CN111162168A - Inorganic-organic hybrid superlattice material with photochromic performance and preparation and application thereof - Google Patents
Inorganic-organic hybrid superlattice material with photochromic performance and preparation and application thereof Download PDFInfo
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Abstract
An inorganic-organic hybridized superlattice material with photochromism performance is green without heating and has strong free radical signal, after being heated, the free radical is quenched and becomes yellow, and after being soaked in ethanol solution and then being irradiated by light, the material is restored to be in an unheated state. The material has an electrical conductivity of 10 without heating‑4S cm‑1Of the sample, the conductivity drop of the sample after thermal discoloration will be nearly 5 orders of magnitude. The material is distinguished from conventional hybrid inorganic-organic materials without heating, the inorganic and organic parts of which are neutral and which retain structural stability even when immersed in waterThe method adopts a light-induced synthesis technology, uses light as energy for opening the superlattice layer, and has the advantages of simple preparation process, high yield and high yield.
Description
Technical Field
The invention belongs to the technical field of inorganic-organic hybrid superlattice materials, and particularly relates to an inorganic-organic hybrid superlattice material with photochromic performance and preparation and application thereof.
Background
The inorganic-organic hybrid material is formed by assembling inorganic components and organic components on a molecular level, and not only can the effect of 'hybrid superiority' of fully playing respective performance advantages of the inorganic materials and the organic materials be achieved through careful design and structural regulation, but also the organic components can generate a synergistic effect with the inorganic components through chemical bonds, so that the hybrid material has a novel function which is not possessed by a single component. The material has important application value in the aspects of photoelectronic devices, solar cells, catalysis, ion exchange, fast ion conductors and the like. Therefore, the preparation of the molecular-based inorganic-organic hybrid material realizes the regulation and control of the optical, electric, magnetic and catalytic performances, deeply researches the association of the material structure and physical properties, and has important significance for finally realizing the practical application of the material.
The metal halide inorganic-organic hybrid material has excellent electrical properties and is easy to prepare into a thin film, so that the metal halide inorganic-organic hybrid material has potential application prospects in the aspects of light-emitting diodes, field effect transistors, solar cells and the like, and becomes one of the most concerned molecular-based hybrid materials. In particular to a lead halide hybrid material (CH) taking methylamine as a cation3NH3PbX3X ═ Cl, Br, I), has received much attention in recent years due to its rapid increase in solar cell conversion efficiency. However, such materials are susceptible to deliquescence in humid environments due to the fact that the inorganic portion is anionic and the organic portion is in cationic form.
Superlattice materials are a class of materials in which two materials are stacked via van der waals interactions. Such materials, which have excellent electrical properties such as superconductivity, high on-off ratio of field effect transistors, etc., are widely used in various electrical devices. On the other hand, because the superlattice material may have the performance which other two-dimensional materials do not have, the conventional methods for synthesizing the superlattice material mainly comprise layer-by-layer peeling recombination, an electrochemical method, a chemical vapor deposition method and the like, and the superlattices synthesized by the methods generally have low yield and poor reproducibility.
Disclosure of Invention
In order to improve the defects of the prior art, the invention aims to provide an inorganic-organic hybrid superlattice material with photochromic performance, a preparation method and application thereof, wherein the conductivity of the inorganic-organic hybrid superlattice material is superior to that of common inorganic-organic hybrid materials, the conductivity of the inorganic-organic hybrid superlattice material is changed by 5 orders of magnitude before and after discoloration, and the superlattice material before discoloration has a photoconductive response to an infrared region.
The purpose of the invention is realized by the following technical scheme:
an inorganic-organic hybrid superlattice material of a type that includes at least one organic layer and at least one inorganic layer, the organic layer being at least one of an EtDAB layer, a MeDAB layer, or a MeBEN layer; the inorganic layer is PbI2A layer; the at least one organic layer is alternately stacked with the at least one inorganic layer.
According to the invention, the organic layer intercalation forms an alternately stacked inorganic-organic hybrid superlattice material in the inorganic layer.
