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In Situ FTIR Spectroscopy for Scanning Accessible Active Sites in Defect-Engineered UiO-66.

ABSTRACT: Three UiO-66 samples were prepared by solvothermal synthesis using the defect engineering approach with benzoic acid as a modulator. They were characterized by different techniques and their acidic properties were assessed by FTIR spectroscopy of adsorbed CO and CD₃CN. All samples evacuated at room temperature contained bridging μ₃-OH groups that interacted with both probe molecules. Evacuation at 250 °C leads to the dehydroxylation and disappearance of the μ₃-OH groups. Modulator-free synthesis resulted in a material with open Zr sites. They were detected by low-temperature CO adsorption on a sample evacuated at 200 °C and by CD₃CN even on a sample evacuated at RT. However, these sites were lacking in the two samples obtained with a modulator. IR and Raman spectra revealed that in these cases, the Zr⁴⁺ defect sites were saturated by benzoates, which prevented their interaction with probe molecules. Finally, the dehydroxylation of all samples produced another kind of bare Zr sites that did not interact with CO but formed complexes with acetonitrile, probably due to structural rearrangement. The results showed that FTIR spectroscopy is a powerful tool for investigating the presence and availability of acid sites in UiO-66, which is crucial for its application in adsorption and catalysis.

SUBMITTER: Butova VV

PROVIDER: S-EPMC10222444 | biostudies-literature | 2023 May

REPOSITORIES: biostudies-literature

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In Situ FTIR Spectroscopy for Scanning Accessible Active Sites in Defect-Engineered UiO-66.

Butova Vera V VV Zdravkova Videlina R VR Burachevskaia Olga A OA Tereshchenko Andrei A AA Shestakova Pavletta S PS Hadjiivanov Konstantin I KI

Nanomaterials (Basel, Switzerland) 20230518 10

Three UiO-66 samples were prepared by solvothermal synthesis using the defect engineering approach with benzoic acid as a modulator. They were characterized by different techniques and their acidic properties were assessed by FTIR spectroscopy of adsorbed CO and CD3CN. All samples evacuated at room temperature contained bridging μ3-OH groups that interacted with both probe molecules. Evacuation at 250 °C leads to the dehydroxylation and disappearance of the μ3-OH ...[more]

PMID: 37242091

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Project description:BackgroundRepair of large-sized bone defects is a challengeable obstacle in orthopedics and evoked the demand for the development of biomaterials that could induce bone repair in such defects. Recently, UiO-66 has emerged as an attractive metal-organic framework (MOF) nanostructure that is incorporated in biomedical applications due to its biocompatibility, porosity, and stability. In addition, its osteogenic properties have earned a great interest as a promising field of research. Thus, the UiO-66 was prepared in this study and assessed for its potential to stimulate and support osteogenesis in vitro and in vivo in a rabbit femoral condyle defect model. The nanomaterial was fabricated and characterized using x-ray diffraction (XRD) and transmission electron microscopy (TEM). Afterward, in vitro cytotoxicity and hemolysis assays were performed to investigate UiO-66 biocompatibility. Furthermore, the material in vitro capability to upregulate osteoblast marker genes was assessed using qPCR. Next, the in vivo new bone formation potential of the UiO-66 nanomaterial was evaluated after induction of bone defects in rabbit femoral condyles. These defects were left empty or filled with UiO-66 nanomaterial and monitored at weeks 4, 8, and 12 after bone defect induction using x-ray, computed tomography (CT), histological examinations, and qPCR analysis of osteocalcin (OC) and osteopontin (OP) expressions.ResultsThe designed UiO-66 nanomaterial showed excellent cytocompatibility and hemocompatibility and stimulated the in vitro osteoblast functions. The in vivo osteogenesis was enhanced in the UiO-66 treated group compared to the control group, whereas evidence of healing of the treated bone defects was observed grossly and histologically. Interestingly, UiO-66 implanted defects displayed a significant osteoid tissue and collagen deposition compared to control defects. Moreover, the UiO-66 nanomaterial demonstrated the potential to upregulate OC and OP in vivo.ConclusionsThe UiO-66 nanomaterial implantation possesses a stimulatory impact on the healing process of critical-sized bone defects indicating that UiO-66 is a promising biomaterial for application in bone tissue engineering.

Dataset Information

In Situ FTIR Spectroscopy for Scanning Accessible Active Sites in Defect-Engineered UiO-66.

Publications

In Situ FTIR Spectroscopy for Scanning Accessible Active Sites in Defect-Engineered UiO-66.

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