Characterization of electronic devices and materials by surface-sensitive analytical techniques

Applications of Surface Science 4 (1980) 4 10—444 © North-Holland Publishing Company

CHARACTERIZATION OF ELECTRONIC DEVICES AND MATERIALS BY SURFACE-SENSITIVE ANALYTICAL TECHNIQUES PH. HOLLOWAY Department of Materials Science and Engineering, University of Florida, Gainesville, Florida 32611, USA and G.E. McGUIRE Materials Characterization Laboratory, Tektronix, Inc., Portland, Oregon 970 77, USA Received 24 July 1979 Revised manuscript received 19 September 1979

Applications of surface-sensitive analytical techniques (Auger electron, X-ray photoelectron, ion scattering and secondary ion mass spectroscopies) in research and development for electronic materials and devices are illustrated. ‘These analytical techniques have been used in all phases of the electronics industry, and their importance and applications are expected to continue to increase.

1. Introduction Research and development in the area of electronic devices and materials has expanded rapidly over the past twenty years since the discovery of the transistor. A number of new technologies have been developed and improved to accomplish the mass production of large and small devices, including vacuum technology, photoresist techniques, dopant implantation and diffusion, thin film deposition, and solid state bonding. Equally important to progress in manufacturing these electronic devices has been improvements in the ability to characterize the topography and composition of small areas and thin layers. For example, scanning and transmission electron microscopy, optical microscopy, ellipsometry and infrared absorption spectroscopy have all been used to characterize topography, structure and composition. But many failures and/or critical materials areas are located at the surface or interfaces of these devices. Some examples are contaminants on the surface, thin gate oxides, delamination of metallization and poor bond strengths. Because of these critical areas, a number of analytical techniques sensitive to the surface and interface have been applied to research and development programs dealing with devices and materials [1—121.Primary amongst these has been Auger electron spectroscopy (AES)

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[3,4,8—10] because it is sensitive to the outer few layers of atoms, can detect both high and low atomic number elements, can achieve very good spatial resolution, and can be used to detect interfaces in conjunction with ion sputtering. Secondary ion mass spectroscopy (SIMS) [4,8—10] has been used often because it is also sensitive to the first few layers of atoms, but in addition it can be used at times to analyze trace elements and is more generally applicable to analysis of insulators (as compared to AES). Two other techniques have been used less often although each has its own unique attributes. X-ray photoelectron spectroscopy (XPS or ESCA electron spectroscopy for chemical analysis) [4,8—10] is sensitive to the outer layers of atoms and is very useful for elemental as well as chemical state (e.g. Si versus SiO2) —

analysis of both conductors and insulators. Ion scattering spectroscopy (ISS) [4,8—10] is the only technique available which is truly sensitive to the surface, i.e. to the very outer layer of atoms. ISS can be used for elemental analysis of both conductors and insulators. In the remainder of this paper, (1) the principles upon which these analytical techniques are based will be discussed briefly, then their application to electronic devices and materials will be discussed under the general headings of (2) general applications, (3) analytical effects, (4) silicon, (5) germanium, (6) compound semiconductors, (7) oxides substrates, (8) molecular beam epitaxy, (9) metallization, (10) resistor and capacitor materials, (11) interconnections, (12) compatibility, and (13) failure analysis. Selected applications of the techniques in each of these categories are illustrated, and the specific examples are supported by a more complete bibliography of categorized publications.

2. Review of techniques General reviews of the experimental techniques may be found in refs. [1—12]. The techniques may be grouped according to whether X-rays (XPS), electrons (AES), or low energy ions (ISS and SIMS) are used for excitation. For the XPS technique shown in fig. 1 photoelectrons are detected for analysis. A flux of X-rays striking a solid will cause ejection of electrons from electron levels with binding energies less than the energy of the incoming photons. The kinetic energy of the photoelectron shown in fig. 1 is given by the energy of the X-ray minus the binding energy of the ejected K shell electron and minus a work function and wave function relaxation term [8]. Since the set of binding energies is unique for a given element, the photoelectron peaks may be used for elemental identification. Core level ionization (fig. 1) leaves the atom in an excited state. De-excitation occurs by an upper level electron (L1 level) decaying to the core hole with the excess energy being transferred to, and causing ejection of, another electron (L23 level) which is by definition an Auger electron. The Auger transitions are denoted by the electron levels involved; thus fig. 1 illustrates the ejection of a KL1L2 ~ electron. The kinetic energy of the Auger electron is given by the differences in binding

