High temperatures and Raman scattering through pulsed spectroscopy and CCD detection

Simon, Patrick; Moulin, B.; Buixaderas, E.; Raimboux, N.; Hérault, Émilie; Chazallon, Bertrand; Cattey, H.; Magneron, N.; Oswalt, J.; Hocrelle, D.

doi:10.1002/jrs.1020

Cited by 41 publications

(39 citation statements)

References 20 publications

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“…More recently, pulsed-laser excitation and gated CCD array detectors have been used for in situ Raman monitoring of diamond film growth [18]. Very recently, a pulsed-laser Raman system, which employs either a gated CCD detector or a Pockels switch has been developed, and Raman spectra in the 2000 K range have been reported [19]. However, in the case of the LHDAC even CW Raman measurements are very rare [20][21][22], while none at all in the time-resolved regime have, to our knowledge, been reported.…”

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“…1 (see also Refs. [13,19]). The detector is triggered by the laser repetition and is appropriately gated; continuous radiation is thus suppressed by a factor that is proportional to the ratio of the pulse interval to the gate width.…”

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“…transparent nitrogen), it is expedient to use spatial filtering to suppress the thermal radiation from the coupler, which typically has a much larger emissivity. Additional suppression of the thermal radiation can be obtained by using blue or even ultraviolet radiation as the Raman excitation source [19,22]. By combining these two methods we have, for example, obtained CW Raman spectra of cubic boron nitride at 2300 K [22,26] at pressures of up to 26 GPa.…”

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“…It is also apparent that the temperature of 1273-1573 K, quoted in Ref. [19] as the limit at which thermal radiation becomes noticeable in Raman spectra, is highly uncertain. It depends on at least the experimental factors described above and also on the sample arrangement and the Raman scattering efficiency.…”

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Pulsed laser Raman spectroscopy in the laser-heated diamond anvil cell

Goncharov

Crowhurst

2005

Review of Scientific Instruments

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We describe the design and operation of a spatially-filtered Raman/fluorescence spectrometer that incorporates a pulsed 532 nm laser excitation source and a synchronized and electronically gated CCD detector. This system permits the suppression of undesired continuous radiation from various sources by a factor of up to 50,000 providing the possibility of acquiring Raman signals at temperatures exceeding 5,000 K.We present performance comparisons of this system with that of a state-of-the-art conventional CW system using a 458 nm excitation source. We also demonstrate that the pulsed system is capable of suppressing an impurity-induced (single nitrogen defects) fluorescence in diamond, and further suggest that this capability can be used to suppress the stress-induced fluorescence in diamond that may appear at pressures near or above 150 GPa.Raman spectroscopy in combination with the DAC is an extremely versatile experimental tool. It is used to investigate the behavior under extreme pressure of many different material properties including vibrational, structural, electronic and elastic [1][2][3][4][5][6][7]. The results of these studies find application in various diverse disciplines including the geoand planetary sciences [1,2,4,5], fundamental physics and chemistry [2,6], and material science [7,8]. Under simultaneous conditions of extreme temperature further information concerning phase changes, chemical kinetics, superconductivity etc. may be obtained. Since the processes described above have very different characteristic time-scales, there is the possibility to separate them using various gated techniques. A technique that has previously been used includes the use of a pair of rotating chopper wheels synchronized to occlude short-lived radiation including the excitation laser light and short-lived fluorescence. This approach has been used to suppress diamond fluorescence in order to permit measurements of ruby fluorescence (the basis of the common pressure scale) above 100 GPa [13][14][15]. The latter process can be separated from the stressinduced diamond fluorescence because it is longer lived (5-20 ms). In another technique the detector is gated to collect the desired signal only when the excitation is present. It has been used for high-temperature Raman measurements at ambient pressure to suppress unwanted thermal radiation. Different types of apparatus have been used including mechanical choppers [16], pulsed lasers and a single-channel gated detector [17]. More recently, pulsed-laser excitation and gated CCD array detectors have been used for in situ Raman monitoring of diamond film growth [18]. Very recently, a pulsed-laser Raman system, which employs either a gated CCD detector or a Pockels switch has been developed, and Raman spectra in the 2000 K range have been reported [19]. However, in the case of the LHDAC even CW Raman measurements are very rare [20][21][22], while none at all in the time-resolved regime have, to our knowledge, been reported. We present here our pulsed Raman system and compar...

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Pulsed laser Raman spectroscopy in the laser-heated diamond anvil cell

Goncharov

Crowhurst

2005

Review of Scientific Instruments

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“…UV excitation and/or pulsed Raman spectroscopy offer two ways to reduce blackbody emission. Simon et al 13 and Mermoux et al 14 show how it is possible to obtain Raman spectra of good quality for materials heated above 1000°C and to monitor their synthesis or their transformation by in situ Raman spectroscopy. Raman studies of minerals at temperatures as high as 2500°C were performed by placing the sample directly in a 300 µm hole drilled in a tantalum or iridium heating wire.…”

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Preface to the special issue on Raman spectroscopy under extreme conditions

Lucazeau¹

2003

J Raman Spectroscopy

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Optical Spectroscopy Methods and High‐Pressure–High‐Temperature Studies

Polian

Simon

Pagès³

2010

Thermodynamic Properties of Solids

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This chapter aims to show how optical spectroscopies contribute to the study of vibrational properties under extreme conditions. Now, what do we mean by extreme conditions? We can take it in the other way and mention that ambient conditions have nothing more special as to permit life on earth -that is already not bad! From the point of view of physics, no particular property occurs at ambient conditions. On the contrary, most of the matter in the universe is under extreme pressure (P) and temperature (T), as it is in planets, stars, and more exotic objects. Studies at high pressure and high temperature are hence only the study of matter in its normal conditions. The reason why geoscientists are much interested in such studies is self-explanatory, but other fields are widely studied. The application of high pressure and high temperature enables to explore the repulsive part of the potential energy (fundamental physics), to provoke phase transformations thereby leading to new structures eventually metastable at ambient conditions (materials sciences), to orient chemical reactions in requested directions (chemistry), and even to crystallize proteins, that otherwise would not happen by using other techniques (biology). Another interest to work under variable conditions is that, obviously, more insight is given into the considered phenomenon, in that the pressure and/or temperature derivatives of the phenomenon become available, thus offering a more complete picture to achieve optimum understanding and/or modeling.There are mainly five experimental methods to probe the vibrational properties of matter: optical spectroscopies (of main interest here), ultrasonics (US), inelastic neutron scattering (INS, cf. Chapter 3), more recently inelastic X-ray scattering (IXS, cf. Chapter 4) -that was made possible due to the introduction of third generation synchrotron radiation facilities -and picosecond (PS) acoustics.INS and IXS are used to determine the dispersion of vibration modes, that is, acoustical as well as optical ones, over the whole Brillouin zone (BZ). The most stringent limitations are the needed sources (national-size ones, i.e., a nuclear reactor for INS and a monochromatized X-ray beam as delivered by a synchrotron for IXS), and a limitation to small momentum transfer (q < 0.1q BZB , where q is the magnitude of the wavevector and BZB is the BZ boundary). An additional limitation for INS is

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High temperatures and Raman scattering through pulsed spectroscopy and CCD detection

Cited by 41 publications

References 20 publications

Pulsed laser Raman spectroscopy in the laser-heated diamond anvil cell

Pulsed laser Raman spectroscopy in the laser-heated diamond anvil cell

Preface to the special issue on Raman spectroscopy under extreme conditions

Optical Spectroscopy Methods and High‐Pressure–High‐Temperature Studies

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