CN110327913B - Nano-flake tungsten oxide/graphene oxide core-shell structure material and preparation method and application thereof - Google Patents

Nano-flake tungsten oxide/graphene oxide core-shell structure material and preparation method and application thereof Download PDF

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CN110327913B
CN110327913B CN201910706959.XA CN201910706959A CN110327913B CN 110327913 B CN110327913 B CN 110327913B CN 201910706959 A CN201910706959 A CN 201910706959A CN 110327913 B CN110327913 B CN 110327913B
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graphene oxide
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structure material
tungsten oxide
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王文静
刘柏雄
万长茂
王子璇
孙强
陈宜
戴天翔
程斌
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Jiangxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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    • B01J35/397Egg shell like
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Abstract

A nano flaky tungsten oxide/graphene oxide core-shell structure material, a preparation method and application thereof. Uniformly mixing tungsten powder and sodium fluoride to obtain mixed powder A; get H2O2And HNO3Uniformly mixing to obtain a mixed solution B; adding a graphene oxide aqueous solution into the mixed solution B to obtain a mixed solution C; slowly adding the mixed powder A into the mixed solution C to obtain a solution E; and (3) placing the solution E in a hydrothermal reaction kettle for hydrothermal reaction, cooling, washing, collecting and drying to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material. The core-shell structure material is of a square single-layer lamellar structure, an inner-layer core is a square tungsten oxide nanosheet, an outer layer is graphene oxide, the thickness of the tungsten oxide single-layer lamellar is 10-30 nm, the length and the width are 100-250 nm, and the coating thickness of the outer-layer graphene oxide is 5-20 nm. The material is applied to the fields of sodium/lithium/magnesium ion batteries, supercapacitors and photocatalysis, and shows excellent performance.

