CN113834856B - 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 film, a preparation method and application thereof. The superlattice film is a three-dimensional porous film containing superlattice materials; superlattice material with chemical formula A.nPbX 2 And wherein a is selected from compounds having a structure as shown in formula 1 or formula 2:R 1 、R 2 、R 3 、R 4 、R 1 ’、R 2 ’、R 3 ’、R 4 'same or different', independently of each other, from C 1‑10 An alkyl group; r is R 5 、R 6 、R 5 ’、R 6 ’、R 7 ’、R 8 'same or different', independently of each other, from C 1‑10 Alkyl, H; x represents halogen; n is more than or equal to 4 and is an integer. The invention adopts a simple infiltration 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, a preparation method and application thereof.
Background
At present, the three-dimensional porous membrane is not easy to be made of two-dimensional materials, and the three-dimensional porous structure made of the two-dimensional materials reported in the prior art is mainly concentrated on the preparation of three-dimensional porous graphene nano-nets, graphene aerogel and graphene foam from graphene sheets, however, the materials are not easy to form a membrane, and particularly are not easy to form a crystalline membrane.
On the other hand, when the superlattice material is made into a large-area film, cracks and the like are likely to occur, and no method for obtaining the superlattice material with a large area is found in the prior art. Porous membranes are very popular for gas sensors due to their multi-stage 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 is represented by the chemical formula A.nPbX 2 And wherein a is selected from compounds having a structure as shown in formula 1 or formula 2:
R 1 、R 2 、R 3 、R 4 、R 1 ’、R 2 ’、R 3 ’、R 4 'same or different', independently of each other, from C 1-10 Alkyl radicals, e.g. C 1-6 Alkyl, exemplified by methyl, ethyl, propyl, or butyl;
R 5 、R 6 、R 5 ’、R 6 ’、R 7 ’、R 8 'same or different', independently of each other, from C 1-10 Alkyl, H, e.g. C 1-6 Alkyl, H, exemplified by methyl, ethyl, H;
x represents halogen, such as F, cl, br or I, preferably I;
n is equal to or greater than 4 and is an integer, preferably n=4.
According to an embodiment of the present invention, in formula 1, R 1 、R 2 、R 3 、R 4 And is the same, selected from methyl or ethyl.
According to an embodiment of the present invention, in formula 1, R 5 、R 6 And is the same, selected from methyl, ethyl or H.
According to an embodiment of the invention, in formula 2, R 1 ’、R 2 ’、R 3 ’、R 4 ' same, selected from methyl or ethylA base.
According to an embodiment of the invention, in formula 2, R 5 ’、R 6 ’、R 7 ’、R 8 ' same, selected from methyl, ethyl or H.
According to an exemplary embodiment of the present invention, A is selected from compounds having a structure as shown in any one of formulas 3 to 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 embodiment of the present invention, the superlattice material may be selected from MeDAB 4PbI 2 ，EtDAB·4PbI 2 Or MeBEN.4PbI 2 。
According to an embodiment of the present invention, the superlattice film includes the above-described superlattice material and a porous base film, the superlattice material being distributed in the surface and pores of the porous base film. Preferably, the superlattice material does not fill all pores of the porous base film.
According to an embodiment of the present invention, the porous base membrane may be selected from fibrous porous membranes, such as filter paper, nylon porous filter membrane, polyethylene porous membrane (PP porous membrane). Preferably, the pore size of the porous base film is 100nm to 10. Mu.m, for example 500nm to 5. Mu.m.
According to an embodiment of the present invention, the superlattice material is supported on the porous base film at a loading of 0.5-2mg/cm 2 For example 0.6-1.5mg/cm 2 Exemplary is 0.7mg/cm 2 、0.8mg/cm 2 、0.836mg/cm 2 、0.9mg/cm 2 、1.0mg/cm 2 、1.2mg/cm 2 。
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 includes a superlattice material and a porous base film, the superlattice material being distributed in surfaces and pores of the porous base film, the superlattice material not filling all pores of the porous base film;
wherein the superlattice material is selected from MeDAB.4PbI 2 ，EtDAB·4PbI 2 Or MeBEN.4PbI 2 ；
The porous substrate membrane is filter paper, a nylon porous filter membrane or a polyethylene porous membrane.
According to an embodiment of the invention, the superlattice film has a morphology substantially as shown in b in fig. 3.
According to an embodiment of the present invention, the preparation process of the superlattice material includes the following steps: combining a compound of the structure represented by formula 1 or formula 2 with PbX 2 Dissolving in N, N-Dimethylformamide (DMF), soaking the film in the solution, taking out, and placing the film under an incandescent lamp for illumination to obtain a green product which is attached to the film to obtain the superlattice material.
