Surface characterization - Analytical Chemistry (ACS Publications)

Surface characterization. G. E. McGuire, M. A. Ray, Steven J. Simko, F. Keith. Perkins, Susan L. Brandow, Elizabeth A. Dobisz, R. J. Nemanich, A. R. C...
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Surface Characterization G. E. McGuire,’ M. A. Ray, Steven J. Simko, F. Keith Perkins, Susan L. Brandow, Elizabeth A. Dobisz, R. J. Nemanich, A. R. Chourasia, and D. R. Chopra MCNC, Center for Microelectronic Systems Technologies, 3021 Cornwallis Road, P.O. Box 12889, Research Triangle Park, North Carolina 27709 Review Contents Introduction Ion Spectrometry Electron Spectroscopy Proximal Probes Optical Characterization of Surfaces X-Rav Techniaues

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INTRODUCTION

Reviews of surface characterization have appeared in Analytical Chemistry every two years since 1977 (1-8). The field continues to grow rapidly and to include an ever increasingdiversity of tools and materials studies. This review is similar to the last one in this series, being written by multiple authors with specialties in one or more of the broad categories of surface analysis in an attempt to highlight important advances in each of these areas. This review begins with literature from January 1991 and ends with literature from December 1992. ION SPECTROMETRY Secondary Ion Mass Spectrometry (SIMS). Over the last several years, the SIMS field, as in most analysis fields, has held a topical conference every two years. To date there have been eight such conferences, SIMS I-SIMS XIII, with the proceedings published in a separate volume by the same name. These volumes should form the basis for any review of SIMS activity. Therefore, this survey will only document articles which were not published in the SIMS conference series. A general review of SIMS, from theory to applications, has been published in an edited volume by Rossiter and Baetzold (AI). A general discussion of SIMS applications, outside of its primary role in the semiconductor industry, was examined (A2),and critical issues in the use of li uid metal ion sources for high-resolution ion imaging were %iscussed(A3). Vickerman has authored three reviews of static SIMS: analysis of organic surfaces (A4), applications to heterogeneous catalysis ( A @ , and discussions of the proposed models for the formation of polyatomic ions during polymer analysis (A6). The applications of SIMS in geochronolgy and cosmology for insight into the evolution of the solar system was reported ( A n . A review of SIMS surface analysis of biomedical materials and biomedicalpolymers was also presented (AB). The importance of depth resolution in SIMS sputtered depth profiling has increased greatly in recent years due primarily to the push toward submicron integrated semiconductor devices. A discussion by Hofmann expounded on the fundamental physical processes which limit depth resolution in sputter rofiiing and on the recent advances toward physicallimitaof &pth resolution (A9). The analyses of depth resolution artifacts are based on Gaussian (normal) statistics that are not always encountered in SIMS analysis. However, they provide a good introduction to the difficulties in sputter profiling. An empirical com arison of impurity profile roadening in Si using N, 0,a n f N e ion beams was examined, and the deca length of the impurity tail was characterized (AlO). The iecay length for Cu, for example, was smallest for Ne, lar er for N, and very large for 0. Enhanced segregation of t u away from the oxide and nitride interfaces is responsible for this effect. This study exemplifies some of the pitfalls inherent in SIMS depth profiling. Another paper reviews the theories of thermal spike mixing and collisional 0003-2700/93/0365-03 1 1R$12.00/0

