Atomic force microscope infrared spectroscopy on 15 nm scale polymer nanostructures

Felts, Jonathan R.; Cho, Han Na; Yu, Min; Bergman, Lawrence A.; Vakakis, Alexander F.; King, William P.

doi:10.1063/1.4793229

Cited by 39 publications

(36 citation statements)

References 41 publications

(47 reference statements)

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“…The ringdown signal was observed at 1340 ± 200 kHz to reduce signal of the AFM cantilever due to pronounced ambient thermal effects at fundamental frequency modes. 53 For AFM-IR imaging, a spatial resolution of 25-100 nm has been previously demonstrated using these conditions. 13,14 In comparison, the spatial resolution for a typical transmission FTIR measurement over a similar wavenumber range is 3-10 microns.…”

Section: Methodsmentioning

confidence: 99%

Nanoscale Chemical-Mechanical Characterization of Nanoelectronic Low-kDielectric/Cu Interconnects

Lo¹,

Dazzi

Marcott³

et al. 2015

ECS J. Solid State Sci. Technol.

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Combined nanoscale chemical and mechanical property characterization has largely been limited by the inability to extend chemical structure identification techniques such as infrared (IR) absorption spectroscopy into the nanometer regime due to diffraction limitations. The recent development of atomic force microscope (AFM) based IR spectroscopy (AFM-IR) has now enabled infrared chemical spectroscopy with resolution well below the diffraction limit. However, the combination of AFM-IR with other AFM based techniques to achieve nanoscale chemical structure-mechanical property characterization has yet to be demonstrated. In this regard, we have combined AFM-IR chemical and contact resonance AFM (CR-AFM) mechanical measurements in the investigation of low dielectric constant (low-k) / Cu damascene structures fabricated using a 90 nm interconnect process technology. We show that the combined AFM-IR and CR-AFM results can be utilized to perform nanoscale chemical-mechanical characterization of both the nano-patterned metal and the low-k dielectric whose mechanical properties are sensitive to chemical modification by the interconnect fabrication process. The continued drive to seek and exploit new materials and phenomena at nanometer dimensions has increased the demand for metrologies capable of characterizing both chemical structure and physical properties at the nanoscale. The nanoelectronics industry in particular has identified metrologies capable of performing nanoscale structureproperty measurements on new materials and devices as an area of critical need in their industry technology roadmap.1,2 Such requirements for nanoscale physical property characterization have readily been met by the development of a range of scanned probe techniques capable of assessing the thermal, 3,4 mechanical, 5,6 and electrical 7,8 properties of materials at the nanoscale. 9 However, the development of nanoscale chemical structure metrologies has been hindered by the difficulty of scaling popular micron-scale techniques such as infrared (IR) absorption spectroscopy [10][11][12] into the nanometer regime due to diffraction limits defined by the Rayleigh equation.13,14 To overcome these limitations, a number of approaches combining optical spectroscopy with scanned probe microscopy (SPM) have been proposed and demonstrated. [13][14][15][16][17][18][19][20] Of these, the atomic force microscope (AFM) IR technique, which is based on photothermally induced resonance (PTIR), 21,22 has recently garnered significant interest due to a demonstrated spatial resolution of 25-100 nm, and a close correlation to micron-scale Fourier transform infrared (FTIR) spectroscopy. 13,14 This combination has resulted in the utilization of AFM-IR in a number of biological, 23-25 polymeric, 26-28 and semiconductor [29][30][31] applications. However, AFM-IR and related techniques have yet to be routinely combined with other AFM based techniques to achieve the ultimate goal of nanoscale structure-property characterization. In this regard, we provide a compelling...

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Section: Methodsmentioning

confidence: 99%

Nanoscale Chemical-Mechanical Characterization of Nanoelectronic Low-kDielectric/Cu Interconnects

Lo¹,

Dazzi

Marcott³

et al. 2015

ECS J. Solid State Sci. Technol.

