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DOE OSTI2016

Supercontinuum Fourier transform spectrometry with balanced detection on a single photodiode

We demonstrate a method of combining a supercontinuum light source with a commercial Fourier transform spectrometer, using a novel approach to dual-beam balanced detection, implemented with phase-sensitive detection on a single light detector. A 40 dB reduction in the relative intensity noise is achieved for broadband light, analogous to conventional balanced detection methods using two matched photodetectors. Unlike conventional balanced detection, however, this method exploits the time structure of the broadband source to interleave signal and reference pulse trains in the time domain, recording the broadband differential signal at the fundamental pulse repetition frequency of the supercontinuum. The method is capable of real-time correction for instability in the supercontinuum spectral structure over a broad range of wavelengths and is compatible with commercially designed spectrometers. A proof-of-principle experimental setup is demonstrated for weak absorption in the 1500-1600 nm region.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1973

A high-resolution Fourier-transform infrared spectrometer.

We have developed a Fourier-transform infrared spectrometer having a resolution of 0.5/cm over the range of wavelength from 1 to 5.5 microns. It has been used to observe the sun over this wavelength range from a Lear Jet flying at an altitude of 14 km, and to observe a number of stars from the ground, using the 229-cm telescope of the Steward Observatory and the 152-cm aluminum-mirror telescope at the Observatorio Astronomico Nacional in the Sierra de San Pedro Martir, Baja California, Mexico. The solar spectrum is given here, while the ground-based spectra are being published separately.

Johnson, H. L.↗

NASA NTRS2003

High Resolution Spectroscopy to Support Atmospheric Measurements

Spectroscopic parameters (such as line position, intensity, broadening and shifting coefficients and their temperature dependences, line mixing coefficients etc.) for various molecular species of atmospheric interest are determined. In order to achieve these results, infrared spectra of several molecular bands are obtained using high-resolution recording instruments such as tunable diode laser spectrometer and Fourier transform spectrometers. Using sophisticated analysis routines (Multispectrum nonlinear least squares technique) these high-resolution infrared spectra are processed to determine the various spectral line parameters that are cited above. Spectra were taken using the McMath-Pierce Fourier transform spectrometer (FTS) at the National Solar Observatory on Kitt Peak, Arizona as well as the Bruker FTS at the Pacific Northwest National Laboratory (PNNL) at Richland, Washington. Most of the spectra are acquired not only at room temperature, but also at several different cold temperatures. This procedure is necessary to study the variation of the spectral line parameters as a function of temperature in order to simulate the Earth's and other planetary atmospheric environments. Depending upon the strength or weakness of the various bands recorded and analyzed, the length(s) of the absorption cells in which the gas samples under study are kept varied from a few centimeters up to several meters and the sample temperatures varied from approximately +30 C to -63 C. Research on several infrared bands of various molecular species and their isotopomers are undertaken. Those studies are briefly described.

Venkataraman, Malathy Devi↗

NASA NTRS1997

Determination of Spectroscopic Properties of Atmospheric Molecules from High Resolution Vacuum Ultraviolet Cross Section and Wavelength Measurements

An account is given of progress during the period 8/l/96-7/31/97 on work on (a) cross section measurements of O2 S-R using a Fourier transform spectrometer (FTS) at the Photon Factory in Japan; (b) the determination of the predissociation linewidths of the Schumann-Runge bands (S-R) of 02; (c) cross section measurements of 02 Herzberg bands using a Fourier transform spectrometer (FTS) at Imperial College; and (d) cross section measurements of H2O in the wavelength region 120-188 nm. The experimental investigations are effected at high resolution with a 6.65 m scanning spectrometer and with the Fourier transform spectrometer. Below 175 nm, synchrotron radiation is most suitable for cross section measurements in combination with spectrometers at the Photon Factory Japan. Cross section measurements of the Doppler limited bands depend on using the very high resolution, available with the Fourier transform spectrometer, (0.025/cm resolution). All of these spectroscopic measurements are needed for accurate calculations of the production of atomic oxygen, the penetration of solar radiation into the Earth's atmosphere, and photochemistry of minor molecules.

