# A multi-modal high pressure and high temperature reaction cell for combined x-ray spectroscopy, scattering, and imaging

Thokozile A. Kathyola, Stephen J. Keylock, Konstantin Ignatyev, Jacob Filik, Jakub Drnec, Paul B. Webb, Anna B. Kroner, Sofia Diaz-Moreno

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Thokozile A. Kathyola, Stephen J. Keylock, Konstantin Ignatyev, Jacob Filik, Jakub Drnec, et al. A multi-modal high pressure and high temperature reaction cell for combined x-ray spectroscopy, scattering, and imaging. Review of Scientific Instruments, 2024, 95 (10), pp.105122. 10.1063/5.0230527. hal-05098748

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# A multi-modal high pressure and high temperature reaction cell for combined x-ray spectroscopy, scattering, and imaging

Thokozile A. Kathyola 🧮 ; Stephen J. Keylock 🧮 ; Konstantin Ignatyev 🧮 ; Jacob Filik 🧮 ; Jakub Drnec 🧮 ; Paul B. Webb 🧮 ; Anna B. Kroner 🧮 ; Sofia Diaz-Moreno 🧮

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# A multi-modal high pressure and high temperature reaction cell for combined x-ray spectroscopy, scattering, and imaging

Cite as: Rev. Sci. Instrum. 95, 105122 (2024); doi: 10.1063/5.0230527

Submitted: 24 July 2024 • Accepted: 1 October 2024 •

Published Online: 23 October 2024

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Thokozile A. Kathyola,<fnref n="1" />,ª ID Stephen J. Keylock,<fnref n="1" /> ID Konstantin Ignatyev,<fnref n="1" /> ID Jacob Filik,<fnref n="1" /> ID Jakub Drnec,<fnref n="2" /> ID Paul B. Webb,⁵ ID Anna B. Kroner,<fnref n="1" /> ID and Sofia Diaz-Moreno<fnref n="1" />,ª ID

## AFFILIATIONS

## ABSTRACT

A free-standing and compact reaction cell for combined *in situ/operando* x-ray spectroscopy, scattering, and imaging measurements at high pressures and high temperatures is described. The cell permits measurements under realistic operating conditions (up to 50 bar and 1000 °C), under static and flow conditions (up to 100 ml/min), over a wide range of hard x-ray energies, variable detection modes (transmission, fluorescence, and scattering), and at all angles of rotation. An *operando* XAS, x-ray fluorescence, x-ray computed tomography, and x-ray diffraction computed tomography case study on the reduction of a heterogeneous catalyst is presented to illustrate the performance of the reaction cell.

© 2024 Author(s). All article content, except where otherwise noted, is licensed under a Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/). https://doi.org/10.1063/5.0230527

## I. INTRODUCTION

The combination of hard x-ray spectroscopy, scattering, and imaging has become increasingly popular in the past decade to unravel structural transitions, and it has been widely applied in heterogeneous catalysis. The high penetration depths of hard x rays permit measurements under industrially relevant conditions, such as high pressure, high temperature, and reactive environments, while the multi-modal approach provides multi-scale mechanistic information on the effects of structure, composition, and species distribution on the performance of the catalyst. Notable advance- ments include the development of experimental setups that permit *in situ/operando* scanning transmission x-ray microscopy (STXM), absorption x-ray computed tomography (XCT), x-ray absorption near edge structure computed tomography (XANES-CT), x-ray fluorescence computed tomography (XRF-CT), x-ray diffraction computed tomography (XRD-CT), and pair distribution function computed tomography (PDF-CT).<fnref n="1" />⁻⁸ However, the previous tomog- raphy studies have been limited to pressures less than 10 bars,

which is below the conditions employed in commercial operations (normally in the range of 20–50 bars). To bridge this pressure gap, we developed a novel *in situ/operando* vitreous (glassy) carbon reac- tion cell (Fig. 1) that can withstand extreme conditions (20–50 bars and up to 1000 °C) and accommodate the combination of multiple complementary techniques.

