OH hydroxyl radicals. When 2-hydroxy benzoic acid is reacted with «OH radical, intermediate product radical with visible purple color is produced (seen in Fig. 1). The amount of MRR a) Fig. 1. eaction of -hydroxyBenzote aid with OH radeal produce diyrony Denzec acid radia! intcmeciate pruct. The vise absorption peak of 300A ‘wavelength presente for dren benzoic rac comparing Wh 300 ‘bsorpaen peak of hydroxy Denzel ai {OH radicals was estimated by measuring the peak intensity and the area of dihydroxy benzoic acid radical intermediate product at about 500mm wavelength, through UV-vis specttophotometer (Shimadau UV-1750), 3. Results and discussion 2.1. Removal characteristics of Si-face SiC wafer ‘Table 1 shows the variation of material removal rate (MRR) of ‘on-axis Si-face SiC wafer polished by different slurries. Using the polishing slurry including only abrasive silica and base without Ha0p, even if pH value of the slurry is 12.5, MRR of SiC water is close to Onmyh. When polished by the slurry with HO, and sil ica, the removal rate could arrive 45 nmjh, On the other side, MRR could increase to 105 nmjh, when adding KOH into the slurry with 0p and silica. In addition, when using the slurry with only H03 and KOH, MRR of Siface SiC wafer approach Onmjh, Therefore, for ‘CMP polishing of Si-face SiC water, oxidant HyO2, alkali KOH and silica abrasive are beneficial for improving the removal, 3.2. XPS analysis ofthe processed surface ig, demonstrates XPS Si2p,,, spectra of on-axis Si-face surface after various treatments for 3h, After the ground wafer immersing. in the solution including H,09. there are only two main peaks due ta Si-C bulk component and Si° component on Si-face surface, a8 shown in the curve-fitting result of Fig. 2a 18], Ibis indicated that the top surface of original ground SIC single crystalline is very dif ficult to produce silicon oxide, even through the immersion of the oxidant. Fig 2billustrates Si2psy» spectra analysis results of polished sur~ face using the sturry including 5 wt HO, and 25 wt silica, Except {or SiC and Si* peak, a small peak of Si” component is also seen ‘on the polished surface, which is corresponding to SiO, bond. tis revealed that silicon oxide layer is formed on Si-face surface after ‘CMP polishing using the slurry including the oxidant, comparing ‘with ionmersing inthe solution including the oxidant, On the other side, Fig. 2c illustrates Si2psj2 spectra analysis, ‘results of polished surface using the slurry including the same con- tent of Swt% H,0;, 25 wt silica and 0.6 wt% KOH, Like Fig, 2b, a small peak of Si component is also detected in Fig. 2c. Itis indi ‘cated that there is also SiO. layer generated on the top polished surface using HO» slurry 2,02 + 2H,0 +0, wo 14,0242 0H @ SiC + 440H 0; > S10, + 2H,0 + C02 @ Si0; + 20H" + Si0;2- + Ho a Both of Fig. 2b and ¢ revealed that SiO» layer is produced on the polished surface using the slurry including 30,3 25 formula (3) shown, itis confirmed that SiC wafer could be oxidized to be Si02 under CMP polishing using the slurry including oxidant and silica Thus, as shown in Table 1, the removal rate of SiC wafer isimproved largely, when polished by the slurry with oxidant. Matsa semoval at (MAR) of fans Sac SIC wale using diferent tse NR azhu et Applied Suce Since Intensity (au) a a Birng energy (eV) (b) z " 2 8 sc Binding every ev) © g Bing energy) ig 2 XPS Sizpan spectsa of on-atis Sac surface after tfeentreatmets for Srey nehoding 5 wt 03,25 wt silica and 0.6 8 KOH, 33. UV-vis spectroscopy measurements As discussed in XPS analysis, when polishing by the slutry wich 20, silicon oxide layeris formed on the surface of Si-face, 50 as to provoke the removal ofS-face; otherwise, even if being immersed inthe olution with H,0,, the surface of Si-face couldn'tbe oxidized H.0; x] \ ‘OH, 0; — Sio, Oxidation a Woveerath om) Fig 3. uv spetoscopy feces treatments of Lee SC wate fo 10m0, ‘sng-bydrony bentole aca a Inder, aunersing inte souton incl Ing sz HO, (b) pelising by the stutyincluing wx #03 () nmesing the sey neuen 5 wes #03 and25 we sca polishing bythe slury ied Ing 522 HO, and 25 esa (e) polshing by