CN111155143A - Preparation method of two-dimensional layered metal organic framework nano material - Google Patents
Preparation method of two-dimensional layered metal organic framework nano material Download PDFInfo
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Abstract
The invention discloses a preparation method of a two-dimensional layered metal organic framework material. The invention prepares a uniform two-dimensional layered metal-organic framework material by electrochemically electrolyzing a metal foil in an organic ligand solution containing oxygen coordination groups. Firstly, 3,6,7,10, 11-hexahydroxy triphenyl is dispersed into deionized water, and an alkaline regulator is added to ensure that the mixture is fully ionized. Then, a metal foil is used as an anode and a cathode, and a certain voltage is applied between the two electrodes to make the ligand migrate to the surface of the anode. Further increasing the voltage to make the anode metal foil start to electrolyze and release metal ions, and further generating a two-dimensional metal organic framework film on the surface of the anode. The invention has the advantages of simple process equipment, accordance with the green preparation concept, lower production cost, shorter preparation period, controllable film layer number and high film conductivity.
Description
Technical Field
The invention belongs to the field of metal organic framework materials, and particularly relates to a preparation method of a two-dimensional layered metal organic framework nano material.
Background
Two-dimensional nanomaterials are materials with one dimension less than 100 nanometers in the geometric dimension. Two-dimensional nanomaterials that have been developed so far are graphene, two-dimensional transition metal chalcogenides, hexagonal boron nitride, borolene, germanene, black scale, two-dimensional organic framework materials, two-dimensional metallo-organic framework materials, and the like. When the geometric size of the material is smaller than a certain size, the nanocarbon material generally exhibits a unique energy band structure and excellent properties due to a surface effect, a quantum size effect, a quantum tunneling effect and a dielectric confinement effect. The two-dimensional nano material has unique physical and chemical properties and wide application prospect.
The two-dimensional metal organic framework nano Material (MOF) is a two-dimensional nano material which is formed by metal ions and organic ligands through coordination bonds and has a regular pore structure. Such materials typically have a large specific surface area and a large number of active sites. By changing the size and the structure of the organic ligand, the structure and the size of the pores of the two-dimensional MOF material can be effectively regulated and controlled. The two-dimensional MOF material has wide application prospects in the fields of gas sensing, catalysis, energy storage, thin film separation and the like. In addition, some MOF materials have excellent electrical and optical properties, and can be used as building units to prepare laminated devices with other two-dimensional nano materials, so that the MOF materials also have wide application prospects in the fields of electronics, photoelectronic devices and the like.
The current methods for preparing the MOF mainly comprise a hydrothermal method, a liquid phase ultrasonic method, an interface growth method, a chemical vapor deposition method and the like. The hydrothermal method is mainly to seal a solution of organic ligand and metal salt in a hydrothermal kettle and make it react at high temperature and high pressure to form coordination compounds (Chemistry of Materials,2012,24(18), 3511). The liquid phase ultrasound method is mainly a method in which an organic ligand and a metal salt are dispersed in a solution by the action of ultrasound and reacted to form a polymer (Nature Energy,2016,1(12), 16184). The materials prepared by the two methods are powder materials, have high yield and are mainly used in the fields of catalysis, energy storage and the like. Interfacial growth methods typically utilize gas-liquid interfaces or liquid-liquid interfacial confinement to produce MOF films (advanced materials,2018,30(10), 1704291.). The film prepared by the method is easy to damage and difficult to prepare on a large scale. The chemical vapor deposition method is a method of preparing a two-dimensional metal organic framework material which has been developed in recent years (naturematrices, 2016,15(3), 304). The method can be used for large-scale preparation, however, the prepared MOF material is composed of nano-scale particles, has low electrical properties and is difficult to be used for optoelectronic devices.
Therefore, other methods for preparing high-quality two-dimensional MOF conductive films are developed, and the large-scale preparation of the high-quality two-dimensional MOF conductive films is a research hotspot in the field of MOF materials.
