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Nanoscale Infrared Imaging Analysis of Carbonaceous Chondrites to Understand Organic-Mineral Interactions During Aqueous Alteration

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Nanoscale Infrared Imaging Analysis of Carbonaceous Chondrites to Understand Organic-Mineral Interactions During Aqueous Alteration Nanoscale infrared imaging analysis of carbonaceous chondrites to understand organic-mineral interactions during aqueous alteration Yoko Kebukawa (癸生川 陽子)a,1, Hanae Kobayashib, Norio Urayamab, Naoki Badenb, Masashi Kondoc, Michael E. Zolenskyd, and Kensei Kobayashia aFaculty of Engineering, Yokohama National University, 240-8501 Yokohama, Japan; bNihon Thermal Consulting Co., Ltd., 160-0023 Tokyo, Japan; cInstrumental Analysis Center, Yokohama National University, 240-8501 Yokohama, Japan; and dAstromaterials Research and Exploration Science, National Aeronautics and Space Administration Johnson Space Center, Houston, TX 77058 Edited by Mark H. Thiemens, University of California at San Diego, La Jolla, CA, and approved December 6, 2018 (received for review September 19, 2018) Organic matter in carbonaceous chondrites is distributed in fine- have applied near-field IR microspectroscopy to carbonaceous grained matrix. To understand pre- and postaccretion history of chondrites and demonstrated organic-phyllosilicates associations (28, organic matter and its association with surrounding minerals, micro- 29). However, the optics and probe settings were not completely scopic techniques are mandatory. Infrared (IR) spectroscopy is a useful sufficient to detect pure near-field signals, and thus the spatial res- technique, but the spatial resolution of IR is limited to a few olution was limited to ∼1 μm. Dominguez et al. (34) reported on micrometers, due to the diffraction limit. In this study, we applied submicron (∼20 nm) mineral identification of the Murchison mete- the high spatial resolution IR imaging method to CM2 carbonaceous orite and a cometary dust particle with near-field IR imaging using chondrites Murchison and Bells, which is based on an atomic force suitable background (i.e., nonnear-field scatterings) suppression, but – −1 microscopy (AFM) with its tip detecting thermal expansion of a the wavelength (wavenumber) range was limited to 800 1,100 cm , sample resulting from absorption of infrared radiation. We confirmed which did not cover characteristic organic absorptions. that this technique permits ∼30 nm spatial resolution organic analysis Alternatively, a high spatial resolution IR imaging technique that for the meteorite samples. The IR imaging results are consistent with detects photothermal-induced resonance using a tunable laser combined with an atomic force microscope was recently de- the previously reported association of organic matter and phyllosili- EARTH, ATMOSPHERIC, veloped and applied to various research fields (35–37). When AND PLANETARY SCIENCES cates, but our results are at much higher spatial resolution. This ob- light is absorbed by the sample, the temperature increase causes servation of heterogeneous distributions of the functional groups of ∼ a characteristic thermal expansion. This thermal expansion drives organic matter revealed its association with minerals at 30 nm spa- the cantilever into oscillation. The oscillation amplitude of the tial resolution in meteorite samples by IR spectroscopy. cantilever is directly proportional to the amount of light absor- bed. The technique covers full mid-IR including ranges for or- meteorites | IR spectroscopy | AFM-IR | organic matter ganic absorption features. Here we report IR imaging analyses of carbonaceous chondrites by atomic force microscopy-based infrared rimitive extraterrestrial materials such as carbonaceous chon- spectroscopy (AFM-IR) that provides IR imaging with spatial Pdrites contain diverse organic matter (OM). Although distinct resolution far below conventional optical diffraction limits. organic grains called “nanoglobules” 100 nm to 1 μminsizeare often found in primitive carbonaceous chondrites (1, 2), they consist Results of roughly 10% or less of the total organics in chondrites (3). The Murchison Meteorite. IR absorption spectra (Fig. 1 A and B)of remaining organics are smaller than nanoglobules and distributed in the Murchison meteorite were obtained using the nano-IR at a fine-grained matrix. To understand pre- and postaccretion history of OM and its interaction with associated minerals, microscopic Significance techniques are mandatory. Scanning electron microscope obser- vation with osmium labeling has demonstrated that OM in car- Spatial relationships between organic matter and minerals are bonaceous chondrites is associated with clay minerals, which may necessary for understanding the formation and evolution of or- have had important trapping and possibly catalytic roles in the ganic matter during aqueous and thermal alteration in their par- evolution of organics in the early solar system (4). ent bodies, as well as preaccretional history. Infrared spectroscopy To obtain molecular structure information at the submicron is a powerful tool to analyze the molecular structures of organic scale, scanning transmission X-ray