CN108300470B - Preparation method of quasi-low-dimensional bismuth-based perovskite nano material - Google Patents

Preparation method of quasi-low-dimensional bismuth-based perovskite nano material Download PDF

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CN108300470B
CN108300470B CN201711417269.XA CN201711417269A CN108300470B CN 108300470 B CN108300470 B CN 108300470B CN 201711417269 A CN201711417269 A CN 201711417269A CN 108300470 B CN108300470 B CN 108300470B
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dimensional bismuth
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唐江
冷美英
陈正午
牛广达
杨颖�
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Huazhong University of Science and Technology
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Abstract

The invention discloses a preparation method of a quasi-low-dimensional bismuth-based perovskite nano material, which comprises the following steps: adopts quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The powder of (a) is used as a raw material, amine is used as a stripping agent, and a solvent is used to obtain a mixture; then, the mixture was treated with a cell crusher, followed by centrifugation, and the supernatant was taken to obtain MA3Bi2X9Of (4) a nanomaterial of (2). The invention can effectively solve the problems of complex synthesis method, lower concentration of the obtained nano material colloidal solution and lower yield of the bismuth-based perovskite nano material compared with the prior art by improving the whole process flow design of the key preparation method, parameter conditions of each step and the like, particularly utilizing strong energy given by a cell crusher and the stripping action of amine to separate the quasi-low-dimensional bismuth-based perovskite material and controlling the types and the proportion of reaction raw materials, the specific power and time of the crushing process and the like.

Description

Preparation method of quasi-low-dimensional bismuth-based perovskite nano material
Technical Field
The invention belongs to the field of photoelectric material preparation, and particularly relates to a preparation method of a quasi-low-dimensional bismuth-based perovskite nano material.
Background
The perovskite nano material has wide application prospect in the field of luminous display due to the advantages of extremely high quantum yield, low cost, simple preparation method and the like.
The perovskite nano material can utilize halogen elements and size effect to adjust the luminescence property (mainly the luminescence wavelength), so that the luminescence spectrum can cover the whole visible light region (400-800nm), and the perovskite nano material has great potential in LED application. However, the research on perovskite nano materials at present mainly aims at Pb base, and the substitution of novel non-toxic elements for Pb and the like has great difficulty due to too high defect concentration or poorer stability of the materials, and only Bi-based perovskite quantum dots subjected to ligand-assisted reprecipitation and Sn-based non-toxic perovskite nano crystals prepared by a thermal injection method are tried to a certain extent, but the preparation process is complex and needs to be further improved.
Disclosure of Invention
Aiming at the above defects or improvement requirements of the prior art, the invention aims to provide a preparation method of a quasi-low-dimensional bismuth-based perovskite nano material, wherein the key preparation method is improved in overall process flow design, parameter conditions of each step and the like, particularly, a cell crusher is used for providing strong energy and the stripping action of amine to separate the quasi-low-dimensional bismuth-based perovskite material, and the problems of complex synthesis method of the bismuth-based perovskite nano material, lower concentration of the obtained nano material colloidal solution and lower yield can be effectively solved compared with the prior art by controlling the types and proportion of reaction raw materials, the specific power and time of the crushing process and the like, and the method can realize the conversion from high-dimensional (such as 3-dimensional) powder or material blocks to low-dimensional (such as 0/1/2-dimensional) nano materials from high to low, the bismuth-based perovskite nano material with or without' is synthesized by a simple synthesis method, and the bismuth-based perovskite nano material prepared by the method has stable performance and excellent performance.
In order to achieve the above object, according to the present invention, there is provided a method for preparing a quasi-low dimensional bismuth-based perovskite nano material, comprising the steps of: adopts quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The powder of (A) is used as a raw material, amine is used as a stripping agent, and a solvent is used to obtain the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9Wherein X is at least one of Cl, Br, I, and a mixture of the solvent capable of dissolving the stripping agent and having a solubility for the stripping agent greater than that for the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9(ii) a solubility of (a); then, the mixture was treated with a cell crusher, followed by centrifugation, and the supernatant was taken to obtain MA3Bi2X9The quasi-low-dimensional bismuth-based perovskite nano material.
