CN114377699A - Preparation method of ultrathin-structure bismuth oxyhalide material - Google Patents

Preparation method of ultrathin-structure bismuth oxyhalide material Download PDF

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CN114377699A
CN114377699A CN202111543192.7A CN202111543192A CN114377699A CN 114377699 A CN114377699 A CN 114377699A CN 202111543192 A CN202111543192 A CN 202111543192A CN 114377699 A CN114377699 A CN 114377699A
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bismuth
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ultrathin
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CN114377699B (en
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何敬敬
牛强
赵长森
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Inner Mongolia Erdos Electric Power Metallurgy Group Co Ltd
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06—Halogens; Compounds thereof
    • B01J27/08—Halides
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties

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Abstract

The invention discloses a preparation method of an ultrathin bismuth oxyhalide material, belonging to the technical field of preparation of nano materials. The method comprises the following steps: (1) dissolving bismuth halide in a solvent, and reacting to obtain a product; the solvent comprises N, N-dimethylformamide and water; (2) and carrying out post-treatment on the product to obtain the ultrathin-structure bismuth oxyhalide material. The invention utilizes a simple low-temperature hydrothermal method to directly dissolve bismuth halide (BiX) substances in a reaction kettle mainly containing N, N-dimethylformamide and a water solvent for reaction, and the ultrathin BiOX material is generated in one step.

Description

Preparation method of ultrathin-structure bismuth oxyhalide material
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of an ultrathin-structure bismuth oxyhalide material.
Background
Bismuth-based materials, the most representative of which is bismuth oxyhalide (BiOX), have unique layered structures, show good photogenerated carrier mobility and high electron-hole pair separation efficiency. Therefore, the bismuth-based photocatalyst has the advantages of a positive Valence Band (VB) potential, no toxicity, good stability and the like, and most of the past researches on BiOX are focused on the visible light-driven bismuth-based photocatalyst in the environmental field, such as dye pollutant degradation photocatalysis in wastewater. Today, itThe research application range is expanded to more fields, such as photocatalytic reduction of CO in the field of energy2And organic materials, even extending to the medical field. Such as bismuth oxyiodide (BiOI) with excellent photocatalytic performance and infrared thermal response bismuth sulfide (Bi)2S3) Combined and synthesized BiOI @ Bi2S3The nanometer diagnosis and treatment material of the semiconductor heterojunction can be used as a contrast agent for CT and photoacoustic imaging, and provides a technology for diagnosis and treatment of medical tumors.
The ideal BiOX photocatalyst has the characteristics of long-life photogenerated charge, proper band gap, full utilization of sunlight, low cost and the like. However, the activity of pure BiOX materials, such as photocatalysis, is limited due to the defects of narrow visible light absorption range, low carrier separation efficiency and the like, and the defects can be improved by changing the morphological structure or constructing a novel bismuth oxyhalide matrix system. Researches show that in the morphology structure, the thinner the corresponding BiOX structure is, the higher the corresponding {001} crystal face proportion is, the higher the defect concentration and the internal electric field intensity are, the higher the photon absorption efficiency and the carrier separation efficiency of the structure are, and the photocatalytic activity is favorably improved. In addition, the key core for constructing the novel bismuth oxyhalide matrix system still lies in the regulation and control of the morphology of the early bismuth oxyhalide matrix structure, and the surface structure of BiOX directly influences the energy band structure of the subsequent new system, thereby influencing the expansion of the catalytic performance in the corresponding application field.
The Chinese patent application CN201910501528.X discloses a method for preparing bismuth oxyhalide nanosheets in one step at normal temperature, which comprises the following steps: dissolving soluble bismuth salt in a solvent a at the normal temperature of 20-35 ℃ until the concentration of bismuth element is 80-400 mM, and carrying out ultrasonic treatment for 5-10 min until the soluble bismuth salt is completely dissolved to obtain a transparent solution A; dissolving soluble halide salt in a solvent B at the normal temperature of 20-35 ℃ until the concentration of the halide salt is 80-400 mM, and performing ultrasonic treatment for 5-10 min until the soluble halide salt KX or NaX is completely dissolved to obtain a transparent solution B; step (3), dropwise adding the solution B into the solution A under the stirring condition at the normal temperature of 20-35 ℃ to form a suspension C; and (4) stirring the mixture C for 1h, centrifuging, washing with deionized water and absolute ethyl alcohol in sequence, washing for 3-4 times respectively, and placing the obtained product in a 65-80 ℃ drying oven for 18-24 h to obtain dry solid powder.