Disclosure of Invention
Based on various short plates in the existing preparation method of the two-dimensional metal organic framework film, the invention provides a preparation method of a two-dimensional MOF film which is green, controllable in layer number, controllable in area and high in conductivity.
The invention provides a method for preparing a two-dimensional metal organic framework film material, which comprises the following steps:
HHTP is dispersed in water, and is added with an alkaline regulator to be ionized, and then reactant solution is obtained by ultrasonic treatment;
electrifying to react by taking metal foils as an anode and a cathode, and obtaining the two-dimensional metal organic framework film material shown in the formula I after the reaction is finished;
the HHTP is 3,6,7,10, 11-hexahydroxy triphenyl;
in the formula I, M is a metal ion.
In the above method, M is selected from any one of the following elements: fe. Co, Ni, Cu and Zn.
The alkaline regulator is at least one selected from ammonia water, sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, tetramethyl ammonium hydroxide solution, ethylenediamine solution and triethylamine solution. Specifically, the water solution can be 1mol/L sodium hydroxide water solution or 1mol/L potassium hydroxide water solution;
in the ultrasonic step, the time is 10min-50 min; specifically, it can be 15min, 20min or 30 min;
the ultrasonic frequency is 50HZ-100 HZ; specifically 60HZ, 70HZ or 80 HZ;
the HHTP concentration in the reactant solution is 0.0001-1.0 mol/L; specifically 0.001, 0.0012, 0.002, 0.0025, 0.005 or 0.01 mol/L;
applying a voltage to the anode and the cathode in the range of 0.3v-10 v; specifically 0.35V, 0.5V, 1.0V, 1.5V, 2.5V or 3V;
the time for applying voltage on the anode and the cathode is 0.2min-200 min; specifically 20min, 25min or 30 min;
applying a voltage between the two electrodes can make the ligand ions migrate to the surface of the anode, and then increasing the voltage further gradually electrolyzes the anode to release the metal ions, so that a coordination reaction occurs between the metal ions and the ligand ions to generate the MOF film on the surface of the anode.
The layer number of the two-dimensional metal organic framework film material is controllable.
The invention has the advantages that:
the two-dimensional layered metal organic framework film prepared by the invention has the advantages of controllable layer number, controllable area, high conductivity, simple operation, low cost, mild reaction condition and capability of meeting the concept of 'green preparation'.
Drawings
FIG. 1 is a theoretical simulation of the material of example 1.
Table 1 shows the unit cell parameters corresponding to the theoretical simulated structure of the material of example 1.
Fig. 2 is an XRD pattern and a theoretically calculated XRD pattern for the two-dimensional metal-organic framework material prepared in example 1.
In fig. 3, (a) is an electron microscope photograph of the two-dimensional metal organic framework material prepared in example 1, and (b) is an atomic force microscope photograph of the two-dimensional metal organic framework material prepared in example 1.
In fig. 4, (a) is a transmission microscope photograph of the two-dimensional metal organic framework material prepared in example 1, and (b) is a high resolution transmission microscope photograph of the two-dimensional metal organic framework material prepared in example 1.
FIG. 5 is a conductivity test of two-dimensional metal organic framework material prepared in example 1.
FIG. 6 is a statistical chart of the thickness and number of layers of two-dimensional metal organic framework films prepared by different reaction times.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1
1) Weighing 32.43mg of 2,3,6,7,10, 11-hexahydroxy triphenyl, dispersing into 50mL of deionized water, dropwise adding 50 microliters of 1mol/L sodium hydroxide aqueous solution, and carrying out 80HZ ultrasonic treatment for 10min to prepare a uniform reactant solution; wherein the molar concentration of HHTP in the solution is 0.002 mol/L;
2) a 1 x 1 cm copper foil was connected to the dc power supply anode and cathode.
3) Controlling the voltage to be 0.5V to ensure that the copper foil is gradually electrolyzed to generate copper ions, and further carrying out coordination reaction with 2,3,6,7,10, 11-hexahydroxy triphenyl ions on the surface of the copper foil. The reaction time was 20 min.
The reaction formula is as follows:
FIG. 1 is a theoretical simulation of the material of example 1.
