SIMS2015 Session DI-TuP: Depth Profiling/Inorganics Poster Session

Tuesday, September 15, 2015 5:20 PM in Grand Ballroom III

Tuesday Afternoon

Time Period TuP Sessions | Topic DI Sessions | Time Periods | Topics | SIMS2015 Schedule

DI-TuP-1 Study on SIMS Depth Profiling of Ru-based Thin Films
Tae Eun Hong, Mi-Rang Byeon, Jong Sung Jin, EuhDuck Jeong (Korea Basic Science Institute, Republic of Korea); Soo-Hyun Kim (Yeungnam University, Republic of Korea)

The downscaling of semiconductor confronts the metallization technology with a large number of challenges. The line resistance of Cu deposited by electro-plating (EP) remarkably rises due to the size effect on the resistivity of the metal film [1].

One possible solution is to maximize the portion of the EP-Cu volume in the dual damascene structure with the thin and conformal diffusion barrier and a seed layer, respectively. The portion of Cu in the dual damascene structures can be increased further by direct plating if the EP of Cu can be achieved on a diffusion barrier without a seed layer. Ru has excellent properties such as low resistivity (7.1 μΩ∙cm), chemical/thermal stability, and immiscibility with Cu. It was also known that Ru adheres well with Cu [2,3], making Ru as a most promising material in the back end of line Cu-wiring as a seed layer or adhesion layer and even as a Cu direct-plateable diffusion barrier.

In this study, Ru films were deposited on a Si wafer using a showerhead-type PEALD reactor (Lucida-M100, NCD Technology), with IMBCH Ru [IMBCH = (η6-1-isopropyl-4-methylbenzene)(η4-cyclohexa-1,3-diene)] as a precursor.

We investigated the compositional characterization of Ru-based thin films using secondary ion mass spectrometry (SIMS). Composition of the films was characterized by SIMS depth profiling whose results were calibrated by RBS. These results will be presented.

[1] S. M. Rossnagel, T. S. Kuan, J. Vac. Sci. Technol. B, 22 (2004) 240.

[2] R. Chan, T. N. Arunagiri, Y. Zhang, O. Chyan, R. M. Wallace, M. J. Kim, T. Q. Hurd, Electrochem. Solid-State Lett., 7

(2004) G154.

[3] H. Kim, T. Koseki, T. Ohba, T. Ohta, Y. Kojima, H. Sato, J. Electrochem. Soc., 152 (2005) G594.

DI-TuP-2 Towards Accurate Determination of Volume Swelling of Silicon Carbide under Heavy Ion Irradiation: A Combination of ToF-SIMS and RBS Study
Ke Jin (Oak Ridge National Laboratory); Zihua Zhu, Jiandong Zhang (Pacific Northwest National Laboratory); Yanwen Zhang (Oak Ridge National Laboratory); William J. Weber (University of Tennessee)

Silicon carbide (SiC) is a promising material in nuclear engineering due to its high strength, good chemical stability and small neutron cross section. In nuclear reactors, extreme radiation condition may lead to degradation of material properties, including volume swelling. The volume swelling of SiC induced by slow heavy ion irradiations at room temperature has been extensively studied in the past decades, but the experimental data are considerably scattered, ranging from 8% to 25% depending on the irradiation conditions and the techniques used for the swelling determination.

In this work, the volume swelling is determined by measuring the depth profile of Au ions implanted into SiC using both time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Rutherford backscattering spectrometry (RBS). In depth profiling, RBS provides the depth information in the unit of areal density (e.g. atom/cm2), while ToF-SIMS provides the absolute depth in the unit of nanometers with the assistance of profilometer. As a result, the density of materials can be extracted from the comparison between these two techniques. The SiC samples were irradiated with 1 and 2 MeV Au ions at both room temperature and high temperature (600 ºc, at which amorphization is not possible) to the ion fluence of 5×1015 cm-2. Our data show that, after high-temperature implantations, the SIMS and RBS results agree well with each other assuming the theoretical density, indicating little volume swelling after irradiation. This result agrees with the previous studies and demonstrates the consistency of the two techniques. In contrast, from room temperature implantations, the extracted densities are ~15% lower than the theoretical value. This result is within the range of previous experimental data and agrees well with the electron energy loss spectroscopy (EELS) study under a similar irradiation condition. This work demonstrates that the combination of RBS and SIMS techniques can provide density information and determine the irradiation-induced volume swelling.
DI-TuP-3 Depth Profiling of Dielectric Films using Room-temperature Direct Bonding in Backside SIMS
Seishi Akahori (Toray Research Center, Inc., Japan)

Backside SIMS is an effective method to investigate the low concentration of dopant and impurities in the semiconductor materials. In particular, Backside SIMS is useful to examine the surface diffusion of dopant without knock-on effect. The samples for Backside SIMS were mounted onto a supporting substrate using a resin as an adhesive and then the samples were polished. The samples were irradiated with an electron beam for the charge neutralization during SIMS measurements. This often causes the destruction of the samples by the adhesive (resin) used for the bonding. To avoid this problem, we developed the new sample preparation method without using the resin. As a result, this method enabled us to analyze more easily insulators and improve the depth resolution using backside SIMS analysis. Recently, we employed a room-temperature direct bonding method (RTDBM).