At present, synthesis of BiOX materials with various shapes has been successfully realized by using methods such as hydrolysis, hydrothermal method, direct precipitation, solvent heat method and template method, but research and development of a low-temperature and simple method for synthesizing BiOX with large surface area and ultrathin structure is a key core for improving electrocatalysis performance and exploring wide application in different fields.
In view of the above, the invention utilizes a simple low-temperature hydrothermal method to directly dissolve a bismuth halide (BiX) substance in a reaction kettle mainly containing N, N-dimethylformamide and a water solvent for reaction, and the ultrathin BiOX material is generated in one step.
Disclosure of Invention
The invention aims to provide a preparation method of an ultrathin-structure bismuth oxyhalide material, which is simple and high in repeatability, and can be used for efficiently preparing an ultrathin-structure bismuth oxyhalide material with an ultra-large surface area
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of an ultrathin-structure bismuth oxyhalide material, which comprises the following steps:
(1) dissolving bismuth halide in a solvent, and reacting to obtain a product; the solvent comprises N, N-dimethylformamide and water;
(2) and carrying out post-treatment on the product to obtain the ultrathin-structure bismuth oxyhalide material.
Preferably, in step (1), the bismuth halide is bismuth iodide (BiI)3) Bismuth bromide (BiBr)3) Bismuth chloride (BiCl)3) And further preferably bismuth iodide.
Preferably, in step (1), the dissolving is carried out in a reaction vessel.
Preferably, in step (1), the operating temperature for the dissolution is 20 to 30 ℃, more preferably 25 ℃.
Preferably, in step (1), the concentration of the bismuth halide is 0.001 to 10mmol/mL after the bismuth halide is dissolved in the solvent.
Preferably, in the step (1), the volume ratio of the N, N-dimethylformamide to the water is 0.01-100: 1, more preferably 0.25 to 1.25: 1, more preferably 1: 1.
preferably, in the step (1), an additive capable of finely controlling the flake structure of the bismuth oxyhalide compound is further added to the solvent, and further preferably, the additive is at least one of sodium citrate, octadecyl trimethyl ammonium bromide (CTAB), citric acid, tartaric acid and sodium benzoate, and further preferably, sodium citrate and/or octadecyl trimethyl ammonium bromide.
Preferably, the molar ratio of the additive to the bismuth halide is 1: 10.
preferably, in the step (1), the solvent further includes an additional solvent capable of finely controlling the sheet structure of the bismuth oxyhalide compound, and further preferably, the additional solvent is at least one of a ketone solvent, an alcohol solvent, cyclohexane and a benzene solvent, and further preferably, an alcohol solvent.
Wherein, the ketone solvent is a ketone solvent commonly used in the art, such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone, diacetone alcohol, etc.; the alcohol solvent is an alcohol solvent commonly used in the art, such as methanol, ethanol, isopropanol, isobutanol, tert-butanol, benzyl alcohol, ethylene glycol, etc., and the benzene solvent is a benzene solvent commonly used in the art, such as toluene, xylene, trimethylbenzene, diphenyl ether, chlorobenzene, etc., which contain benzene ring
Preferably, the volume ratio of the additional solvent to water is 0-10: 1.
Preferably, in the step (1), the reaction temperature is 25-200 ℃, and the reaction time is 0-72 h; further preferably, the reaction temperature is 120-180 ℃, and the reaction time is 10-15 h.
Preferably, the step (2) is specifically: and cooling the product, washing the powder with a water/alcohol mixed solution, centrifuging and drying to obtain the ultrathin-structure bismuth oxyhalide material.
As a specific embodiment of the present invention, the water/alcohol mixed solution is a mixture of water and ethanol in a volume ratio of 1: 1 to prepare a mixed solution.
The invention has the beneficial effects that:
(1) the method has strong universality, and because each BiOX has a similar layered crystal structure, the band structure of the BiOX can be easily and accurately regulated and controlled by changing the type and the content of halogen atoms. Thus, with BiI3、BiBr3And BiCl3The bismuth source can be used for obtaining BiOI, BiOBr and BiOCl ultrathin sheet materials in an environment containing N, N-dimethylformamide and water;
(2) the process is simple and cost-effective, bismuth halide and additives can be directly dissolved in a reaction kettle containing N, N-dimethylformamide and water, and ultrathin sheets can be directly obtained at low temperature without further treatment;
(3) the structure precise control mode is simple to operate, and the shape of the sheet structure can be precisely controlled by directly adding additives such as alcohol solvents or sodium citrate and the like into the precursor;
(4) the synthesized BiOX has an ultrathin structure, an ultrathin bismuth oxyhalide base is obtained, and the thickness of a structural sheet is less than 30 nm.
