CN108383160B - Preparation method and application of metal element doped BiOCl nanosheet material - Google Patents

Preparation method and application of metal element doped BiOCl nanosheet material Download PDF

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CN108383160B
CN108383160B CN201810323242.2A CN201810323242A CN108383160B CN 108383160 B CN108383160 B CN 108383160B CN 201810323242 A CN201810323242 A CN 201810323242A CN 108383160 B CN108383160 B CN 108383160B
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metal element
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chloride
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biocl nanosheet
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刘恩辉
周勇
韩秀莉
洪伟峰
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Xiangtan University
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract

The invention relates to a preparation method and application of a metal element doped BiOCl nanosheet material. The method adopts bismuthate, a doping source, a reducing agent, a chlorine source and an auxiliary agent as raw materials, and synchronously acts the mechanical force of high-energy ball milling on oxidation reduction, doping and chlorination reactions, and then obtains the metal element doped BiOCl nanosheet material through heat treatment, washing for impurity removal, solid-liquid separation and drying. The molar ratio of the doped metal element to the bismuth element in the obtained material is (0.01-0.3): 1, the material is composed of nanosheets with the plane size of 20-500 nm and the thickness of 1-20 nm, and the specific surface area is 3-300 m2(ii) in terms of/g. The invention has simple process, easy realization of industrial production, low manufacturing process cost and environmental protection; the prepared metal element doped BiOCl nanosheet material has wide application in the fields of supercapacitors, alkaline secondary batteries, lithium ion batteries, photocatalysts, pearlescent pigments, medicines and the like.