According to an embodiment of the present invention, the compound of formula 1 or formula 2 is mixed with PbX 2 The molar ratio of (2) is 1 (4-10), for example 1 (4-8), and is exemplified by 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, and exemplified as 5mL:1mmol.
According to an embodiment of the invention, the membrane is immersed in the solution for a time of 0.5-5min, for example 1min.
According to an embodiment of the present invention, the compound of formula 1 or formula 2 is mixed with PbX 2 Having the meaning as described above.
The invention also provides a preparation method of the superlattice film, which comprises the following steps:
(1) Combining a compound of the structure represented by formula 1 or formula 2 with PbX 2 Dissolving in N, N-Dimethylformamide (DMF) to obtain a mixed solution;
(2) And soaking the porous substrate film in the mixed solution, taking out the soaked porous substrate film, and carrying out light treatment on the porous substrate film until the substrate color is changed from pale yellow to green, so as to obtain the superlattice film.
According to an embodiment of the present invention, in step (1), the compound of formula 1 or formula 2 is mixed with PbX 2 The molar ratio of (2) is 1 (4-10), for example 1 (4-8), and is exemplified by 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, and exemplified as 5mL:1mmol.
According to an embodiment of the present invention, in step (2), the soaking time is not too long, for example 0.5-5min, such as 1-3min, and exemplified by 1min.
According to an embodiment of the present invention, the compound of formula 1 or formula 2, pbX 2 And the porous base film both have the meanings as described above.
According to an exemplary scheme of the invention, the preparation method of the superlattice film comprises the following steps:
(1) MeDAB, etDAB or MeBEN and PbI 2 Dissolving in DMF to obtain a mixed solution;
(2) And soaking the porous substrate film in the mixed solution, taking out the soaked porous substrate film, and carrying out light treatment on the porous substrate film until the substrate color is changed from pale yellow to green, so as to obtain the superlattice film.
The invention also provides the superlattice material and the superlattice film prepared by the method.
The invention also provides application of the superlattice film in explosive detection. Preferably, the explosive is a nitro-containing explosive; examples are PA (picric acid), RDX (cyclotrimethylene trinitroamine), NB (nitrobenzene), DNB (dinitrobenzene), TNT (trinitrotoluene).
The invention has the beneficial effects that:
the invention provides a superlattice film containing superlattice materials, a preparation method and application thereof. The invention adopts a simple infiltration method to synthesize the three-dimensional porous membrane (the size on paper is 29.6 cm) of the superlattice material in a large area. Compared with other three-dimensional porous synthesis, the film disclosed by the invention is simple and easy to prepare, and can be grown into a large-area film.
1. The experimental method is simple, and the pure superlattice material and the film containing the superlattice material 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 into green, has strong free radical signal, is responsive to the vapor of the explosive, and is free radical quenched after being heated, and is not responsive to the vapor of the explosive. Can be used for detecting the nitro-containing explosive.
Drawings
Fig. 1 is a schematic diagram of the preparation process of the superlattice film in example 1.
Fig. 2 is a powder diffraction pattern of superlattice thin films prepared using different porous base films.
Fig. 3 is an SEM topography of the sample of example 1: a. blank nylon membrane; etDAB 4PbI 2 A superlattice thin film; etDAB 4PbI 2 SEM element mapping diagram of superlattice thin film.
FIG. 4 is a sample of example 1EtDAB 4PbI 2 Current/voltage graphs for the composite and annealed samples of superlattice thin films.
FIG. 5 is example 1 EtDAB.4PbI 2 Results of the test for the airtight properties of the superlattice film: a) The response of the sample immediately after synthesis in an explosive vapor atmosphere, b) the non-response of the electrode in an explosive vapor atmosphere after annealing.
Detailed Description
The technical scheme of the invention will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
Example 1
As shown in FIG. 1The preparation process is shown, 0.461g PbI 2 (1 mmol) and 0.118g of EtDAB (EtDAB means N, N, N ', N' -tetraethylbenzidine (Et) 2 NC 6 H 4 C 6 H 4 NEt 2 ) Dissolving in 5mL of DMF (N, N-dimethylformamide) to obtain a mixed solution; a commercially available nylon porous filter membrane is taken as a base membrane, soaked in the mixed solution for 1 minute, taken out and placed under an incandescent lamp for illumination, and the color of the base membrane is changed from pale yellow to green (as shown in figure 1).
XRD powder diffraction results prove that the green product grown on the substrate is superlattice material EtDAB.4PbI 2 (a) in FIG. 2), illustrating the inclusion of EtDAB 4PbI 2 The superlattice film is successfully prepared.