mixing as bounds for bilayer profile broadening (A1I). Zalm applies the expressions for collisional mixing, which were developed under high-energy bombardment, and provides a concise analytical formula for ion beam mixing (A12). In most previous discussions of depth resolution, the role of s utter-induced surface topography has not been considered: Secondary ion yield changes resulting from topographical changes in the surface have been reported for Cs+ and 02+depth profilin in Si (A13,A14), and 0 2 + depth profiling in GaAs (A15) and InP (A16). Significant improvement in depth resolution of Cr-Ni layers was reported for normal incidence SIMS analysis with an 02+ion beam (A17). The normal incidence beam produced the least amount of surface topography. To elevate this problem, sample rotation has proven very useful. Sample rotation has provided improved depth resolution in implanted samples and at interfaces during SIMS depth profiling ( A l G A 2 0 ) . Finally, the influence of photolithographically obtained submicron surface topography on SIMS depth profiles was explored to demonstrate the difficulty of obtaining on-chip analysis (A21). The assumption that the measured profile is always broader than the actual profile may not be the case for samples with topographical features. Still, on-chip analyses must be carried out, and therefore, test structures for Si wafer analysis have been developed which yield acceptable depth resolution (A22, A23). High depth resolution is required for the &doped semiconductor sam les and layered semiconductor structures. A review of SIMi! a plied to compound semiconductor structures and 6-dopetf layers is reported (A24). SIMS profiles have been simulated by convolution of the profile with the resolution function using 6-doped layers (A25), and the implication and possible limits for deconvolution from the &doped layers was examined (A26). 6-doped Be layers in MBE GaAs layers have been measured and reveal a dopant impurity width of 20 A (A27). High dynamic range profiling along with high depth resolution is alwa s essential. High dynamic range profiling can be obtainedrby creating mesa structures in the sample using the ion beam and then profiling as usual (A28). Dynamic range optimization for As and Sb implants in Si is also reported (A29). A solution to the difficult problem of quantitative do ant depth profiles in silicided structures was obtained by knith along with an estimate of the errors involved (A30). Finally, a test methodology has been developed for profiling shallow junctions (650 "C showed a T,of 85-91 K. Also, the orientation of the deposited film depended on the substrate temperature. Extended X-ray Absorption Fine Structure (EXAFS). The oscillations occurring on the high-energy side of an X-ray absorption edge (30-1000 eV) are commonly known as extended X-ray absorption fine structure (EXAFS) (E21). EXAFS has now emerged as a widely used technique for the investigation of electronic structure and the local threedimensional environment surrounding specific atoms in materials where the popular techniques of X-ray diffraction (XRD) and neutron diffraction have failed. The experiment consists of XAS measurement. When the incident X-ray energy exceeds the threshold excitation energy to photoeject the core electron, the outgoing photoelectron wave from a central absorbing atom interferes constructively or destructively with the photoelectron waves backscattered from atoms in the first coordination shell. The interference, which is ANALYTICAL CHEMISTRY, VOL. 65, NO. 12, JUNE 15, 1993