In a further preferred embodiment of the present invention, the raw material MA is the pseudo-low-dimensional bismuth-based perovskite material3Bi2X9The amount of the powder of (4) is in the range of 0.02 to 0.1 mmol.
In a further preferred embodiment of the present invention, the amine as the release agent is at least one of butylamine, n-octylamine, and oleylamine;
the solvent is any one of n-octane, n-hexane, toluene and a methanol/n-octane mixed solvent.
In a further preferred embodiment of the present invention, in the mixture, the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The ratio of the amounts of substances of both the amine and the powder of (1): 15 to 62.5;
the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The ratio of the amount of the substance of (2) to the volume of the solvent is 0.04mmol: 6-15 ml.
As a further optimization of the invention, the mixture also comprises oleic acid as a ligand, and the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The ratio of the amount of the oleic acid to the amount of the powder of (1) to the amount of the oleic acid is 1:37.5 to 75.
In a further preferred embodiment of the present invention, the mixture is treated by the cell crusher at a power of 200 to 400W for 30 to 60 minutes, the duty ratio of the cell crusher is 1/3 to 1/2, and the continuous ultrasonic treatment time is 1 second.
Compared with the prior art, the technical scheme of the invention synthesizes the green, environment-friendly and high-fluorescence quantum yield MA by adopting a novel synthesis method of 'from high to low, from existence to nonexistence' of a crushing method (especially a ligand-assisted crushing method)3Bi2X9The perovskite nano material can solve the problem that the synthesis method of the bismuth-based perovskite nano material in the prior art is complex on one hand, and can overcome the defects of low concentration and low yield of the nano material colloidal solution obtained in the prior art on the other handThe invention has important significance for the research of the performance and the luminology of the novel semiconductor nano material.
The existing perovskite nano material synthesis methods are all processes of 'growing nuclei from nothing to nothing' and mainly aim at Pb-based perovskite materials. Compared with Pb-based perovskite, Bi-based perovskite is not only environment-friendly, but also quasi-low-dimensional material, i.e. octahedral framework is low-dimensional structure, and MA+Inserted in an octahedral framework (quasi low dimensional materials are identical in that the crystal structure contains low latitude structural parts compared with standard low dimensional materials, except that 1. the low latitude structure in quasi low latitude materials is composed of anionic octahedra, the low latitude structure in standard low latitude materials is composed of atoms directly, 2. the low latitude structure in quasi low latitude materials is unbalanced in charge and requires electrostatic force to provide electrostatic force to keep the charge balance, so that MA + cations are located near the low latitude structure, and in standard low latitude materials, the low latitude structure is electrically neutral and is combined by Van der Waals force to form a macroscopic material).
Quasi-low-dimensional bismuth-based perovskite material MA used in the invention3Bi2X9The powder raw material of (3) can be prepared by the preparation method in the prior art, such as an anti-solvent precipitation method, a solvent volatilization method and the like; as for the powder raw material, a large number of quasi-low-dimensional structures are connected together through ionic bonds, and a single quasi-low-dimensional bismuth-based perovskite nano material cannot be obtained generally; the invention uses amine as a stripping agent and uses a solvent to carry out ultrasonic treatment, so that single nano materials which are mutually separated can be obtained, and the quasi-low-dimensional bismuth-based perovskite nano material products are in a single separated state under a microscope and can be used. The invention also preferably uses oleic acid as a ligand, so that the oleic acid is attached to the surface of the separated nano material to play a role in protection, thereby preparing the nano material capable of stably existing.
The invention particularly controls the quasi-low-dimensional bismuth-based perovskite material MA used3Bi2X9The amount of the powder, the ratio of the stripping agent to the powder, the specific power and time of the pulverizing process, will beLow-dimensional bismuth-based perovskite material MA3Bi2X9The amount of the powder material is controlled to be not more than 0.1mmol, which can ensure that the powder is uniformly peeled off (mainly because the amount of the powder used is proportional to the volume of the solvent, while the ultrasonic wave used in the pulverization process is generated by a vibrating rod, the energy is weakened along with the increase of the distance, and the solution volume is too large, which can cause that a large amount of the powder cannot be uniformly peeled off); taking the solvent as n-octane as an example, the quasi-low-dimensional bismuth-based perovskite material MA in the mixture3Bi2X9The ratio of the amounts of the powder, the amine and the n-octane of (1): 15-62.5: 1000-2250, controlling the power used in the crushing process to 200-400W, controlling the treatment time to 30-60 minutes, and detaching the quasi-low-dimensional bismuth-based perovskite material by using strong energy given by a cell crusher and the stripping effect of amine, thereby realizing the preparation of the quasi-low-dimensional bismuth-based perovskite nano material with good stability and other properties.