According to the invention, one of the organic layers of the superlattice material has a thickness of
For example
The thickness of one inorganic layer in the superlattice material is
For example
For example, an organic layer has a thickness of
A thickness of an inorganic layer of
According to the present invention, the inorganic-organic hybrid superlattice material has a molar ratio of organic layer to inorganic layer of 1:0.1-5, preferably 1:1-4.5, such as 1: 2-4. Illustratively, the molar ratio of the organic layer to the inorganic layer is 1: 4. When the molar ratio exceeds this range, the organic layer cannot be intercalated into the inorganic layer any more, or it can also be understood that there is not enough room in the inorganic layer to accommodate more organic layers.
According to the invention, the thickness of the inorganic-organic hybrid superlattice material is 10-1000nm, such as 200-800nm, such as 300-600 nm.
According to the invention, the inorganic-organic hybrid superlattice material has a unit cell parameter of
α＝90°,β＝95.72(2)°,γ＝90°,
In the present invention, the EtDAB means N, N, N ', N' -tetraethylbenzidine (Et)2NC6H4C6H4NEt2) The MeDAB is N, N, N ', N' -tetramethylbenzidine (Me)2NC6H4C6H4NMe2) The MeBEN is N, N, N ', N' -tetramethyl-p-phenylenediamine (Me)2NC6H4NMe2)。
According to the invention, the superlattice material has color-changing properties, and the inorganic-organic hybrid superlattice material is green, in which material electrons are transferred from a lead iodide layer to an organic layer, forming radical electrons; after heat treatment (such as heating to 100-; the color change is due to the disappearance of free radicals in the superlattice material, and as shown in fig. 5 for an example, the response value of the heated superlattice material to the intensity of the free radicals is zero, and if a yellow sample obtained after the heating treatment is placed in an ethanol solution and is illuminated, electrons in the material are transferred again, and the material is changed into the original green color.
According to the invention, the superlattice material has photoconductive response performance, the response of the superlattice material to the photoconduction can be widened to an infrared region, but the superlattice material after heating and color change has the photoconductive response only under the light with the wavelength of less than 645 nm.
According to the invention, the conductivity of the superlattice material is 10-4S·cm-1The magnitude is that the conductivity of the superlattice material after heating and color change is reduced by 5 magnitudes, namely 10-9S·cm-1Magnitude.
In the invention, the conductivity test method comprises the following steps: dispersing the synthesized material on a silicon wafer substrate, coating silver adhesive on two sides of a single crystal, and connecting gold wires. Conductivity was tested on the KEITHLEY 4200-SCS. The variable temperature conductivity is realized by the combination of Lake ShoreCrX-VF and KEITHLEY 4200-SCS.
The invention also provides a preparation method of the inorganic-organic hybrid superlattice material, which comprises the following steps:
1) dissolving an inorganic material and an organic material in an organic solvent to prepare a mixed solution;
2) adding an anti-solvent into the mixed solution obtained in the step 1) to obtain a precipitate;
3) performing illumination treatment on the precipitate obtained in the step 2) to prepare the inorganic-organic hybrid superlattice material;
wherein, in the step 1), the inorganic material is selected from PbI2The organic material is selected from one of EtDAB, MeDAB or MeBEN.
According to the invention, the organic solvent of step 1) is selected from N, N' -dimethylformamide.
According to the present invention, the molar ratio of the organic material to the inorganic material in the mixed solution of step 1) is 1:0.1 to 5, preferably 1:1 to 4.5, for example 1:2 to 4.
According to the invention, the anti-solvent of step 2) is acetonitrile and chlorobenzene, and a yellow precipitate can be obtained after the anti-solvent is added.
According to the present invention, the amount of the antisolvent to be added in step 2) is not particularly limited, and it is sufficient to ensure complete precipitation. Illustratively, the anti-solvent is added in an amount of 10mL of acetonitrile and 30mL of chlorobenzene per 1mL of the mixed solution.
According to the invention, the illumination treatment in step 3) can be illumination under an incandescent lamp, a xenon lamp, an ultraviolet lamp or an infrared lamp; the illumination time is 1-2 hours.
According to the invention, a green product can be obtained after light treatment.
The invention also provides the application of the inorganic-organic hybrid superlattice material, which is used for a memory device.
The present invention also provides a method of varying the conductivity of the above inorganic-organic hybrid superlattice material, the method comprising:
s1) heat treating the inorganic-organic hybrid superlattice material.
The heating temperature is 100-200 ℃; the heating time is 1-2 hours. The conductivity of the superlattice material is 10-4S·cm-1The magnitude is that the conductivity of the superlattice material after heating and color change is reduced by 5 magnitudes, namely 10-9S·cm-1Magnitude.