Parkinson, W. H.↗

NASA NTRS2011

Fast Imaging Detector Readout Circuits with In-Pixel ADCs for Fourier Transform Imaging Spectrometers

Focal plane arrays (FPAs) with high frame rates and many pixels benefit several upcoming Earth science missions including GEO-CAPE, GACM, and ACE by enabling broader spatial coverage and higher spectral resolution. FPAs for the PanFTS, a high spatial resolution Fourier transform spectrometer and a candidate instrument for the GEO-CAPE mission are the focus of the developments reported here, but this FPA technology has the potential to enable a variety of future measurements and instruments. The ESTO ACT Program funded the developed of a fast readout integrated circuit (ROIC) based on an innovative in-pixel analog-to-digital converter (ADC). The 128 X 128 pixel ROIC features 60 ?m pixels, a 14-bit ADC in each pixel and operates at a continuous frame rate of 14 kHz consuming only 1.1 W of power. The ROIC outputs digitized data completely eliminating the bulky, power consuming signal chains needed by conventional FPAs. The 128 X 128 pixel ROIC has been fabricated in CMOS and tested at the Jet Propulsion Laboratory. The current version is designed to be hybridized with PIN photodiode arrays via indium bump bonding for light detection in the visible and ultraviolet spectral regions. However, the ROIC design incorporates a small photodiode in each cell to permit detailed characterization of the ROICperformance without the need for hybridization. We will describe the essential features of the ROIC design and present results of ROIC performance measurements.

focal plane arrays (FPAs)↗

DOE OSTI2018

Early Stage Detection of Stress Due to Copper on Maize (Zea mays L.) by Laser-Induced Fluorescence and Infrared Spectroscopy

Laser-induced fluorescence (LIF) and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy has been applied for the nondestructive, label free, and rapid analyses of the impact of copper (25, 50, and 75 μM) on maize seedlings at an early stage before the changes appear visually on the plant. The LIF measurement has been used to detect the signs of stress in the photosynthetic pigment. The integrated areal intensity and increasing fluorescence intensity ratios indicate decrease in the photosynthetic pigments in the leaves of maize plants stressed with copper. The ATR-FTIR technique has been utilized to estimate the changes arising in the cell wall polysaccharides, amino acid, secondary structure of protein and lipid content of the leaves of control and copper-treated maize seedlings. The second derivative and curve fitting analyses have been applied for the enhancement of the spectral variations and quantitative estimation of the changes arising in the biochemical profile. The result shows an increase in the pectin, lignin, amino acid, and protein content and reduction in the amount of cellulose and lipid in the leaves of maize seedlings due to the treatment of copper. This study indicates the toxic response of copper by hampering the growth and reduction in the photosynthetic pigments and biochemical content of the maize seedlings. This study also demonstrates the feasibility of the spectroscopic techniques (LIF and ATRFTIR) as a rapid, label free, and nondestructive probe for the assessment of stress and monitoring of crops.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Photoluminescent and Thermoluminescent Studies of Dy{sup 3+} and Eu{sup 3+} Doped Y{sub 2}O{sub 3} Phosphors

Eu{sup 3+} doped and Dy{sup 3+} codoped yttrium oxide (Y{sub 2}O{sub 3}) phosphors have been prepared using solid-state reaction technique (SSR). The prepared phosphors were characterized by X-ray diffractometer (XRD), energy dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM) and Fourier transforms infrared spectroscopy (FTIR) techniques. Photoluminescence (PL) and Thermoluminescence (TL) properties were studied in detail. PL emission spectra were recorded for prepared phosphors under excitation wavelength 254 nm, which show a high intense peak at 613 nm for Y{sub 2}O{sub 3}:Dy{sup 3+}, Eu{sup 3+} (1:1.5 mol %) phosphor. The correlated color temperature (CCT) and CIE analysis have been performed for the synthesized phosphors. TL glow curves were recorded for Eu{sup 3+}doped and Dy{sup 3+}codoped phosphors to study the heating rate effect and dose response. The kinetic parameters were calculated using peak shape method for UV and γ exposures through computerized glow curve deconvolution (CGCD) technique. The phosphors show second order kinetics and activation energies varying from 5.823 × 10{sup − 1} to 18.608 × 10{sup − 1} eV.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

Polyaniline-Modified TiO{sub 2}, a Highly Effective Photo-catalyst for Solid-Phase Photocatalytic Degradation of PVC