Drawings
FIG. 1 is a MA implemented in accordance with the present invention3Bi2X9The structure diagram of the unit cell corresponds to Cl (1D), Br (2D) and I (0D) from left to right respectively, wherein I (0D), Br (2D) and Cl (1D) correspond to 0-dimensional-MA respectively3Bi2I9Quasi 2-dimensional-MA3Bi2Br9And quasi-1-dimensional-MA3Bi2Cl9The structure of (1);
FIG. 2 is a MA implemented in accordance with the present invention3Bi2Br9An absorption spectrum of the nanomaterial;
fig. 3 is a MA implemented in accordance with the present invention3Bi2Br9A fluorescence spectrum of the nanomaterial;
fig. 4 is a MA implemented in accordance with the present invention3Bi2Cl9Electron microscopy of nanomaterials.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The preparation method of the quasi-low-dimensional bismuth-based perovskite nano material comprises the following steps: adopts quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The powder of (X ═ Cl, Br, I) is used as a raw material, an amine is added as a stripping agent, and n-octane is used as a solvent (other solvents may be used as long as they can simultaneously satisfy the condition that the perovskite material is insoluble or slightly soluble and the stripping agent is soluble; for example, n-hexane, toluene, a mixed solvent of methanol and n-octane, etc.) may be used; the quasi-low-dimensional bismuth-based perovskite material is detached by utilizing strong energy given by a cell crusher and the stripping action of amine, so that the synthesis of a new nano material from high to low and from existence to nonexistence is realized; centrifuging, collecting supernatant to obtain a compound of formula MA3Bi2X9Of (4) a nanomaterial of (2).
The invention can also utilize a ligand auxiliary crushing method (correspondingly, ligand material raw materials need to be added), as shown in figure 1, the manufacturing principle is as follows: 1) adopts quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The method comprises the following steps of (X ═ Cl, Br and I) powder is used as a raw material, amine is added to serve as a stripping agent to assist in crushing of the quasi-low-dimensional bismuth-based perovskite material, and n-octane which cannot dissolve the quasi-low-dimensional bismuth-based perovskite material is used as a solvent; 2) the cell crusher is utilized to provide strong energy to cooperate with the stripping effect of amine to separate the quasi-low-dimensional bismuth-based perovskite material, so as to realize the synthesis of new nano materials from high to low and from existence to nonexistence; 3) centrifuging, collecting supernatant to obtain a compound of formula MA3Bi2X9Of (4) a nanomaterial of (2).
The invention relates to a preparation method of a quasi-low-dimensional bismuth-based perovskite nano material, which comprises the following preparation steps and key points: 1) the molar value of the quasi-low-dimensional bismuth-based perovskite material powder is 0.02-0.1 mmol, and the powder is crushed by a cell crusher; 2) the amine is used as a stripping agent, the amine comprises amine types with different C chain lengths such as butylamine, n-octylamine, oleylamine and the like, and the molar ratio of the raw material powder to the amine to the solvent n-octane is 1: 15-62.5: 1000 to 2250; 3) oleic acid serves as a ligand to protect the resulting quantum dots and to disperse them in n-octane.
In the invention, various selected materials are selected from elements with high abundance in the earth crust, the resources are rich, the environment is friendly because no toxic component is contained, and the perovskite structure and the adjustable light-emitting range thereof enable the perovskite structure to become a low-cost pollution-free light-emitting nano material with development potential.