Description

Preparation method and application of metal element doped BiOCl nanosheet material
Technical Field
The invention relates to a preparation method and application of a metal element doped BiOCl nanosheet material, and belongs to the field of novel functional materials.
Background
Bismuth oxychloride is an important functional material, and has wide application in the fields of electrode active materials, catalysts, pigments, cosmetics, gas sensors, electronic materials, medical materials and the like due to the unique microstructure and physicochemical properties, no toxicity and low cost. In order to further improve the performance of the BiOCl material, metal element doping is an important means.
The structure and performance of the material are closely related to the preparation process. The existing methods for synthesizing ultrafine functional powder can be classified into physical methods and chemical methods according to the synthesis principle. These methods have been widely used for powder synthesis, but have respective disadvantages. The physical method can prepare the ultra-fine particles with easily controlled particle size, but the required equipment is expensive; the chemical method has low cost, is easy to adjust the particle size through process control, but has complex process flow and is likely to bring environmental pollution. The mechanochemical method combines a physical method with a chemical method, and the basic principle is that the energy provided by a reactant through a grinding process improves the chemical activity of the reactant, so that the reaction which is usually required to be carried out at a high temperature can be rapidly carried out at a lower temperature. The mechanochemical synthesis method is a synthesis method with low price, environmental protection, high efficiency and high controllability, and the preparation method ensures that the structure and the performance of the material have more design possibilities and is easy for industrial production.
Sarwan et al Applied Surface Science 258(2011) 247-. Yang et al [ Phys.chem.chem.Phys.16(2014)21349-21355] prepared a tungsten-doped bismuth oxychloride material by a solvothermal method by using bismuth nitrate, tungsten chloride, potassium chloride and urea as raw materials and ethylene glycol as a solvent and researching the photocatalytic performance of the tungsten-doped bismuth oxychloride material. Zhang et al [ Applied Catalysis B: Environmental 221(2018)320-328] uses bismuth nitrate, sodium chloride and cobalt chloride as raw materials, uses ethylene glycol and Triton X-100 as additives, prepares a cobalt-doped BiOCl material by a hydrothermal method, and researches the photocatalytic performance of degrading bisphenol A under visible light. Dou et al Separation and Purification Technology 162(2016) 114-.
The invention patent (application publication No. CN 103421511A) discloses a rare earth ion doped bismuth oxyhalide luminescent material and a preparation method thereof, wherein bismuth nitrate, rare earth nitrate and potassium halide are mixed according to a certain molar ratio and dissolved in a solvent, a surfactant is added and stirred uniformly, and then the pH of the solution is adjusted and transferred into a reaction kettle for hydrothermal reaction to prepare the rare earth ion doped bismuth oxyhalide luminescent material. The invention patent (application publication No. CN 105478149A) discloses preparation of a tin-doped bismuth oxychloride visible light catalyst, which is characterized in that a bismuth nitrate solution with a certain concentration is dropwise added into a tin chloride solution with a certain concentration under the condition of stirring, then a sodium hydroxide solution is dropwise added into a mixed solution of the bismuth nitrate solution and the tin chloride solution to adjust the pH value for reaction for 2 hours, and a tin-doped BiOCl material is prepared after washing and drying. The invention patent [ application publication No. CN105032452A ] discloses a preparation method of a K-doped BiOCl photocatalyst with high visible light activity, and the preparation method comprises the steps of adding a certain amount of potassium nitrate, ammonium chloride and citric acid into a bismuth nitrate solution, and heating and evaporating the solvent at 250-400 ℃ to prepare the K-doped BiOCl material.
At present, many researches on the preparation of BiOCl materials doped with metal elements mainly include a hydrothermal method, a solvothermal method, a sol-gel method and the like. However, these methods generally have the problems of complicated synthesis process, high cost, etc.
Disclosure of Invention
The invention aims to provide a preparation method and application of a metal element doped BiOCl nanosheet material. The molar ratio of the doped metal element to the bismuth element in the prepared material is (0.01-0.3): 1, the material is composed of nanosheets with the plane size of 20-500 nm and the thickness of 1-20 nm, and the specific surface area is 3-300 m2/g。
The invention is realized by the following technical scheme:
a preparation method of a metal element doped BiOCl nanosheet material comprises the following steps:
(1) uniformly mixing bismuthate, a doping source, a reducing agent, a chlorine source and an auxiliary agent according to a molar ratio (the ratio of the amount of substances) of 1 (0.01-0.3) to 0.25-2 to 0.001-0.3 to obtain a raw material mixture;
(2) putting the raw material mixture obtained in the step (1) and grinding balls into a ball mill according to the mass ratio of 1 (0.5-100), and carrying out ball milling for 0.2-20 h under a protective atmosphere;
(3) and (3) placing the ball-milled mixture obtained in the step (2) in a high-temperature furnace for heat treatment at 100-600 ℃ for 0.5-10 h, washing and removing impurities of the heat-treated product with distilled water and absolute ethyl alcohol respectively, and then carrying out solid-liquid separation and drying to obtain the metal element doped BiOCl nanosheet material.
Further, the bismuthate is one or more than two of sodium bismuthate, lithium bismuthate, potassium bismuthate and magnesium bismuthate.
Furthermore, the doping source metal element is one or more than two of iron, copper, nickel, cobalt, titanium, manganese and rare earth, and the doping source is one or more than two of simple substances, oxides, hydroxides, oxalates, acetates, citrates, nitrates, carbonates, sulfates and halides of the metal elements.
Furthermore, the reducing agent is one or more than two of doping source metal element reduction substance, metal bismuth powder, carbon powder, sulfite, formaldehyde (or paraformaldehyde), formic acid, reducing sugar and phenol.
Further, the chlorine source is a compound containing chloride ions, preferably one or more of hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride, zinc chloride, ferric chloride, cupric chloride, aluminum chloride, calcium chloride, and magnesium chloride.
