A multi-molecular beam/infrared reflection absorption spectroscopy apparatus for probing mechanisms and kinetics of heterogeneously catalyzed reaction from ultrahigh vacuum to near-ambient pressure conditions

Carsten Schröder; Philipp A. Haugg; Timo Görgens; Sergej Romaker; Henrik Gross; Swetlana Schauermann

doi:10.1063/5.0237747

journal article Jan 01, 2025

A multi-molecular beam/infrared reflection absorption spectroscopy apparatus for probing mechanisms and kinetics of heterogeneously catalyzed reaction from ultrahigh vacuum to near-ambient pressure conditions

Carsten Schröder

Philipp A. Haugg

Timo Görgens

Sergej Romaker

Henrik Gross Swetlana Schauermann

Review of Scientific Instruments Vol. 96 No. 1 · AIP Publishing

View at Publisher Save 10.1063/5.0237747

Abstract

A novel multi-molecular beam/infrared reflection absorption spectroscopy (IRAS) apparatus is described, which was constructed for studying mechanisms and kinetics of heterogeneously catalyzed reactions following a rigorous surface science approach in the pressure range from ultrahigh vacuum (UHV, 1 × 10−10 mbar) to near-ambient pressure (NAP, 1000 mbar) conditions. The apparatus comprises a preparation chamber equipped with standard surface science tools required for the preparation and characterization of model heterogeneous catalysts and two reaction chambers operating at different pressure ranges: in UHV and in the variable pressure range up to NAP conditions. The UHV reaction chamber contains two effusive molecular beams (flux up to 1.1 × 1015 molecules cm−2 s−1), a quadrupole mass spectrometer, a Fourier-Transform (FT) IRA spectrometer, and a molecular beam monitor for beam aligning. This combination of the methods allows us to independently dose different reactants on the surface in a highly controlled way while simultaneously monitoring the evolution of gaseous products by QMS and recording the evolution of the surface species by FT-IRAS. The second reaction chamber operating in the variable pressure range is equipped with polarization-modulation-IRAS and three gas dosers and is designed as a small reactor, which can be operated in a continuous flow mode. The sample prepared under well-controlled UHV conditions can be in situ transferred between all chambers, thus allowing for investigations of structure–reactivity relationships over model surfaces. In this contribution, we provide a detailed description of the apparatus and the test measurements of the different crucial parts of the apparatus in the variable pressure range.

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References

69

[1]

Chem. Eng. Process. (2011) 10.1016/j.cep.2011.05.024

[2]

Catal. Today (2009) 10.1016/j.cattod.2008.11.002

[3]

Catalytic reactor for operando spatially resolved structure–activity profiling using high-energy X-ray diffraction

Birte Wollak, Diego Espinoza, Ann-Christin Dippel et al.

Journal of Synchrotron Radiation 2023 10.1107/s1600577523001613

[4]

Adv. Catal. (1989) 10.1016/s0360-0564(08)60017-6

[5]

Metal Catalysts for Heterogeneous Catalysis: From Single Atoms to Nanoclusters and Nanoparticles

Lichen Liu, Avelino Corma

Chemical Reviews 2018 10.1021/acs.chemrev.7b00776

[6]

J. Catal. (2003) 10.1016/s0021-9517(02)00073-8

[7]

Surf. Sci. (1967) 10.1016/0039-6028(67)90005-2

[8]

J. Catal. (1974) 10.1016/0021-9517(74)90039-6

[9]

J. Catal. (2003) 10.1016/s0021-9517(02)00112-4

[10]

Acc. Chem. Res. (2015) 10.1021/acs.accounts.5b00237

[11]

Coord. Chem. Rev. (2021) 10.1016/j.ccr.2021.214179

[12]

Catal. Rev.—Sci. Eng. (1997) 10.1080/01614949708006469

[13]

Angew. Chem., Int. Ed. (2015) 10.1002/anie.201410738

[14]

Prog. Surf. Sci. (2000) 10.1016/s0079-6816(00)00019-8

[15]

Top. Catal. (1994) 10.1007/bf01492278

[16]

Surf. Sci. Rep. (1998) 10.1016/s0167-5729(98)00002-8

[17]

Catal. Today (2007) 10.1016/j.cattod.2006.12.005

[18]

Phys. Chem. Chem. Phys. (2007) 10.1039/b700365j

[19]

Annu. Rep. Prog. Chem., Sect. C: Phys. Chem. (2004) 10.1039/b313667c

[20]

Catal. Lett. (2009) 10.1007/s10562-009-0224-4

[21]

Appl. Spectrosc. (1993) 10.1366/0003702934415273

[22]

Rev. Sci. Instrum. (2001) 10.1063/1.1329902

[23]

Rev. Sci. Instrum. (2018) 10.1063/1.5021641

[24]

J. Chem. Phys. (2016) 10.1063/1.4940318

[25]

Photoelectron spectroscopy under ambient pressure and temperature conditions

D. Frank Ogletree, Hendrik Bluhm, Eleonore D. Hebenstreit et al.

Nuclear Instruments and Methods in Physics Researc... 2009 10.1016/j.nima.2008.12.155

[26]

Catal. Rev. (2007) 10.1080/01614948308079666

[27]

J. Vac. Sci. Technol., A (1991) 10.1116/1.577664

[28]

Surf. Sci. Rep. (2017) 10.1016/j.surfrep.2017.02.002

[29]

Rev. Sci. Instrum. (2000) 10.1063/1.1318919

[30]

J. Phys. Chem. C (2013) 10.1021/jp401867g

[31]

J. Catal. (2012) 10.1016/j.jcat.2012.03.009

[32]

Rev. Sci. Instrum. (2016) 10.1063/1.4945113

[33]

Rev. Sci. Instrum. (2013) 10.1063/1.4792673

[34]

Rev. Sci. Instrum. (2020) 10.1063/5.0026171

[35]

Rev. Sci. Instrum. (2022) 10.1063/5.0081102

[36]

Phys. Rev. Lett. (2002) 10.1103/physrevlett.89.046101

[37]

Top. Catal. (2000) 10.1023/a:1019101109313

[38]

Science (2017) 10.1126/science.aam9035

[39]

Catal. Lett. (2014) 10.1007/s10562-014-1417-z

[40]

Surf. Sci. Rep. (2013) 10.1016/j.surfrep.2013.10.003

[41]

Rev. Sci. Instrum. (2005) 10.1063/1.2140449

[42]

Chem. Soc. Rev. (2014) 10.1039/c3cs60374a

[43]

Rev. Sci. Instrum. (2009) 10.1063/1.3257677

[44]

Rev. Sci. Instrum. (2024) 10.1063/5.0210860

[45]

Phys. Chem. Chem. Phys. (2021) 10.1039/d1cp03436g

[46]

J. Phys. Chem. C (2009) 10.1021/jp902138q

[47]

Faraday Trans. (1996) 10.1039/ft9969204683

[48]

Cell Rep. Phys. Sci. (2024) 10.1016/j.xcrp.2024.101890

[49]

Rev. Sci. Instrum. (2019) 10.1063/1.5093487

[50]

Rev. Sci. Instrum. (2013) 10.1063/1.4803933

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Published: Jan 01, 2025
Vol/Issue: 96(1)

Authors

C

Carsten Schröder