2-D elemental mapping of an extreme ultraviolet-irradiated PET with a compact near edge X-ray fine structure spectromicroscopy

Abstract We present a near edge X-ray fine structure (NEXAFS) spectromicroscopy, that was developed based on a compact laboratory laser-plasma soft X-ray light source. The presented approach to spectromicroscopy is different from the usual synchrotron-based one when the series of full-field microscopy images are obtained at different energies. Herein, spatially localized NEXAFS spectra are obtained using a broad-band SXR emission, and the microscopic image is obtained by a raster scanning. The plasma is formed by the interaction of nanosecond laser pulses with a double stream gas puff target. The laser plasma source was optimized for efficient soft X-ray emission from a krypton plasma in the range ~2 nm to 5 nm wavelength radiation (energy of ~250 eV – 620 eV). This emission is used to acquire simultaneously emission and absorption spectra of soft X-ray light from the source and from the investigated sample. The spectra were acquired from a small area of PET polymer ~30 × 30 μm2 in size. A raster scanning was implemented to obtain 2-D elemental composition maps. A chemical (elemental) composition of EUV-irradiated PET was investigated. The data are in agreement with the reference measurements and the theoretical values. EUV irradiated PET spectra are showing hydrogen decrease in the PET structure due to the EUV irradiation. In the paper, a detailed information about the source, the system, the spectral measurements and the results are presented and discussed.

[1]  J. Brash,et al.  Characterization of Biomaterials by Soft X-Ray Spectromicroscopy , 2010, Materials.

[2]  C. Bittencourt,et al.  NEXAFS spectromicroscopy of suspended carbon nanohorns , 2013 .

[3]  A. Schertel,et al.  Surface analysis of partially crystalline and amorphous poly(ethylene terephthalate) samples by X-ray absorption spectroscopy (NEXAFS) , 1996 .

[4]  S. D. Stasio,et al.  Comparative NEXAFS Study on Soot Obtained from an Ethylene/ Air Flame, a Diesel Engine, and Graphite , 2006 .

[5]  H. Ade,et al.  NEXAFS imaging of synthetic organic materials , 2012 .

[6]  J. Sedlmair.  Soft x-ray spectromicroscopy of environmental and biological samples , 2011 .

[7]  Henryk Fiedorowicz,et al.  Characterization of multi-jet gas puff targets for high-order harmonic generation using EUV shadowgraphy , 2012 .

[8]  T. Harada,et al.  Development of a flat-field grazing-incidence XUV spectrometer and its application in picosecond XUV spectroscopy. , 1984, Applied optics.

[9]  Ian McNulty,et al.  Interlaced zone plate optics for hard X-ray imaging in the 10 nm range , 2017, Scientific Reports.

[10]  Harald Ade,et al.  Trends in the Carbonyl Core (C 1S, O 1S) → π*C=O Transition in the Near-Edge X-ray Absorption Fine Structure Spectra of Organic Molecules , 2002 .

[11]  A. Tivanski,et al.  Hygroscopic behavior of individual submicrometer particles studied by X-ray spectromicroscopy. , 2010, Analytical chemistry.

[12]  Cherno Jaye,et al.  NEXAFS Sensitivity to Bond Lengths in Complex Molecular Materials: A Study of Crystalline Saccharides. , 2015, The journal of physical chemistry. B.

[13]  Adam P. Hitchcock,et al.  Introduction of Soft X-Ray Spectromicroscopy as an Advanced Technique for Plant Biopolymers Research , 2015, PloS one.

[14]  I. Tanaka,et al.  Electron energy loss near-edge structures of cubic Si3N4 , 2001 .

[15]  Andrzej Bartnik,et al.  Extreme ultraviolet tomography using a compact laser-plasma source for 3D reconstruction of low density objects. , 2014, Optics letters.

[16]  Andrzej Bartnik,et al.  Simultaneous treatment of polymer surface by EUV radiation and ionized nitrogen , 2012 .