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Characterization of electronic devices and materials

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energies of the three levels (EK EL1 EL2 3) minus a correction term for work function difference and electron wave function’relaxations (similar to that for XPS). The core level ionization which initiates the Auger process can be caused by either X-rays, electrons or ions. By convention AES refers to electron excitation. While data for XPS are usually taken as the number N(E) of electrons with a particular energy E versus that energy, AES data are normally taken as dN(E)/dE versus F spectra with a potential-modulation differentiation scheme [4,7,8, 10]. Differentiation suppresses the high background caused by inelastically scattered electrons. Signal processing can be used to increase the sensitivity and decrease the time required for Auger analysis in both the derivative and the N(E) mode. The low energy ion techniques of ISS and SIMS are shown in fig. 2. When ions impinge upon a solid there is a finite probability (~10~)that they will undergo an elastic collision with surface atoms and lose an amount of energy determinated by the mass of the scattering atom and the scattering angle (fig. 2); therefore the mass of elements in a solid may be determined by energy-analyzing the scattered ions. ISS refers to the elastic scattering of ions with initial energies of about 4 keV or less. Only ions elastically scattered from the outer layer of surface atoms are detected in this technique, since ions which penetrate beyond the outer layer are rapidly neutralized. —~

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In addition to elastic collisions some ions suffer inelastic collisions with surface atoms, causing the ejection of these atoms (sputtering). Other primary ions penetrate a short distance into the lattice where they lose their kinetic energy and create energy cascades which may also cause sputtering of material from the solid as either charged or neutral atoms and molecules. By collecting and mass-analyzing the sputtered secondary ions the elemental composition of the solid can be determined. When molecules are collected as secondary ions their cracking patterns may allow identification of the parent molecule. In all four cases, the experimental techniques are sensitive to the surface region of solids. Because the mean free path of low-energy electrons in solids is short, the AES and XPS signals originate in the outer S A to 20 A of the sample. The energy cascade in SIMS causes ejection of ions from the outer 10 A, while ion scattering in ISS occurs at the outermost layer of atoms. All of the techniques are capable of elemental analysis, although the elemental sensitivity factor for SIMS depends greatly upon the matrix. For example pure gold is difficult to detect with SIMS because of the low secondary ion yield, but small amounts of gold in an oxide matrix can easily be detected. For AES, XPS and ISS, the variation in elemental sensitivity over the periodic table is about a factor of ten. The detection limits of AES, XPS and ISS are similar, i.e. 0.1—0.5 at.%, while in some cases, the detection limit for SIMS can be 1 ppm or better. Most techniques give good resolution of one element over another, except that it is sometimes difficult to resolve elements with ISS when their atomic numbers are high and close together. All four techniques can be quantified in selected instances using standards, but general quantification is still an area of research. At times, problems can be solved only by knowing both the elements present

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and their chemical state (e.g. metal versus oxide). XPS has been used extensively to determine chemical state, and a large body of data is being accumulated upon which to base conclusions. The Auger electron peak shape and energy, and in some instances, the “cracking pattern” in SIMS can also be used to determine chemical state. All of these techniques use sputter removal of surface atoms to determine the distribution of elements with depth, therefore depth analysis is destructive. In addition, the electron beam for AES and ion beam for ISS/SIMS can be focussed to a small size, therefore these three techniques are capable of resolving features in the plane of the surface. A surface area ~l mm in diameter is typically sampled in XPS measurements.

