Review—Laser Ablation Ionization Mass Spectrometry (LIMS) for Analysis of Electrodeposited Cu Interconnects

Grimaudo, Valentine; Moreno‐García, Pavel; Riedo, Andreas; López, Alena Cedeño; Tulej, Marek; Wiesendanger, Reto; Würz, Peter; Broekmann, Peter

doi:10.1149/2.0221901jes

Cited by 17 publications

(12 citation statements)

References 73 publications

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“…Hence, the signal variations along depth can be used to isolate local inhomogeneity providing that applied laser power densities are sufficiently stable in the course of the specific measurement campaign. Our laboratory studies indicate that with a depth resolution in the sub‐micrometer range, regions of interests, such as individual mineralogical grains or mineralogical layers, can be detected relatively easily within the sample illustrating the high sensitivity of our miniature LIMS system 28,29,34,35,39 …”

Section: Methodsmentioning

confidence: 82%

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Isotope abundance ratio measurements using femtosecond laser ablation ionization mass spectrometry

et al. 2020

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Accurate isotope ratio measurements are of high importance in various scientific fields, ranging from radio isotope geochronology of solids to studies of element isotopes fractionated by living organisms. Instrument limitations, such as unresolved isobaric inferences in the mass spectra, or cosampling of the material of interest together with the matrix material may reduce the quality of isotope measurements. Here, we describe a method for accurate isotope ratio measurements using our laser ablation ionization time-of-flight mass spectrometer (LIMS) that is designed for in situ planetary research. The method is based on chemical depth profiling that allows for identifying micrometer scale inclusions embedded in surrounding rocks with different composition inside the bulk of the sample. The data used for precise isotope measurements are improved using a spectrum cleaning procedure that ensures removal of low quality spectra. Furthermore, correlation of isotopes of an element is used to identify and reject the data points that, for example, do not belong to the species of interest. The measurements were conducted using IR femtosecond laser irradiation focused on the sample surface to a spot size of 12 μm. Material removal was conducted for a predefined number of laser shots, and time-of-flight mass spectra were recorded for each of the ablated layers. Measurements were conducted on NIST SRM 986 Ni isotope standard, trevorite mineral, and micrometer-sized inclusions embedded in aragonite. Our measurements demonstrate that element isotope ratios can be measured with accuracies and precision at the permille level, exemplified by the analysis of B, Mg, and Ni element isotopes. The method applied will be used for in situ investigation of samples on planetary surfaces, for accurate quantification of element fractionation induced by, for example, past or present life or by geochemical processes.

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Section: Methodsmentioning

confidence: 82%

“…Our laboratory studies indicate that with a depth resolution in the sub-micrometer range, regions of interests, such as individual mineralogical grains or mineralogical layers, can be detected relatively easily within the sample illustrating the high sensitivity of our miniature LIMS system. 28,29,34,35,39…”

Section: Depth Profiling Analysismentioning

confidence: 99%

Isotope abundance ratio measurements using femtosecond laser ablation ionization mass spectrometry

et al. 2020

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“…For the analysis of sample purity, several analytical methodologies combined with depth profiling were developed. They are summarised in detail in a recent comprehensive review [184].…”

Section: Semiconductor Industrymentioning

confidence: 99%

Current Progress in Femtosecond Laser Ablation/Ionisation Time-of-Flight Mass Spectrometry

et al. 2021

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The last decade witnessed considerable progress in the development of laser ablation/ionisation time-of-flight mass spectrometry (LI-TOFMS). The improvement of both the laser ablation ion sources employing femtosecond lasers and the method of ion coupling with the mass analyser led to highly sensitive element and isotope measurements, minimisation of matrix effects, and reduction of various fractionation effects. This improvement of instrumental performance can be attributed to the progress in laser technology and accompanying commercialisation of fs-laser systems, as well as the availability of fast electronics and data acquisition systems. Application of femtosecond laser radiation to ablate the sample causes negligible thermal effects, which in turn allows for improved resolution of chemical surface imaging and depth profiling. Following in the footsteps of its predecessor ns-LIMS, fs-LIMS, which employs fs-laser ablation ion sources, has been developed in the last two decades as an important method of chemical analysis and will continue to improve its performance in subsequent decades. This review discusses the background of fs-laser ablation, overviews the most relevant instrumentation and emphasises their performance figures, and summarizes the studies on several applications, including geochemical, semiconductor, and bio-relevant materials. Improving the chemical analysis is expected by the implementation of laser pulse sequences or pulse shaping methods and shorter laser wavelengths providing current progress in mass resolution achieved in fs-LIMS. In parallel, advancing the methods of data analysis has the potential of making this technique very attractive for 3D chemical analysis with micrometre lateral and sub-micrometre vertical resolution.

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“…In this work, we employ a collinear (same axis of propagation) depth profiling laser system with two temporally separated pulses for the Laser Ablation Ionization Mass Spectrometry (LIMS) technique with our miniature reflectron‐type TOF mass analyzer designed for space applications 12,26–29 . The implemented double‐pulse (DP) method increases the ionization efficiencies of the LA process, which results in higher spatial resolution in depth profiling experiments.…”

Section: Introductionmentioning

confidence: 99%

UV post‐ionization laser ablation ionization mass spectrometry for improved nm‐depth profiling resolution on Cr/Ni reference standard

Grimaudo

Tulej

Riedo

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale Laser ablation combined with mass spectrometry forms a promising tool for chemical depth profiling of solids. At irradiations near the ablation threshold, high depth resolutions are achieved. However, at these conditions, a large fraction of ablated species is neutral and therefore invisible to the instrument. To compensate for this effect, an additional ionization step can be introduced. Methods Double‐pulse laser ablation is frequently used in material sciences to produce shallow craters. We apply double‐pulse UV femtosecond (fs) Laser Ablation Ionization Mass Spectrometry to investigate the depth profiling performance. The first pulse energy is set to gentle ablation conditions, whereas the second pulse is applied at a delay and a pulse energy promoting the highest possible ion yield. Results The experiments were performed on a Cr/Ni multi‐layered standard. For a mean ablation rate of ~3 nm/pulse (~72 nJ/pulse), a delay of ~73 ps provided optimal results. By further increasing the energy of the second pulse (5–30% higher with respect to the first pulse) an enhancement of up to 15 times the single pulse intensity was achieved. These conditions resulted in mean depth resolutions of ~37 and ~30 nm for the Cr and Ni layers, respectively. Conclusions It is demonstrated on the thin‐film standard that the double‐pulse excitation scheme substantially enhances the chemical depth profiling resolution of LIMS with respect to the single‐pulse scheme. The post‐ionization allows for extraordinarily low ablation rates and for quantitative and stoichiometric analysis of nm‐thick films/coatings.

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Review—Laser Ablation Ionization Mass Spectrometry (LIMS) for Analysis of Electrodeposited Cu Interconnects

Cited by 17 publications

References 73 publications

Isotope abundance ratio measurements using femtosecond laser ablation ionization mass spectrometry

Isotope abundance ratio measurements using femtosecond laser ablation ionization mass spectrometry

Current Progress in Femtosecond Laser Ablation/Ionisation Time-of-Flight Mass Spectrometry

UV post‐ionization laser ablation ionization mass spectrometry for improved nm‐depth profiling resolution on Cr/Ni reference standard

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