The weight difference before and after film infiltration was measured to find EtDAB 4PbI 2 The mass of the porous nylon filter membrane loaded on the porous nylon filter membrane is about 0.836mg cm -2 。
The size of the synthesized superlattice film can be adjusted according to the size of the substrate, and the film with the same size can be obtained by selecting the substrate with the same size.
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) by SEM test. Via EtDAB 4PbI 2 After infiltration, a portion of the wells were EtDAB 4PbI 2 The material plugs but still leaves a portion of the hole (b in fig. 3). SEM elemental analysis tests show that Pb, I, C and N elements are uniformly distributed on the substrate film.
The substrate film can also be replaced by filter paper or commercial pp film to obtain EtDAB.4PbI containing substrate 2 Is a superlattice film of the device. XRD powder diffraction results for the two films are shown in FIGS. 2 b) and c).
Example 2: electrode fabrication and current-voltage testing on superlattice porous membrane
The superlattice film with a relatively large shape (about 15cm in diameter) prepared in example 1 was selected, the shape of the gold interdigital electrode was plated on the film under the protection of a mask, and the electrode was led out with silver colloid on both sides. The electrodes were placed in a Lake Shore CRX-VF sample chamber and evacuated, and tested for voltage VS current curves at different temperatures using the KEITHLEY 4200-SCS. And then the above-mentioned implementationThe electrode prepared by the superlattice film in situ is heated to 100 ℃ 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 just synthesized 2 After the electrode is made, controlling the voltage to be 5V and the current to be 10 -8 On the order of a, the conductivity of the sample after heat fading drops by approximately 3.
Example 3: gas sensitive performance testing on superlattice porous films
The superlattice porous film of example 1 was vapor deposited with the interdigital electrodes, silver paste was applied to both sides of the interdigital electrodes, and gold wires were connected. The electrode is placed in a glass tube, the flow rate of dry air blown out from a steel bottle is controlled by a gas flowmeter, the flow rate is controlled by a three-way valve, a sample baseline is run under the dry air atmosphere, and then the detection capability of the sample to the vapor atmosphere of the nitroexplosive is tested by using saturated steam components of the explosive solid. By controlling the voltage to 5V, the change in current under different atmospheres was detected on Ji Shili 2602B. The green sample film synthesized was responsive to the explosive vapors, but the response disappeared after thermal annealing (fig. 5).
As can be seen from FIGS. 5 a) and 5 b), the as-synthesized EtDAB 4PbI 2 The response values for 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 2.63min. In addition, the electrode is used for acetone, ammonia, benzene, ethylbenzene and CO 2 Common gases such as methanol have good anti-interference performance.
Example 4
This embodiment differs from embodiment 1 in that: with N, N, N ', N' -tetramethylbenzidine (formula Me) 2 NC 6 H 4 C 6 H 4 NMe 2 Abbreviated as MeDAB) was substituted for EtDAB in an amount of 0.1g.
Preparation of MeDAB 4 PbI-containing product 2 Is a superlattice film of the device.
Example 5
This embodiment differs from embodiment 1 in that: in the form of N, N, N'N' -tetramethyl-p-phenylenediamine (chemical formula Me 2 NC 6 H 4 NMe 2 Abbreviated as MeBEN) in an amount of 0.1g.
Preparation of the composition containing MeBEN.4PbI 2 Is a superlattice film of the device.
Example 6
This embodiment differs from embodiment 1 in that: filter paper was used as the porous base film.
Example 7
This embodiment differs from embodiment 1 in that: commercially available PP films were 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, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (23)
1. A superlattice film, characterized in that the superlattice film is a three-dimensional porous film containing a superlattice material;
the superlattice material is represented by the chemical formula A.nPbX 2 And wherein a is selected from compounds having a structure as shown in formula 1 or formula 2:
R 1 、R 2 、R 3 、R 4 、R 1 ’、R 2 ’、R 3 ’、R 4 'same or different', independently of each other, from C 1-10 An alkyl group;
R 5 、R 6 、R 5 ’、R 6 ’、R 7 ’、R 8 'same or different', independently of each other, from C 1-10 Alkyl, H;
x represents halogen;
n is more than or equal to 4 and is an integer.
2. The superlattice film of claim 1, wherein R 1 、R 2 、R 3 、R 4 、R 1 ’、R 2 ’、R 3 ’、R 4 ' are independently selected from C 1-6 An alkyl group;
R 5 、R 6 、R 5 ’、R 6 ’、R 7 ’、R 8 ' are independently selected from C 1-6 An alkyl group.
