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 PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 61
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 45
- 239000011258 core-shell material Substances 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002060 nanoflake Substances 0.000 title description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 32
- 239000011812 mixed powder Substances 0.000 claims abstract description 23
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- 239000010410 layer Substances 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000002356 single layer Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 8
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 8
- 238000007146 photocatalysis Methods 0.000 claims abstract description 7
- 230000001699 photocatalysis Effects 0.000 claims abstract description 7
- 239000002135 nanosheet Substances 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001425 magnesium ion Inorganic materials 0.000 abstract description 5
- 229910052708 sodium Inorganic materials 0.000 abstract description 5
- 239000011734 sodium Substances 0.000 abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 14
- 239000011858 nanopowder Substances 0.000 description 7
- 238000011065 in-situ storage Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000011257 shell material Substances 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
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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
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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