A series of polyaniline-modified TiO{sub 2} photo-catalysts (TiO{sub 2}@PANI) were prepared via an in-situ polymerization of aniline onto TiO{sub 2} nanoparticles. The Fourier-transform infrared spectroscopy (FT-IR) and thermogravimetric analyses (TGA) confirmed that the polyaniline (PANI) successfully grafted on the TiO{sub 2} NPs. The X-ray diffraction (XRD) patterns showed that the crystalline structure of the TiO{sub 2} did not change during the preparation of PANI. Photodegradable nanocomposites were prepared by embedding the photocatalysts into the commercial poly(vinyl chloride) (PVC) samples. The nanocomposite films were compared against pure PVC and PVC-TiO{sub 2} films for their photodegradation performances. The photocatalytic activity of the TiO{sub 2}@PANI catalysts improved with an increase in the inorganic/organic molar ratio. With the TiO{sub 2} aniline molar ratio of 10, the PVC-TiO{sub 2}@PANI nanocomposite film lost about 67% of its weight after 720 h irradiation under UV. Meanwhile, the pure PVC and PVC-TiO{sub 2} control films lost about 12 and 45% of their initial weights, respectively. Results showed that the rate at which the PVC is photodegraded can be controlled by the amount of the TiO{sub 2} NPs as well as the initial TiO{sub 2} aniline molar ratio. The SEM micrograms indicated a rougher and more porous surface for the irradiated PVC-TiO{sub 2}@PANI compared with controls. .

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Effect of Alkali Treatment on Mechanical and Morphological Properties of Pineapple Leaf Fibre/Polyester Composites

In this study, our aim is to analyze the influence of fibre treatments and different fibre loading on mechanical, physical and chemical properties of pineapple leaf fibre reinforced polyester composites (PALF/PE). Fibre treatments were carried out with 1 N NaOH and KOH for 1 h. The untreated and treated PALF/PE composites were fabricated with 25 wt%, 35 wt% and 45 wt% fibre loadings by compression molding technique. Fourier Transform Infrared Spectroscopy (FTIR) was used to understand the effects of chemical treatment on PALF mechanical test results revealed that 45 wt% of PALF/PE composites treated with NaOH showed a 35% increase in tensile strength compared to untreated PALF/PE composites. The tensile modulus and the flexural module are also the highest at 45 wt% of KOH treated composites. The highest impact strength of 70 J/m was obtained for PALF/PE composites with NaOH treated fibres at 25% fibre loading. The results show that the fibre treatments in terms of the flexural and inter-laminar shear strength of composites were not effective. SEM of the tensile fractured specimen of PALF/PE composites revealed the changes in fibre characteristics due to the alkali treatment and less fibre pull-out at higher fibre loading. Overall we conclude that 1 N NaOH, 45 wt% treated PALF/PE composites satisfactorily and effectively improved both the mechanical and morphological properties. Obtained composites would be promising for construction materials, furniture and automotive components due to their superior strength and modulus at higher fibre loading.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Novel Biocide Based on Cationic Derivative of Psyllium: Surface Modification and Antibacterial Activity

To circumvent the problems (such as volatilization, photolytic decomposition, chemical instability, easy permeability through the skin) associated with low molecular weight antimicrobial agents, our strategy employed graft copolymerization of cationic monomer with the polymeric substrate viz. psyllium husk. The surface graft concentration of quaternary ammonium ion on psyllium was optimized by measuring the extent of grafting in the microwave-induced process. The surface modification of graft copolymers was evident by different physico–chemical techniques like {sup 13}C nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), X-ray diffractometer (XRD), differential scanning calorimetry (DSC), Thermo gravimeteric analysis (TGA), and viscometric study. The synthesized water soluble product resulted good antibacterial activity against Gram positive Staphylococcus aureus and Bacillus anthracis but failed to produce any antibacterial activity against Gram negative Salmonella typhi and Escherichia coli. The reason to failure has been explained on the basis of differences in the electrokinetic property between Gram-positive and Gram-negative bacteria. Optimum minimum inhibitory concentration (MIC) for the polymeric grade which showed good biocidal effect evaluated by both zone of inhibition and absorbance is found at 1000 µg/ml.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Adsorption of Iron(III) and Copper(II) by Bacterial Cellulose from Rhodococcus sp. MI 2

