Simultaneous neutron powder diffraction and Raman spectroscopy – an approach of combining two complementary techniques

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Raphael Finger ◽  
Thomas C. Hansen ◽  
Holger Kohlmann
Keyword(s):  
Raman Spectroscopy ◽  
Neutron Diffraction ◽  
Amorphous Materials ◽  
Lead Sulfate ◽  
Phase Identification ◽  
Ambient Conditions ◽  
Raman Spectroscopic ◽  
Sapphire Single Crystal ◽  
Complementary Techniques

Abstract Diffraction techniques are well-established methods for crystal structure determination as well as phase identification and quantification. Raman spectroscopy can be a valuable complementary characterization technique, because in contrast to the former it yields also information on amorphous materials and it is a probe for short-range structural effects. The herein presented setup allows for simultaneous neutron diffraction and Raman spectroscopy, shown with a sample of lead sulfate under ambient conditions as a proof of principle. In order to fulfil requirements of both methods, a sapphire single-crystal is used as a sample holder. Practical considerations for successful simultaneous in situ neutron diffraction and Raman spectroscopic measurements are given.

Mapping gold nanoparticles on and in edible leaves in situ using surface enhanced Raman spectroscopy

RSC Advances ◽  
2016 ◽  
Vol 6 (65) ◽  
pp. 60152-60159 ◽  
Author(s):  
Zhiyun Zhang ◽  
Huiyuan Guo ◽  
Yingqing Deng ◽  
Baoshan Xing ◽  
Lili He
Keyword(s):  
Gold Nanoparticles ◽  
Raman Spectroscopy ◽  
Surface Enhanced Raman Spectroscopy ◽  
Mapping Technique ◽  
Raman Spectroscopic ◽  
Surface Enhanced ◽  
Surface Enhanced Raman ◽  
Spinach Leaves

A surface enhanced Raman spectroscopic (SERS) mapping technique was applied to qualitatively detect and characterize gold nanoparticles on and in spinach leaves in situ.

Evaluation of Residual Stresses Within Plasma-Sprayed Zirconia (ZrO2-Y2O3 8%wt) Coatings

1998 ◽  
Author(s):  
N. Baradel ◽  
L. Bianchi ◽  
F. Blein ◽  
A. Freslon ◽  
M. Jeandin ◽  
...  
Keyword(s):  
Neutron Diffraction ◽  
Thermal Spraying ◽  
Thermomechanical Properties ◽  
Hole Drilling ◽  
Stabilized Zirconia ◽  
Incremental Hole Drilling ◽  
Complementary Techniques ◽  
Plasma Sprayed ◽  
Steel Substrates

Abstract Thermal spraying induces stresses, which strongly influence thermomechanical properties of the deposits. To study both generation and influence of these stresses, various techniques could be used separately and/or concurrently. "In-situ" curvature, neutron diffraction and incremental hole drilling methods are often presented as complementary techniques. In this study, partially stabilized zirconia coatings, performed onto steel substrates at various spraying temperatures, have allowed to compare these three different methods.

Prototype Raman Spectroscopic Sensor for in Situ Mineral Characterization on Planetary Surfaces

1998 ◽  
Vol 52 (4) ◽  
pp. 477-487 ◽  
Author(s):  
Alian Wang ◽  
Larry A. Haskin ◽  
Enriqueta Cortez
Keyword(s):  
Raman Spectroscopy ◽  
Planetary Surfaces ◽  
Detailed Characterization ◽  
Raman Spectroscopic ◽  
Fine Grained ◽  
Target Rock ◽  
Reaction With Water ◽  
Probe Head

Raman spectroscopy has the potential to provide definitive identification and detailed characterization of the minerals that comprise rocks and soils on planetary surfaces. We have designed a probe head for Raman spectroscopy that is suitable for use on a spectrometer deployed by a rover or a lander on the surface of a planet such as Mars, the Moon, or an asteroid. The probe head is lightweight, low power, rugged, and simple. It is based on a tiny distributed feedback diode laser and volume holographic components. A protective shell surrounds the probe head and serves as a mechanical stop for the mechanical arm of a planetary rover or lander during placement of the probe head onto the surface of a rock or soil. Pressing the shell against the rough surface of a target rock or soil also places the sampling objective of the probe head in rough focus, and the probe head is designed to be tolerant of focusing errors of ∼5 mm. A breadboard version of the probe head gave spectra of high quality on clean crystals of diamond, sulfur, calcite, quartz, and olivine. The results are qualitatively comparable to those obtained by using a conventional micro-Raman spectrometer on fine-grained travertine and on difficult specimens of basaltic lavas and impactites whose original mineralogy had been altered by reaction with water and air.