Description

Nano-flake tungsten oxide/graphene oxide core-shell structure material and preparation method and application thereof
Technical Field
The invention relates to a preparation method of a core-shell structure nanosheet layer material, and particularly relates to a preparation method of an in-situ synthesized nano flaky tungsten oxide/graphene oxide core-shell structure material.
Background
Tungsten trioxide is a stable n-type semiconductor material and is widely applied to photocatalysis, electrochemical catalysis and the like. In recent years, with the intensive research on lithium/sodium ion batteries, tungsten trioxide has also been widely used in electrochemical energy storage, and has been studied mainly as a negative electrode material for lithium/sodium ion batteries. However, the nanometer tungsten trioxide has the defects of slow charge transfer rate, few surface reaction active sites, easy recombination of photo-generated electron hole pairs and the like, and the application field of the nanometer tungsten trioxide is greatly limited. Graphene oxide, as a novel two-dimensional carbon material, has a large specific surface area, excellent electrical conductivity, good mechanical properties, and high chemical and thermal stability, and is widely used in the electrochemical field.
In recent years, although tungsten trioxide/graphene oxide composite materials have been extensively studied by researchers as battery negative electrode materials, few reports have been made on two-dimensional nanocomposite materials in which tungsten trioxide is used as a core and graphene oxide is used as a shell.
Disclosure of Invention
The invention aims to provide the preparation method for in-situ synthesis of the nano flaky tungsten oxide/graphene oxide core-shell structure material, which is simple to operate, low in reaction temperature and short in reaction period, and the prepared tungsten oxide/graphene oxide core-shell structure material is single in structure and high in purity.
In order to achieve the purpose, the invention adopts the following technical scheme:
1) uniformly mixing tungsten powder and sodium fluoride according to the mass ratio of 10: 1-10: 3 to obtain mixed powder A;
2) respectively taking 5-15 ml of H with the mass concentration of 30%2O2And 5-15 ml of HNO with the mass concentration of 69%3Uniformly mixing to obtain a mixed solution B;
3) adding 2-6 ml of graphene oxide aqueous solution with the mass concentration of 0.05% -0.15% into the mixed solution B to obtain a mixed solution C;
4) slowly adding 1-8 g of the mixed powder A into the mixed solution C, and stirring until the mixed powder A is fully dissolved to obtain a solution E;
5) and (3) placing the solution E in a hydrothermal reaction kettle for hydrothermal reaction at 120-200 ℃, and after the reaction is finished, cooling, washing, collecting and drying to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material.
The size of the tungsten powder is 2-3 mu m.
The graphene oxide is of a micron-sized single-layer graphene oxide structure.
The stirring is magnetic stirring or ultrasonic dispersion.
The filling ratio of the solution E in the hydrothermal reaction kettle is 35-75%.
The reaction time is 20-35 h.
The washing is carried out for 3-5 times by adopting absolute ethyl alcohol for centrifugal washing, and the collection is centrifugal collection.
The drying temperature is 50-80 ℃, and the drying time is 12-16 h.
The core-shell structure material prepared by the preparation method is of a square single-layer lamellar structure, the inner-layer core is a square tungsten oxide nanosheet, the outer layer is graphene oxide, the thickness of the tungsten oxide single-layer lamellar is 10-30 nm, the length and the width are 100-250 nm, and the coating thickness of the outer-layer graphene oxide is 5-20 nm.
The nano flaky tungsten oxide/graphene oxide core-shell structure material prepared by the preparation method is applied to the fields of sodium/lithium/magnesium ion batteries, supercapacitors and photocatalysis.
Compared with the prior art, the invention has at least the following beneficial effects:
the method adopts in-situ one-step synthesis of the tungsten oxide/graphene oxide core-shell structure nano powder, does not need large-scale equipment and harsh reaction conditions, does not need a morphology control agent, has easily obtained raw materials, low cost and high yield, does not need post-treatment, is environment-friendly, and can be suitable for large-scale production.
The tungsten oxide/graphene oxide core-shell structure nano powder prepared by the method has a core-shell structure with tungsten oxide as a core and graphene oxide as a shell. The nano powder with the core-shell structure is applied to the fields of sodium/lithium/magnesium ion batteries and photocatalysis, and shows excellent performance.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of the nano-flake tungsten oxide/graphene oxide core-shell structure material powder prepared in example 1 of the present invention;
fig. 2 and 3 are Scanning Electron Microscope (SEM) photographs and Transmission Electron Microscope (TEM) photographs of the nano-flake tungsten oxide/graphene oxide core-shell structure material powder prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example 1:
1) uniformly mixing 2-3 mu m tungsten powder and sodium fluoride according to a mass ratio of 10:1 to obtain mixed powder A;
2) respectively taking 5ml of H with the mass concentration of 30 percent2O2And 5ml of HNO with the mass concentration of 69 percent3Mixing evenly to obtain a mixed solution B;
3) adding 2ml of a 0.05 mass% micron-sized graphene oxide aqueous solution with a single-layer structure into the mixed solution B to obtain a mixed solution C;
4) slowly adding 1g of the mixed powder A into the mixed solution C, and obtaining a solution E after the mixed powder A is fully dissolved by magnetic stirring;
5) and (3) placing the solution E in a hydrothermal reaction kettle according to the filling ratio of 35% for hydrothermal reaction at 160 ℃ for 22 hours, cooling after the reaction is finished, centrifugally washing for 3 times by adopting absolute ethyl alcohol, centrifugally collecting, and drying at 50 ℃ for 12 hours to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material.