the slur) including 54% 0; Buy sia and 8 KOH, to produce Si0,. Why can Si-face SiC wafer carry out oxidation reac tion through CMP polishing using the slurry including HO. but ‘not through immersing inthe solution with H0,? We tried to use LUVjvis spectrometry to explore the reason ofthe difference, Fig. 3 shows UVjvis spectroscopy of different treatments of Si-face SiC wafer with H0; using 2-hydroxy benzoic acid as an indicator. The absorption wavelength of dihydroxy benzoic acid intermediate product radical is about 500m, while the peak of about 300 nmis ascribed to benzene ring of2-hydroxy benzoic acid AAs can be seen in Fig. 3, itis obvious that all of five spectroscopy curves demonstrate the peak at 300 nm, whether immersing or pol {ishing of Si-face using H; 0p. On the other side, the peak of 500 am is only shown in the curve when polishing by the slurry including 0p and silica in Fig. 2d and e, but the peak of detecting hydroxyl radical (OH) doesn't be observed in otier three curves, ‘When immersing in the solution with 1205, itis indicated that 1,0) itself is very difficult to produce #OH radicals, resulting in none of radicals being measured, as shown in Fig. 3a; thus. acc ng to formula (2)-Si-face is very difficult tobe oxidized to generate SiO, without «OH radicals, in coincidence with XPS analysis of Fig. 2a. As shown in formula (1) in general, HzO, could be cecom- posed slowly to produce H,0 and 0, at room temperature, but isn't powerful enough to react with SiC single crystal, Fig. 3b demon- strated none of the peak at 500mm, which proves that it is very hard to produce measurable «OH radicals by merely using 202 under polishing condition, resulting in extremely low MRR of Si- face as shown in Table 1d. None of the peak of 500mm in Fi. 3¢ alfirms that the static abrasive silica isn't active enough to induce 102 produce observable «OH radicals, ehrough immersing in the slurry with #03 and silica Only if polishing by the slurry including H20z and silica, the peak of 500nm could appear, as illustrated in Fig. 3d. On the other side ‘when adding KOH into the polishing slurry with HO, and silica ‘omic step | ultra-smooth surface Ee — Ss “otubte : OFF» SIO64 ¥ Zhou tapped Suse Science 216 (2014) 62-648 pnt) en any pain i 7 ‘. ita 300300 a0 ton iio 300 ad at —Fa0 Fig5. Thevavatio ofthe atomiestep-ecace oyphology ope steels the ier vestments using the diferent ingredients ough APM measurement <1 yn? td 25 vats iea fr Oh. Ra: 00539 (eater ness i the solution with 0.6 wl: KOI fo: 3h, Ra: 0.0592 mn @ fer smersing us the soltion with Swe 1,0; for 3h, Ra: 0.0567 am: () poised by the srry with 5 wi HO; fe: C2, a: 0.1521 (0) plished by testy with 25 ws sia for 0.5 Ra: 0071S nag) crossectional Image along te nes betwen A, andi (a) (h)eoss-secuobl image along the lines betwee E and (4)zh et Applied Swce Science 4s shown in Fig. 3¢, the intensity of the peak with $00nm climbs up to 0.1 from 0.08. It is revealed that the content of «OH radical increases indeed in the existence of KOH, Consequently itis revealed that enough «OH radicals could be motivated to generate during CMP polishing using the oxidant and the abrasive, as shown in formula (2); thus, adequate «OH radical could help to promote the oxidation of Si-face SiC wafer, so as to ‘obtain effective removal of the wafer. In addition, the amount of «0H radicalsis very ew and the char- acteristic peak absorbance is only below 0.1, itis indicated that the oxidation of Si-face is very difficult to be completed resulting in ow removal rate of Si-face, as reported by our research and other lit- ceratures. The UV results help us to investigate deeply the removal ‘mechanism of SiC wafer, and lead us to look for more appropriate ‘oxidant to improve the removal of SiC wafer 34, Removal model ond AFM measurements of polished surface As we known, during CMP process, chemical reaction and mechanical abrasion have been considered as the twa basic fac- tors for the removal ofthe material. Towards highly chemical inert and hard Si-ace SiC wafer, the effective removal is very difficult to ‘be completed. Based on the discussed above, the CMP mechanism lof