The method further comprises the following steps:
s2) placing the sample obtained after the heating treatment into an ethanol solution, and carrying out light treatment.
The illumination treatment can be illumination under an incandescent lamp, a xenon lamp, an ultraviolet lamp or an infrared lamp; the illumination time is 1-2 hours.
The invention has the beneficial effects that:
1. the inorganic-organic hybrid superlattice material with photochromic performance is green without being heated and hasStrong free radical signal, and after heating, the material turns yellow due to the quenching of the free radicals, and after soaking in ethanol solution and light treatment, the material returns to the unheated state. The inorganic-organic hybrid superlattice material has an electrical conductivity of 10 without heating-4S·cm-1Of the sample, the conductivity drop of the sample after thermal discoloration will be nearly 5 orders of magnitude. The inorganic-organic hybrid superlattice material is different from the traditional inorganic-organic hybrid material (inorganic components are in an anionic form, organic components are in a cationic form, and the deliquescence is easy) when the inorganic-organic hybrid superlattice material is not heated, and both the inorganic part and the organic part of the inorganic-organic hybrid superlattice material are neutral, so that the structural stability is still maintained even if the inorganic-organic hybrid superlattice material is soaked in water.
2. The preparation method of the inorganic-organic hybrid superlattice material with photochromic performance has the following advantages: compared with the preparation and purification of other inorganic-organic hybrid materials, the preparation of the compound of the inorganic-organic hybrid superlattice material is simple and easy; no by-product is generated in the reaction process, and only a reagent for analyzing the purity is used, the purification is not needed; can be prepared under relatively mild conditions without complex equipment; the green crystalline product can be directly obtained.
3. The preparation method of the invention adopts a light-induced synthesis technology, uses light as energy for opening the superlattice layer, and has simple preparation process operation, high yield and large output.
Drawings
Fig. 1 is a schematic structural view of the superlattice material prepared in example 1.
Fig. 2 is a transmission electron micrograph of lead iodide and the superlattice material prepared in example 1.
Fig. 3 is a powder diffraction pattern of the superlattice material prepared in example 1.
Fig. 4 is a graph showing the performance test of the superlattice material prepared in example 1 under different conditions.
Fig. 5 is a free radical intensity spectrum of the superlattice material prepared in example 1 and the heat treated superlattice material.
Detailed Description
The preparation method of the present invention will be described in further detail with reference to specific examples. 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.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Example 1
0.020g of PbI2And 0.0033g EtDAB in 1mLDMF (N, N' -dimethylformamide) to give a pale yellow clear solution, 10mL acetonitrile and 30mL chlorobenzene as anti-solvents were added to the clear solution to give a yellow precipitate, and the reaction mixture was placed under an incandescent lamp to give about 0.021g dark green product, noted EtDAB 4PbI2Wherein 4 represents EtDAB and PbI2In a molar ratio of 1: 4.
Fig. 1 is a schematic structural view of the superlattice material prepared in example 1. It comprises an EtDAB layer and PbI2Layer, and the EtDAB layer and PbI2The layers are stacked alternately.
FIG. 2 is a transmission electron micrograph of lead iodide and the superlattice material prepared in example 1, and the structure of the superlattice material is further confirmed from FIG. 2, wherein the EtDAB layer has a thickness of about
The PbI2The thickness of the layer is
Fig. 3 is a powder diffraction pattern of the superlattice material prepared in example 1. Based on the powder diffraction pattern, the inorganic-organic can be calculatedThe unit cell parameter of the hybrid superlattice material is
α＝90°,β＝95.72(2)°,γ＝90°,
Example 2
The greenish black sample piece (marked as a synthetic sample) prepared in example 1 and having a relatively large shape was picked up, gold was plated on both ends of the piece under the protection of a mask plate, and electrodes were led out on the gold by silver paste. The conductivity of the synthesized sample was obtained by placing the electrode in a Lake Shore CRX-VF sample chamber, evacuating, and testing the voltage VS current curve at different temperatures using KEITHLEY 4200-SCS.
Heating the sample prepared in the embodiment 1 to 100 ℃ in situ, and preserving the heat for 2 hours to obtain a yellow sample, and recording the yellow sample as a heating discoloration sample; and testing the voltage VS current curve of the heating color-changing sample at different temperatures to obtain the conductivity of the heating color-changing sample.
