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However, the covalent chemistry of this kind of 2D materials is still barely explored. Herein, the covalent functionalization with silanes of a magnetic NiFe\u2010LDH is reported. The synthetic route consists of a topochemical approach followed by anion exchange reaction with surfactant molecules prior to covalent functionalization with the (3\u2010aminopropyl)triethoxysilane (APTES) molecules. The functionalized NiFe\u2010APTES was fully characterized by X\u2010ray diffraction, infrared spectroscopy, electron microscopy, thermogravimetric analysis coupled with mass spectrometry and <jats:sup>29<\/jats:sup>Si solid\u2010state nuclear magnetic resonance, among others. The effect on the electronic properties of the functionalized LDH was investigated by a magnetic study in combination with M\u00f6ssbauer spectroscopy. 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