Table 1 shows the unit cell parameters corresponding to the theoretical simulated structure of the material of example 1.
TABLE 1 cell parameters corresponding to theoretical simulated structures of the materials of example 1
FIG. 2 is an XRD pattern and a theoretical calculation XRD pattern of a two-dimensional metal organic framework material prepared in example 1, and the two-dimensional MOF prepared by the invention is completely consistent with a theoretical simulation.
Fig. 3 (a) is a scanning electron microscope photograph of the two-dimensional metal-organic framework material prepared in example 1, which shows that the layered metal-organic framework material prepared in the present invention. Fig. 3 (b) is an afm photograph of two-dimensional metal-organic framework material prepared in example 1, which further proves that the layered metal-organic framework thin film is prepared according to the present invention.
Fig. 4 (a) is a transmission photograph of the two-dimensional metal organic framework material prepared in example 1, and fig. 4 (b) is a high-resolution transmission photograph of the selected region of the two-dimensional metal organic framework material prepared in example 1, which proves that the two-dimensional material has a six-membered ring pore structure, and the measured value is consistent with the theoretical value.
FIG. 5 is a conductivity test of the two-dimensional metal organic framework material prepared in example 1, and the conductivity is 0.09S-cm-1On the left and right, much higher than the conductivity of MOF films reported at present.
Example 2
1) Weighing 16.21mg of 2,3,6,7,10, 11-hexahydroxy triphenyl, dispersing into 50mL of deionized water, dropwise adding 25 microliters of 1mol/L potassium hydroxide aqueous solution, and carrying out 50HZ ultrasonic treatment for 30min to prepare a uniform reactant solution; wherein the molar concentration of HHTP in the solution is 0.001 mol/L;
2) a 1 x 1 cm copper foil was connected to the dc power supply anode and cathode.
3) Controlling the voltage to be 0.35V to ensure that the copper foil is gradually electrolyzed to generate copper ions, further carrying out coordination reaction with 2,3,6,7,10, 11-hexahydroxy triphen ions on the surface of the anode, and changing the reaction time to obtain MOF films with different thicknesses.
FIG. 6 shows the thickness and the corresponding number of layers of two-dimensional MOF produced by atomic force microscopy at different reaction times.
Example 3
1) Weighing 81.05mg of 2,3,6,7,10, 11-hexahydroxy triphenyl, dispersing into 50mL of deionized water, dropwise adding 50 microliters of ammonia water solution, and carrying out 70HZ ultrasonic treatment for 15min to prepare a uniform reactant solution; wherein the molar concentration of HHTP in the solution is 0.005 mol/L;
2) a 1 x 1 cm cobalt foil was connected to the dc power supply anode and cathode.
3) Controlling the voltage to be 3.0V to ensure that the cobalt foil is gradually electrolyzed to generate cobalt ions, and further carrying out coordination reaction with 2,3,6,7,10, 11-hexahydroxy triphenyl ions on the surface of the anode for 20 min. To obtain Co3(HHTP)2A MOF film.
Example 4
1) Weighing 162.1mg of 2,3,6,7,10, 11-hexahydroxy triphenyl, dispersing into 50mL of deionized water, dropwise adding 25 microliters of triethylamine solution, and performing 60HZ ultrasonic treatment for 20min to prepare a uniform reactant solution; wherein the molar concentration of HHTP in the solution is 0.01 mol/L;
2) a 1 x 1 cm nickel foil was connected to the dc power supply anode and cathode.
3) Controlling the voltage to be 2.5V to ensure that the nickel foil is gradually electrolyzed to generate nickel ions, and further carrying out coordination reaction with 2,3,6,7,10, 11-hexahydroxy triphenyl ions on the surface of the anode for 20 min. Obtaining Ni3(HHTP)2A MOF film.
Example 5
1) Weighing 40.53mg of 2,3,6,7,10, 11-hexahydroxy triphenyl, dispersing into 50mL of deionized water, dropwise adding 25 microliters of tetramethylammonium hydroxide solution, and performing 50Hz ultrasound for 30min to prepare a uniform reactant solution; wherein the molar concentration of HHTP in the solution is 0.0025 mol/L;
2) 1X 1 cm of iron foil was connected to the anode and cathode of a DC power supply.
