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1.
Rev Sci Instrum ; 86(3): 033706, 2015 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-25832237

RESUMO

An Atomic Force Microscope (AFM) has been integrated in a miniature high-pressure flow reactor for in-situ observations of heterogeneous catalytic reactions under conditions similar to those of industrial processes. The AFM can image model catalysts such as those consisting of metal nanoparticles on flat oxide supports in a gas atmosphere up to 6 bar and at a temperature up to 600 K, while the catalytic activity can be measured using mass spectrometry. The high-pressure reactor is placed inside an Ultrahigh Vacuum (UHV) system to supplement it with standard UHV sample preparation and characterization techniques. To demonstrate that this instrument successfully bridges both the pressure gap and the materials gap, images have been recorded of supported palladium nanoparticles catalyzing the oxidation of carbon monoxide under high-pressure, high-temperature conditions.

2.
Rev Sci Instrum ; 85(8): 083703, 2014 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-25173272

RESUMO

To enable atomic-scale observations of model catalysts under conditions approaching those used by the chemical industry, we have developed a second generation, high-pressure, high-temperature scanning tunneling microscope (STM): the ReactorSTM. It consists of a compact STM scanner, of which the tip extends into a 0.5 ml reactor flow-cell, that is housed in a ultra-high vacuum (UHV) system. The STM can be operated from UHV to 6 bars and from room temperature up to 600 K. A gas mixing and analysis system optimized for fast response times allows us to directly correlate the surface structure observed by STM with reactivity measurements from a mass spectrometer. The in situ STM experiments can be combined with ex situ UHV sample preparation and analysis techniques, including ion bombardment, thin film deposition, low-energy electron diffraction and x-ray photoelectron spectroscopy. The performance of the instrument is demonstrated by atomically resolved images of Au(111) and atom-row resolution on Pt(110), both under high-pressure and high-temperature conditions.

3.
Rev Sci Instrum ; 80(7): 074501, 2009 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-19655969

RESUMO

We discuss the design, operation, and performance of a vacuum setup constructed for use in zero (or reduced) gravity conditions to initiate collisions of fragile millimeter-sized particles at low velocity and temperature. Such particles are typically found in many astronomical settings and in regions of planet formation. The instrument has participated in four parabolic flight campaigns to date, operating for a total of 2.4 h in reduced-gravity conditions and successfully recording over 300 separate collisions of loosely packed dust aggregates and ice samples. The imparted particle velocities achieved range from 0.03 to 0.28 m s(-1) and a high-speed, high-resolution camera captures the events at 107 frames/s from two viewing angles separated by either 48.8 degrees or 60.0 degrees. The particles can be stored inside the experiment vacuum chamber at temperatures of 80-300 K for several uninterrupted hours using a built-in thermal accumulation system. The copper structure allows cooling down to cryogenic temperatures before commencement of the experiments. Throughout the parabolic flight campaigns, add-ons and modifications have been made, illustrating the instrument flexibility in the study of small particle collisions.


Assuntos
Temperatura Baixa , Aceleradores de Partículas/instrumentação , Ausência de Peso , Desenho Assistido por Computador , Cobre , Poeira , Desenho de Equipamento , Gelo , Movimento (Física) , Vácuo
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