CN115433464A - Preparation method of interconnected non-close-packed binary superstructure - Google Patents
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Abstract
The invention relates to the technical field of materials and nanotechnology, in particular to a preparation method of an interconnected non-close-packed binary superstructure. Mainly aiming at the problem that replaceable elements are more limited to inorganic nanoparticles, and most of reports show that the prepared binary superstructure is often a close-packed structure, the following technical scheme is provided: dispersing the mixed solution into an organic solvent containing a ligand in an ultrasonic mode, then uniformly mixing the mixed solution with a colloid nanocrystalline solution coated by the ligand, and completing the preparation of the interconnected non-close-packed binary superstructure by a gas-liquid interface assembly method. The invention uses hydrolyzable zeolite imidazole ester framework material with special shape as the construction element of the binary superstructure, and utilizes the characteristics of local slow hydrolysis and condensation in the assembly process to realize one-step assembly and construction of the non-close-packed binary superstructure material, and simultaneously, the type and size of the other nano-particles as the element have strong adjustability.
Description
Technical Field
The invention relates to the technical field of materials and nanotechnology, in particular to a preparation method of an interconnected non-close-packed binary superstructure.
Background
Self-assembly is an important way for creating new materials, and various different building elements can be constructed into an ordered superstructure by self-assembly. The material can not only embody the unique nano effect of the nano particles, but also show the integration property different from the nano particles.
At present, a plurality of different types of construction elements can be constructed into a superstructure material with regular structure and complex shape through interaction of intermolecular force, electrostatic force and the like by self-assembly. Compared with a single-component superstructure material, the dual superstructure material is poor in structure adjustability, low in performance integration level and the like, the dual superstructure material is formed by two different elements, the structure is more complex, and meanwhile, the performance integration is higher based on the synergistic effect of different components. Although it is reported that various binary superstructures can be prepared by replacing components in the binary superstructures, the replaceable moieties are more limited to inorganic nanoparticles, while most of the prepared binary superstructures are reported to tend to be close-packed structures.
Therefore, it is necessary to develop a simple, efficient and universal assembly method to construct non-close-packed superstructure materials with novel structural interconnections. In view of this, we propose a method for the preparation of interconnected non-close-packed binary superstructures.
Disclosure of Invention
The invention aims to provide a preparation method of an interconnected non-close-packed binary superstructure, aiming at the problems that replaceable elements in the background technology are more limited to inorganic nanoparticles, and most of reports show that the prepared binary superstructure is often a close-packed structure.
The technical scheme of the invention is as follows: a method for preparing an interconnected non-close-packed binary superstructure comprises the following steps:
the method comprises the following steps: mixing 300-1200mgZn (CH) 3 COO) 2 ·2H 2 Dissolving O in 5-20mL of water, and recording as A solution; the mixed solution of 5-20mL2.58M2-methylimidazole and 5-20mL0.54mMCTAB is denoted as a solution B; rapidly adding the solution A into the solution B under stirring, stirring for 15 seconds, and standing at room temperature for 2 hours; obtaining ZIF-8 powder through the steps of centrifuging, drying and grinding;
step two: preparation of oleic acid coated ferroferric oxide (Fe) by pyrolysis of iron oleate, manganese oleate and mixture of cobalt oleate and iron oleate 3 O 4 ) Manganese monoxide (MnO) and cobalt ferrite (CoFe) 2 O 4 ) A nanoparticle;
step three: dispersing 15-25mg of truncated cube metal organic framework powder into 10mL of solution, and performing ultrasonic treatment for 5-20 minutes to obtain a stable dispersion system;
step four: uniformly mixing the dispersion system obtained in the step three with 1-5mg/mL of nano-particle solution modified by oleic acid according to the equal volume;
step five: and volatilizing and assembling the mixed solution obtained in the fourth step of 20-50 mu L by using a gas-liquid interface assembly method to obtain a two-dimensional film, and obtaining the final interconnected non-close-packed binary superstructure material through the steps of film fishing and drying.
Preferably, in the first step, the ZIF-8 powder metal-organic framework is in the shape of a truncated cube, and the metal-organic framework is a zeolite imidazole ester framework material.
Preferably, the solution in step three is 1.5-2.5% (v/v) oleic acid in n-hexane.