The following are specific examples:
example one
The preparation method of the quasi-low-dimensional bismuth-based perovskite nano material comprises the following specific steps:
step 1: cleaning a glass bottle; for example, deionized water, acetone, isopropanol and deionized water can be used for sequentially cleaning a white glass bottle for ten minutes respectively, and then the white glass bottle is dried by a nitrogen gun;
step 2: adding 0.02mmol of MA3Bi2Br9Adding the mixture into a glass bottle, adding 5mL of n-octane and 0.5mL of oleic acid into the bottle in sequence to serve as a solvent and a ligand respectively, and then adding 100uL of n-octylamine to serve as a stripping agent;
wherein, the raw material MA3Bi2Br9Is quasi 2-dimensional bismuth-based perovskite powder;
and step 3: putting the glass bottle into a cell crusher to adjust the power to 45 (namely the power is 300W) and start crushing for 30 minutes;
and 4, step 4: taking out the suspension in the glass bottle, centrifuging the suspension at 8000rpm, and taking the supernatant to obtain a light yellow Bi-based perovskite nanosheet colloidal solution.
Example two
The preparation method of the quasi-low-dimensional bismuth-based perovskite nano material comprises the following specific steps:
step 1: cleaning a glass bottle; sequentially cleaning a white glass bottle with deionized water, acetone, isopropanol and deionized water for ten minutes respectively, and then blowing the white glass bottle with a nitrogen gun;
step 2: adding 0.02mmol of MA3Bi2I9Adding into a glass bottle, adding 5mL of n-octane into the bottleAnd 0.5mL of oleic acid are respectively used as a solvent and a ligand, and then 200uL of n-octylamine is added as a stripping agent;
wherein, the raw material MA3Bi2I9Quasi-0-dimensional bismuth-based perovskite powder;
and step 3: putting the glass bottle into a cell crusher, adjusting the power to 45, and starting crushing for 30 minutes;
and 4, step 4: taking out the suspension in the glass bottle, centrifuging the suspension at 8000rpm, and taking the supernatant to obtain the light red Bi-based perovskite quantum dot colloidal solution.
EXAMPLE III
The preparation method of the quasi-low-dimensional bismuth-based perovskite nano material comprises the following specific steps:
step 1: cleaning a glass bottle; sequentially cleaning a white glass bottle with deionized water, acetone, isopropanol and deionized water for ten minutes respectively, and then blowing the white glass bottle with a nitrogen gun;
step 2: adding 0.02mmol of MA3Bi2Cl9Adding the mixture into a glass bottle, adding 5mL of n-octane and 0.5mL of oleic acid into the bottle in sequence to serve as a solvent and a ligand respectively, and then adding 100uL of n-octylamine to serve as a stripping agent;
wherein, the raw material MA3Bi2Cl9Is quasi-1-dimensional bismuth-based perovskite powder;
and step 3: putting the glass bottle into a cell crusher, adjusting the power to 45, and starting crushing for 30 minutes;
and 4, step 4: taking out the suspension in the glass bottle, centrifuging the suspension at 8000rpm, and taking the supernatant to obtain a white Bi-based perovskite nanowire colloidal solution.
Taking the first embodiment using the quasi-2-dimensional bismuth-based perovskite powder as an example, in the original powder raw material, a large number of multi-layer nanosheets are tightly combined and stacked together due to the action of atomic/molecular interaction forces such as ionic bonds, and the quasi-low-dimensional bismuth-based perovskite nano material on the microscopic scale cannot be obtained, but the preparation method in the first embodiment can be used for obtaining the mutually-separated quasi-low-dimensional bismuth-based perovskite nano material on the microscopic scale; the surface of the quasi-low-dimensional bismuth-based perovskite nano material obtained by treatment can be combined with oleic acid to form a nano material nano sheet which exists stably; and, if the supernatant containing the nanosheets obtained by this treatment (the supernatant may be used as an intermediate product or as a final product) is dried, the nanosheet materials therein will remain in a state of being separated from each other.
The adopted raw material quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The powder of (a) may be commercially available, or may be prepared by itself by a conventional preparation method (e.g., antisolvent precipitation, solvent evaporation, etc.).