Time-of-flight neutron diffraction studies of clay-fluid interactions under basin conditions

Clay Minerals ◽  
2000 ◽  
Vol 35 (1) ◽  
pp. 283-290 ◽  
Author(s):  
N. T. Skipper ◽  
G. D. Williams ◽  
A. V. C. de Siqueira ◽  
C. Lobban ◽  
A. K. Soper
Keyword(s):  
Neutron Diffraction ◽  
Sedimentary Basin ◽  
Time Of Flight ◽  
Ambient Conditions ◽  
Isotopic Labelling ◽  
Fluid Systems ◽  
High Pressure High Temperature ◽  
Temperature Sample ◽  
Fluid Interactions

AbstractNeutron diffraction experiments can provide an extremely high-resolution structural picture of clay-fluid systems. Here we describe the application of time-of-flight neutron scattering to hydrated clays, including discussion of issues such as isotopic labelling, sample containment, and data analysis. Recent studies of hydrated vermiculites under ambient conditions are used as an example. We then describe a new high-pressure/high-temperature sample environment that is being used to study clay-fluid interactions, in situ under hydrostatic sedimentary basin conditions. This environment enables us to approximate conditions encountered during burial, at depths of up to 10 km.

scholarly journals Control of zeolite pore interior for chemoselective alkyne/olefin separations

Science ◽  
2020 ◽  
Vol 368 (6494) ◽  
pp. 1002-1006 ◽  
Author(s):  
Yuchao Chai ◽  
Xue Han ◽  
Weiyao Li ◽  
Shanshan Liu ◽  
Sikai Yao ◽  
...  
Keyword(s):  
Neutron Diffraction ◽  
Neutron Scattering ◽  
Inelastic Neutron Scattering ◽  
Inelastic Neutron ◽  
Ambient Conditions ◽  
Efficient Removal ◽  
Reversible Binding ◽  
Lower Olefins ◽  
In Situ Neutron Diffraction

The efficient removal of alkyne impurities for the production of polymer-grade lower olefins remains an important and challenging goal for many industries. We report a strategy to control the pore interior of faujasite (FAU) zeolites by the confinement of isolated open nickel(II) sites in their six-membered rings. Under ambient conditions, Ni@FAU showed remarkable adsorption of alkynes and efficient separations of acetylene/ethylene, propyne/propylene, and butyne/1,3-butadiene mixtures, with unprecedented dynamic separation selectivities of 100, 92, and 83, respectively. In situ neutron diffraction and inelastic neutron scattering revealed that confined nickel(II) sites enabled chemoselective and reversible binding to acetylene through the formation of metastable [Ni(II)(C2H2)3] complexes. Control of the chemistry of pore interiors of easily scalable zeolites has unlocked their potential in challenging industrial separations.

In situ defect quantification and phase identification during flash sintering using Raman spectroscopy

2021 ◽  
Author(s):  
Shannon E. Murray ◽  
Guangxin Lv ◽  
Soumitra S. Sulekar ◽  
David G. Cahill ◽  
Daniel P. Shoemaker
Keyword(s):  
Raman Spectroscopy ◽  
Phase Identification ◽  
Flash Sintering ◽  
Defect Quantification

scholarly journals A double-walled sapphire single-crystal gas-pressure cell (type III) for in situ neutron diffraction

2022 ◽  
Vol 55 (1) ◽  
Author(s):  
Raphael Finger ◽  
Thomas C. Hansen ◽  
Holger Kohlmann
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Ambient Pressure ◽  
Functional Materials ◽  
Gas Pressure ◽  
Elastic Neutron ◽  
Type Iii ◽  
Pressure Cell ◽  
Sapphire Single Crystal

In situ neutron diffraction is an important characterization technique for the investigation of many functional materials, e.g. for hydrogen uptake and release in hydrogen storage materials. A new sapphire single-crystal gas-pressure cell for elastic neutron scattering has been developed and evaluated; it allows conditions of 298 K and 9.5 MPa hydrogen pressure and 1110 K at ambient pressure. The pressure vessel consists of a sapphire single-crystal tube of 35 mm radius and a sapphire single-crystal crucible as sample holder. Heating is realized by two 100 W diode lasers. It is optimized for the D20 diffractometer, ILL, Grenoble, France, and requires the use of a radial oscillating collimator. Its advantages over earlier sapphire single-crystal gas-pressure cells are higher maximum temperatures and lower background at low and high diffraction angles. The deuterium uptake in palladium was followed in situ for validation, proving the potential of the type-III gas-pressure cell for in situ neutron diffraction on solid–gas reactions.

Feasibility of Detecting Barrier Layer to Low-k Transition in Copper Cmp Using Raman Spectroscopy

2005 ◽  
Vol 867 ◽  
Author(s):  
S. Kondoju ◽  
C. Juncker ◽  
P. Lucas ◽  
S. Raghavan ◽  
P. Fischer ◽  
...  
Keyword(s):  
Raman Spectroscopy ◽  
Spectroscopic Method ◽  
Spectroscopic Techniques ◽  
Vibrational Modes ◽  
Si Substrate ◽  
Raman Spectroscopic ◽  
Barrier Layers ◽  
Copper Cmp ◽  
Low K

AbstractIn copper CMP, transitions from copper to barrier as well as barrier to dielectric layer are typically sensed in situ using an optical reflectance technique. Spectroscopic techniques such as Raman, which allow monitoring the vibrational modes of silicon and low-k layers, have interesting potential for detecting these transitions. In this paper the use of Raman spectroscopy in detecting in situ removal of barrier layers from CDO materials is reported. Intensities of Raman peaks characteristic of Si-Si vibrations from Si substrate and C-H vibrations from low-k materials have been used for monitoring CDO layer thickness and detecting removal of Ta overlayer. An abrasion cell is integrated with a Raman spectrometer to demonstrate the feasibility of Raman monitoring in-situ. Capabilities and limitations of the Raman spectroscopic method are discussed.

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