Si-face SiC wafer is illustrated in Fig. 4, Under a certain CMP downward pressure and rotation speed. instantaneous high temperature and friction movement occurs on SiC wafer surface when the water collide with polishing pad and abrasive, which promote H30; decomposition to release enough amount of eOH radicals to drive the SiC reaction, in the presence of «01 radicals SiC could carry out oxidation reaction to produce softer and higher chemical activity Sid, layer [18.22], which can react with OH released by alkali to generate soluble Si032~ (for- ula (4)) [33.34) and be removed by the abrasive silica particles simultaneously, resulting in effective removal of SiC wafer. (is believed that the formatian of soluble and softer silicon oxide layer fon the surface plays a critical role in the removal of SiC wafer. On the other side, when using silica nanoparticle as the abra- sive in our developed slutty, none of defects like scratches or pits are observed on polished SiC surface. Especially the surface ‘with atomic step-terrace structure morphology and extremely iow roughness Raof about 0.06 nmis achieved by AFM measurement, as shown in Fig. 5a Fig. Sg demonstrates cross-sectional image of Ay and Ay in Fiz 5a, which indicates the step height is about 0.251m, in agreement with the theoretical thickness of one bilayer of Si and C atoms in SiC crystalline [35]. Because the hardness of sil- ca nanoparticle abrasive approaches to silicon oxide layer on the polished surface, the mechanical removal brought by the abrasive should become quite fine and accurate 50 as to obtain atomically ultra-smooth surface, Furthermore, we would try to observe the precise change of atomic step-terrace morphology on the ultra-smooth surface to study the removal mechanism through AFM measurement. AS demonstrated in Fig. 5, itis revealed that the atomic step mor- phology on the surfaces after immersing or polishing by different ingredients have remarkable variations. First the effect of the oxidant H,02 towards atomic step mor- phology is studied. As shown in Fig. Se, when polished by the solution of only H303 for 0.2h, alarge number of high “brightness granules are observed clearly on atomic step surface. As seen from the cross-sectional image shown in Fig. 5g, the height of highlight pparts is about 05-1.0 rm, much higher than the step height of orig inal Si-C bilayer with 0.25 nm; thus, itis inferred thas the highlight _granules belongs to the generated silicon oxide via the oxidation of SiC. Therefore, itis confirmed defintely that silicon oxide could be produced by H.02 under CMP condition from visual AFM measure ment, Otherwise, due to the absence of the mechanical grading of the abrasives, the produced silicon oxide during polishing process is very hard to be removed, so that the atomic step morphology in Fig, Se reflects obviously the generation ofa great amount of oxide by the slurry only with H,02, But not by the slurry including H02 and abrasive shown in Fig, 5b, On the other side, as demonstrated in Fig. 5d. after immersing by the solution with H,03. the atomic step morphology couldn't present distinct high brightness oxide yet, still similar to the previous surface shown in Fig, 5¢. Therefore ‘AFM atomic step measurement results confirms further that SiC wafer could be oxidized using 1,03 in CMP environment, but not available after immersing in H20>, ‘Subsequently, the effect of silica abrasive is discussed, Based on the discussed above, only ifremaining a very few oxide granules on the previous polished ultra-smooth surface, the slurry with silica abrasive (even without H1,02) would also bring very small removal of Si-face, resulting in the removal results of Table | and the ret ference [36]. As shown in Fig. f, there are a great many tiny pits ‘on the atomic terrace, Because silica abrasives could remove the residual oxide, the original positions of the granular oxide divert to nanomerc pits. Thus, it is deferred that the removal of Si-face is proportional to the amount of residual oxide on the surface, when using only silica abrasive. In addition, iis seen obviously chat the produced oxide at the step-edge