3. General applications There are a number of articles illustrating how these surfaces sensitive analytical techniques may be applied to electronic devices and materials (see refs. [13—41]). Deal [16] has discussed the application of surface analysis to the areas of silicon substrate fabrication, thermal oxidation, photomasking and cleaning, diffusion, dielectric deposition, metallization and chip protection. He concludes that surface sensitive analytical techniques have impacted and/or will impact all of these areas of semiconductor processing. This conclusion is reinforced in a survey by Holloway [22] where specific applications of surface analyses were cited in the areas of substrate and substrate processing, deposited films, patterning, interconnections and compatibility. The application of AES to microelectronic technology has been emphasized by Morabito [32] and McGuire and Holloway [29] McGuire and Holloway have also compared the use of AES and XPS for electronic research and development, and Grunthaner [20] has illustrated many problems that can be solved by XPS analysis. Similarly, Dobrott et al. [17] have illustrated some consideration in analyzing electronic samples with SIMS using an ion microprobe, and have determined some detection limits for this analysis technique. Dobrott et al. have illustrated some considerations in achieving spatial resolution in the plane of the surface with an ion microprobe. Spatial resolution in the plane of the surface can also be achieved in AES by focussing an electron beam to a very small spot. MacDonald et al. [28] have illustrated this technique with beams focussed to ~0.2 pm, and Christou [13] has discussed the incorporation of the electron energy analyzer into a scanning electron microscope for analysis of <0.1 pm spots. To complete a three-dimensional compositional analysis, the concentration distribution with depth must be known. Sputter profiling for depth analysis has been illustrated in several publications [17,20,29,31], but MacDonald and Riach [27] have directly addressed the problem and illustrated some results obtained by sputter removing surface atoms from thin films. .

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4. Effects of analytical techniques As with any analytical technique, those sensitive to the surface region of solids may cause damage in the sample being analyzed, and this damage may interfere with the analysis. The different types of damage reported are summarized in refs. [10] and [42—58]. The observed effects include electron stimulated adsorption and oxidation [45,49,52], electron stimulated desorption [50,5 1], breaking of chemical bonds [43,56], heating of the sample [10], migration of mobile species [44], Auger peak shape changes due to chemical shifts [48], and artifacts due to sputtering [54,57,58]. Thomas [56] first demonstrated that SiO2 was susceptible to decomposition by electron irradiation. This apparently occurs due to collisional excitation of bonding electrons to non-bonding orbitals; this causes disintegration of the SiO2 molecule. Thus analysis must be performed at very low electron doses [48]. The local heating caused by a beam focussed onto a substrate has not been studied properly. Data for titanium hydride suggest that temperatures ofseveral hundred degrees Centrigrade can be created by a focussed electron beam for AES. Beam heating may be significant in samples of poor thermal conductivity, such as Si02. Beyond causing phase changes, high local heating causes material to diffuse rapidly. Chou et al. [44] have found that chlorine incorporated in Si02 films can move during AES analysis. This results from a higher mobility due to local heating and a high driving force caused by trapped electrons creating electric fields. This effect may be reduced by cooling the specimen towards liquid nitrogen temperatures. Sputtering the surface with inert gas ions (e.g. Art) can cause damage [54,57,58]. Wehner [58] has reviewed the possible effects such as amorphous sputtered layers, preferential sputter removal of elements, the “knock-on” effect, surface roughness, etc. Most of these effects have been observed for electronic materials. For example, sputtering of GaAs has led to preferential removal of As leaving a Ga-rich surface layer [54]. Thus a number of possibilities exist for introducing artifacts into the analytical data. With the help of an experienced analyst, most of these effects can be avoided.

5. Silicon Silicon and its compounds have been the most studied electronic material. This of course results from the dominance of silicon-based technology in the semiconductor industry. In order to make the impact of surface analysis upon this material and technology more easily comprehended, the silicon category will be discussed according to subcategories. (a) General. General aspects of the analysis of silicon are discussed in refs. [59—79] in addition to those in the applications section (section 3). The general distribution of secondary electrons from Si surfaces has been studied by Allie and Gervais [59]. Studies of clean Si surfaces have shown that the surface atoms may be arranged dif-