The samples prepared in example 1 above and their thermochromic samples were tested for photoconductivity at different wavelengths. By adopting the electrode preparation method, the Xe lamp and the laser are used as light sources, and the optical filter is used for obtaining the photoconductive performance under different wavelengths.
Fig. 4 is a performance test chart of the superlattice material under different conditions. Specifically, a) in fig. 4 is an electrode pattern. B) in FIG. 4 is a conductivity test of the sample prepared in example 1 and its thermochromic sample. As can be seen from b) of FIG. 4, the conductivity of the sample prepared in example 1 increased with increasing temperature, and the conductivity was 4.66X 10 at 300K-4S·cm-1When the temperature is raised to 350K, the conductivity is raised to 2.12X 10-3S·cm-1(ii) a C) in FIG. 4 is the photoconduction of the samples prepared in example 1 under different illumination. D) in FIG. 4 is photoconduction of a thermochromic sample under different illumination. E) in FIG. 4 is the photoconductive performance of the sample prepared in example 1 and its thermochromic sample under a 808nm laser. F) in FIG. 4 is the photoconductive performance of the sample prepared in example 1 and its thermochromic sample under a 1064nm laser.
As can be seen from the above FIG. 4, the conductivity of the sample after heating was reduced to 6.99X 10-9S·cm-1. This change in conductivity can be cycled at least 5 times or more. The photocurrent of the sample prepared in example 1 was 1.42 times higher than that of the sample irradiated with Xe lamp. The photocurrent of the sample after heating under the Xe lamp was 15 times that of the original. In addition, the samples prepared in example 1 all have a photoconductive response to the ultraviolet-visible-infrared region, while the samples after heating have a photoconductive response only to light before 645 nm.
Example 3
Heating the sample prepared in the embodiment 1 to 100 ℃ in situ, preserving the heat for 2 hours, then cooling to obtain a yellow sample, recording the yellow sample as a heating color-changing sample, respectively testing the free radical strength of the synthesized sample and the heating color-changing sample, wherein a testing instrument selects an Electron-Paramagnetic Resonance spectrometer (EPR), the testing condition is normal temperature testing, and the magnetic field range is 3353-3688G.
Fig. 5 is a free radical intensity spectrum of the superlattice material prepared in example 1 and the heat treated superlattice material. As can be seen from fig. 5, the sample prepared in example 1 has a strong electron paramagnetic resonance signal, indicating that the sample has free radicals. After the heating treatment, the electron paramagnetic resonance signal of the heated color-changing sample almost disappears, which shows that the free radical disappears.
Example 4
0.020g of PbI2And 0.0027g MeDAB in 1mL DMF (N, N' -dimethylformamide) to give a pale yellow clear solution, 10mL acetonitrile and 30mL chlorobenzene as anti-solvents were added to the clear solution to give a yellow precipitate, and the reaction mixture was placed under an incandescent lamp to give about 0.021g of a dark green product, designated MeDAB 4PbI2Wherein 4 represents MeDAB and PbI2In a molar ratio of (a).
Example 5
0.020g of PbI2And 0.0020g MeBEN was dissolved in 1mL of DMF (N, N' -dimethylformamide) to give a pale yellow clear solution, 10mL of acetonitrile and 30mL of chlorobenzene were added as anti-solvents to give a yellow precipitate, and the reaction mixture was placed under an incandescent lamp to give about 0.021g of a dark green product, designated MeBEN 4PbI2Wherein 4 represents MeBEN and PbI2In a molar ratio of (a).
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. An inorganic-organic hybrid superlattice material, wherein the superlattice material comprises at least one organic layer and at least one inorganic layer, and the organic layer is at least one of an EtDAB layer, a MeDAB layer or a MeBEN layer; the inorganic layer is PbI2A layer; the at least one organic layer is alternately stacked with the at least one inorganic layer.
2. The superlattice material as in claim 1, wherein the intercalation of the organic layers into the inorganic layers forms an alternating stack of inorganic-organic hybrid superlattice material.
