Synthesis strategies towards amorphous porous carbons with selective oxygen functionalization for the application as reference material
Synthesis strategies towards amorphous porous carbons with selective oxygen functionalization for the application as reference material
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DOI：
10.1016/j.carbon.2020.09.030
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发表时间：
2021-01-01
期刊：
影响因子：
10.9
通讯作者：
Etzold, Bastian J. M.
中科院分区：
文献类型：
--
作者：
Herold, Felix;Leubner, Oliver;Etzold, Bastian J. M.
碳表面官能化，特别是氧表面基团的操纵已被证明是在许多应用中获得高性能材料的关键。尽管碳表面化学的控制在许多技术相关的应用中具有巨大的潜力，但对无定形和多孔碳的表面氧化物的定性和定量分析仍然具有挑战性。在这项研究中，我们尝试对具有高氧负载量的聚合物衍生的多孔炭进行选择性的有机化学功能化，目的是建立程序升温脱附(TPD)和漫反射红外傅里叶变换光谱(DRIFT)的分析标准。在此背景下，氧化碳材料与锂铝氢化物(LiAlH4)的定量化学还原被用作合成具有定义的氧表面基团(羟基和醚)系综的碳材料的关键。基于这种还原策略，基于保护基团化学的选择性LiAlH4还原导致醛、酮和醌作为表面官能团，并研究了化学接枝选择性地引入苯酯、甲醚和羧酸。通过漂移光谱、TPD、X-射线光电子能谱和滴定方法对所有材料作为分析标准的适用性进行了评估。(C)2020爱思唯尔有限公司。保留所有权利。
Manipulation of carbon surface functionalization and especially of oxygen surface groups has been demonstrated to be key for obtaining high performance materials in a multitude of applications. Although control of carbon surface chemistry offers large potential in many technical relevant applications, qualitative and quantitative analysis of surface oxides for amorphous and porous carbons remains challenging. In this study, we attempt selective, organic chemistry-based functionalization of a polymer-derived porous model carbon featuring high oxygen loadings, with the aim to establish analytical standards for temperature programmed desorption (TPD) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). In this context, quantitative chemical reduction of an oxidized carbon material with lithium aluminum hydride (LiAlH4) is utilized as the key for the synthesis of carbon materials with defined ensembles of oxygen surface groups (hydroxyl groups and ethers). Based on this reduction strategy, selective LiAlH4 reduction based on protection group chemistry leads to aldehydes, ketones and quinones as surface functional groups and chemical grafting is studied for the selective introduction of phenyl esters, methyl ethers and carboxylic acids. All materials are evaluated with respect to the applicability as analytical standard by DRIFT spectroscopy, TPD, X-ray photoelectron spectroscopy and titration methods. (C) 2020 Elsevier Ltd. All rights reserved.