Preferably, the nanoparticles in step four are ferroferric oxide (Fe) 3 O 4 ) Manganese monoxide (MnO), cobalt ferrite (CoFe) 2 O 4 ) Any one or more of them.
Preferably, the solution A in the first step is 300mgZn (CH) 3 COO) 2 ·2H 2 O and 5mL of water, and the solution B is a mixed solution of 5mL 2.58M2-methylimidazole and 5mL 0.54mMCTAB.
Preferably, the solution A in the first step is 600mgZn (CH) 3 COO) 2 ·2H 2 O and 10mL of water, and the solution B is a mixed solution of 10mL2.58M2-methylimidazole and 10mL0.54mMCTAB.
Preferably, the solution A in the first step is 1200mgZn (CH) 3 COO) 2 ·2H 2 O and 20mL of water, and the solution B is a mixed solution of 20mL2.58M2-methylimidazole and 20mL0.54mMCTAB.
Compared with the prior art, the invention has the following beneficial technical effects:
1. firstly synthesizing metal organic framework powder, dispersing the metal organic framework powder into an organic solvent containing a ligand in an ultrasonic mode, then uniformly mixing the metal organic framework powder with a colloidal nanocrystal solution coated by the ligand, and completing preparation of an interconnected non-close-packed binary superstructure by a gas-liquid interface assembly method;
2. the invention uses a slowly hydrolysable and coagulable metal organic framework as an assembly element, so that an interconnected non-close-packed structure is formed in the hydrolysis and coagulation processes, and meanwhile, the specific combination of a coagulation position and ligand-coated nano particles enables nano crystals to gather and surround the periphery of an interconnected part to form an interconnected non-close-packed binary superstructure;
3. the invention uses hydrolyzable zeolite imidazole ester framework material with special shape as the construction element of the binary superstructure, and utilizes the characteristics of local slow hydrolysis and condensation in the assembly process to realize one-step assembly and construction of the non-close-packed binary superstructure material, and simultaneously, the type and size of the other nano-particles as the element have strong adjustability.
Drawings
FIG. 1 shows oleic acid-modified Fe 3 O 4 Interconnected non-close-packed binary superstructure ZIF-8/Fe formed by co-assembling nanoparticles and ZIF-8 3 O 4 Transmission electron microscopy and energy spectroscopy;
FIG. 2 is a transmission electron micrograph of interconnected non close-packed binary superstructures ZIF-8/MnO formed by co-assembling dioleic acid modified MnO nanoparticles with ZIF-8 according to an embodiment of the present invention;
FIG. 3 is a trioleic acid modified CoFe example of the invention 2 O 4 Interconnected non-close-packed binary superstructure ZIF-8/CoFe formed by co-assembling nanoparticles and ZIF-8 2 O 4 Transmission electron micrograph (D).
Detailed Description
The technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
Example one
As shown in fig. 1, the method for preparing an interconnected non-close-packed binary superstructure provided by the invention comprises the following preparation steps:
the method comprises the following steps: at room temperature, 300mgZn (CH) 3 COO) 2 ·2H 2 Dissolving O in 5mL of water, and recording as A solution; the mixed solution of 5mL2.58M2-methylimidazole and 5mL0.54mMCTAB is recorded as solution B; slowly stirring, quickly adding the solution A into the solution B, stirring for 15 seconds, and standing at room temperature for 2 hours; obtaining truncated cube ZIF-8 powder through the steps of centrifugation, drying, grinding and the like;
step two: 9g of iron oleate, 2.15g of oleic acid and 50g of octadecene were charged into a 100mL three-necked flask, N 2 Gradually heating to 120 deg.C under protection, vacuumizing for 1 hr, and vacuumizing and N-charging for 3 times 2 Operation, finally in N 2 Heating to 320 ℃ in the atmosphere and stirring at constant temperature for 1 hour to complete the synthesis of particles; finally adding 50mL of ethanol, centrifugally washing, dispersing in 10mL of normal hexane, and finishing Fe coated with oleic acid 3 O 4 Preparing nano particles;
step three: adding 25mg of truncated cube ZIF-8 powder into 10mL1.5% (v/v) normal hexane solution of oleic acid, and performing ultrasonic treatment for 10 minutes to uniformly disperse the mixture to obtain stable colloidal solution;
step four: mixing the dispersion obtained in the third step with oleic acid-modified 2mg/mL Fe 3 O 4 Uniformly mixing the nanoparticle solution according to the equal volume;
step five: volatilizing and assembling 20 mu L of mixed solution obtained in the fourth step by using a gas-liquid interface assembly method to obtain a two-dimensional film, and obtaining interconnected non-close-packed binary ZIF-8/Fe through the steps of film fishing and drying 3 O 4 A superstructure.