microscopy (STXM) com- matter and identification of minerals. However, its spatial reso- bined with carbon X-ray absorption near-edge structure spec- lution is limited due to the diffraction limit. Recently, the atomic troscopy (C-XANES) is so far the most suitable method. The force microscopy (AFM) based IR nanospectroscopy was de- STXM with C-XANES provides molecular structure information veloped and applied in various scientific fields to overcome the at the ∼40 nm spatial resolution and is often applied to various extraterrestrial materials including carbonaceous chondrites (5– diffraction limit of IR. We applied the AFM-based IR nano- spectroscopy to carbonaceous chondrites and studied organic- 12), Antarctic micrometeorites (13, 14), interplanetary dust ∼ particles (IDPs) (15, 16), and cometary particles recovered from mineral associations at the 30 nm spatial resolution. Comet 81P/Wild 2 by the Stardust mission (17–20). Fourier transform infrared (FTIR) microspectroscopy is a Author contributions: Y.K. designed research; Y.K., H.K., and M.K. performed research; – H.K., N.U., and N.B. contributed new reagents/analytic tools; Y.K. analyzed data; and Y.K., well-established technique for extraterrestrial materials (15 17, M.E.Z., and K.K. wrote the paper. 21–27), as well as imaging analyses (28–32). IR spectroscopy The authors declare no conflict of interest. provides information about not only molecular structures of OM similar to C-XANES, but also mineral identification, and thus This article is a PNAS Direct Submission. could be a complementary method to STXM/C-XANES. How- Published under the PNAS license. ever, the spatial resolution of IR is limited to a few micrometers 1To whom correspondence should be addressed. Email: [email protected]. (roughly equal to wavelength) due to the diffraction limit. The This article contains supporting information online at www.pnas.org/lookup/suppl/doi:10. scanning near-field optical microscopy technique allows one to 1073/pnas.1816265116/-/DCSupplemental. obtain IR spectra at submicrometer spatial resolution (33). We www.pnas.org/cgi/doi/10.1073/pnas.1816265116 PNAS Latest Articles | 1of6 Downloaded by guest on September 25, 2021 locations indicated in Fig. 1C. The IR spectra indicated in red − showed absorption bands at ∼3,400 and 1,640 cm 1, and are assigned to structural and/or absorbed H Oofhydroussilicatesat − 2 2,960, 2,930, and 2,860 cm 1; assigned to the aliphatic C–H − − stretching modes at around 1,435 cm 1; assigned to CO 2 of − − 3 carbonates at around 1,150 cm 1;assignedtoSO2 of sulfates; − 4 and at around 1,000 cm 1, assigned to the Si-O stretching modes of silicates. The spot in green (Fig. 1C) was dominated by sulfates with lesser silicates, and spots in blue are mainly silicates with less OH and sulfates. These features were mostly consistent with the IR spectra of the Murchison meteorite obtained with conventional micro-FTIR (Fig. 2) (38). However, the nano-IR spectra reflected more local characteristics, e.g., a spot with abundant aliphatic CH and sulfates that are less significant in the conventional micro- FTIR spectra obtained for larger areas (100 × 100 μm2). Fig. 3 shows 3 × 3 μm2 IR absorption maps with the IR source − − tunedto1,000cm1 corresponding to SiO, 1,150 cm 1 correspond- − − ing to sulfates, 1,730 cm 1 corresponding to C = O, 2,920 cm 1 −1 corresponding to aliphatic CH2, 2,960 cm corresponding to −1 aliphatic CH3, and 3,400 cm corresponding to OH. Some part of the silicates (Fig. 3A, Lower Right) overwrapped with the OH-rich area that indicated phyllosilicates. Fig. 4 shows the CH2/ −1 CH3 peak intensity ratio map generated from 2,920 cm (CH2) −1 map and 2,960 cm (CH3) map after image shift correction using the AFM image. Bells Meteorite. IR absorption spectra (Fig. 5 A and B) of the Bells meteorite were obtained using the nano-IR at locations indicated in Fig. 2. IR spectra of Murchison and Bells meteorites obtained using a con- Fig. 5C. None of the five points showed the OH absorption band in ventional micro-FTIR (38). this area. One of these points showed dominant absorptions at − around 2,950 cm 1 assigned to aliphatic C–H, as well as at − − ∼1,730 cm 1 assigned to C = O, ∼1,600 cm 1 assigned to aromatic Discussion − − C = C, at around 1,450 cm 1 assigned to carbonates, at ∼1,200 cm 1 Spatial Resolution. The diffraction limit is roughly equivalent to the − − − assigned to sulfates and/or C–O, and at ∼950 cm 1 assigned to wavelength, e.g., ∼3.3 μmat3,000cm 1 and ∼10 μmat1,000cm 1. silicates. The other spots showed dominant silicate peaks at around Point spectra a few micrometer-sized areas from our meteorite −1 −1 1,000 cm , and some peaks at 1,450, 1,200, and 1,150 cm .The samples (Figs. 1 and 5) clearly showed that the spatial resolution in nano-IR spectra did not resemble the IR spectra of the Bells me- our nano-IR analysis was beyond the diffraction limit. The IR maps teorite obtained by the conventional technique (Fig. 2), probably (Figs. 3 and 6) also confirmed that the actual spatial resolution was due to heterogeneities of the meteorite since the analyzed area was at least 30 nm, e.g., based on the C = O hot spot in the Murchison × μ 2 only 2 1 m .
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