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ferently than would be expected from the bulk crystal structure. Grant and Haas [64] have shown that this may or may not result from impurities on the surface; Si{l 11 } (2 X 1) and (7 X 7) rearrangements are characteristic of a clean surface rather than of a contaminated surface. Sachse et al. [75] have shown that ion bombardment may cause the surface of Si to change from crystalline to amorphous. The thickness of the damaged layer is a function of time and energy, and some annealing studies were performed. The surface does not always change drastically as a result of interactions. For example silicon films can be epitaxially grown on sapphire and Chang [60], Didenko et al. [62] and Joyce et al. [69] have studied this epitaxial growth with techniques including AES and SIMS. The effects of substrate orientation, temperature, and surface structure upon the epitaxial and electrical properties were studied. At other times, the surface reorganizes, e.g. the interaction of hydrogen with Si has been studied by Hagstrum and co-workers [72,76],and von Roedern et al. [79]. They could clearly see changes in the XPS and other spectra which indicated hydrogen-induced change in the structure of the surface. (b) Contamination and cleaning. Control of contamination is critical to the successful production of electronic devices, and surface analysis has proven very useful in this area (refs. [80—92]). Yang et al. [91] used AES to show that carbon is a contaminant commonly left on silicon surfaces by common cleaning techniques. Sputtering removed carbon, but activated the surface towards reaction with atinospheric gases. Plasma treatments were shown to provide the cleanest surfaces. Chang [82] has shown that high temperature oxidations also remove carbon, but metallic impurities may appear on the surface as a result of the treatment. Another impurity which affects electrical performance at very low concentrations is sodium. Grunthaner and Maserjain [85], and Lyo and Komiya [88] have studied the distribution and chemical state of Na in Si02 using AES and XPS. A number of different chemical states was observed for sodium, and it was mobile under some conditions of analysis. Techniques to minimize the effects of Na were discussed. (c) Electronic structure. The electronic configuration of clean and contaminated Si surfaces has been studied by surface analysis (refs. [93—i10]). Amelio [93] first recorded the Auger spectra from clean Si and tried to deduce the density of filled states from these measurements. As shown by Houston and L.agally [179], and others, there is not always a direct correspondence since s or p bonding character may be emphasized differently in Auger emission. The same is true in XPS and in a modification of this technique where photons in the ultra-violet region are used for excitations (UPS). Pandey [97], Rowe and co-workers [l00—l06], Rubio et al. [107], and Sebenne et al. [108,109] have used UPS to study the electronic structure of the surface. They have identified electronic surface states which may eventually be correlated with electrical properties of the material. Hamann [96] has theoretically analyzed the clean surface of Si. He has calculated the energy levels of these surface states and successfully related them to the atomic rearrangement which occurs on clean surfaces. These results provide hope that interfacial states may eventually be analyzed in a similar manner.

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(d) Dopants. Surface analysis has been used to study the formation of dopantrich surface oxides (glasses), diffusion of dopants, and implantation of dopants (refs. [111—125]).Gallon et al. [117] have shown thatPontheSisurfaceeliminates the reconstructed arrangement; with phosphorous present the atomic arrangement of the outer layer has a symmetry (or lattice) that is equivalent to that produced by cutting the bulk lattice. Several studies have shown that both P and B segregate at the Si/SiO2 interface [111—114,121,1231. The chemical state of the dopant in the oxide layer has been studied [121], and segregation coefficients reported. Levenson et al. [119], and Thomas and Morabito [124] have determined calibration factors and detection limits for dopants in silicon. A number of investigators have used AES and SIMS to study dopant diffusion profiles [112,120,122,126]. Because of the lower detection limits for SIMS, it is clearly favored for this type of analysis. (e) Silicides. Since the thin film silicide reaction to form ohmic contacts is critical to semiconductor technology, surface analysis has been extensively applied to this problem (refs. 127—143]). Bindell et al. [127], and Robinson and co-workers [123,140] have shown that the silicide formation is usually controlled by the kinetics of diffusion. Blattner et al. [129] studied the effect ofvarious oxidizing ambients on siicide formation. Robinson [134,1401, and Thomas and Terry [142] have clearly shown that silicide formation causes chemical shifts in the Si Auger electron peaks (shape and energy changes), and Boyer et al. [130] have studied similar shifts in XPS data. Danyluk and McGuire [133] used XPS chemical shifts to conclude that Pt Si~O~ compounds were formed during heat treatments and that these compounds interfered with chemical etchings of integrated circuits. This conclusion is disputed by data reported by Rand and Roberts [139], who conclude that only SiO2 is causing these problems. (f) Silicon—metal interactions. Silicide formation is important, but other silicon— metal interactions can occur and affect device characteristics (refs. [144—154]). Nakamura et al. [148] have studied the interaction between Al and Si films. At times Si can be transported through Al and form Si02 layers on its surface. Hiraki and co-workers [146,149] have used AES to study the chemical state of Si in noble metals (e.g. Au) and conclude that “metallic” Si exists under these conditions. Some important silicon—metal phenomena occur right on the surface, e.g. Schottky barrier formation. A number of investigators have studied these phenomena [145, 151—154]. (g) Implantation. AES and SIMS have been used a number of times to investigate the average depth and range of implanted ions (refs. [92,120,124,155—162]). Care must be taken to avoid artifacts when measuring the depth profiles by sputtering, but spectra from AES and SIMS [120], and AES and ellipsometry [155] have compared well and reinforce the conclusion that good profiles can be produced. The experimental profiles have been compared to theoretical calculations to develop predictive capabilities. (h) Silicon oxide and oxidation. The structure and rate of formation of Si02 has been studied in greater detail than all other areas of Si technology (refs. [44,46,48,