Modified cellulose from the pellicle produced by Rhodococcus sp. MI 2 was more efficient at removing Fe(III) and Cu(II) from aqueous solution than similarly modified cellulose from Komagataeibar xylinus TISTR 998. This study first describes the modification of the cellulose to produce mercerized bacterial cellulose (MBC), phosphorylated bacterial cellulose (PBC), acid–base cellulose and diethylenetriamine bacterial cellulose (EABC). Their efficacy as adsorbents to adsorb Fe(III) and Cu(II) was then determined. In aqueous solution at pH 4 at initial Fe(III) concentration of 20 mg/L, PBC reached adsorption equilibrium within 195 min. At pH 5 in an initial Cu(II) concentration of 75 mg/L, EABC reached adsorption equilibrium within 210 min. Molecular structures and chemical bonds were examined by Fourier transform infrared spectroscopy (FT-IR) and physical morphologies by scanning electron microscopy. The adsorption kinetics of MBC, PBC and EABC showed good agreement with the proposed pseudo-second order model and the adsorption isotherm was best described by the Freundlich model. Our study determined optimal conditions, molecular structures, physical morphologies and adsorption kinetics. The cellulose produced by the new strain Rhodococcus sp. MI 2 was highly efficient at adsorbing and removing metal ions from aqueous solution.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Effect of Nanoclay Addition on the Biodegradability and Performance of Starch-Based Nanocomposites as Mulch Films

The biodegradation and performance of potential agricultural mulch films prepared from native and oxidized corn starch nanocomposites with chitosan-modified bentonite were studied under simulated soil test conditions. Samples were removed at different times and their wet and dry weights were registered. A photographic register of films appearance was also included. Bio-physicochemical changes along biodegradation progress were followed by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TG). Results indicate that all samples degraded in a three step process and that they almost fully degrade by 100 days of testing. The chemical modification of starch and the addition of fillers did not produce significant differences in biodegradation rate. Microbial attack, mainly by fungal microorganisms started at the end of the first week and produced a 50% weight loss in approximately 35 days. Biological assays indicate that germination was negatively affected by proposed starch-based films.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Effect of Annealing Temperature on Structural, Morphological, Optical and Magnetic Properties of NiFe{sub 2}O{sub 4} Thin Films

Nickel ferrite (NiFe{sub 2}O{sub 4}) thin films have been deposited on glass substrates by a chemical spray pyrolysis technique at 350 {sup ∘}C substrate temperature. The deposited films were annealed at four different temperatures (400, 450, 500 and 550 {sup ∘}C), and the effect of annealing temperature on the structural, morphological, optical and magnetic properties were studied. The annealed films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), UV-visible spectroscopic analysis and vibrating sample magnetometer (VSM). XRD patterns showed that the NiFe{sub 2}O{sub 4} is oriented along (311) plane, which enhances peak intensity with respect to the annealing temperature. The analysis of XRD pattern revealed the formation of single-phase cubic spinel structure. The FT-IR spectrum of NiFe{sub 2}O{sub 4} thin films showed strong absorption peaks around 616 and 353 cm{sup − 1} which indicates the cubic spinel crystal structure of the films. FE-SEM micrographs show that the grain size increases with an increase in annealing temperature. The grain size varies between ∼ 19 and ∼ 28 nm, confirming the nanocrystalline nature of the prepared thin films. The optical properties of the films were studied by an absorbance spectrum in the range of 300 to 800 nm. The results showed that the energy band gap decreased with the increase of annealing temperature. Magnetic properties of NiFe{sub 2}O{sub 4} thin films exhibit a strong dependence on the annealing temperature. The saturation magnetization increases from ∼ 68.29 to ∼ 205.24 emu/cm{sup 3} with increasing annealing temperature, which is in favour of modern electronic device miniaturization.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

Infrared Spectroscopic Study of Magnetic Behavior of Dysprosium Doped Magnetite Nanoparticles

Dysprosium doped magnetite (Fe{sub 3−x}Dy{sub x}O{sub 4} with x = 0.0–0.1) nanoparticles have been synthesized using the co-precipitation method. Magnetic characterization using vibrating sample magnetometer (VSM) has revealed an enhancement in the saturation magnetization with Dy{sup 3+} doping. The occupancy of the dopant ions in magnetite lattice has been probed using Fourier transform infrared spectroscopy (FTIR). The shifting of ν{sub 2} (Fe–O) band at 452 cm{sup − 1} for undoped samples to 443 cm{sup − 1} for dysprosium-doped samples is indicative of occupancy of dysprosium at the octahedral site. X-ray diffraction (XRD) patterns have been used to calculate the strain and lattice constant. The strain is found to increase with doping level and attained a maximum value for the x = 0.03. This increase in the strain can be attributed to occupancy of large diameter Dy{sup 3+} ions at the octahedral site of spinel structure of the magnetite lattice.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Electrochemical Investigations of Magnetic Co{sub 3}O{sub 4} Nanoparticles as an Active Electrode for Supercapacitor Applications