[17]  Sophie-Charlotte Gleber,et al.  Characterization of refractory organic substances by NEXAFS using a compact X-ray source , 2011, Journal of Soils and Sediments.

[18]  A. Bartnik,et al.  Physical and chemical modifications of PET surface using a laser-plasma EUV source , 2010 .

[19]  Andrzej Bartnik,et al.  Laser-plasma EUV source dedicated for surface processing of polymers , 2011 .

[20]  J. Lambert,et al.  Structural and elemental investigations of isolated aquatic humic substances using X-ray photoelectron spectroscopy , 2000, Fresenius' journal of analytical chemistry.

[21]  Andrzej Bartnik,et al.  A compact, quasi-monochromatic laser-plasma EUV source based on a double-stream gas-puff target at 13.8 nm wavelength , 2010 .

[22]  Y. Ouchi,et al.  POLARIZED NEXAFS SPECTROSCOPIC STUDIES OF POLY(BUTYLENE TEREPHTHALATE), POLY(ETHYLENE TEREPHTHALATE), AND THEIR MODEL COMPOUNDS , 1998 .

[23]  L. Lemelle,et al.  2D/3D Microanalysis by Energy Dispersive X-ray Absorption Spectroscopy Tomography , 2017, Scientific Reports.

[24]  H. Ågren,et al.  A theoretical study of the near-edge x-ray absorption spectra of some larger amino acids , 1998 .

[25]  K. Prince,et al.  X-ray spectroscopy of heterocyclic biochemicals: xanthine, hypoxanthine, and caffeine. , 2012, The journal of physical chemistry. A.

[26]  Andrzej Bartnik,et al.  Compact laser plasma EUV source based on a gas puff target for metrology applications , 2005 .

[27]  Andrzej Bartnik,et al.  Strong extreme ultraviolet emission from a double-stream xenon/helium gas puff target irradiated with a Nd:YAG laser , 2000 .

[28]  A. P. Smith,et al.  Use of near Edge X-Ray Absorption Fine Structure Spectromicroscopy to Characterize Multicomponent Polymeric Systems , 2001 .

[29]  H. Ade,et al.  NEXAFS spectromicroscopy of polymers: overview and quantitative analysis of polyurethane polymers , 1999 .

[30]  Andrzej Bartnik,et al.  A Compact “Water Window” Microscope with 60 nm Spatial Resolution for Applications in Biology and Nanotechnology , 2015, Microscopy and Microanalysis.

[31]  Kang Xia,et al.  XANES Studies of Oxidation States of Sulfur in Aquatic and Soil Humic Substances , 1998 .

[32]  D. Sparks,et al.  Soft X-ray spectromicroscopy study of mineral-organic matter associations in pasture soil clay fractions. , 2014, Environmental science & technology.

[33]  Andrzej Bartnik,et al.  Compact system for near edge X-ray fine structure (NEXAFS) spectroscopy using a laser-plasma light source. , 2018, Optics express.

[34]  Harald Ade,et al.  CALIBRATED NEXAFS SPECTRA OF SOME COMMON POLYMERS , 2003 .

[35]  Andrzej Bartnik,et al.  Spectral investigations of photoionized plasmas induced in atomic and molecular gases using nanosecond extreme ultraviolet (EUV) pulses , 2014 .

[36]  M. W. George,et al.  Energy Dispersive XAFS: Characterization of Electronically Excited States of Copper(I) Complexes , 2013, The journal of physical chemistry. B.

[37]  B. L. Henke,et al.  X-Ray Interactions: Photoabsorption, Scattering, Transmission, and Reflection at E = 50-30,000 eV, Z = 1-92 , 1993 .

[38]  Stanislaus S. Wong,et al.  Near-edge X-ray absorption fine structure spectroscopy as a tool for investigating nanomaterials. , 2006, Small.