Evaluating Silicon using Raman Microscopy

Applications | 2024 | Thermo Fisher ScientificInstrumentation
RAMAN Spectroscopy, Microscopy
Industries
Materials Testing, Semiconductor Analysis
Manufacturer
Thermo Fisher Scientific

Summary

Importance of the Topic


Silicon is a foundational material across semiconductor devices, microelectronics, lithium-ion batteries and advanced alloys. Understanding its molecular and structural properties is critical to ensure optimal performance, reliability and manufacturing quality. Raman microscopy delivers non-destructive, spatially resolved insights into chemical identity, crystallinity and mechanical strain, making it an essential analytical tool for both research and industrial quality control.

Goals and Study Overview


This application note illustrates how Raman microscopy reveals key characteristics of various silicon-based materials. The study demonstrates component identification and distribution in aluminum alloys, evaluation of silicon anode morphology, phase mapping in nickel silicide thin films, 3-D imaging of silicon nanoribbons and visualization of stress-induced strain in semiconductor nanomembranes and LOCOS structures.

Methodology and Instrumentation


Raman spectroscopy probes vibrational modes of chemical bonds and lattice phonons, producing a molecular fingerprint that shifts with changes in crystallinity and mechanical strain. Imaging mode acquires spectra at defined spatial intervals to build chemical and structural maps. Instruments employed include:
  • Thermo Scientific DXR3 Raman Microscope (532 nm excitation, confocal mode)
  • Thermo Scientific DXR3xi Raman Imaging Microscope (455 nm or 532 nm lasers, 100× or 50× metallurgical objectives)
  • Parameters such as laser power (1–6 mW), pixel sizes (0.1–1 µm) and sampling volumes tailored to sample type

Main Results and Discussion


Key findings from diverse sample types include:
  • Silicon in Aluminum Alloys: Raman imaging at 520 cm⁻¹ identified finely dispersed Si particles (3–25 wt %) in aluminum foil. Image analysis yielded size distributions (6–151 µm²) for 81 particles, informing strength and castability correlations.
  • Silicon Anode Materials: Nano-scaled silicon powders were evaluated using multivariate curve resolution. Progressive red-shifts and peak broadening of the 520 cm⁻¹ band indicated decreasing crystallinity and particle size, guiding anode design to mitigate volume expansion.
  • Nickel Silicide Thin Films: Raman peak integration at 362, 290, 215, 196 and 109 cm⁻¹ mapped monosilicide (NiSi) and residual Ni₂Si phases in MOS contacts. Spatial homogeneity and minor phase distributions were visualized after thermal processing.
  • Silicon Nanoribbons: Confocal 3-D Raman imaging of 220 nm silicon ribbons on PDMS captured peak area, position and spectral correlations. Peak shifts from 520.8 to 522.8 cm⁻¹ quantified compressive strain, while correlation maps revealed fluorescent contaminants.
  • Stress-Induced Strain in Nanomembranes and LOCOS Structures: Raman peak shift maps of a Si₀.₇₀₄Ge₀.₂₉₆ nanomembrane (41 nm) and LOCOS patterned wafers highlighted tensile or compressive strain zones. Shifts from 520.7 down to 512.4 cm⁻¹ and peak broadening identified stress gradients induced by lattice mismatch and oxide islands.

Benefits and Practical Applications


Raman microscopy offers:
  • Non-destructive chemical and structural identification at µm to sub-µm scales
  • Quantitative crystallinity assessment and strain mapping for device performance optimization
  • Rapid imaging workflows suitable for R&D, QA/QC and failure analysis
  • Cross-platform compatibility with complementary techniques (AFM, SEM)

Future Trends and Opportunities


Advancements likely include integration of operando Raman measurements in battery cycling, higher-throughput mapping for manufacturing inline inspection, deeper 3-D and correlative multimodal imaging, as well as AI-driven spectral analysis. Flexible electronics, quantum devices and next-generation power materials will benefit from enhanced spatial and temporal resolution of strain and composition.

Conclusion


This review highlights the versatility of Thermo Scientific DXR3 and DXR3xi Raman microscopes for comprehensive evaluation of silicon-based materials. From alloy inclusions to nanoscale anode powders, silicide interconnects, flexible nanoribbons and strained semiconductor layers, Raman imaging provides indispensable data on composition, crystallinity and mechanical effects. Continued expansion of methods and instrumentation will drive deeper insights in materials science and device engineering.

References


  1. Mueller MG, Fornabaio M, Zagar G, Mortensen A. Microscopic strength of silicon particles in aluminum-silicon alloy. Acta Materialia. 2016;105:165–175.
  2. USDA. How is aluminum foil made? (usda.gov).
  3. Je M, Han DY, Ryu J, Park S. Constructing pure Si anodes for advanced lithium batteries. Acc Chem Res. 2023;56:2213–2224.
  4. Sethuraman VA, Chon MJ, Shimshak M, Van Winkle N, Guduru PR. In situ measurement of biaxial modulus of Si anode for Li-ion batteries. Electrochem Commun. 2010;12:1614–1617.
  5. Lee PS, Mangelinck D, Pey KL, Shen Z, Ding J, Osipowicz T, et al. Micro-Raman spectroscopy investigation of nickel silicides and nickel (platinum) silicides. Electrochem Solid-State Lett. 2000;3(3):153–155.
  6. Chatterjee P, Pan Y, Stevens EC, Ma T, Jiang H, Dai LL. Controlled morphology of thin film silicon integrated with environmentally responsive hydrogels. Langmuir. 2013;29:6495–6501.
  7. Cavallo F, Turner KT, Lagally MG. Facile fabrication of ordered crystalline-semiconductor microstructures on compliant substrates. Adv Funct Mater. 2014;24:1730–1735.
  8. De Wolf I. Micro-Raman spectroscopy to study local mechanical stress in silicon integrated circuits. Semicond Sci Technol. 1996;11:139–154.
  9. Moroz V, Strecker N, Xu X, Smith L, Bork I. Modeling the impact of stress on silicon processes and devices. Mater Sci Semicond Process. 2003;6:27–36.
  10. Ma L, Qiu W, Fan X. Stress/strain characterization in electronic packaging by micro-Raman spectroscopy: A review. Microelectron Reliab. 2021;118:114045.
  11. Sanchez-Perez JR. Sample data provided by University of Wisconsin–Madison group.

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