CN113834856A - Large-size superlattice film and preparation method and application thereof - Google Patents
Large-size superlattice film and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a large-size superlattice thin film and a preparation method and application thereof. The superlattice film is a three-dimensional porous film containing a superlattice material; the superlattice material has a chemical formula of A. nPbX2Wherein A is selected from compounds having a structure represented by formula 1 or formula 2:
R1、R2、R3、R4、R1’、R2’、R3’、R4' same or different, independently from each other selected from C1‑10An alkyl group; r5、R6、R5’、R6’、R7’、R8' same or different, independently from each other selected from C1‑10Alkyl, H; x represents halogen; n is not less than 4 and is an integer. The invention adopts a simple immersion method to synthesize the three-dimensional porous membrane of the superlattice material in a large area.
Description
Technical Field
The invention belongs to the field of superlattice materials, and particularly relates to a large-size superlattice film and a preparation method and application thereof.
Background
At present, a three-dimensional porous membrane is very difficult to prepare from a two-dimensional material, and the preparation of a three-dimensional porous structure from a two-dimensional material reported in the prior art mainly focuses on preparing graphene sheets into a three-dimensional porous graphene nano-mesh, graphene aerogel and graphene foam, but the materials are difficult to form into a membrane, and particularly difficult to become a crystalline membrane.
On the other hand, a superlattice material is made into a large-area film, which is easy to crack, and a method for obtaining the superlattice material with a large area is not found in the prior art. Porous membranes are very popular for gas sensors because of their hierarchical structure of pores.
Disclosure of Invention
The invention provides a superlattice film, which is a three-dimensional porous film containing superlattice materials;
the superlattice material has a chemical formula of A.nPbX2Wherein A is selected from compounds having a structure represented by formula 1 or formula 2:
R1、R2、R3、R4、R1’、R2’、R3’、R4' same or different, independently from each other selected from C1-10Alkyl radicals, e.g. C1-6Alkyl, illustratively methyl, ethyl, propyl, or butyl;
R5、R6、R5’、R6’、R7’、R8' same or different, independently from each other selected from C1-10Alkyl, H, e.g. C1-6Alkyl, H, exemplified by methyl, ethyl, H;
x represents halogen, such as F, Cl, Br or I, preferably I;
n is 4 or more and is an integer, preferably, n is 4.
According to an embodiment of the present invention, in formula 1, R1、R2、R3、R4And is selected from methyl or ethyl.
According to an embodiment of the present invention, in formula 1, R5、R6And is selected from methyl, ethyl or H.
According to an embodiment of the present invention, in formula 2, R1’、R2’、R3’、R4' same, selected from methyl or ethyl.
According to an embodiment of the present invention, in formula 2, R5’、R6’、R7’、R8' same, selected from methyl, ethyl or H.
According to an exemplary embodiment of the invention, a is selected from compounds having a structure as shown in any one of formulas 3-5:
wherein the compound of formula 3 is abbreviated as MeDAB, the compound of formula 4 is abbreviated as EtDAB, and the compound of formula 5 is abbreviated as MeBEN.
According to an exemplary aspect of the invention, the superlattice material may be selected from MeDAB 4PbI2，EtDAB·4PbI2Or MeBEN 4PbI2。
According to an embodiment of the present invention, the superlattice film comprises the superlattice material described above and a porous base film, the superlattice material being distributed on a surface and in pores of the porous base film. Preferably, the superlattice material does not fill all of the pores of the porous base film.
According to an embodiment of the present invention, the porous base film may be selected from a fiber-based porous membrane, such as filter paper, a nylon porous filter membrane, a polyethylene porous membrane (PP porous membrane). Preferably, the pore size of the porous base membrane is from 100nm to 10 μm, for example from 500nm to 5 μm.