3) Controlling the voltage to be 1.0V to enable the iron foil to be gradually electrolyzed to generate iron ions, and further carrying out coordination reaction with 2,3,6,7,10, 11-hexahydroxy triphenyl ions on the surface of the anode for 25min to obtain Fe3(HHTP)2A MOF film.
Example 6
1) Weighing 20.26mg of 2,3,6,7,10, 11-hexahydroxy triphenyl, dispersing into 50mL of deionized water, dropwise adding 25 microliters of ethylenediamine solution, and carrying out 80HZ ultrasonic treatment for 20min to prepare a uniform reactant solution; wherein the molar concentration of HHTP in the solution is 0.0012 mol/L;
2) a 1 x 1 cm zinc foil was connected to the dc power supply anode and cathode.
3) Controlling the voltage to be 1.5V to ensure that the zinc foil is gradually electrolyzed to generate zinc ionsThe Zn is further subjected to coordination reaction with 2,3,6,7,10, 11-hexahydroxy triphenyl ions on the surface of the anode for 30min to obtain Zn3(HHTP)2A MOF film.
Claims (8)
1. A method for preparing a two-dimensional metal organic framework thin film material, comprising:
HHTP is dispersed in water, and is added with an alkaline regulator to be ionized, and then reactant solution is obtained by ultrasonic treatment;
electrifying to react by taking metal foils as an anode and a cathode, and obtaining the two-dimensional metal organic framework film material shown in the formula I after the reaction is finished;
the HHTP is 3,6,7,10, 11-hexahydroxy triphenyl;
in the formula I, M is a metal ion.
2. The method of claim 1, wherein: the M is selected from any one of the following elements: fe. Co, Ni, Cu and Zn.
3. The method according to claim 1 or 2, characterized in that: the alkaline regulator is at least one selected from ammonia water, sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, tetramethyl ammonium hydroxide solution, ethylenediamine solution and triethylamine solution.
4. A method according to any one of claims 1 to 3, wherein: in the ultrasonic step, the time is 10min-50 min;
the ultrasonic frequency is 50HZ-100 HZ.
5. The method according to any one of claims 1 to 4, wherein: the HHTP concentration in the reactant solution is 0.0001-1.0 mol/L.
6. The method according to any one of claims 1 to 4, wherein: and applying voltage to the anode and the cathode in the range of 0.3v-10 v.
7. The method according to any one of claims 1 to 6, wherein: the time for applying the voltage on the anode and the cathode is 0.2min-200 min.
8. The method according to any one of claims 1 to 7, wherein: the layer number of the two-dimensional metal organic framework film material is controllable.
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| CN114632547A (en) * | 2022-02-25 | 2022-06-17 | 武汉工程大学 | Preparation method and application of two-dimensional conductive MOF nanosheet loaded gold nanoparticle composite material |
| CN114854214A (en) * | 2021-02-03 | 2022-08-05 | 中国科学院化学研究所 | In-situ growth graphene two-dimensional covalent organic framework composite material and preparation method thereof |
| CN115926188A (en) * | 2023-01-10 | 2023-04-07 | 天津大学 | Salphen-based metal organic framework material, and preparation method and application thereof |
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| CN113235118A (en) * | 2021-05-17 | 2021-08-10 | 苏州大学 | Electrochemical synthesis method of conductive metal organic framework anode |
| CN114632547A (en) * | 2022-02-25 | 2022-06-17 | 武汉工程大学 | Preparation method and application of two-dimensional conductive MOF nanosheet loaded gold nanoparticle composite material |
| CN115926188A (en) * | 2023-01-10 | 2023-04-07 | 天津大学 | Salphen-based metal organic framework material, and preparation method and application thereof |
| CN115926188B (en) * | 2023-01-10 | 2023-09-05 | 天津大学 | Salphen-based metal organic framework material, preparation method and application |
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