3. A superlattice material as claimed in claim 1 or 2, wherein one of the organic layers in the superlattice material has a thickness of
For example
The thickness of one inorganic layer in the superlattice material is
For example
For example, an organic layer has a thickness of
A thickness of an inorganic layer of
4. A superlattice material as claimed in any one of claims 1-3, wherein the inorganic-organic hybrid superlattice material has a molar ratio of organic to inorganic layers in the range of 1:0.1-5, preferably 1:1-4.5, such as 1: 2-4. Illustratively, the molar ratio of the organic layer to the inorganic layer is 1: 4.
Preferably, the inorganic-organic hybrid superlattice material has a unit cell parameter of
α＝90°,β＝95.72(2)°,γ＝90°,
5. The superlattice material as claimed in any one of claims 1-4, wherein the thickness of the inorganic-organic hybrid superlattice material is 10-1000nm, such as 200-800nm, such as 300-600 nm.
6. The superlattice material as claimed in any one of claims 1-5, wherein the superlattice material has color shifting properties.
Preferably, the superlattice material has photoconductive response performance, the response of the superlattice material to the photoconduction can be widened to an infrared region, but the superlattice material after heating and color changing has the photoconductive response only under the light with the wavelength of less than 645 nm.
Preferably, the conductivity of the superlattice material is 10-4S·cm-1The magnitude is that the conductivity of the superlattice material after heating and color change is reduced by 5 magnitudes, namely 10-9S·cm-1Magnitude.
7. A method of making an inorganic-organic hybrid superlattice material as claimed in any one of claims 1-6, wherein the method comprises the steps of:
1) dissolving an inorganic material and an organic material in an organic solvent to prepare a mixed solution;
2) adding an anti-solvent into the mixed solution obtained in the step 1) to obtain a precipitate;
3) performing illumination treatment on the precipitate obtained in the step 2) to prepare the inorganic-organic hybrid superlattice material;
wherein, in the step 1), the inorganic material is selected from PbI2The organic material is selected from one of EtDAB, MeDAB or MeBEN.
8. The method according to claim 7, wherein the organic solvent of step 1) is selected from N, N' -dimethylformamide.
Preferably, the molar ratio of the organic material to the inorganic material in the mixed solution of step 1) is 1:0.1 to 5, preferably 1:1 to 4.5, for example 1:2 to 4.
Preferably, the anti-solvent of step 2) is acetonitrile and chlorobenzene, and after adding the anti-solvent, a yellow precipitate can be obtained.
Preferably, the anti-solvent of step 2) is added in an amount of 10mL of acetonitrile and 30mL of chlorobenzene per 1mL of the mixed solution.
Preferably, the illumination treatment in step 3) may be illumination under an incandescent lamp, a xenon lamp, an ultraviolet lamp, an infrared lamp; the illumination time is 1-2 hours.
9. Use of an inorganic-organic hybrid superlattice material as claimed in any one of claims 1-6 in a memory device.
10. A method of conductivity variation of an inorganic-organic hybrid superlattice material as claimed in any one of claims 1-6, said method comprising:
s1) heat treating the inorganic-organic hybrid superlattice material.
Preferably, the heating temperature is 100-200 ℃; the heating time is 1-2 hours. The conductivity of the superlattice material is 10-4S·cm-1The magnitude is that the conductivity of the superlattice material after heating and color change is reduced by 5 magnitudes, namely 10-9S·cm-1Magnitude.
Preferably, the method further comprises:
s2) placing the sample obtained after the heating treatment into an ethanol solution, and carrying out light treatment.
The illumination treatment can be illumination under an incandescent lamp, a xenon lamp, an ultraviolet lamp or an infrared lamp; the illumination time is 1-2 hours.
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| CN113834856A (en) * | 2020-06-24 | 2021-12-24 | 中国科学院福建物质结构研究所 | Large-size superlattice film and preparation method and application thereof |
| CN115739121A (en) * | 2022-11-14 | 2023-03-07 | 中国科学院福建物质结构研究所 | Metal-coated composite semiconductor material and preparation method and application thereof |
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| CN113834856A (en) * | 2020-06-24 | 2021-12-24 | 中国科学院福建物质结构研究所 | Large-size superlattice film and preparation method and application thereof |
| CN113834856B (en) * | 2020-06-24 | 2023-07-21 | 中国科学院福建物质结构研究所 | Large-size superlattice film and preparation method and application thereof |
| CN115739121A (en) * | 2022-11-14 | 2023-03-07 | 中国科学院福建物质结构研究所 | Metal-coated composite semiconductor material and preparation method and application thereof |
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