According to an embodiment of the present invention, a loading amount of the superlattice material on the porous base film is 0.5-2mg/cm2For example, 0.6 to 1.5mg/cm2Exemplary is 0.7mg/cm2、0.8mg/cm2、0.836mg/cm2、0.9mg/cm2、1.0mg/cm2、1.2mg/cm2。
According to an embodiment of the present invention, the specification (e.g., size, shape) of the superlattice film is determined by the porous base film.
According to an exemplary aspect of the present invention, the superlattice film comprises a superlattice material and a porous base film, the superlattice material is distributed on the surface and in the pores of the porous base film, and the superlattice material does not fill all the pores of the porous base film;
wherein the superlattice material is selected from MeDAB 4PbI2，EtDAB·4PbI2Or MeBEN 4PbI2；
The porous basement membrane is filter paper, a nylon porous filter membrane or a polyethylene porous membrane.
According to an embodiment of the present invention, the superlattice film has a morphology substantially as shown by b in fig. 3.
According to an embodiment of the present invention, the process for preparing the superlattice material comprises the following steps: a compound with a structure shown in formula 1 or formula 2 and PbX2Dissolving in N, N-Dimethylformamide (DMF), soaking the membrane in the solution, taking out, and placing the membrane under an incandescent lamp for illumination to obtain a green product attached to the membrane as the superlattice material.
According to an embodiment of the present invention, the compound having the structure represented by formula 1 or formula 2 is reacted with PbX2In a molar ratio of 1 (4-10), such as 1 (4-8), illustratively 1: 4.
According to an embodiment of the present invention, the volume molar ratio of the N, N-dimethylformamide to the compound of the structure represented by formula 1 or formula 2 may be (1-10) mL:1mmol, for example (2-8) mL:1mmol, illustratively 5mL:1 mmol.
According to an embodiment of the invention, the soaking time of the membrane in the solution is 0.5-5min, e.g. 1 min.
According to an embodiment of the present invention, the compound having the structure represented by formula 1 or formula 2 is reacted with PbX2Have the meaning as described above.
The invention also provides a preparation method of the superlattice thin film, which comprises the following steps:
(1) a compound with a structure shown in formula 1 or formula 2 and PbX2Dissolving in N, N-Dimethylformamide (DMF) to obtain a mixed solution;
(2) and soaking the porous base membrane in the mixed solution, taking out the soaked porous base membrane, and performing light treatment on the porous base membrane until the color of the base changes from light yellow to green to obtain the superlattice film.
According to an embodiment of the present invention, in step (1), the compound having a structure represented by formula 1 or formula 2 is reacted with PbX2In a molar ratio of 1 (4-10), such as 1 (4-8), illustratively 1: 4.
According to an embodiment of the present invention, in step (1), the volume molar ratio of the N, N-dimethylformamide to the compound of the structure represented by formula 1 or formula 2 may be (1-10) mL:1mmol, for example (2-8) mL:1mmol, illustratively 5mL:1 mmol.
According to an embodiment of the invention, in step (2), the soaking time is not longer, for example, 0.5-5min, such as 1-3min, and is exemplary 1 min.
According to an embodiment of the present invention, the compound of the structure represented by formula 1 or formula 2, PbX2And the porous base film have the meanings as described above.
According to an exemplary embodiment of the present invention, the method for preparing the superlattice thin film comprises the following steps:
(1) mixing MeDAB, EtDAB or MeBEN with PbI2Dissolving in DMF to obtain a mixed solution;
(2) and soaking the porous base membrane in the mixed solution, taking out the soaked porous base membrane, and performing light treatment on the porous base membrane until the color of the base changes from light yellow to green to obtain the superlattice film.
The invention also provides a superlattice material and a superlattice film prepared by the method.
The invention also provides application of the superlattice thin film in explosive detection. Preferably, the explosives are nitro-group-containing explosives; examples are PA (picric acid), RDX (cyclotrimethylenetrinitramine), NB (nitrobenzene), DNB (dinitrobenzene), TNT (trinitrotoluene).