3. The superlattice film of claim 1, wherein R 1 、R 2 、R 3 、R 4 、R 1 ’、R 2 ’、R 3 ’、R 4 ' are independently selected from methyl, ethyl, propyl or butyl;
R 5 、R 6 、R 5 ’、R 6 ’、R 7 ’、R 8 ' are independently selected from methyl, ethyl, H.
4. The superlattice film of claim 1, wherein X is I.
5. The superlattice film of claim 1, wherein n = 4.
6. The superlattice film of claim 1, wherein in formula 1, R 1 、R 2 、R 3 、R 4 Identical, selected from methyl or ethyl;
and/or, in formula 1, R 5 、R 6 Identical, selected from methyl, ethyl or H;
and/or, in formula 2, R 1 ’、R 2 ’、R 3 ’、R 4 ' same, selected from methyl or ethyl;
and/or, in formula 2, R 5 ’、R 6 ’、R 7 ’、R 8 ' same, selected from methyl, ethyl or H.
7. The superlattice film according to claim 1, 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.
8. The superlattice film of claim 7, wherein the superlattice material is selected from the group consisting of MeDAB 4PbI 2 ，EtDAB·4PbI 2 Or MeBEN.4PbI 2 。
9. The superlattice film according to any one of claims 1-6, wherein the preparation process of the superlattice material comprises the steps of: combining a compound of the structure represented by formula 1 or formula 2 with PbX 2 Dissolving in N, N-dimethylformamide, soaking a porous substrate film in the solution, taking out, and placing the porous substrate film under an incandescent lamp for illumination to obtain a green product which is attached to the porous substrate film to obtain the superlattice material.
10. The superlattice film according to claim 9, wherein the compound of formula 1 or formula 2 is mixed with PbX 2 The molar ratio of (2) is 1 (4-10);
the volume molar 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, 1mmol;
the infiltration time of the porous substrate film in the solution is 0.5-5min.
11. The superlattice film of any one of claims 1-8, wherein the superlattice film comprises the superlattice material and a porous base film, the superlattice material being distributed in surfaces and pores of the porous base film.
12. The superlattice film of claim 11, wherein the superlattice material does not fill all pores of the porous base film.
13. A superlattice film according to claim 11 or 12, wherein said porous base film is selected from fibrous porous films.
14. The superlattice membrane of claim 13, wherein the porous base membrane is selected from filter paper, a ni Long Duokong filter membrane, a polyethylene porous membrane.
15. A superlattice membrane according to claim 11 or 12, characterized in that the pore size of the porous base membrane is 100nm-10 μm.
16. A superlattice film according to claim 11 or 12, wherein the superlattice material is present on the porous base film at a loading of 0.5-2mg/cm 2 。
17. The superlattice film of claim 8, wherein the superlattice film comprises a superlattice material and a porous base film, the superlattice material being distributed in surfaces and pores of the porous base film, the superlattice material not filling all pores of the porous base film;
wherein the superlattice material is selected from MeDAB.4PbI 2 ，EtDAB·4PbI 2 Or MeBEN.4PbI 2 ；
The porous substrate membrane is filter paper, a nylon porous filter membrane or a polyethylene porous membrane.
18. A method of preparing a superlattice film as defined in any one of claims 1-17, wherein the method of preparing comprises the steps of:
(1) Combining a compound of the structure represented by formula 1 or formula 2 with PbX 2 Dissolving in N, N-dimethylformamide to obtain a mixed solution;
(2) And soaking the porous substrate film in the mixed solution, taking out the soaked porous substrate film, and carrying out light treatment on the porous substrate film until the substrate color is changed from pale yellow to green, so as to obtain the superlattice film.
19. The method according to claim 18, wherein in the step (1), the compound having the structure represented by formula 1 or formula 2 is mixed with PbX 2 The molar ratio of (2) is 1 (4-10);
in the step (1), the volume molar 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, namely 1mmol;
in the step (2), the soaking time is 0.5-5min.
20. The method of preparation according to claim 18, characterized in that the method of preparation comprises the steps of:
(1) MeDAB, etDAB or MeBEN and PbI 2 Dissolving in N, N-dimethylformamide to obtain a mixed solution;
(2) And soaking the porous substrate film in the mixed solution, taking out the soaked porous substrate film, and carrying out light treatment on the porous substrate film until the substrate color is changed from pale yellow to green, so as to obtain the superlattice film.
21. Use of the superlattice film as defined in any one of claims 1-17 for explosives detection.
22. The use of claim 21, wherein the explosive is a nitro-containing explosive.
23. The use according to claim 21 or 22, wherein the explosive is picric acid, cyclotrimethylene trinitramine, nitrobenzene, dinitrobenzene, trinitrotoluene.
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