The RTDBM was used for various materials including semiconductors (MEMS, LED, Power devices etc.). In this method called the surface activated bonding (SAB), oxide film and absorption layer are removed from the wafer surface irradiated with atoms or ions in a high vacuum and dangling bond is generated on the activated surfaces. These activated surfaces which have dangling bond immediately bond only by touching each other.

In this work, we investigated the depth profiling of insulating samples, which were stacked the dielectric films (SiN/SiO2) on a silicon wafer, with/out the RTDBM using a magnetic sector SIMS(CAMECA 6f or 7f).

DI-TuP-5 SIMS Investigation of the Outer Oxide Layer of Cladding Material after Irradiation
Stephane Portier, Matthias Martin (Paul Scherrer Institute, Switzerland)

Zirconium-based alloys are widely used in nuclear industry mainly as cladding for nuclear fuel in power plants. Due to, both coolant and irradiation effects an outer oxide layer is formed on the cladding and modifies its mechanical and thermal properties and behaviour. These modifications can generate a risk for the exploitation of the nuclear fuel and then necessitate to be investigated. During the oxide growth process, boron and lithium, present in the cooling water for neutron absorption control and cladding corrosion control respectively, are trapped in the oxide layer and diffuse through it.

In this work, SIMS depth profiles have been performed using the shielded ATOMIKA 4000 SIMS installed in the Hot Lab Division of the Paul Scherrer Institute. Both lithium and boron profiles have been investigated using Ga+ and Cs+ primary ions through the cladding oxide layer (average thickness about 4 μm) of M5™ cladding material. The crater depths have been measured using an optical interferometer.

The obtained profiles indicate that the oxide layer is divided in two sub-layers. In particular an 800 nm-1μm thick layer, at the metal oxide interface, is strongly Li and B depleted and may play a protective role against lithium and boron diffusion through the oxide layer. This sub-layer also shows electrical properties widely different from the rest of the oxide layer.

DI-TuP-6 Electrochemical, X-ray Photoelectron and Time-of-Flight Secondary Ion Mass Spectrometry Studies of The Corrosion-resistance Properties Oxide Films on Ni-Cr-Mo Alloys
Xiangrong Zhang (The University of Western Ontario); Heng-Yong Nie, David Shoesmith (The University of Western Ontario, Canada)

Nickel-chromium-molybdenum alloys exhibit exceptional corrosion resistance and are widely used in the chemical processing industry. This resistance is generally attributed to the passive film whose properties appear dominated by the Cr/Mo contents of the alloys.

We have been studying the properties of these films as a function of applied potential, pH, temperature and solution composition using a range of electrochemical and surface analytical techniques. These techniques include polarization and voltammetric experiments, electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). In addition, we have used the measurement of oxygen reduction currents as an indicator of surface reactivity and as a probe to detect the redox transformations which occur in the oxide.

Using these techniques, it is possible to clarify the changes in the oxide film which could eventually lead to its breakdown and a susceptibility to localized corrosion. While passivity is generally attributed to the presence of a Cr(III)-dominated barrier layer, ToF SIMS shows that the segregation of oxidized Mo (and, to a lesser degree, W) to the outer regions of the film is an essential feature maintaining passivity when exposure conditions become particularly aggressive at positive potentials, low pH and high temperatures.

By combining the impedance characteristics of the oxide film and the XPS/ToF-SIMS evidence for the distribution of cationic species within the film, we have defined the redox transformations occurring in the oxide and interpreted their importance in determining the resistance of these alloys to crevice corrosion.
DI-TuP-9 Differentiation of Crystalline and Amorphous Phases in Photo-Thermo-Refractive Glass by SIMS
Mikhail Klimov (AMPAC, University of Central Florida); L.B. Glebov, L. Glebova (CREOL, University of Central Florida)
Photo-Thermo-Refractive Glass (PTRG) is a complex material combining properties of amorphous and crystalline components in the same matrix. PTRG is one of the leading photosensitive materials in holographic gratings production and is a new optical material for lasers. Even though PTRG application is quite mature, the precise way of its working is still under intense investigation. Current paper presents SIMS investigation in this question. Cs and O2 primary ions were used to generate secondary clusters that provide not only elemental but also structural information on composition of the PTRG. Crystalline phase of NaF, that presumably responsible for photosensitivity of PTRG was differentiated by appropriate choice of detected clusters from Na and F bound in amorphous matrix and its concentration was profiled in depth. Choices of secondary clusters and their sensitivity to NaF crystallinity are discussed. Results on PTRG virgin and irradiated samples as well as a holographic grating are presented.
Time Period TuP Sessions | Topic DI Sessions | Time Periods | Topics | SIMS2015 Schedule