The core-shell structure material synthesized in situ by the method is a square single-layer lamellar structure, the inner-layer core is a square tungsten oxide nanosheet, the outer layer is graphene oxide, the thickness of the tungsten oxide single-layer lamellar is 10-30 nm, the length and the width are 100-250 nm, and the coating thickness of the outer-layer graphene oxide is 5-20 nm. The core-shell material is applied to the fields of sodium/lithium/magnesium ion batteries and photocatalysis. Especially when applied to a sodium ion battery, the electrolyte shows excellent electrochemical performance.
As can be seen from fig. 1, the prepared composite material is a composite material of tungsten trioxide and graphene oxide.
As clearly shown in FIG. 2, the prepared nano-powder is a single-layer sheet structure with uniform size, the size of 100-200nm and the thickness of about 20-30 nm.
As can be further seen from fig. 3, the prepared nano monolayer sheet is tungsten oxide with the length and width of about 100nm, and the outer layer is uniformly coated with a graphene oxide layer with the thickness of about 15 nm. Further proves that the prepared material has a core-shell structure.
Example 2:
1) uniformly mixing 2-3 mu m tungsten powder and sodium fluoride according to a mass ratio of 10:1.5 to obtain mixed powder A;
2) respectively taking 8ml of H with the mass concentration of 30 percent2O2And 8ml of HNO with the mass concentration of 69 percent3Uniformly mixing to obtain a mixed solution B;
3) adding 2.5ml of a 0.1 mass percent micron-sized graphene oxide aqueous solution into the mixed solution B to obtain a mixed solution C;
4) slowly adding 2.5g of the mixed powder A into the mixed solution C, and performing ultrasonic dispersion to obtain a solution E after the mixed powder A is fully dissolved;
5) and (3) placing the solution E in a hydrothermal reaction kettle according to a filling ratio of 75% for hydrothermal reaction at 180 ℃ for 24 hours, cooling after the reaction is finished, centrifugally washing for 3 times by adopting absolute ethyl alcohol, centrifugally collecting, and drying at 60 ℃ for 14 hours to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material.
Example 3:
1) uniformly mixing 2-3 mu m tungsten powder and sodium fluoride according to a mass ratio of 10:3 to obtain mixed powder A;
2) 10ml of H with the mass concentration of 30 percent are respectively taken2O2And 10ml of HNO with the mass concentration of 69 percent3Uniformly mixing to obtain a mixed solution B;
3) adding 4ml of a 0.13 mass% micron-sized graphene oxide aqueous solution into the mixed solution B to obtain a mixed solution C;
4) slowly adding 5.2g of the mixed powder A into the mixed solution C, and obtaining a solution E after the mixed powder A is fully dissolved by magnetic stirring;
5) and (3) placing the solution E in a hydrothermal reaction kettle according to the filling ratio of 35% for hydrothermal reaction at 160 ℃ for 30 hours, cooling after the reaction is finished, centrifugally washing for 5 times by adopting absolute ethyl alcohol, centrifugally collecting, and drying at 80 ℃ for 16 hours to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material.
Example 41:
1) uniformly mixing 2-3 mu m tungsten powder and sodium fluoride according to a mass ratio of 10:2 to obtain mixed powder A;
2) respectively taking 15ml of H with the mass concentration of 30 percent2O2And 12ml of HNO with the mass concentration of 69 percent3Uniformly mixing to obtain a mixed solution B;
3) adding 5ml of a 0.08 mass percent micron-sized graphene oxide aqueous solution into the mixed solution B to obtain a mixed solution C;
4) slowly adding 8g of the mixed powder A into the mixed solution C, and performing ultrasonic dispersion to obtain a solution E after the mixed powder A is fully dissolved;
5) and (3) placing the solution E in a hydrothermal reaction kettle according to the filling ratio of 50% for hydrothermal reaction at 120 ℃ for 35 hours, cooling after the reaction is finished, centrifugally washing for 4 times by adopting absolute ethyl alcohol, centrifugally collecting, and drying at 70 ℃ for 13 hours to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material.
Example 5:
1) uniformly mixing 2-3 mu m tungsten powder and sodium fluoride according to a mass ratio of 10:2.5 to obtain mixed powder A;
2) 12ml of H with the mass concentration of 30 percent are respectively taken2O2And 15ml of HNO with the mass concentration of 69 percent3Uniformly mixing to obtain a mixed solution B;
3) adding 6ml of a 0.15 mass% micron-sized graphene oxide aqueous solution into the mixed solution B to obtain a mixed solution C;
4) slowly adding 6g of the mixed powder A into the mixed solution C, and performing ultrasonic dispersion to obtain a solution E after the mixed powder A is fully dissolved;
5) and (3) placing the solution E in a hydrothermal reaction kettle according to the filling ratio of 60% for hydrothermal reaction at 200 ℃ for 20 hours, cooling after the reaction is finished, centrifugally washing for 5 times by adopting absolute ethyl alcohol, centrifugally collecting, and drying at 80 ℃ for 12 hours to obtain the nano flaky tungsten oxide/graphene oxide core-shell structure material.
Compared with the prior art, the invention at least has the following beneficial effects:
the method adopts in-situ one-step synthesis of the tungsten oxide/graphene oxide core-shell structure nano powder, does not need large-scale equipment and harsh reaction conditions, does not need a morphology control agent, has easily obtained raw materials, low cost and high yield, does not need post-treatment, is environment-friendly, and can be suitable for large-scale production.
The tungsten oxide/graphene oxide core-shell structure nano powder prepared by the method has a core-shell structure with tungsten oxide as a core and graphene oxide as a shell. The nano powder with the core-shell structure is applied to the fields of sodium/lithium/magnesium ion batteries and photocatalysis, and shows excellent performance.