Drawings
FIG. 1 is an XRD pattern of the BiOI prepared in example 1;
FIG. 2 is an SEM and TEM image of the BiOI prepared in example 1;
FIG. 3 is an SEM of the BiOI prepared in example 2;
FIG. 4 is an XRD pattern of BiOCl prepared in example 3;
FIG. 5 is an SEM image of BiOCl prepared in example 3.
Fig. 6 is an SEM image of the bio i prepared in example 4.
Fig. 7 is an SEM image of the bio i prepared in comparative example 1.
Fig. 8 is an SEM image of the bio i prepared in comparative example 2.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. The following is merely an exemplary illustration of the scope of the invention as claimed, and various changes and modifications of the invention of the present application may be made by those skilled in the art based on the disclosure, which also fall within the scope of the invention as claimed.
The "ranges" disclosed herein are in the form of lower and upper limits. There may be one or more lower limits, and one or more upper limits, respectively. The given range is defined by the selection of a lower limit and an upper limit. The selected lower and upper limits define the boundaries of the particular range. All ranges that can be defined in this manner are inclusive and combinable, i.e., any lower limit can be combined with any upper limit to form a range. For example, ranges of 60-120 and 80-110 are listed for particular parameters, with the understanding that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values 1 and 2 are listed, and if the maximum ranges 3, 4, and 5 are listed, the following ranges are all contemplated: 1-2, 1-4, 1-5, 2-3, 2-4 and 2-5.
In the present invention, unless otherwise stated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, a numerical range of "0 to 5" indicates that all real numbers between "0 to 5" have been listed herein, and "0 to 5" is only a shorthand representation of the combination of these numbers.
In the present invention, all embodiments and preferred embodiments mentioned herein may be combined with each other to form a new technical solution, if not specifically stated.
In the present invention, all the technical features mentioned herein and preferred features may be combined with each other to form new technical solutions, if not specifically mentioned.
The present invention will be further described below by way of specific examples. The various chemicals used in the examples of the present invention were obtained by conventional commercial routes unless otherwise specified.
Example 1
Preparing the BiOI ultrathin slice with ethanol added solvent: 36.8mg of bismuth iodide (BiI) are weighed out3) Dispersing in a reaction kettle containing solvent composed of 6mL of N, N-Dimethylformamide (DMF), 2mL of ethanol and 6mL of water, and dissolving with stirring or ultrasonic dissolving at room temperature for 5minThen the mixture is put into an oven with the temperature of 140 ℃ for reaction for 12 hours. After natural cooling, the mixture was washed with water/alcohol (1: 1 by volume), and the resulting powder was collected by centrifugation and dried overnight in a vacuum oven at 60 ℃.
Fig. 1 is an XRD pattern of the synthesized bio i. It can be seen that the actual synthesized powder structure matches the standard card PDF # 10-445 for BiOI.
Fig. 2 is SEM and TEM pictures of the synthesized bio i. A, B, C, D in the figure represent the appearance at different magnifications and different positions, and it can be seen that the actual synthesized BiOI powder is in the form of flakes; TEM breakthrough showed the thickness of the thin sheet of bio i to be around 13 nm.
Example 2
With the assistance of an octadecyl trimethyl ammonium bromide additive, the preparation of the BiOI ultrathin slice comprises the following steps: 36.8mg of BiI are weighed36.3mg of octadecyl trimethyl ammonium bromide, dispersed in a reaction vessel containing a solvent consisting of 6mL of DMF, 10mL of ethanol and 24mL of water, dissolved by stirring or ultrasonic dissolution at room temperature for 5min, and then placed in an oven at 140 ℃ to react for 12 h. After natural cooling, the mixture was washed with water/alcohol (1: 1 by volume), and the resulting powder was collected by centrifugation and dried overnight in a vacuum oven at 60 ℃.
Fig. 3 is an SEM picture of a bio i prepared with addition of octadecyl trimethyl ammonium bromide additive. A, B in the figure represent the appearance of different magnifications, it can be seen that the BiOI powder synthesized from octadecyl trimethyl ammonium bromide still presents a flake-like structure, with a flake thickness of less than 30 nm.
Example 3
Preparation of BiOCl ultrathin sheets: weigh 19.7mg BiCl3Dispersing in a reaction kettle containing a solvent consisting of 6mL of DMF, 10mL of ethanol and 24mL of water, stirring at room temperature for dissolving or ultrasonically dissolving for 5min, then placing in a 160 ℃ oven, and reacting for 12 h. After natural cooling, the mixture was washed with water/alcohol (1: 1 by volume), and the resulting powder was collected by centrifugation and dried overnight in a vacuum oven at 60 ℃.
Fig. 4 is an XRD pattern of the synthesized BiOCl. It can be seen that the actual synthesized powder structure matches BiOCl's standard card PDF # 06-249.