The reaction cell design and development was informed by a previous *in situ* SCT, XANES-CT, XRF-CT, and XRD-CT setup (operating at ≤4 bar) developed at Diamond Light Source<fnref n="2" />⁻⁴ and glassy carbon tube cells for *operando* high pressure and high tem- perature x-ray absorption spectroscopy (XAS) measurements.⁹⁻¹¹ Our cell has successfully been used at Diamond (beamlines I18¹<fnref n="2" /> and K11)¹³ and at the ESRF (beamline ID31)¹⁴ to investigate multi-scale structural variations during heterogeneous catalysis, gas adsorption, and metal corrosion processes. Various combinations of spectroscopy, scattering, and imaging over wide ranges of energy (7–75 keV) and spatial resolution (2–50 µm) afforded by the dif- ferent beamlines have been explored. In this paper, we present an *operando* XAS, XRF, SCT, and XRD-CT study on a dynamic and

<footnote n="1">¹Diamond Light Source, Didcot, Oxfordshire OX11 0DE, United Kingdom</footnote>

<footnote n="2">²The European Synchrotron Radiation Facility, 71 Av. des Martyrs, 38000 Grenoble, France</footnote>

<footnote n="3">³School of Chemistry, University of St Andrews, St Andrews KY16 9ST, United Kingdom</footnote>

<footnote>ªAuthors to whom correspondence should be addressed: thokozile.kathyola@diamond.ac.uk and sofia.diaz-moreno@diamond.ac.uk</footnote>
heterogeneous catalyst to illustrate the application of the developed reaction cell.

## II. CELL DESIGN

Figure 1 shows the schematics and a picture of the multi-modal high pressure and high temperature reaction cell. A list of the components required to build the cell (Table S1) and a technical drawing of the bespoke cell base (Fig. S1) are provided in the supplementary material. The main component is a 75 mm glassy carbon tube (Hochtemperatur Werkstoffe GmbH; Sigradur G) with a 3 mm inner diameter (ID) and 10 mm outer diameter (OD). One advantage of glassy carbon is that it has low x-ray absorbance, which permits thicker walls without significantly reducing the ability to measure XAS/XANES-CT at relatively low x-ray energies from about 7 keV.⁹ It is also amorphous with low concentration of impurities,¹⁵,¹⁶ which makes it ideal for XRD-CT and XRF-CT measurements. To increase x-ray transmittance and fluorescence, the wall thickness of the 15 mm middle section [Fig. 1(a)] was reduced to 1.5 mm by machining down the glassy carbon with an abrasive power file. Quartz wool plugs at each end of the tube are used to keep the sample in the mid-section and minimize the dead volume in the cell. Due to the opaque nature of glassy carbon, a graduated 2.5 mm wooden rod was used to ensure that quartz wool plugs filled up the entirety of the 30 mm ends of the tube. The glassy carbon tube has good torsional rigidity during tomography measurements and

can withstand the strain exerted at the top by a 10 mm compression tube fitting (Swagelok), modified 10 mm to 1/16 in. reducing T-piece (Swagelok), 1/16 in. gas outlet stainless steel tubing (Swagelok), and 0.5 mm OD Type K thermocouple (RS Components). It is also well supported at the bottom by a bespoke stainless steel base with holes for M3 screws to connect to a beamline rotation stage and welded on Swagelok 10 mm and a 1/16 in. male connectors for the tube bottom and a gas inlet fitting. The gas inlet and outlet stainless steel tubing are loosely coiled up (one to three 150 mm diameter loops) to reduce the strain on the cell. Consequently, the cell can rotate up to 360° without any breakages or obstructions during tomography scans. The full angle rotation ensures less distortions/artifacts in image reconstructions, angle dependent XRD-CT analysis, and improved XRF-CT of highly attenuating samples.