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53,57,59,70,163—205]). A number of areas have been studied including the growth of the oxides. Studies of the initial stages of oxidation have shown that a chemisorbed oxygen layer is first established, then an oxide layer is formed [163,171, 172]. In fact, Raider et al. [193] conclude that true Si02 may not be formed on Si surfaces which have been chemically etched and exposed to room temperature air for short periods of time. Once the S1O2 layer is formed, the interface between Si02/Si remains in doubt [168,174,175,178,197,204]. This interface is important because electrically active energy states are associated with it. Studies to date indicate that the interface is sharp, with some measurements showing a width of~2 nm [174,175]. However the nature of the interface is still in doubt. In some models, the interface consists of isolated islands of Si in an SiO2 matrix. In other models, a sub-oxide transition layer is postulated [168]. The topic is still being actively investigated, but no clear correlations have been found between surface analysis and electrical data. A similar controversy involves the structure of silicon monoxide (SiO). Some data indicate that SiO exists as a unique species in the solid state [177,189,192] while other data suggest that SiO is simply a mixture of Si and SiO2 [1811. In fact some investigators suggest that SiO is the transition from oxide to element at the SiO2/Si interface [168]. This topic is also still controversial, however it appears that SiO is a true compound. Other aspects of Si02 have been studied. For example, its electronic structure has been investigated [170,180,194] and the density of filled valence states measured by Auger peak shape analysis [179]. Sweet and Holloway [200] measured the interfacial oxide thickness on Si—Ge alloys and correlated thickness changes with changes in the contact resistance to sputtered deposited W contact films. (i) Silicon nitride. Thin films of silicon nitride are used to passivate devices and to serve as charge storage films in non-volatile memories. As a result, a significant number of investigators have studied the nitrides (refs. [164,165,182—184,206— 221)]. The nitride films have been prepared in three ways. One method is to directly react hot Si with nitrogen-containing gases [208,213], but the reaction proceeds very slowly and the product often contains large amounts of oxygen. However, this reaction is still very important because some N can be found at the Si/SiO2 interface after heating [212,219] and this may influence the electrical properties of devices. A second more common method of depositing nitride films is chemical vapor deposition (CVD) from a silane—ammonia mixture. Studies of CVD films have shown that they contain oxygen and hydrogen as well as nitrogen [211,213,219— 221]. The properties of the nitride films vary with the incorporation of 0 and H, but quantitative correlations between the composition and electrical properties are very limited [219]. Ogata [217] has reported studies of the diffusion in Al in these nitride films. The third method for deposition of silicon nitride is to use a plasma. Studies of these films are less numerous although they have been shown to have incorporated impurities [219]. (j) Silicon carbide. A limited amount of work has been reported on silicon car-

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bide (refs. [59,74,164,165,222—224]). Most of these studies involve electron beam cracking of CO and CO2 onto the Si surface and subsequent carbide formation. Distinct chemical shifts are observed in the Si and C Auger peaks which positively identify carbide formation [222].