Further, the auxiliary agent is one or more than two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, hexadecyl trimethyl ammonium bromide, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, triethanolamine, ethylene glycol, glycerol, nonionic surfactant, saccharide and soluble starch.
Further, the protective atmosphere is one or more than two of nitrogen, argon, carbon dioxide and air.
Furthermore, the rotating speed of the ball mill is 30-3000 rpm.
Further, the ball mill is selected from various types on the market; the grinding balls are one or more than two of agate balls, corundum balls, zirconia balls, ceramic balls and stainless steel balls.
The metal element-doped BiOCl nanosheet material obtained by the preparation method is applied to the fields of supercapacitors, alkaline secondary batteries, lithium ion batteries, photocatalysts, pearlescent pigments, medicines and the like.
The invention has the beneficial effects that:
(1) the method has the advantages of simple preparation process, mild process conditions, easy industrial production, environment-friendly production process, high product purity and easy control of the micro-morphology and size of the product.
(2) The metal element doped BiOCl nanosheet material prepared by the method disclosed by the invention is wide in application, and can be applied to the fields of supercapacitors, alkaline secondary batteries, lithium ion batteries, photocatalysts, pearlescent pigments, medical intermediates and the like.
Drawings
Fig. 1 is a scanning electron microscope image of the iron-doped BiOCl nanosheet material prepared in example 1.
Figure 2 is a scanning electron microscope image of the copper-doped BiOCl nanoplatelets prepared in example 2.
Fig. 3 is a cyclic voltammetry test chart of a secondary alkaline electrode composed of the cobalt-doped BiOCl nanosheet prepared in example 3 and nickel hydroxide at different scanning rates.
Fig. 4 is a nitrogen sorption desorption isotherm plot of the manganese-doped BiOCl nanosheet material prepared in example 4.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific examples, but the present invention is not limited to the examples.
Example 1
(1) Uniformly mixing 2mmol of sodium bismuthate, 0.6mmol of metal bismuth powder, 0.01mmol of ferric ammonium oxalate, 2mmol of potassium chloride and 0.02mmol of polyvinylpyrrolidone to obtain a raw material mixture; adding the raw material mixture and a corundum grinding ball into a ball mill according to the mass ratio of 1:60, introducing air, carrying out ball milling for 8 hours under the condition that the rotating speed is 800rpm, carrying out constant-temperature heat treatment on the ball-milled mixture for 5 hours at 300 ℃, washing a heat-treated product by using deionized water and absolute ethyl alcohol to remove impurities, carrying out solid-liquid separation by adopting filtration, and finally carrying out vacuum drying on a solid product obtained by filtration for 12 hours at 90 ℃ to obtain the 5% iron-doped BiOCl nanosheet material.
(2) And (3) characterizing the iron-doped BiOCl nanosheet material obtained in the example 1 by adopting a JEOLJEM-3010 type scanning electron microscope, wherein the iron-doped BiOCl nanosheet material is composed of square nanosheets with the thickness of 5-10 nm and the plane size of 200-400 nm as shown in figure 1.
Example 2
(1) Uniformly mixing 2mmol of potassium bismuthate, 2mmol of sodium sulfite, 0.016mmol of copper acetate, 2mmol of ammonium chloride and 0.01mmol of polyethylene glycol to obtain a raw material mixture; adding the raw material mixture and a porcelain ball grinding ball into a ball milling tank according to the mass ratio of 1:100, introducing nitrogen, carrying out ball milling for 6h under the condition of the rotating speed of 1500rpm, carrying out constant-temperature heat treatment on the ball-milled mixture for 3h at 400 ℃, washing a heat-treated product by using deionized water and absolute ethyl alcohol to remove impurities, carrying out solid-liquid separation by adopting filtration, and finally drying a solid product obtained by filtration at 110 ℃ for 10h to obtain the 8% copper-doped BiOCl nanosheet material.
(2) And (3) characterizing the copper-doped BiOCl nanosheet material obtained in the example 2 by adopting a JEOLJEM-3010 type scanning electron microscope, wherein the material is composed of square nanosheets with the thickness of 5-10 nm and the plane size of about 300nm as shown in FIG. 2.
Example 3
(1) Uniformly mixing 2mmol of magnesium bismuthate, 0.5mmol of paraformaldehyde, 0.2mmol of cobalt sulfate, 2mmol of sodium chloride and 0.03mmol of sodium dodecyl benzene sulfonate to obtain a raw material mixture; adding the raw material mixture and zirconia ball grinding balls into a ball-milling tank according to the mass ratio of 1:70, introducing carbon dioxide, carrying out ball milling for 6h under the condition that the rotating speed is 1000rpm, carrying out constant-temperature heat treatment on the ball-milled mixture for 4h at 300 ℃, washing a heat-treated product by using deionized water and absolute ethyl alcohol to remove impurities, carrying out solid-liquid separation by adopting filtration, and finally drying a solid product obtained by filtration at 120 ℃ for 10h to obtain the 10% cobalt-doped BiOCl nanosheet material.
(2) Preparing the prepared sample into an electrode plate, assembling the electrode plate, a nickel hydroxide positive plate and 6mol/L KOH solution into an alkaline secondary battery, and performing cyclic voltammetry on the constructed secondary alkaline battery at room temperature by adopting a CHI660A electrochemical workstation manufactured by Shanghai Chenghua company. As shown in FIG. 3, the cyclic voltammetry curves of the cell at different scanning rates have good reversibility of the redox peak at higher scanning rates, and show good electrochemical performance.
Example 4
(1) Uniformly mixing 2mmol of sodium bismuthate, 1mmol of reducing sugar, 0.016mmol of manganese sulfate, 2mmol of sodium chloride and 0.06mmol of hexadecyl trimethyl ammonium bromide to obtain a raw material mixture; adding the raw material mixture and stainless steel ball grinding balls into a ball-milling tank according to the mass ratio of 1:50, introducing nitrogen, carrying out ball milling for 15h under the condition that the rotation speed is 900rpm, carrying out constant-temperature heat treatment on the ball-milled mixture for 3h at 400 ℃, washing a heat-treated product by using deionized water and absolute ethyl alcohol to remove impurities, carrying out solid-liquid separation by adopting filtration, and finally drying a solid product obtained by filtration for 12h at 80 ℃ to obtain the 8% manganese-doped BiOCl nanosheet material.
(2) The sample material was tested using a TriStar II 3020 model specific surface area and pore size distribution apparatus, as shown in FIG. 4, the manganese-doped BiOCl nanoplatelet material had a specific surface area of 12.8m2/g。