Prior to pressuring the glassy carbon tube, a burst pressure of about 70 bars was estimated using the Barlow formula.¹⁰ This was based on the wall thickness (1.5 mm) and OD (6 mm) of the middle section, glassy carbon yield strength (1380 bars), and a discretionary safety factor of 10. The cell has been tested up to 500 °C at 10 °C/min and 20 bars of helium (He) and hydrogen (H₂) without fault. Gas-tight graphite ferrules (Greyhound Chromatography; Cole Palmer) were used for the Swagelok connections to the glassy carbon and thermocouple, while the gas inlet and outlet utilize stainless-steel ferrules. The flexibility of the graphite ferrules makes them reusable, along with the glassy carbon tube and Swagelok fittings. Since the ferrules are rated to about 450 °C, hot air blowers were directed

<figure><img src="image_11.png" /><figcaption>FIG. 1. Schematics of the multi-modal high pressure and high temperature reaction cell detailing (a) its components and (b) the arrangement of the hot air blowers for scattering and transmission measurements; (c) a picture of the cell at the ESRF beamline ID31.</figcaption></figure>
<figure><img src="image_12.png" /><figcaption>FIG. 2. Temperature calibration curves for a glassy carbon tube with and without a sample under static conditions and at ambient pressure.</figcaption></figure>

toward the sample area in the middle of the tube [Figs. 1(b) and 1(c)]. The hot air blowers (Leister AG; 800 W) can go up to 750 °C, but measurements of the temperature inside the tube with and without a sample [e.g., iron (III) oxide (Fe₂O₃) powder] show that this translates to about 520 °C (Fig. 2). A PID benchtop controller (Omega Engineering Ltd.) coupled with a Type K thermocouple was used to record the empty tube/sample temperature and remotely control the power supplied to the hot air blowers as a function of the set point. The thermocouple tip was placed at the top of the sample to ensure that it was excluded from the tomography sinograms. A thermal infrared (IR) imaging camera (Optris GmBH) can also be included to non-destructively measure the vertical and horizontal temperature profiles of the sample bed (Fig. S2). The setup is adaptable and, if required, can permit the use of alternative heat sources (e.g., IR heaters) to achieve higher temperatures, providing they do not obstruct or affect the x-ray beam, detectors, cameras, and/or optical microscopes. It is advisable to utilize flame-retardant thermal insulating sheets to protect ancillary equipment, especially in experimental hutches with confined sample areas.

Another notable design consideration was the inclusion of ancillary equipment such as mass flow controllers (Bronkhorst UK Ltd./Premier Control Technologies Ltd.), pressure transducers (Keller Druckmesstechnik AG/Applied Measurements Ltd.), pressure controllers (Bronkhorst UK Ltd./Premier Control Technologies Ltd.), and mass spectrometers (Pfeiffer/EcoCat) that can tolerate high pressures (20–50 bars) and high flowrates (10–100 ml/min) of toxic, flammable, and corrosive gases. These can be connected to the cell base and reducing T-piece [Fig. 1(a)] via 1/16 in. Swagelok steel tubing and fittings. The gas outlet also allows for connections to local exhaust ventilation systems and optional product traps. Overall, the free-standing reaction cell is portable and uses commercially available standard connections, which makes it easily adaptable to equipment at different beamlines and facilities. It has been commissioned and used at the beamline I18 (Diamond) for simultaneous scanning SCT, XRF-CT, and XRD-CT (8–17 keV) and point XANES (7 and 9 keV) using a 4 × 4 µm² (FWHM) monochromatic beam. It has

also been used at beamline ID31 (ESRF) for scanning XRD-CT and PDF-CT (75 keV) using a 4 × 6 µm² (FWHM) monochromatic beam and at beamline K11 (Diamond) for full field SCT (22 keV) using a polychromatic beam with a 1.4 × 1.2 mm² field of view and 2D XRD (33 eV) using a 50 × 50 µm² (FWHM) monochromatic beam.