6. Germanium Because of the lesser importance in the semiconductor industry, the number of surface analysis investigations of Ge are much less than for Si (refs. [64,98,105, 170,194,202,225—235]). Techniques to clean Ge surfaces have been studied [228] as well as the formation of oxide upon these surfaces [225,227,235]. The electronic structure of Ge surfaces has been studied with XPS, UPS and electron energy loss measurements [226,230,231,233]. These data provide insight into the density of filled states, density of unfilled states above the Fermi energy, intervalency transitions, plasma losses and surface states. Mityagin et al. [232] have studied the growth of GaAs on Ge surfaces. Knotek [229] and Santilli and Haneman [234] have used AES and XPS to measure the contamination levels in crystalline and amorphous Ge, and to correlate differences in contamination with changes in electronic transport properties.

7. Compound semiconductors With the increasing interest in compound semiconductor devices, the use of surface analysis to study these materials is increasing. As with Si, these uses will be illustrated by subdividing the major category. (a) General. General aspects of compound semiconductors analysis are discussed in refs. [54,64,73,203,236—258]. Chemical preparation of the surfaces has been studied [238], and compositional profiles into the bulk have been measured [225]. The distribution of implanted dopants has been studied [240,2421 along with dopant redistribution upon heat treatment. (b) Contamination and cleaning. As described in refs. [259—263], a limited amount of work has been reported on contaminants of compound semiconductors. Uebbing [262,263] reports that carbon contamination severely attenuates the photoyield of GaAs—Cs—O photosurfaces. In fact, one monolayer of C caused the photoyield to approach zero. Chen [26] has studied the surfaces of GaAs contaminated with Na. Alexandre [259] has proposed that a surface gettering of alkali impurities can be created on GaAs by ion implanting then heat treating the sample to cause segregation to the surface from the bulk. Shiota et al. [261] have studied techniques for chemically preparing GaAs surfaces. If the surface is improperly etched, non-stoichiometry and thick oxides may result.

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(c) Electronic structure. The electronic structure of compound semiconductor surfaces has been extensively studied (refs. [106,226, 230—232, 264—285]). The density of filled and empty electronic energy states has been studied by photoernission using X-rays, ultraviolet photons and continuously variable energy photons from a synchrotron [273,274,278,281]. Pianetta et al. [281] conclude that the Fermi energy of GaAs was pinned at midgap because of extrinsic states. Chemisorbed oxygen caused surface reconstruction which changed this extrinsic state and changed the surface electronic structure. The existence of surface states on GaAs has been established by a number of studies [266—270,272,275,280—285]. Thc surface state may result from the surface reconstruction observed for GaAs [64, 266]. The association between energy states and interfaces between Ga and GaAs has been studied by Bachrach and Bianconi [265]. They see evidence for a redistribution of charge between Ga and As as the interface is created. (d) corn pound semiconductor reactions. Surface studies of reactions on compound semiconductors are described in refs. [52,232,286—313], however, the majority of these references deal with the formation of oxides on GaAs surfaces [287,

289,292—294,300—302 ,304—308 ,3 10,312]. Oxides grown by thermal, anodic, or plasma treatments have been studied. The optical and physical properties vary depending upon the preparation technique and the parameters used in a particular technique. Oxide growth was influenced by the amount of water in tile atmosphere [293] and the oxide was rich in Ga because of both evaporation and rejection of As from the oxide film [287,292,302,310,312]. However the amount of As redistribution and the compounds formed depended upon experimental technique and crystalline orientation [307]. The initial stages of oxidation have been studied by Pianetta et al. [305,306]. (e) compound semiconductor contacts. The formation of electrical contacts to compound semiconductors involves a number of very complex material reactions,

as illustrated in refs. [314—331]. The reactions involving Ni/Au—Ge films on GaAs have been studied by Robinson and co-workers [32 6—328] and by Anderson et ai.

[314]. The reactions are complex in that Ni diffuses inward and Ga diffuses outward. The rearrangement of these deposited layers was correlated with changes in the contact resistance and barrier energy. The use of other metals for contacts upon

GaAs has been reported [316—319,321,325,329,330] and in general, complex metallurgical reactions can be observed upon high temperature heat treating. There have been some studies of the relationship between surface states on the Ill-—V semiconductors and the Schottky barrier formation [320,323]. (f) Compound semiconductorprocessing A limited number of studies of processing have been reported in refs. [90,332—335]. Bayliss et ai. [332] reported that GaP decomposed when it was electron bombarded [332]. They also reported on structural and compositional changes upon heating GaAs, lnP and GaP in vacuum

[333]. Gerner et al. [335J and Chang [334] have used AES to study films of Ga~Al1 ~As films grown by liquid phase epitaxy.