This attempt reports on cobalt oxide (Co{sub 3}O{sub 4}) nanoparticles (NPs) prepared through the traditional chemical reflux method to examine the behavior of supercapacitor performance. The synthesized NPs were characterized using several analytical tools such as ultraviolet-visible spectroscopy (UV), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) pattern, and scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX). Moreover, the electrochemical performance was analyzed using galvanostatic charge and discharge studies (GCD), cyclic voltammetry (CV) studies as well as electrochemical impedance spectroscopy (EIS). The cubical phase of Co{sub 3}O{sub 4} was identified from the XRD pattern and also the average crystalline size was measured by Scherrer’s equation. FTIR confirmed the functional group of Co{sub 3}O{sub 4} NPs. SEM images revealed the hexagonal-shaped nanoflakes-like morphology of the sample. From the elemental analysis, the formation of pure Co{sub 3}O{sub 4} NPs by means of high purity and composition ratio of cobalt with oxygen was found. Vibrating sample magnetometer (VSM) plot scrutinized the magnetic performance of Co{sub 3}O{sub 4} NPs{sub .} The Co{sub 3}O{sub 4} NPs modified electrode has delivered maximum specific capacitance as 1413 Fg{sup −1} at a current density of 1 Ag{sup −1} which maintains tremendous cycling stability within the retention ratio of 98.4% after 1000 cycles. .

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Structural and Magnetic Behavior of BaAl{sub x}Cr{sub y}Fe{sub 11}O{sub 19} (x + y = 1) Hexagonal Ferrites

The present study aims to analyze barium hexagonal ferrite and its derivation behavior using sol-gel auto-combustion co-doped with Al{sup 3+}/Cr{sup 3+}ions. Also, the effects of dopants on structural and magnetic properties of prepared samples were investigated. To this purpose, the finest powders were preheated at 500 °C for 1 h and calcinated at 900 °C about 2 h. Then, the magnetic powders were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), and vibrating sample magnetometer (VSM). The XRD patterns show the magnetoplumbite phase. According to the Scherrer equation applied, inserting ions led to a decrease in lattice parameters (a and c) and crystallite size. The morphology of synthesized samples was observed by FESEM and proved the hexagonal shapes of the prepared samples. The nanoparticles sizes were recorded between 59 and 79 nm. Moreover, the magnetic properties of prepared samples were specified by VSM. The saturation magnetization (M{sub s}) and remnant magnetization (M{sub r}) of the synthesized magnetic powders were decreased by inserting Al{sup 3+}/Cr{sup 3+} ions, while coercivity (H{sub c}) increased from 5215 to 7178 Oe. .

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Control of optical absorption and fluorescence spectroscopies of natural melanin at different solution concentrations

The source of the optical properties of natural melanin persists as an impressive conundrum, hindering a thorough comprehension of the complicated photo-protective contribution of these extensive natural pigments and the pragmatic design of revolutionary bioinspired materials for optoelectronic functionalities. Melanin is a natural pigment distributed in vivo, and provides protection from the sun rays, exhibiting a strong wide-band UV–visible absorption. In the present study, we investigated the optical properties of natural melanin at different pH concentrations within the framework of experimental techniques, namely, UV–visible absorption, Fourier transform infrared spectroscopy (FTIR), and fluorescence spectroscopies. The results indicate that the optical absorption and fluorescence of natural melanin are enhanced within the near-UV and visible regimes with an increase in the solution concentration, are dependent on the pH level, and can impact the emergence of a broad band of visible absorption. The variations in the optical absorption spectra of natural melanin solutions at various pH levels will demonstrate novel rational strategies for controlling their optical properties for potential optoelectronic applications.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2018

Synthesis and Characterization of Silicon Nanowires by Electroless Etching

Silicon nanowires (SiNWs) were synthesized by two-step electroless etching of p-type Si (100) wafer and characterized by field emission scanning electron microscopy, UV–Vis spectroscopy, x-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and Raman spectroscopy. The vibrational signature at 1108 and 2087 cm{sup −1} confirmed SiNWs were passivated by both oxygen and hydrogen atoms. Raman peak at 517 cm{sup −1} indicated crystalline SiNWs with tailing toward redshift due to Fano effect. The Si(2p) and Si(2s) core orbital spectra of SiNWs were found at 99.8 and 150.5 eV, respectively. Moreover, the reflection of SiNWs is minimized to ~ 1 to 5% in the 650-nm wavelength.

77 NANOSCIENCE AND NANOTECHNOLOGY↗