The invention has the beneficial effects that:
the invention provides a superlattice thin film containing a superlattice material, and a preparation method and application thereof. The invention adopts a simple immersion method to synthesize a three-dimensional porous membrane (the size on the paper is 29.6cm) of a superlattice material in a large area. Compared with other three-dimensional porous synthesis, the preparation of the film is simple and easy, and the film can be grown into a large-area film.
1. The experimental method is simple, and pure superlattice materials and films containing the superlattice materials can be obtained by a room-temperature solution method. Compared with the traditional method, the method has high yield and good reproducibility.
2. The compound is synthesized to be green, has strong free radical signals, responds to the explosive steam, and is quenched after being heated, and does not respond to the explosive steam. Can be used for detecting explosives containing nitro groups.
Drawings
Fig. 1 is a schematic diagram of the process for preparing the superlattice thin film in example 1.
Fig. 2 is a powder diffraction pattern of superlattice thin films prepared using different porous substrate films.
FIG. 3 is an SEM topography for the sample of example 1: a. a blank nylon membrane; EtDAB.4 PbI2A superlattice thin film; c. EtDAB 4PbI2SEM elemental mapping of superlattice thin films.
FIG. 4 shows EtDAB.4PbI of example 12Current/voltage plots for the synthesized and annealed samples of the superlattice thin film.
FIG. 5 shows EtDAB.4PbI of example 12Results of hermetic properties test of superlattice thin films: a) the response of the sample under an explosive vapor atmosphere was synthesized, b) no response of the electrode under an explosive vapor atmosphere after annealing.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
According to the preparation process shown in FIG. 1, 0.461g of PbI is added2(1mmol) and 0.118g EtDAB (EtDAB means N, N, N ', N' -tetraethylbenzidine (Et)2NC6H4C6H4NEt2) Dissolved in 5mL of DMF (N, N-dimethylformamide) to obtain a mixed solution; a commercially available nylon porous filter membrane was used as a basement membrane, soaked in the above mixed solution for 1 minute, taken out and placed under an incandescent lamp for illumination, and the color of the basement membrane changed from light yellow to green (see fig. 1).
XRD powder diffraction results prove that the green product grown on the substrate is a superlattice material EtDAB.4PbI2(see a) in FIG. 2), illustrating that EtDAB.4PbI is contained2The superlattice thin film is successfully prepared.
After weighing, the weight difference before and after the membrane infiltration is found to be EtDAB.4PbI2The mass of the carrier on the nylon porous filter membrane is about 0.836mg cm-2。
The size of the synthesized superlattice thin film can be adjusted according to the size of the substrate, and the larger film can be obtained by selecting the larger substrate.
Through SEM tests, the pore diameter of the pores of the blank nylon membrane was found to be several hundred nanometers to several micrometers (a in fig. 3). Through EtDAB 4PbI2After wetting, part of the pores were etched DAB.4PbI2The material is blocked but still leaving part of the hole (b in fig. 3). The element Pb, I, C and N are uniformly distributed on the basement membrane through SEM element analysis tests.
The base membrane can be replaced by filter paper or commercial pp membrane to obtain different base membrane containing EtDAB.4PbI2The superlattice thin film of (1). The XRD powder diffraction results for both films are shown in b) and c) of fig. 2.
Example 2: electrode manufacturing and current-voltage testing on superlattice porous membrane
The superlattice film prepared in example 1 and having a relatively large shape (the diameter is about 15cm) is selected, gold interdigital electrodes are plated on the film under the protection of a mask, and the electrodes are led out by silver paste on two sides. The electrode was placed in a Lake Shore CRX-VF sample chamber and evacuated and tested for voltage VS current curves at different temperatures using KEITHLEY 4200-SCS. Then, the electrode prepared by the superlattice film in the embodiment 1 is heated to 100 ℃ in situ and annealed for 2 hours to obtain a yellow sample; the thermochromic samples were tested for voltage VS current curves at different temperatures (see fig. 4). FIG. 4 shows that: sample EtDAB.3.9 PbI as-synthesized2After the electrode is manufactured, the voltage of 5V is controlled, and the current is 10-8The magnitude of A, the conductivity drop of the sample after heat fading will be nearly 3.