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8. Oxide substrates

Surface analysis techniques have been used to study both the surface and grain boundary composition of oxide substrates (e.g. A1

2O3 ceramics, sapphire, quartz,

etc., see refs. [336—347]). Sundahl [343—3451 and Conley [336,337] used AES to measure the surface composition of A12O3 ceramic substrates after firing and after chemical etching. They demonstrated that Ca and other elements segregated to and were removed from the A12O3 surface upon firing and etching respectively. The presence of these surface impurities increased the adhesion strength of deposited Ta2N and metal overlayers. Vig et al. [346,347] have shown that ultraviolet radiation in air may be used to remove carbonaceous contaminants from quartz surfaces. This improved adhesion of deposited films. Interfacial segregation can affect properties other than film adhesion. Johnson and Stein [340] have shown that impurities in A12O3 may segregate to the grain boundaries and lower the fracture strength of the material.

9. Molecular beam epitaxy (MBE) Because growth of epitaxial films is critically dependent upon the structure and cleanliness of the surface, surface analysis has and continues to provide information critical to improvement in the MBE process (refs. [348—357]). A typical example is analysis of the surface composition during film deposition [348,350]. Foxon and Joyce [353] have used such measurements to characterize phenomena occurring during growth. Along with others, they have shown that group V elements of

compound semiconductors are more volative than group III elements, therefore the vapor phase roust be enriched in the group V elements. At higher temperatures the difference in volatility between different group III elements can cause compositonal changes. Ploog and Fischer [356] have shown that the Sn dopant segregates to the surface of GaAs during deposition and can cause changes in electrical properties. At times, the surface concentration of Sn was three orders of magnitude higher than the bulk composition.

10. Metallization A number of different aspects of the metailization of electronic devices has been studied with surface analysis (refs. [137,339,345,358—406]). For example Thomas [402] has shown that In is enriched on the surface of evaporated Au—In films. The

incorporation of impurities during the deposition process has been studied. Thomas and Haas [401] have measured the incorporation of C and 0 into nichrome films from residual gases in the deposition system. The effects of these impurities upon eutectic bonding processing were considered. Andrews and Morabito [358] have

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shown that Al and Mg impurities in sputter-deposited Pt films originate from sput-

tering of the substrate holders. The impurities can cause undesirable etching of PtSi and resistive paths in the device. Coating the substrate holders with Pt eliminated the problem. Oxide formation on the metal films has been studied. Chang et al. [361] have shown that thick oxide can be formed on Al if processing conditions are not carefully controlled. Koudelkova et al. [389] have studied the films formed on Al by treatment in a chromate solution. The passivating film was found to consist of hydrated Cr (+3) oxide, hydrated Al (+3) oxide, and Cr (+6) species which were largely chlorides. The effects of various deposition conditions have been studied. Besides oxides, surface analysis has been used to study contaminants on the metallization. Christou and Day [367] have studied fluorine contamination in the Ti—Pt—Au system, and Isoyama et al. [387] and Holloway and Bushmire [380] have studied organic contamination on Al and Au surfaces, respectively. Holloway and Bushmire showed that photoresist was a common contaminant on Au metallized hybrid microcircuits. They demonstrated that ozone or ultraviolet radiation in air could be used to remove this photoresist. Besides analyzing the surface, a large number of metallization studies have used sputter profiling for depth analysis of thin films. This is particularly important since deposited metal films have a large concentration of grain boundaries, dislocations and vacancies. Accelerated diffusion, particularly along grain boundaries, has been reported many times in thin films. Wildman et al. [406] studied the Cu/Al system, Tompkins and Pinnel [403,404] studied Cu/Au and Ni/Au, Holloway and Nelson [381,394] studied Cr/Au, Hall et al. [374,375] studied Cu/Au and Pd/Au, McGuire et a!. [369,393] studied Cr/Pt and Pt/Au, Chang and Quintana [364] studied Pt/Au and Hwang and Balluffi [385,386] studied Ag/Au. The data show that the rates of interdiffusion are much higher in the presence of grain boundaries. The analysis of the data can be very complicated however. Holloway et al. [381,382], Hwang and Balluffi [385,386], and Hall and Morabito [376] have discussed techniques of data analysis. Panousis and Hail [397] and Holloway and Nelson [383] have discussed the effects of grain boundary diffusion on soldering, thermocompression bonding and film resistivity. Surface analysis has also been used to study metal surfaces of electrical contacts. Haque [377] has studied the surface composition of contact metals and has observed both surface segregation and preferential contamination effects. Umemoto et al. [405] have determined the thickness of oxide on Ru and Rh which will prevent polymerization of organic molecules on the contact but yet will not cause significant increase in the contact resistance.

