Room-Temperature Synthesis of UiO-66 and Thermal Modulation of Densities of Defect Sites

Matthew R. DeStefano; Timur Islamoglu; Sergio J. Garibay; Joseph T Hupp; Omar K. Farha

doi:10.1021/acs.chemmater.6b05115

Room-Temperature Synthesis of UiO-66 and Thermal Modulation of Densities of Defect Sites

Matthew R. DeStefano, Timur Islamoglu, Sergio J. Garibay, Joseph T Hupp, Omar K. Farha

Northwestern University

Research output: Contribution to journal › Article › peer-review

141 Citations (Scopus)

Abstract

UiO-66 is an archetypal zirconium-based metal-organic framework (MOF) that is constructed from hexanuclear zirconium oxide clusters as secondary building units (SBUs) and 1,4-benzenedicarboxylate (bdc) linkers. For the first time, a room-temperature solution-based synthesis is reported for UiO-66 and several of its derivatives, UiO-66-X (X = NH₂, OH, or NO₂), resulting in materials that are as porous and crystalline as those made at elevated temperatures. In addition, via modulation of the temperature at which UiO-66 is synthesized, the number of defect sites can be varied. It was found through N₂ sorption isotherm analysis and potentiometric acid-base titrations that increasing the synthesis temperature from 25 to 130 °C results in a systematic decrease in the number of defect sites in UiO-66. The results suggest that, with respect to this synthetic procedure, a maximal number of defect sites is achieved [∼1.3 missing linkers per Zr₆O₄(OH)₄(bdc)₆] at a temperature of 45 °C.

Original language	English
Pages (from-to)	1357-1361
Number of pages	5
Journal	Chemistry of Materials
Volume	29
Issue number	3
DOIs	https://doi.org/10.1021/acs.chemmater.6b05115
Publication status	Published - Feb 14 2017

ASJC Scopus subject areas

Chemistry(all)
Chemical Engineering(all)
Materials Chemistry

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abstract = "UiO-66 is an archetypal zirconium-based metal-organic framework (MOF) that is constructed from hexanuclear zirconium oxide clusters as secondary building units (SBUs) and 1,4-benzenedicarboxylate (bdc) linkers. For the first time, a room-temperature solution-based synthesis is reported for UiO-66 and several of its derivatives, UiO-66-X (X = NH2, OH, or NO2), resulting in materials that are as porous and crystalline as those made at elevated temperatures. In addition, via modulation of the temperature at which UiO-66 is synthesized, the number of defect sites can be varied. It was found through N2 sorption isotherm analysis and potentiometric acid-base titrations that increasing the synthesis temperature from 25 to 130 °C results in a systematic decrease in the number of defect sites in UiO-66. The results suggest that, with respect to this synthetic procedure, a maximal number of defect sites is achieved [∼1.3 missing linkers per Zr6O4(OH)4(bdc)6] at a temperature of 45 °C.",

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AU - DeStefano, Matthew R.

AU - Islamoglu, Timur

AU - Garibay, Sergio J.

AU - Hupp, Joseph T

AU - Farha, Omar K.

PY - 2017/2/14

Y1 - 2017/2/14

N2 - UiO-66 is an archetypal zirconium-based metal-organic framework (MOF) that is constructed from hexanuclear zirconium oxide clusters as secondary building units (SBUs) and 1,4-benzenedicarboxylate (bdc) linkers. For the first time, a room-temperature solution-based synthesis is reported for UiO-66 and several of its derivatives, UiO-66-X (X = NH2, OH, or NO2), resulting in materials that are as porous and crystalline as those made at elevated temperatures. In addition, via modulation of the temperature at which UiO-66 is synthesized, the number of defect sites can be varied. It was found through N2 sorption isotherm analysis and potentiometric acid-base titrations that increasing the synthesis temperature from 25 to 130 °C results in a systematic decrease in the number of defect sites in UiO-66. The results suggest that, with respect to this synthetic procedure, a maximal number of defect sites is achieved [∼1.3 missing linkers per Zr6O4(OH)4(bdc)6] at a temperature of 45 °C.

AB - UiO-66 is an archetypal zirconium-based metal-organic framework (MOF) that is constructed from hexanuclear zirconium oxide clusters as secondary building units (SBUs) and 1,4-benzenedicarboxylate (bdc) linkers. For the first time, a room-temperature solution-based synthesis is reported for UiO-66 and several of its derivatives, UiO-66-X (X = NH2, OH, or NO2), resulting in materials that are as porous and crystalline as those made at elevated temperatures. In addition, via modulation of the temperature at which UiO-66 is synthesized, the number of defect sites can be varied. It was found through N2 sorption isotherm analysis and potentiometric acid-base titrations that increasing the synthesis temperature from 25 to 130 °C results in a systematic decrease in the number of defect sites in UiO-66. The results suggest that, with respect to this synthetic procedure, a maximal number of defect sites is achieved [∼1.3 missing linkers per Zr6O4(OH)4(bdc)6] at a temperature of 45 °C.

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