Example 3: gas sensitive performance testing on superlattice porous films
The superlattice porous film in example 1 is vapor-plated with interdigital electrodes, silver paste is coated on two sides of the interdigital electrodes, and gold wires are connected. And (3) placing the electrode in a glass tube, controlling the flow of dry air blown out from a steel cylinder through a gas flowmeter, controlling through a three-way valve, running a sample baseline in dry air atmosphere, and testing the vapor atmosphere detection capability of the sample on the nitro explosives by using saturated vapor components passing through the explosive solid. By controlling the voltage to 5V, the change in current under different atmospheres was detected on the custard 2602B. The synthesized green sample film responded to the explosive vapors, but the response disappeared after thermal annealing (fig. 5).
From FIGS. 5a) and 5b) it can be seen that EtDAB.4PbI has just been synthesized2The response values of the film to PA, RDX, NB, DNB and TNT were 43%, 81%, 51%, 68% and 79%, respectively, with response times of 0.20, 0.89, 0.32, 0.48 and 0.34min and recovery times of 2.61, 5.98, 4.88, 6.21 and 2.63 min. In addition, the electrode is used for acetone, ammonia gas, benzene, ethylbenzene and CO2Common gases such as methanol and the like have good anti-interference performance.
Example 4
The present embodiment is different from embodiment 1 in that: with N, N, N ', N' -tetramethylbenzidine (formula Me)2NC6H4C6H4NMe2Abbreviated as MeDAB) in an amount of 0.1g instead of EtDAB.
The prepared product contains MeDAB.4PbI2The superlattice thin film of (1).
Example 5
The present embodiment is different from embodiment 1 in that: with N, N, N ', N' -tetramethyl-p-phenylenediamine (formula Me)2NC6H4NMe2Abbreviated as MeBEN) in an amount of 0.1g instead of EtDAB.
The preparation method comprises the step of preparing the MeBEN.4PbI2The superlattice thin film of (1).
Example 6
The present embodiment is different from embodiment 1 in that: filter paper was used as the porous base membrane.
Example 7
The present embodiment is different from embodiment 1 in that: a commercially available PP film was used as the porous base film.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A superlattice film, characterized in that the superlattice film is a three-dimensional porous film containing a superlattice material;
the superlattice material has a chemical formula of A.nPbX2Wherein A is selected from compounds having a structure represented by formula 1 or formula 2:
R1、R2、R3、R4、R1’、R2’、R3’、R4' same or different, independently from each other selected from C1-10Alkyl radicals, e.g. C1-6Alkyl, illustratively methyl, ethyl, propyl, or butyl;
R5、R6、R5’、R6’、R7’、R8' same or different, independently from each other selected from C1-10Alkyl, H, e.g. C1-6Alkyl, H, exemplified by methyl, ethyl, H;
x represents halogen, such as F, Cl, Br or I, preferably I;
n is 4 or more and is an integer, preferably, n is 4.
2. The superlattice film as claimed in claim 1, wherein R in formula 11、R2、R3、R4And is selected from methyl or ethyl.
Preferably, in formula 1, R5、R6And is selected from methyl, ethyl or H.
Preferably, in formula 2, R1’、R2’、R3’、R4' same, selected from methyl or ethyl.
Preferably, in formula 2, R5’、R6’、R7’、R8' same, selected from methyl, ethyl or H.
3. The superlattice film according to claim 1 or 2, wherein a is selected from compounds having a structure as shown in any one of formulas 3-5:
wherein the compound of formula 3 is abbreviated as MeDAB, the compound of formula 4 is abbreviated as EtDAB, and the compound of formula 5 is abbreviated as MeBEN.
