In Situ Investigation of Non‐Isothermal Decomposition of Pt Acetylacetonate as One‐Step Size‐Controlled Synthesis of Pt Nanoparticles

Abstract

Interest in the development of state-of-the-art methods for synthesis of Pt nanoparticles is dictated by both unique properties of platinum itself and the wide range of platinum nanoparticles applications. Platinum acetylacetonate and platinum nanoparticles produced by the thermal decomposition of Pt(acac) 2 are studied via in situ X-ray diffraction and Raman spectroscopy, thermal gravimetry, scanning (SEM), and transmission electronic microscopy (TEM). The experiments are made at heating rates of 1 and 5 K min À1 . A comparative analysis of SEM, TEM, and XRD data highlights the formation of coarse Pt particles with sizes of %60-160 nm, which are composed of nanoparticles with dimensions of 1.9 and 4.1 nm for 1 K min À1 -and 5 K min À1 -heating rates, respectively. The desirable average size of nanoparticles upon their synthesis can thus be achieved by a simple tuning of the heating rate of acetylacetate thermal decomposition. The present results open up the possibility to use a trivial non-isothermal thermal decomposition method in the synthesis of both supported and unsupported nanoparticles of predetermined size for other chemical elements such as Pd, Ni, Co, etc. from their acetylacetonates.

Gas-Phase Synthesis of PtMo Alloy Electrocatalysts with Enhanced Activity and Durability for Oxygen Reduction Reaction

“…38 The second weight loss observed between 150 and 250 °C was attributed to the thermal decomposition of Pt(acac) 2 and Mo(CO) 6 . 39,40 In this step, Pt metal seeds were formed by reducing the power of CO gas, which was derived from the decomposition of Mo(CO) 6 . The XPS analysis revealed that the metallic Mo peak, located at 228.3 eV, was not detected in the Mo 3d spectrum of PtMo/ C-200 (Figure 2c).…”

“…The first weight loss observed at approximately 100 °C results from the vaporization of residual H 2 O in the powder samples . The second weight loss observed between 150 and 250 °C was attributed to the thermal decomposition of Pt(acac) 2 and Mo(CO) 6 . , In this step, Pt metal seeds were formed by reducing the power of CO gas, which was derived from the decomposition of Mo(CO) 6 . Mo false( CO false) 6 false( normalg false) ↔ Mo false( CO false) 6 false( ads false) → Mo false( ads false) + 6 CO false( normalg false) …”

Controlled Synthesis of Platinum and Silver Nanoparticles Using Multivalent Ligands

“…Mostly, organometallic precursors have been used for the preparation of bimetallic nanoalloy particles [50][51][52]. To the best of our knowledge, only a few reports are available on the preparation of PtNPs and AgNPs using platinum (II) acetylacetonate (Pt(acac) 2 ) [53][54][55] and silver (I) acetylacetonate (Ag(acac)) [44,56] as precursors, respectively.…”

Non-Isothermal Decomposition as Efficient and Simple Synthesis Method of NiO/C Nanoparticles for Asymmetric Supercapacitors

“…Since the capacitance of oxide-based composites strongly depends on their microstructural characteristics that may differ at various synthesis conditions and component ratios, the development of an efficient and simple synthesis method that would ensure the production of composite electrode materials with optimal specific electrochemical properties is a relevant task. Furthermore, it was previously shown [ 22 , 23 ] that non-isothermal decomposition of Pt acetyl acetonate enables access to Pt/C nanoparticles whose surface area can reach 100 m 2 /g. This synthesis method is very simple and requires only two stages; moreover, no washing, filtering or subsequent drying of a specimen are required.…”