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dependent on the incident X-ray energy and nearest-neighbor distance, is reflected as oscillations on the high-energy side of a discontinuity in the X-ray absorption spectrum. Fourier transform analysis of EXAFS yields structural information such as nearest-neighbor distances, coordination numbers, and t es of nearest neighbors (E22). The short-range order of E a F S allows structural information to be obtained from amorphous and dispersed materials that lack sufficient longran e order which is re uired for analysis by conventional XRb. Materials studie! by EXAFS include heterogeneous catalysts, glasses, intermetallic alloys, polymers, proteins, catalysis, and metal sites in bioinorganic materials. EXAFS studies are conducted in laboratories using bremsstrahlung radiation from conventional or rotating anode X-ray tubes. The advent of high-flux synchrotron radiation sources with broad and smooth spectral ranges has extended the application of EXAFS to metastable systems and systems having a very low concentration of elements of interest. As the availability of synchrotron facilities increases, the potential applications of EXAFS will widen further. Several review articles have appeared recently highlighting the importance and applications of EXAFS (E23). In recent years the local geometric and electronic structures of the high-temperature superconductors have been extensivelystudied using EXAFS. Mustre et al. (E24)have studied the axial oxygen contributions to the Cu K edge in the temperature ran e of 10-105 K. They found two nearly equallypopulatecfO(4) sites 0.13 A apart. The site separation was found to decrease by 0.02 A in a re ion near T,. The effect of Ni substitutionon the copper site t a s been examined by Szunyogh et al. (E25)for the concentration range of 0-0.15 in YBaz(Cul,Ni,)307 sample. Significant differences were observed in the partial densities of states, the Fermi level, and the DOS at the Fermi level in the case when Cu(l! sublattice was doped. The study of Bridges et al. (E%) showed that, for low Ni concentrations, the Ni substitutes nearly uniformly on both Cu sites. A t higher Ni concentrations, the NiO were present as an impurity phase. The values of T,was found to decrease linearly with Ni concentration, approaching zero at a Ni concentration of 8.5 atom % . Yang et al. (E27) studied the YBa~(Cul-,M,)307a, where M = Fe, Co, Ni, and Zn. The study was directed to determine the important material parameters, such as the location of dopants, valence of dopants, structuralchanges,modifications of electronic densities of states, and distribution of holes. The local structure of BaBi,Pbl,03 has been studied by De Groot et al. (E28)and Boyce et al. (E29)for the various values of x . De Groot et al. found that the oxygen 1s spectra did not show the pre eak structures common in the doped copper oxide supercon uctors. Boyce et al. observed two Bi-0 distances. These distances and their separations were found to decrease with increasing Pb concentration. The local structure around Bi atoms in Bal-,K,BiOa has been studied by Salem-Sugui et al. (E30) for 0 < x < 0.4 and in the temperature range 13-300 K. The ordered breathing modet e distortion in BaBiO3 was found to be replaced by a isordered distortion of the same type when K was substituted into the Ba site. The superconducting T1-Ca-Ba-Cu-0 thin films were investigated by DiMarzio et al. (E31). Improvement in the superconducting transition increased the CuOz plane orientation parallel to the substrate. The Ndz-,Ce,CuOp has been studied by Oyanagi et al. (E32)in the Cu K and 6 e L3 regions at various oxygen partial pressures. The reduction in the pressure was found to enhance the electron density at the copper sites, without changing the oxygen deficiency. Studying the Cu 1s and 2p region in such a material, Lederman et al. (E33)observed two possibilities: (1)Ce causes a decrease in the Cu valence, and (2) Ce causes a shift in the Cu 1s position. Tan et al. (E34)have established the valence of Ce as 3+ in Ce-doped NdzCuO4. Tranquada et al. (E35)probed the localized states in Laz-,Ba,Cu04 and studied their delocalization. A localized hole was found around the Ba site, while no delocalized holes were detected at the La L3 edge. The average distance between Cu and the apical oxygen remained essentially unchanged by Sr doping. Tan et al. (E36) studied the rare earth site ordering in Laz,R,Sr,CuO~ for R = Sm, Eu, Gd, and Tb. They observed two inequivalent sites for the rare earths. Utilizing the measurements in the CuK edge in the Bi-Pb-Sr-Ca-Cu oxide superconductor in the temperature range from 26.9 to 300 K,