Claims (5)

1. The preparation method of the metal element-doped BiOCl nanosheet material is characterized in that the metal element-doped BiOCl nanosheet material is applied to an alkaline secondary battery, the molar ratio of the doped metal element to the doped bismuth element in the material is (0.01-0.3): 1, the material is composed of nanosheets with the plane size of 20-500 nm and the thickness of 1-20 nm, and the specific surface area is 3-300 m2(ii)/g; the preparation method comprises the following steps:
(1) uniformly mixing bismuthate, a doping source, a reducing agent, a chlorine source and an auxiliary agent according to the molar ratio of 1 (0.01-0.3) to (0.25-2) to (0.001-0.3) to obtain a raw material mixture;
(2) putting the raw material mixture obtained in the step (1) and grinding balls into a ball mill according to the mass ratio of 1 (0.5-100), and carrying out ball milling for 0.2-20 h under a protective atmosphere;
(3) placing the ball-milled mixture obtained in the step (2) in a high-temperature furnace, performing heat treatment for 0.5-10 hours at 100-600 ℃, washing and removing impurities of a product after the heat treatment with distilled water and absolute ethyl alcohol respectively, and then performing solid-liquid separation and drying to obtain a metal element doped BiOCl nanosheet material;
the chlorine source is one or more than two of sodium chloride, potassium chloride, ammonium chloride, zinc chloride, ferric chloride, copper chloride, aluminum chloride, calcium chloride and magnesium chloride;
the reducing agent is one or more than two of a reduction substance doped with source metal elements, metal bismuth powder, carbon powder, sulfite, formaldehyde, paraformaldehyde, formic acid, reducing sugar and phenol;
the auxiliary agent is one or more than two of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, hexadecyl trimethyl ammonium bromide, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, triethanolamine, ethylene glycol, glycerol, nonionic surfactant, saccharide substances and soluble starch.
2. The method for preparing a metal element-doped BiOCl nanosheet material as claimed in claim 1, wherein the bismuthate is one or more of sodium bismuthate, lithium bismuthate and potassium bismuthate.
3. The method for preparing a metal element-doped BiOCl nanosheet material according to claim 1, wherein the doping source metal element is one or more of iron, copper, nickel, cobalt, titanium, manganese and rare earth; the doping source is one or more than two of simple substances, oxides, hydroxides, oxalates, acetates, citrates, nitrates, carbonates, sulfates and halides of the metal elements.
4. The method for preparing a metal element-doped BiOCl nanosheet material according to claim 1, wherein the protective atmosphere is one or more of nitrogen, argon, carbon dioxide and air.
5. The preparation method of the metal element doped BiOCl nanosheet material according to claim 1, wherein the ball mill is selected from various commercially available models; the grinding balls are one or more than two of agate balls, corundum balls, zirconia balls, ceramic balls and stainless steel balls; the rotating speed of the ball mill is 30-3000 rpm.
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