is more than that on the terrace from Fig, Se, Thus it’s also deferred that step-edge atoms can be removed easily by the abrasive nanoparticles, compared with the terrace atoms, besides the higher activity of step-edge atoms [37] Eventually, we would explore the influence of alkali KOH in (CMP process. When immersing inthe solution of KOH, the residual oxide on the surface is decreased, as shown in fig, 5c Is indi cated that KOH could react with silicon oxide. On the other side Fig. Sb by the slurry including HO, and abrasive (without KOH) demonstrates that the produced oxide granules on atomic step _morphology appears to be not reduced clearly unexpectedly, com- pared with Fig. 5a by the slury including KOH, HO; and abrasive Actually, as discussed in previous UV-vis spectroscopy analysis, under the existence of KOH, hydroxyl radical density increases, so that the amount of created oxide increases during CMP procedre; ‘meanwhile, KOH could react with the oxide to remove the oxide companying with silica abrasive abrading. Asa result, the addition ‘of KOH in CMP process could accelerate the generation ofthe oxide instead, resulting in non-decrement of the oxide on atomic step morphology despite ofthe dissolution of alkali. Thus, the introduc tion of alkali KOH could improve largely the removal of Si-face SiC water: Asdiscussed above, it's very unique to study the effect of the oxi- dant. abrasive and alkali towards the removal mechanism of Si-face SiC wafer, through investigating the variation of atomic step mor- phology on the ultra-smooth surface. On one side, on the surface of Siface SIC wafer, silicon oxide layer is produced by the oxidant #0; and alkali KOH under CMP polishing condition; on the other sie, the oxide layer is removed by silica nanoparticle atomic scale ‘wear and the dissolution of alkali. With a simultaneous repeating process of the generation and removal ofthe oxide layer, the global planarization with atomically smooth and extremely low Ra surface is realized. 4. Conclusion In the study, XPS, UV-vis spectroscopy and AFM analysis has bbeen conducted to investigate CMP removal mechanism of Si-face SiC wafer. XPS Si2p,_ spectra results reveals that silicon oxide layer is formed on Si-face surface, when polished by the slury with oxi- dant H20z, but the oxide couldn't be produced by immersing. in the solution with H,03. UV-vis spectroscopy results proves that Ot radical could be generated only under CMP polishing by theoe thou et al Applied sufce Science 315 (2014) 43-648 slutty with H,02 and silica particles, so as to promote oxidation (of Si-face to realize the effective removal. The analysis of XPS and UV-vis spectroscopy results isin accordance with the variation of MRR of Si-race SiC wafer using different slurries. It is confirmed that the formation of soluble and soft silicon oxide layer on the surface plays a critical role in the removal of SiC wafer. On the ‘other side, ultra-smooth polished surface with atomic step struc- ‘ture morphology and extremely low Raof about 0.06 nmis achieved using the developed slurry with silica nanoparticle abrasive. Its innovative that the chemical reaction and interaction behavior on. ‘the polished surface are studied through investigating the varis- tion of atomic step morphology, which reveals that CMP removal mechanism involves a simultaneous process of surface chemical reaction and nanoparticle atomic scale abrasion. The relative anal- ysis and removal mechanism exploration would be contributing to ‘design CMP system, cevelop slurries, and improve the removal and surface quality of SiC wafer, as well as other CMP materials, ‘Acknowledgements ‘This research has been supported by National Natural Science Foundation of China (No. 91223202), National Key Basic Research, Program of China (873 Program, No. 2011CBO13102), and Inter- national Science & Technology Cooperation Program of China (No. 2011DFA73410), and the Foundation for Innovative Research Groups of the National Natural Science Foundation of China (No. 51321092) References IM] Vt tis, KL. zhang Fane, W. Di Miroeletran. 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