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Koizumi et al. (E37) determined the interatomic distance and mean square relative displacement in the system. The Cu K and Pb L3 edges in PbBaSrY1,CaXCu3O,+a and Pb~Sr~Y1-,Ca~Cu308+a systems have been measured by Yamaguchi et al. (E38). The Cu K-edge position was found to be shifted to higher energy retaining the CUI+feature while Pb appeared in mixed states of 2+ and 4+. The terbium-iron amorphous films have been studied by Takayama et al. (E39). The Co-Fe multilayers have been studied b Boher et al. (E40). Harris et al. (E411investi ated the Fe-Tg alloy films. Magnetic properties and local orfering during thermal annealing of amorphous Fe,5Ni&5Si16 films have been studied by Oliver et al. (E42). The position of Zr within the unit cell of SmzCo17 has been determined b Rabenberg et al. (E43). The temperature-dependent EXAF8 measurements have been carried out by Marcus et al. (E44) on gold (Au55) clusters made by the Schmid process. The noncubic symmetry in garnet structures, A3B5012 (for A = Y and Gd; B = Fe, Ga, and Al) have been studied by Dong and Lu (E45). The EXAFS of alkali metal halides (NaBr, KBr, RbCl) as a function of pressure of 0-8 GPa has been investigated by Freund et al. (E46). Himpsel et al. (E47) have studied the Ca 2p soft X-ray absorption edge in Ca metal, CaSiz, CaO, CaFz, BaFz on CaFz, and Ca and CaFz on Si(ll1). In semiconductor technology also EXAFS has been utilized to study the types of bonding and to reveal the local structure. The ionicity and bonding in amorphous silicon nitride, Sil- Ny has been studied by Bayliss and Gurman (E48). $he structuralstudy of coordination defects in amorphous gallium arsenide has been investigated by Udron et al. (E49). A comprehensive study of short-range order in a-Sil-,C,:H has been undertaken by Meneghini et al. (E50). Thin-film amorphous Si0,:H system has been investigated for the bond length (E51). The focal structure and bonding configurations in amorphous GaAsP films were studied by Baker et al. (E52). The atomic-scalestructure of a-Sidn,:H thin films has been determined by Edwards et al. (E53). The structure of hydrogenated amorphous Si-C alloy films have been studied by Pascarelli et al. (E54). The strain and bond distortions in epitaxial Ge,Sil, on Si(OO1) have been investigated by Woicik et al. (E55). Surface EXAFS (SEXAFS) has been found to provide valuable information about the surface morphology and the adsorption of gases on the surfaces of materials. Haase (E56) has reviewed the application of EXAFS to adsorbates. The surface local structure of S-Cu(ll1) has been studied by Kitajima et al. (E57). By studying the reconstruction in the system (2 X 1) oxygen-silver(llO), Becker et al. (E58) have shown that oxygen adsorbs close to the surface, inducing a reconstruction of the missing-row type. The electron-donor pro erties of K adsorbed on TiOz(100)were investi ated by Praihakaran et al. (E59). Monolayers of coadsorbe! Ba and 0 on a single crystal of W(100) were investigated by Shih et al. (E60). They observed the stoichiometry to be nearly 1:2 for Ba:O on W. Jiang et al. (E61)performed a study on epitaxial Cu layers on a Ag(001) surface covered by an epitaxial Au. The surface structure was observed to be free from distortion due to anomalous dispersion effects and it was different from that of normal fcc Cu. The chemisorption of Na on Al(111) has been studied by Schmalz et al. (E62).The crystallographic structure of epitaxial iron films grown on Cu(100) depends upon their thickness and their growth temperature, as shown by Magnan et al. (E63). The local bonding structure of Sb on Si(ll1)has been studied by Woicik et al. (E64). Richter et al. (E65)have studied the local and long-range bonding properties of Si(OO1) 2 1-Sb interface. Photoemission induced EXAFS has been also utilized for surface structure determination. Kim et al. (66)studied the Na-Si(100) 2 X 1 and Cs-Si(100) 2 X 1 interfaces. The structure of AI-Si(ll1) interfaces for 1.1and 2.2 monolayers of A1 coverages has been investigated by Mangat et al. (67). The average Si-Si and Si-A1 nearest-neighbor distances as determined by them are 2.47 0.04 A. The Bi-InP(110) interface was studied for 0.35 and 0.9 monolayer of Bi coverages by Choudhary et al. (E68).Their results show that, for 0.9 monolayer, Bi rows epitaxially and the P-Bi bond length is 2.42 f 0.05 A study of atomic geometries of Ag-InP(110) interfaces for 0.5- and 1-8,metal coverages has been performed by Mangat et al. (E69).