### III. CELL PERFORMANCE

The capability of the multi-modal reaction cell (Fig. 1) was explored with a case study on the reduction of a precipitated sodium promoted iron (III) oxide (Fe₂O₃/Na) Fischer-Tropsch catalyst. The cell was loaded with 20 mg of Fe₂O₃/Na powder (~88 µm grain size) mixed with 120 mg of amorphous glass beads (~100 and 200 µm from Sigma-Aldrich). Pure H₂ was constantly flowed through the system at 20 ml/min to maintain 20 bar of pressure. The catalyst bed was heated from ambient temperature to 220, 320, and 420 °C at 10 °C/min and monitored *operando* using XAS (7 keV), XRF (17 keV), SCT (17 keV), and XRD-CT (17 and 75 keV). Mass spectrometry measurements (not shown here) were collected simultaneously with spectroscopy and tomography. Fluorescence yield and transmission Fe K-edge XANES spectra were collected at the Diamond beamline I18, and the data were reduced using Athena in the Demeter software package.¹⁷ Complementary XRF, SCT, and XRD-CT data were collected at 17 keV in the same instrument. The sample was rastered across a 4 × 4 µm² (FWHM) beam size to give XRF maps of about 3 × 8 mm² using vertical and horizontal steps of 20 µm. About 278 translation steps and 181 rotations in 1° steps were used for three to four SCT and XRD-CT slices. In contrast, a 75 keV monochromatic x-ray beam focused to a 4 × 6 µm² (FWHM) size was used to collect the XRD-CT data at beamline ID31 at the ESRF. In this case, 350 translation steps and 181 rotations in 1° steps were used. XRD lateral scans were also collected over 8–11 mm using steps of 500 µm. In both experiments, the sample was translated vertically by about 3 mm to obtain slices at the top, middle, and bottom of the catalyst bed. The data were processed and analyzed using Python scripts (provided by beamlines I18 and ID31) and DAWN.¹⁸

XRF was used at beamline I18 to map out the catalyst bed [Fig. 3(a)] and identify optimal cross sections at the top, middle, and bottom to collect XAS, SCT, and XRD-CT. Figure 3(b) shows a fluorescence yield Fe K-edge XANES spectrum of the pre-reduction catalyst at ambient temperature and 20 bars of H₂. Characteristic Fe₂O₃ features due to 1s → 3d (7114 eV) and 1s → 4p (7123 eV) electronic transitions are evident.¹,¹⁹,²⁰ Complementary SCT [Fig. 3(c)] determined the distribution of the catalyst among the glass beads. The SCT mainly showed the highly absorbing big catalyst particles and/or agglomerates, while the XRD-CT [Fig. 3(d)] also spatially resolved the small particles spread across the glass beads and inner walls of the glassy carbon tube. However, extraction of the XRD patterns from the different particles/agglomerates was very challenging as the ~200 µm glass beads limited the penetration depth of the x rays at 17 keV and the scattering of the crystalline sample.

The extraction of the XRD patterns was possible using the data collected at ID31. The higher 75 keV energy coupled with smaller ~100 µm glass beads resulted in higher resolution XRD-CT reconstructions [Fig. 3(e)]. The XRD patterns extracted from the tomography data collected at 20 bars of H₂ and ambient temperature, 220, 320, and 420 °C are shown in Fig. 4. As expected, the XRD at ambient temperature shows distinctive Fe₂O₃ reflections with
<figure><img src="image_13.png" /><figcaption>FIG. 3. Operando (a) XRF, (b) XAS, (c) XCT, and [(d) and (e)] XRD-CT data of a Fe₂O₃/Na catalyst collected at ambient temperature and 20 bar of H₂.</figcaption></figure>

<figure><img src="image_14.png" /><figcaption>FIG. 4. Operando XRD of the reduction of the Fe₂O₃/Na catalyst by H₂ to α-Fe via Fe₃O₄ and FeO from ambient temperature to 420 °C at 20 bars.</figcaption></figure>

relatively intense (104) and (110) Bragg peaks in the low Q region.¹⁹ The Fe₂O₃ is stable up to 220 °C and then it reduces to iron (II, III) oxide (Fe₃O₄) at 320 °C. The formation of Fe₃O₄ is indicated by the appearance of distinguishing (220), (311), (511), and (440) peaks at 2.1, 2.5, 3.0, and 3.1 Å⁻¹ respectively. Traces of metallic iron (α-Fe) were detected at 320 °C, but it was more dominant at 420 °C with

a very intense (110) peak at 3.1 Å⁻¹. Relatively small peaks due to (200) and (220) iron (II) oxide (FeO) reflections are also present at 420 °C. Notably, FeO has previously eluded detection and is generally assumed to not be a stable intermediate in the reduction of unsupported Fe₂O₃-based Fischer–Tropsch catalysts.¹,¹⁹,²⁰ Further analysis of the XRD-CT is required to determine correlations between the formation of the different Fe species in the mixed systems at 320 and 420 °C and the morphology/distribution of the catalyst particles.