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“…In keeping with previous reports of AFM-IR analysis for nanofilm specimens, the maximum peak-to-peak probe deflection was recorded. 47 Despite the small sampling volume, AFM-IR spectra displayed peak positions and shapes which closely match the fingerprint region of bulk ATR FTIR spectra, AFM-IR mapping was performed to provide a detailed picture of chemical heterogeneity.…”

Section: Afm-ir Analysismentioning

confidence: 99%

Insights into Epoxy Network Nanostructural Heterogeneity Using AFM-IR

Morsch

Liu

Lyon

et al. 2015

ACS Appl. Mater. Interfaces

108

115

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The first direct observation of a chemically heterogeneous nanostructure within an epoxy resin is reported. Epoxy resins comprise the matrix component of many high performance composites, coatings and adhesives, yet the molecular network structure that underpins the performance of these industrially essential materials is not well understood. Internal nodular morphologies have repeatedly been reported for epoxy resins analysed using SEM or AFM, yet the origin of these features remains a contentious subject, and epoxies are still commonly assumed to be chemically homogeneous. Uniquely, in this contribution we use the recently developed AFM-IR technique to eliminate previous differences in interpretation, and establish that nodule features correspond to heterogeneous network connectivity within an epoxy phenolic formulation.

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“…Because the PTIR signal varies both in time and frequency (Figure 6), noise can be reduced by applying a time-frequency signal transformation (such as the Morlet wavelet transform) and by filtering the signal for times longer than the cantilever ring down and for frequencies not corresponding to the cantilever bending modes (119,120). By virtue of reduced noise, this method yields a 32-fold reduction in the need for pulse averaging (120), resulting in a corresponding throughput increase.…”

Section: Photothermal-induced Resonancementioning

confidence: 97%

“…PTIR characterization has been applied to investigate a wide array of samples including bacteria (28,29,(103)(104)(105)(106), cells (107)(108)(109)(110), lipids (111), proteins (112), polymers (30,(113)(114)(115)(116)(117)(118)(119)(120)(121), drugs (122,123), quantum dots (124), plasmonic nanostructures (97,(125)(126)(127), metal-organic frameworks (128), and organo-trihalide perovskites (129). PTIR setups require a pulsed, spectrally narrow, wavelength-tunable laser source; an AFM tip operating in contact mode; and far-field optics to focus light under the tip.…”

Section: Photothermal-induced Resonancementioning

confidence: 99%

Infrared Imaging and Spectroscopy Beyond the Diffraction Limit

Centrone

2015

Annual Rev. Anal. Chem.

234

275

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Progress in nanotechnology is enabled by and dependent on the availability of measurement methods with spatial resolution commensurate with nanomaterials' length scales. Chemical imaging techniques, such as scattering scanning near-field optical microscopy (s-SNOM) and photothermal-induced resonance (PTIR), have provided scientists with means of extracting rich chemical and structural information with nanoscale resolution. This review presents some basics of infrared spectroscopy and microscopy, followed by detailed descriptions of s-SNOM and PTIR working principles. Nanoscale spectra are compared with far-field macroscale spectra, which are widely used for chemical identification. Selected examples illustrate either technical aspects of the measurements or applications in materials science. Central to this review is the ability to record nanoscale infrared spectra because, although chemical maps enable immediate visualization, the spectra provide information to interpret the images and characterize the sample. The growing breadth of nanomaterials and biological applications suggest rapid growth for this field.

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Atomic force microscope infrared spectroscopy on 15 nm scale polymer nanostructures

Cited by 39 publications

References 41 publications

Nanoscale Chemical-Mechanical Characterization of Nanoelectronic Low-kDielectric/Cu Interconnects

Nanoscale Chemical-Mechanical Characterization of Nanoelectronic Low-kDielectric/Cu Interconnects

Insights into Epoxy Network Nanostructural Heterogeneity Using AFM-IR

Infrared Imaging and Spectroscopy Beyond the Diffraction Limit

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