Preferably, the superlattice material is selected from MeDAB 4PbI2，EtDAB·4PbI2Or MeBEN 4PbI2。
4. The superlattice thin film as claimed in any one of claims 1 to 3,the preparation method is characterized in that the preparation process of the superlattice material comprises the following steps: a compound with a structure shown in formula 1 or formula 2 and PbX2Dissolving the film in N, N-dimethylformamide, soaking the film in the solution, taking out, and placing the film under an incandescent lamp for illumination to obtain a green product attached to the film, wherein the green product is the superlattice material.
Preferably, the compound with the structure shown in the formula 1 or the formula 2 and PbX are adopted2The molar ratio of (1) to (4-10).
Preferably, the volume mol ratio of the N, N-dimethylformamide to the compound with the structure shown in the formula 1 or the formula 2 is (1-10) mL:1 mmol.
Preferably, the soaking time of the membrane in the solution is 0.5-5min, e.g. 1 min.
Preferably, the compound with the structure shown in the formula 1 or the formula 2 and PbX are adopted2Have the meaning as claimed in claim 1 or 2.
5. The superlattice film according to any one of claims 1 to 4, wherein said superlattice film comprises said superlattice material according to any one of claims 1 to 4 and a porous base film, said superlattice material being distributed over a surface and pores of said porous base film. Preferably, the superlattice material does not fill all of the pores of the porous base film.
Preferably, the porous base membrane is selected from a fiber-based porous membrane, such as filter paper, a nylon porous filter membrane, a polyethylene porous membrane. Preferably, the pore size of the porous base membrane is from 100nm to 10 μm, for example from 500nm to 5 μm.
Preferably, the loading amount of the superlattice material on the porous base membrane is 0.5-2mg/cm2。
6. The superlattice film according to any one of claims 1-5, wherein said superlattice film comprises a superlattice material and a porous base film, said superlattice material being distributed over a surface and pores of said porous base film, said superlattice material not filling all pores of said porous base film;
wherein the superlatticeThe material is selected from MeDAB.4 PbI2，EtDAB·4PbI2Or MeBEN 4PbI2；
The porous basement membrane is filter paper, a nylon porous filter membrane or a polyethylene porous membrane.
Preferably, the superlattice film has a morphology substantially as shown as b in fig. 3.
7. A method for preparing a superlattice thin film as claimed in any one of claims 1 to 6, characterized in that said method comprises the steps of:
(1) a compound with a structure shown in formula 1 or formula 2 and PbX2Dissolving in N, N-Dimethylformamide (DMF) to obtain a mixed solution;
(2) and soaking the porous base membrane in the mixed solution, taking out the soaked porous base membrane, and performing light treatment on the porous base membrane until the color of the base changes from light yellow to green to obtain the superlattice film.
8. The method according to claim 7, wherein in the step (1), the compound having the structure represented by formula 1 or formula 2 is reacted with PbX2The molar ratio of (1) to (4-10).
Preferably, in the step (1), the volume molar ratio of the N, N-dimethylformamide to the compound having the structure shown in the formula 1 or the formula 2 is (1-10) mL:1 mmol.
Preferably, in the step (2), the soaking time is 0.5-5 min.
9. The method for producing a superlattice thin film according to claim 7 or 8, characterized by comprising the steps of:
(1) mixing MeDAB, EtDAB or MeBEN with PbI2Dissolving in DMF to obtain a mixed solution;
(2) and soaking the porous base membrane in the mixed solution, taking out the soaked porous base membrane, and performing light treatment on the porous base membrane until the color of the base changes from light yellow to green to obtain the superlattice film.
10. Use of a superlattice thin film as claimed in any one of claims 1-6 for explosive detection. Preferably, the explosives are nitro-group-containing explosives; preferred are PA (picric acid), RDX (cyclotrimethylenetrinitramine), NB (nitrobenzene), DNB (dinitrobenzene), TNT (trinitrotoluene).
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