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Catalysis is one of the many important applications of EXAFS. The silicon oxide- rafted dinuclear molybdenum catalyst derived from Mo2(6Ac)4 was studied for catalytic activity for propene by Zhuang et al. (E70). The structures of bimetallic cop er-platinum particles in freshly reduced and out assed Cu t-NaY zeolites were characterized by Tzou et al. &I). The SiO2-supported Pd-Cr catalysts prepared by using mixed inorganic salts of the metals were studied by Borgna et al. (E72). These catalysts have been found to be 100% selective for the formation of butenes in the process of partial hydro enation of l,&butadiene. One atomic layer of niobium oxife layer prepared on a Si02 surface has been synthesized and studied by Asakura and Iwasawa (E73). Evidence of a Nb-Si bond with bond length of 0.327 f 0.003 nm was found on the surface. The system was found to be more active and selective for CzH4 formation from CzHzOH in the temperature range 373-573 K. The study of Dooryhee et al. (E74)on nickel-exchanged Y zeolite was focused on the location of the Ni2+ ions in the hydrated form of the zeolite, the environment and evidence of movement of Ni2+ions upon heating the zeolite, and the changes in local environment of the Ni brought about by subsequent reduction in H. The characterization (E75) of Re surface species, derived by treating HSRe3(C0)12adsorbed on -pA1203in H at 400 K, revealed an average Re-Re coordination number of 2, the Re-Re distance to be 2.67 A, and the Re-0 distance to be 2.05 A. The structure and electronic state of molybdenum subcarbonyl s ecies encaged in alkali-metal cation-exchanged zeolites have t e e n studied by Okamoto et al. (E76). Matsumoto and Tanabe (E77) have investigated the catalytic behavior and structure of active species on Cu-Y zeolite in the oxidation of carbon monoxide. The adsorption of perrhenate, ermanganate, molybdate, tungstate, and chromate on A1283 has been studied by Mulcahy et al. (E78).The nickel-molybdenum-sulfur structure in carbon-supported and alumina-supported nickel-molybdenum catalysts was studied by Louwers and Prins (E79). Zhang et al. (E80) investigated the oxidation leaching of copper atoms from palladium-copper particles in Y zeolite. Maloney et al. (E81) have studied the osmium carbonyl clusters in basic Y zeolite. A study of platinum particles in L-zeolite saturated with H2 at room temperature and after desorption of H2 in He has been performed by McHugh et al. (E82).The polymerization of pyrrole over palladium- and tin dioxide-supported KL zeolite has been studied by Larsen et al. (E83).

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ACKNOWLEDGMENT We acknowledge Chemical Abstracts Service for providing access to STN International to aid in the literature search used in the preparation of this work. A.R.C. acknowledges and D.R.C. acknowledge support from the Robert A. Welch Foundation, Grant T-0643. F.K.P. acknowledges support as a NRC/NRL Co-Operative Research Associate. LITERATURE CITED 1NTRODUCTION (1) Kane, P. F.; Larrabee, G. 8. Anal. Chem. 1977,49, 22lR-230R. (2) Kane, P. F.; Larrabee, 0. 8. Anal. Chem. 1979,57, 308R-317R. (3) Larrabee, G. B.; Shaffner, T. J. Anal. Chem. 1981,53. 163R-174R. (4) Bowling, R. A.; Larrabee, 0. 8. Anal. C b m . 1983. 55, 133R-156R. (5) Bowling. R. A.; Shaffner, T. J.; Larrabee, G. B. Anal. Chem. 1985, 57, 130R-15 1R. (6) McGuire, G. E. Anal. Chem. 1987,59, 294R-308R. (7) Fulghum, J. E.; McOuire, G. E.; Musselman, I.H.; Nemanich, R. J.; White, J. M.; Chopra, D. R.; Chourasla, A. R. Anal. Chem. 1989,67, 24313-269R. (8) Ray, M. A.; McGuire, G. E.; Musselman. I. H. Nemanich, R. J.; Chopra, D. R. Anal. Chm. 1991, 83, 99R-118R. ION SPECTROMETRY (Al) Greenikf, C. M.; White, J. M. Secondary-Ion Mass Spectrometry. I n PhySlCalMethods of Chemlshy,Rossiter, B. W., Baetzold, R. C., Eds.; Wiiey and Sons: New York, 1993;Vol. 9A, pp 321-81. (A2) Stevle, F. A. Surf. Interface Anal. 1992, 78, 81-6. (A3) LevCSetti, R.; Hallegot, P.; Glrod, C.; Chabala. J. M.; LI, J.; Sodonis, A.; Wolbach. W. Surf. Scl. 1991,246, 94-106. (A4) Paul, A. J.; Vlckerman, J. C. Phibs. Trans. R. SOC.London 1990,A333, 147. (A5)Reed. N. M.;Vldterman. J. C. NATOASISer. (Fundem.AspectsofHeterog. Catel. Stud. Part. Beams) 1991,8265, 357-92. (A61 Leggett, G. J.; Vlckerman, J. C. Int. J. Mass Spectrom. Ion Processes 1992, 122, 281-319.

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