11. Resistor and capacitor material Studies of materials used for resistors and capacitors are reported in refs. [407--

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423

417]. Huttemann et al. [410] have studied the effect of light elements such as N, C and 0 in Ta and tantalum nitride films for capacitors. Variations of electrical properties with these impurities have been discussed. Adams and Kramer [408] have studied the oxidation of tantalum nitride after reactive-sputter deposition. Growth of the oxide followed a parabolic rate law, but the adhesion and contact resistance to metal overlayers were not affected until the material had been stored for several months. Baitinger et al. [409] have shown that reactions can occur at the interface between nichrome resistor films and Al to form insulating A1203 films and subsequent high contact resistance.

12. Interconnections The effects of surface contamination upon solid and liquid state bonding have been studied with surface analysis (refs. [418—425]). Gray [420] investigated the causes for lack of adhesion during eutectic bonding of Au—Si prçforms. Surface segregation and compound formation of bulk impurities were the cause of this problem. McGuire et al. [424] have correlated the amount of surface impurities present on solids versus the concentration of impurities in electropolating baths. They conclude that concentrations above one ppm of certain metals (e.g. Cu in Au) could cause significant decreases in thermocompression bond strengths. Holloway and Long [421,422] have shown that Cr203 films as thin as 1 nm can interfere with ther-

mocompression bonding. They also studied teclmiques to remove Cr2 03 films from Au surfaces. Bushmire and Holloway [418] used AES to measure the thickness of photoresist films on Au surfaces and to determine when the photoresist interfered with Au/Au bonding as performed by different techniques. They showed that ultrasonic bonding was least sensitive to contamination while compliant bonding was most sensitive.

13. Compatibility Even though this is an extremely important area where surface analysis has the potential for large impact, the number of studies reported in the literature is very limited (refs. [426—428]). Smith et al. [428] have studied the glasses used to passivate Si devices, and Paulsen and Kirk [427] have shown that under some conditions, the phosphorous in PSG glass can accelerate the corrosion of Al. Christou and Wilkins [426] and Grunthaner et al. [338] have studied the effects of alkali and halide impurities on surface migration of metallization. This migration caused filamentary growth and shorted circuits in some devices. Elimination of halide and alkali contaminants and of moisture can prevent this surface migration problem.

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/ c’haracterization of electronic devices and

materials

14. Failure analysis Again, this is a very important area of electronic device processing, and surface analysis has proven to be very valuable. Unfortunately, however, the number of literature publications is very low compared to the importance of the application (refs. [429—440]). It would be interesting to give the reader a complete review of the failure analysis topic. This is another review in itself; therefore, we will illustrate the subject with only three examples. AES was used by Holloway and Long [422] to show that poor lead frame thermocompression bond strengths resulted from a thin layer of Cr 203 on the surface. A chemical cleaning technique was developed to remove the Cr203. Marcus et al. [438] used scanning AES to show that Ag was deposited during electropolating and resulted in poor adherence of Ni electropolate to Ni substrate. Finally, Brown et al. [429] used AES and SIMS to show that an organometallic grain refiner could be codeposited with electropolated Cu in areas of low current density. This organometallic deposition resulted in delayed solder joint failures.

15. Summary It is quite obvious from the pre~edingdiscussion and the list of references that surface-sensitive analytical techniques are now quite important to the electronic industry. It is useful both for research into basic materials phenomena and for development of new technologies for producing electronic devices. This importance will continue to grow as the electronic industry expands into new areas.

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