Oleic acid modified Fe in this example 3 O 4 And (3) a transmission electron microscope and an energy spectrum of an interconnected non-close-packed binary superstructure formed by co-assembling the nanoparticles and the ZIF-8. As can be seen from FIGS. 1a-1b, ZIF-8 particles were bonded to each other in a head-to-head fashion with significant gaps between the particles and a ring of nanoparticles surrounded by the junction. From the spectrum of FIG. 1c, the interconnect structure contains ZIF-8 and Fe 3 O 4 And the distribution of the elements indicates that the superstructure is in an interconnected, non-close-packed form.
Example two
As shown in fig. 2, the present invention provides a method for preparing an interconnected non-close-packed binary superstructure, which further includes the following steps:
the method comprises the following steps: at room temperature, 600mgZn (CH) 3 COO) 2 ·2H 2 Dissolving O in 10mL of water, and marking as A solution; a mixed solution of 10mL of 2.58M 2-methylimidazole and 10mL of 0.54 mL of MCTAB was designated as a solution B; rapidly adding the solution A into the solution B under stirring, stirring for 15s, and standing at room temperature for 2 hours; obtaining truncated cube ZIF-8 powder through operations of centrifugation, drying and grinding;
step two: 6mmol MnO powder (ex Aladdin), 8.5mL oleic acid and 18mL octadecene were added to a 100mL three-necked flask, N 2 Gradually heating to 120 deg.C under protection, vacuumizing for 1 hr, and vacuumizing and charging N for 3 times 2 Operation, finally in N 2 Heating to 320 ℃ in the atmosphere and stirring at constant temperature for 2 hours to complete a particle synthesis experiment; finally, 100mL of ethanol is added, and after centrifugal washing, the mixture is dispersed in 20mL of normal hexane to complete the preparation of the manganese monoxide (MnO) nano particles coated by the oleic acid;
step three: adding 25mg of truncated cube ZIF-8 powder into 10ml L2.0% (v/v) oleic acid normal hexane, and performing ultrasonic treatment for 10 minutes to uniformly disperse the mixture to obtain a stable colloidal solution;
step four: uniformly mixing the dispersion system obtained in the step three with a MnO nanoparticle solution of 3mg/mL modified by oleic acid according to the equal volume;
step five: and volatilizing and assembling 35 mu L of the mixed solution obtained in the fourth step by using a gas-liquid interface assembly method to obtain a two-dimensional film, and obtaining an interconnected non-close-packed binary ZIF-8/MnO superstructure through the steps of film fishing and drying.
In the embodiment, mnO nanoparticles modified by oleic acid and ZIF-8 are assembled together to form a transmission electron microscope with an interconnected non-close-packed binary superstructure. ZIF-8 particles are mutually connected in a head-to-head mode, obvious gaps are formed among the particles, and a circle of MnO nano particles are distributed at the connecting part.
EXAMPLE III
As shown in fig. 3, the present embodiment of the method for preparing an interconnected non-close-packed binary superstructure further includes the following steps:
the method comprises the following steps: 1200mgZn (CH) at room temperature 3 COO) 2 ·2H 2 Dissolving O in 20mL of water, and marking as A solution; a mixed solution of 20mL2.58M2-methylimidazole and 20mL of 0.54mMCTAB is taken as a solution B; and quickly adding the solution A into the solution B under stirring, stirring for 15 seconds, and standing at room temperature for 2 hours. And (3) obtaining the truncated cube ZIF-8 powder through operations of centrifugation, drying and grinding.
Step two: 5.6g of iron acetylacetonate, 2.0g of cobalt acetylacetonate, 4.5g of oleic acid, 21.0g of oleylamine and 25mL of benzyl ether were placed in a 100mL three-necked flask and mixed uniformly, and N 2 Gradually heating to 120 deg.C under protection, vacuumizing for 1 hr, and vacuumizing and N-charging for 3 times 2 Operation, finally in N 2 Heating to 200 ℃ in the atmosphere and keeping the temperature constant for 90 minutes, then continuously heating to 295 ℃ and keeping the temperature constant for 1 hour to finish the particle synthesis experiment; finally adding 50 ethanol, centrifugally washing, dispersing in 10mL of normal hexane, and finishing the oleic acid coated CoFe 2 O 4 And (4) preparing.