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (5)

1. A preparation method of a quasi-low-dimensional bismuth-based perovskite nano material is characterized by comprising the following steps: adopts quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The powder of (A) is used as a raw material, amine is used as a stripping agent, and a solvent is used to obtain the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9Wherein X is one of Cl, Br and I, and the solvent is capable of dissolving the stripping agent and has a solubility for the stripping agent greater than that for the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The solvent is any one of n-octane, n-hexane, toluene and a methanol/n-octane mixed solvent; then, the mixture is treated by a cell crusher, and the energy applied by the cell crusher and the stripping effect of amine can overcome the defect of the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9Separating the bismuth-based perovskite material with quasi-low dimension by ionic bond in the powder, centrifuging, and collecting the supernatant to obtain the compound of formula MA3Bi2X9The quasi-low-dimensional bismuth-based perovskite nano material;
wherein the amine as the stripping agent is at least one of butylamine, n-octylamine, and oleylamine;
when X is Cl, the raw material is quasi-1-dimensional bismuth-based perovskite nano material MA3Bi2Cl9Obtained powder of the formula MA3Bi2X9The quasi-low-dimensional bismuth-based perovskite nano material has a chemical formula of MA3Bi2Cl9The nanowire of (a);
when X is Br, the raw material is quasi 2-dimensional bismuth-based perovskite nano material MA3Bi2Br9Obtained powder of the formula MA3Bi2X9The quasi-low-dimensional bismuth-based perovskite nano material has a chemical formula of MA3Bi2Br9A nanosheet of (a);
when X is I, the raw material is quasi-0-dimensional bismuth-based perovskite nano material MA3Bi2I9Obtained powder of the formula MA3Bi2X9The quasi-low-dimensional bismuth-based perovskite nano material has a chemical formula of MA3Bi2I9The quantum dot of (1).
2. The method for producing a quasi-low-dimensional bismuth-based perovskite nanomaterial as claimed in claim 1, wherein the quasi-low-dimensional bismuth-based perovskite material MA as the raw material3Bi2X9The amount of the powder of (4) is in the range of 0.02 to 0.1 mmol.
3. The method for preparing the quasi-low dimensional bismuth-based perovskite nano-material as claimed in claim 1, wherein in the mixture, the quasi-low dimensional bismuth-based perovskite material MA3Bi2X9The ratio of the amounts of substances of both the amine and the powder of (1): 15 to 62.5;
the quasi-low-dimensional bismuth-based perovskite material MA3Bi2X9The ratio of the amount of substance of (a) to the volume of the solvent was 0.04mmol:6ml ~ 15 ml.
4. The method for preparing the quasi-low dimensional bismuth-based perovskite nano-material as claimed in any one of claims 1 to 3, wherein the mixture further comprises oleic acid as a ligand, and the quasi-low dimensional bismuth-based perovskite material MA3Bi2X9The ratio of the amount of the oleic acid to the amount of the powder of (1) to the amount of the oleic acid is 1:37.5 to 75.
5. The preparation method of the quasi-low dimensional bismuth-based perovskite nano material as claimed in any one of claims 1 to 3, wherein the cell crusher is used for processing the mixture under the power of 200W-400W for 30-60 minutes, the duty ratio of the cell crusher is 1/3-1/2, and the continuous ultrasonic time is 1 second.
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CN106390985A (en) * 2016-08-31 2017-02-15 中国科学院新疆理化技术研究所 Preparation method of ultrathin H1.78Sr0.78Bi0.22Nb2O7 nano-sheet
CN106433619A (en) * 2016-09-27 2017-02-22 华中科技大学 Preparation method of Bi-based perovskite quantum dot material
CN106631816A (en) * 2016-12-23 2017-05-10 浙江大学 Preparation method of atomic-scale thickness two-dimensional perovskite nanosheet by liquid phase stripping

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Publication number Priority date Publication date Assignee Title
CN106390985A (en) * 2016-08-31 2017-02-15 中国科学院新疆理化技术研究所 Preparation method of ultrathin H1.78Sr0.78Bi0.22Nb2O7 nano-sheet
CN106433619A (en) * 2016-09-27 2017-02-22 华中科技大学 Preparation method of Bi-based perovskite quantum dot material
CN106631816A (en) * 2016-12-23 2017-05-10 浙江大学 Preparation method of atomic-scale thickness two-dimensional perovskite nanosheet by liquid phase stripping

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