Fig. 5 is an SEM picture of the synthesized BiOCl. It can be seen that the actually synthesized BiOCl exhibits a lamellar structure with uniform morphology.
Example 4
36.8mg of BiI are weighed3Dispersing in a reaction kettle containing a solvent consisting of 6mL of DMF and 24mL of water, stirring at room temperature for dissolving or ultrasonically dissolving for 5min, then putting in an oven at 140 ℃, and reacting for 12 h. After natural cooling, the mixture was washed with water/alcohol (1: 1 by volume), and the resulting powder was collected by centrifugation and dried overnight in a vacuum oven at 60 ℃.
Fig. 6 is an SEM picture of the prepared bio i without the addition of additives and additional solvent. A, B in the figure represent the appearance of different magnifications, and it can be seen that the synthesized BiOI powder exhibits a heterogeneous morphology, a flake-like structure.
Comparative example 1
In contrast to example 1, the solvent was replaced with the same volume of water for N, N-dimethylformamide. That is, 36.8mg of bismuth iodide (BiI) was weighed3) Dispersing in a reaction kettle containing a solvent consisting of 12mL of water and 2mL of ethanol, stirring at room temperature for dissolving or ultrasonically dissolving for 5min, then placing in an oven at 140 ℃, and reacting for 12 h. After natural cooling, washing and centrifugal drying are carried out.
Fig. 7 is an SEM picture of the prepared BiOI. As can be seen, the synthesized BiOI has a random agglomeration blocky shape.
Comparative example 2
In contrast to example 1, water was replaced with the same volume of N, N-dimethylformamide in the solvent. That is, 36.8mg of bismuth iodide (BiI) was weighed3) Dispersing in a reaction kettle containing a solvent consisting of 12mL of N, N-Dimethylformamide (DMF) and 2mL of ethanol, stirring at room temperature for dissolving or ultrasonically dissolving for 5min, then placing in an oven at 140 ℃, and reacting for 12 h. After natural cooling, washing and centrifugal drying are carried out.
Fig. 8 is an SEM picture of the prepared BiOI. A, B in the figure represent the appearance of different magnifications, and it can be seen that the synthesized BiOI exhibits a sheet-like lamination and a petal-like morphology.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. A preparation method of an ultrathin structure bismuth oxyhalide material is characterized by comprising the following steps:
(1) dissolving bismuth halide in a solvent, and reacting to obtain a product; the solvent comprises N, N-dimethylformamide and water;
(2) and carrying out post-treatment on the product to obtain the ultrathin-structure bismuth oxyhalide material.
2. The method according to claim 1, wherein in the step (1), the bismuth halide is at least one of bismuth iodide, bismuth bromide and bismuth chloride.
3. The method according to claim 1, wherein in the step (1), the bismuth halide is bismuth iodide.
4. The method according to claim 1, wherein the dissolving in step (1) is carried out in a reaction kettle, and the dissolving is carried out at an operating temperature of 20-30 ℃, preferably 25 ℃.
5. The method according to claim 1, wherein in the step (1), the concentration of the bismuth halide is 0.001 to 10mmol/mL after the bismuth halide is dissolved in the solvent.
6. The method according to claim 1, wherein in the step (1), the volume ratio of N, N-dimethylformamide to water is 0.01 to 100: 1, preferably 0.25 to 1.25: 1, more preferably 1: 1.
7. the production method according to claim 1, wherein in the step (1), an additive capable of finely controlling the flake structure of the bismuth oxyhalide compound is added to the solvent; preferably, the additive is at least one of sodium citrate, octadecyl trimethyl ammonium bromide, citric acid, tartaric acid and sodium benzoate; further preferably sodium citrate and/or octadecyl trimethyl ammonium bromide; preferably, the molar ratio of the additive to the bismuth halide is 1: 10.
8. the preparation method according to claim 1, wherein in the step (1), the solvent further comprises an additional solvent capable of finely controlling the sheet structure of the bismuth oxyhalide compound, preferably, the additional solvent is at least one of a ketone solvent, an alcohol solvent, cyclohexane and a benzene solvent, and more preferably, the additional solvent is an alcohol solvent; preferably, the volume ratio of the additional solvent to water is 0-10: 1.
9. The preparation method according to claim 1, wherein in the step (1), the reaction temperature is 25-200 ℃, and the reaction time is 0-72 h; preferably, the reaction temperature is 120-180 ℃, and the reaction time is 10-15 h.
10. The preparation method according to claim 1, wherein the step (2) is specifically: and cooling the product, washing the powder with a water/alcohol mixed solution, centrifuging and drying to obtain the ultrathin-structure bismuth oxyhalide material.
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