Step three: adding 25mg of truncated cube ZIF-8 powder into 10mL2.5% (v/v) oleic acid n-hexane, and performing ultrasonic treatment for 10 minutes to uniformly disperse the powder to obtain a stable colloidal solution;
step four: mixing the dispersion of step three with oleic acid-modified 5mg/mL CoFe 2 O 4 Uniformly mixing the nanoparticle solution according to the equal volume;
step five: assembling method by using gas-liquid interfaceVolatilizing and assembling 50 mu L of mixed solution obtained in the fourth step to obtain a two-dimensional film, and obtaining interconnected non-close-packed binary ZIF-8/CoFe through the steps of film fishing and drying 2 O 4 A superstructure.
Oleic acid modified CoFe in this example 2 O 4 And the nanoparticles and the ZIF-8 are assembled together to form the transmission electron microscope with the interconnected non-close-packed binary superstructure. ZIF-8 particles are connected with each other in a head-to-head mode, and a circle of CoFe is obviously accumulated at the connection part 2 O 4 And (3) nanoparticles.
The above embodiments are only some preferred embodiments of the present invention, and many alternative modifications and combinations of the above embodiments may be made by those skilled in the art based on the technical solution of the present invention and the related teachings of the above embodiments.
Claims (7)
1. A preparation method of an interconnected non-close-packed binary superstructure is characterized by comprising the following steps:
the method comprises the following steps: 300-1200mgZn (CH) 3 COO) 2 ·2H 2 Dissolving O in 5-20mL of water, and marking as A solution; the mixed solution of 5-20mL2.58M2-methylimidazole and 5-20mL0.54mMCTAB is denoted as a solution B; rapidly adding the solution A into the solution B under stirring, stirring for 15 seconds, and standing at room temperature for 2 hours; obtaining ZIF-8 powder through the steps of centrifuging, drying and grinding;
step two: preparation of oleic acid coated ferroferric oxide (Fe) by pyrolysis of iron oleate, manganese oleate and a mixture of cobalt oleate and iron oleate 3 O 4 ) Manganese monoxide (MnO) and cobalt ferrite (CoFe) 2 O 4 ) A nanoparticle;
step three: dispersing 15-25mg of truncated cube metal organic framework powder into 10mL of solution, and performing ultrasonic treatment for 5-20 minutes to obtain a stable dispersion system;
step four: uniformly mixing the dispersion system obtained in the step three with 1-5mg/mL nano-particle solution modified by oleic acid according to the equal volume;
step five: and volatilizing and assembling the mixed solution obtained in the fourth step of 20-50 mu L by using a gas-liquid interface assembly method to obtain a two-dimensional film, and obtaining the final interconnected non-close-packed binary superstructure material through the steps of film fishing and drying.
2. The method of claim 1, wherein in step one, the ZIF-8 powder metal organic framework is in the shape of a truncated cube, and the metal organic framework is a zeolitic imidazolate framework material.
3. The method of claim 1, wherein the solution in step three is 1.5-2.5% (v/v) n-hexane of oleic acid.
4. The method of claim 1, wherein the nanoparticles in step four are iron oxide (Fe) 3 O 4 ) Manganese monoxide (MnO), cobalt ferrite (CoFe) 2 O 4 ) Any one or more of them.
5. The method of claim 1, wherein the solution A in step one is 300mg Zn (CH) 3 COO) 2 ·2H 2 O and 5mL of water, and the solution B is a mixed solution of 5mL 2.58M2-methylimidazole and 5mL 0.54mMCTAB.
6. The method of claim 1, wherein the solution A in step one is 600mg Zn (CH) 3 COO) 2 ·2H 2 O and 10mL of water, and the solution B is a mixed solution of 10mL2.58M2-methylimidazole and 10mL0.54mMCTAB.
7. The method for preparing an interconnected non-close-packed binary superstructure according to claim 1, wherein the solution A in the first step is1200mgZn(CH 3 COO) 2 ·2H 2 O and 20mL of water, and the solution B is a mixed solution of 20mL2.58M2-methylimidazole and 20mL0.54mMCTAB.
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