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Here, we demonstrate a protocol for the two-step synthesis of single-crystalline core-shells using a non-isostructural metal-organic framework (MOF) pair, HKUST-1 and MOF-5, which have well-matched crystal lattices.
Because of their designability and unprecedented synergistic effects, core-shell metal-organic frameworks (MOFs) have been actively examined recently. However, the synthesis of single-crystalline core-shell MOFs is very challenging, and thus a limited number of examples have been reported. Here, we suggest a method of synthesizing single-crystalline HKUST-1@MOF-5 core-shells, which is HKUST-1 at the center of MOF-5. Through the computational algorithm, this pair of MOFs was predicted to have the matched lattice parameters and chemical connection points at the interface. To construct the core-shell structure, we prepared the octahedral- and cubic-shaped HKUST-1 crystals as a core MOF, in which the (111) and (001) facets were mainly exposed, respectively. Via the sequential reaction, the MOF-5 shell was well-grown on the exposed surface, showing a seamless connect interface, which resulted in the successful synthesis of single-crystalline HKUST-1@MOF-5. Their pure phase formation was proved by optical microscopic images and powder X-ray diffraction (PXRD) patterns. This method presents the potential of and insights into the single-crystalline core-shell synthesis with different kinds of MOFs.
MOF-on-MOF is a type of hybrid material comprising two or more different metal-organic frameworks (MOFs)1,2,3. Owing to the various possible combinations of constituents and structures, MOF-on-MOFs provide varied novel composites with remarkable properties, which have not been achieved in single MOFs, offering great potential in many applications4,5,6. Among the various types of MOF-on-MOFs, a core-shell structure in which one MOF surrounds another has the advantage of optimizing the....
CAUTION: Before conducting the experiment, thoroughly read and comprehend the material safety data sheets (MSDSs) of the chemicals used in this protocol. Wear appropriate protective gear. Utilize a fume hood for all synthesis procedures.
1. Synthesis of cubic HKUST-1
NOTE: The experimental procedure was based on a previously reported method14. For core-shell synthesis, 10 pots were synthesized at a time. Therefore, 10 pots of t.......
According to the two calculated structures of the HKUST-1@MOF-5 core-shell system14, in both the (001) and (111) planes, the Cu sites from the metal nodes of HKUST-1 and the oxygen sites from the carboxylates of MOF-5 are well-matched as the chemical connection points at the interface between the two MOFs (Figure 1). Therefore, cubic and octahedral crystals of HKUST-1, in which the (001) and (111) planes are exposed, respectively, were synthesized as the core MOFs for.......
In this protocol, cubic- and octahedral-shaped HKUST-1 crystals were synthesized, referring to a previously reported method14. For the synthesis of HKUST-1, H3BTC solution was added while heating and stirring the solution of Cu(NO3)2·2.5H2O to prevent the precipitation of H3BTC as the temperature decreased. Subsequently, acetic acid was added immediately to prevent fast nucleation and ensure the growth of a large single crystal. As soon a.......
This work was supported by the National Research Foundation of Korea (NRF) Grant funded by the Ministry of Science and the ICP (No. NRF-2020R1A2C3008908 and 2016R1A5A1009405).
....Name | Company | Catalog Number | Comments |
Acetic acid | DAEJUNG | 1002-4400 | Synthesis of HKUST-1 (protocol steps 1.4, and 2.4) |
Copper(II) nitrate hemipentahydrate | Sigma Aldrich | 223395-100G | Synthesis of HKUST-1 (protocol steps 1.1, and 2.1) |
D2 PHASER | Bruker AXS | DOC-B88-EXS017-V3 | Powder X-ray diffraction |
Digital stirring hot plate | Thermo Scientific | SP131320-33Q | Hotplate for heating and stirring (protocol steps 1.2, and 2.2) |
Direct-Q3UV water purification system | MILLIPORE | ZRQSVP030 | Deionized water (protocol steps 1.1, and 2.1) |
Ethyl alcohol anhydrous, 99.9% | DAEJUNG | 4023-4100 | Synthesis of HKUST-1 (protocol steps 1.2, and 2.2) |
Forced convection oven (OF-02P/PW) | JEIO TECH | EDA8136 | Oven for heating reaction (protocol steps 1.5, 2.5, and 3.4) |
N,N-diethylformamide | TCI | D0506 | Synthesis of HKUST-1@MOF-5 (protocol step 3.1) |
N,N'-Dimethylformamide | DAEJUNG | 6057-4400 | Synthesis of HKUST-1 (protocol steps 1.1, and 2.1) |
Stereo microscopes | Nikon | SMZ745T | Optical Microscope |
Terephthalic acid | Sigma Aldrich | 185361-500G | Synthesis of HKUST-1@MOF-5 (protocol step 3.1) |
Trimesic acid | Sigma Aldrich | 482749-100G | Synthesis of HKUST-1 (protocol steps 1.2, and 2.2) |
Ultrasonic cleaner | BRANSONIC | CPX-952-338R | Sonicator with bath for dissolving solution (protocol step 3.1) |
Zinc nitrate hexahydrate | Sigma Aldrich | 228737-100G | Synthesis of HKUST-1@MOF-5 (protocol step 3.1) |
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