## IV. CONCLUSION

We have designed and developed a free-standing and compact reaction cell for high pressure and high temperature *in situ/operando* spectroscopy, scattering, and imaging measurements. The capabilities of this setup have been explored by looking at technologically relevant multi-phase and multi-component systems such as the Fischer–Tropsch synthesis. The primary aim was to develop an easily accessible/reproducible tool that provides holistic information on how bulk structure, morphology, composition, and distribution contribute to the overall performance of functional materials. The multi-technique cell has successfully been used at different beamlines and facilities and is readily available to Diamond Light Source users. Further development is under way to optimize the cell for XRF-CT and XANES-CT measurements and for operations at pressures greater than 20 bars. Previous attempts at XRF-CT have been constrained by high attenuation, thus we are investigating methods
to improve data acquisition. These methods include improving sample loading/dilution, modifying the cell geometry, and utilizing two fluorescence detectors.

## SUPPLEMENTARY MATERIAL

The **supplementary material** contains a list of the components required to build the cell, a technical drawing of the bespoke stainless steel cell base, and an infrared image of vertical and horizontal temperature profiles.

## ACKNOWLEDGMENTS

This work was carried out with the support of Diamond Light Source, beamline I18 (Proposal No. SP31385), the EPSRC Interface with the Future (InfUSE) Prosperity Partnership (Grant No. EP/V038044/1), and the European Synchrotron Radiation Facility (Proposal No. A-5651; DOI:10.15151/ESRF-ES-1226450390). We thank Stuart Bartlett (Diamond), Sylvia Britto (Diamond), Huw Shiel (Imperial College London), and James Le Houx (Diamond) for their aid with some of the data collection.

## AUTHOR DECLARATIONS

### Conflict of Interest

The authors have no conflicts to disclose.

### Author Contributions

All authors contributed to the work presented in this paper. T.A.K., K.I., P.B.W., A.B.K., and S.D.-M. contributed to the conception and design of the experiments. T.A.K., S.J.K., K.I., J.D., and A.B.K. provided technical support. T.A.K., K.I., P.B.W., A.B.K., and S.D.-M. performed the experiments. T.A.K. and J.F. analyzed the data. T.A.K. wrote the manuscript, which was edited by K.I. and S.D.-M.

**Thokozile A. Kathyola:** Conceptualization (equal); Data curation (equal); Formal analysis (equal); Investigation (equal); Methodology (equal); Project administration (equal); Validation (equal); Visualization (equal); Writing – original draft (equal); Writing – review & editing (equal). **Stephen J. Keylock:** Investigation (equal); Methodology (equal). **Konstantin Ignatyev:** Formal analysis (equal); Investigation (equal); Methodology (equal); Resources (equal); Software (equal); Validation (equal); Writing – review & editing (equal). **Jacob Filik:** Data curation (equal); Formal analysis (equal); Investigation (equal); Methodology (equal); Software (equal); Validation (equal); Visualization (equal). **Jakub Drnec:** Data curation (equal); Investigation (equal); Resources (equal); Software (equal); Visualization (equal). **Paul B. Webb:** Conceptualization (equal); Investigation (equal); Methodology (equal); Validation (equal). **Anna B. Kroner:** Conceptualization (equal); Investigation (equal); Methodology (equal); Resources (equal); Validation (equal). **Sofia Diaz-Moreno:** Conceptualization (equal); Data curation (equal); Funding acquisition (equal); Investigation (equal); Methodology (equal); Project administration (equal); Resources (equal); Supervision (equal); Validation (equal); Writing – review & editing (equal).

## DATA AVAILABILITY

The data that support the findings of this study are available within the article and its **supplementary material**.

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