Claims (10)

1. A preparation method of a nano flaky tungsten oxide/graphene oxide core-shell structure material is characterized by comprising the following steps:
1) uniformly mixing tungsten powder and sodium fluoride according to the mass ratio of 10: 1-10: 3 to obtain mixed powder A;
2) respectively taking 5-15 ml of H with the mass concentration of 30%2O2And 5-15 ml of HNO with the mass concentration of 69%3Uniformly mixing to obtain a mixed solution B;
3) adding 2-6 ml of graphene oxide aqueous solution with the mass concentration of 0.05% -0.15% into the mixed solution B to obtain a mixed solution C;
4) slowly adding 1-8 g of the mixed powder A into the mixed solution C, and stirring until the mixed powder A is fully dissolved to obtain a solution E;
5) placing the solution E in a hydrothermal reaction kettle for hydrothermal reaction at 120-200 ℃, cooling, washing, collecting and drying after the reaction is finished, and obtaining the nano flaky tungsten oxide/graphene oxide core-shell structure material;
the core-shell structure material is of a square single-layer lamellar structure, an inner-layer core is a square tungsten oxide nanosheet, an outer layer is graphene oxide, the thickness of the tungsten oxide single-layer lamellar is 10-30 nm, the length and the width are 100-250 nm, and the coating thickness of the outer-layer graphene oxide is 5-20 nm.
2. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the size of the tungsten powder is 2-3 mu m.
3. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the graphene oxide is of a micron-sized single-layer graphene oxide structure.
4. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the stirring is magnetic stirring.
5. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the filling ratio of the solution E in the hydrothermal reaction kettle is 35-75%.
6. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the reaction time is 20-35 h.
7. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the washing is carried out for 3-5 times by adopting absolute ethyl alcohol for centrifugal washing, and the collection is centrifugal collection.
8. The preparation method of the nano flaky tungsten oxide/graphene oxide core-shell structure material according to claim 1, which is characterized in that: the drying temperature is 50-80 ℃, and the drying time is 12-16 h.
9. The nano flaky tungsten oxide/graphene oxide core-shell structure material prepared by the preparation method according to claim 1, which is characterized in that: the core-shell structure material is of a square single-layer lamellar structure, an inner-layer core is a square tungsten oxide nanosheet, an outer layer is graphene oxide, the thickness of the tungsten oxide single-layer lamellar is 10-30 nm, the length and the width are 100-250 nm, and the coating thickness of the outer-layer graphene oxide is 5-20 nm.
10. The nano flaky tungsten oxide/graphene oxide core-shell structure material prepared by the preparation method according to claim 1, which is characterized in that: the nano flaky tungsten oxide/graphene oxide core-shell structure material is applied to the field of supercapacitors or photocatalysis.
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石墨烯基复合材料的合成及相关电化学性能研究;黄猛;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140915(第09期);第3.3.2节和第3.5节 *
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