Preparation method of cation-modified molybdenum oxide or tungsten oxide nanowire with large specific surface area

A technology of tungsten oxide nanowires and large specific surface area, applied in the direction of molybdenum oxide/molybdenum hydroxide, tungsten oxide/tungsten hydroxide, nanotechnology, etc., can solve the problem of small specific surface area of ​​nanowires, limited development and application, and high crystal density and other problems, to achieve the effect of rich surface hydroxyl groups, stable synthesis method, and simple equipment

Active Publication Date: 2018-06-15
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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Problems solved by technology

[0004] However, due to the high crystal density, the currently prepared molybdenum oxide and tungsten oxide nanowires have the following problems: (1) The diameter is generally relatively large, resulting in a small specific surface area of ​​the nanowires, generally less than 100 m 2 / g, and no specific surface area greater than 200 m 2 / g related reports; (2) The synthesis scale is small, the output is low, and the volume of the self-pressurized reactor used is generally less than 100 mL. These two insufficient factors seriously limit the development and application of molybdenum oxide and tungsten oxide one-dimensional nanowires.

Method used

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  • Preparation method of cation-modified molybdenum oxide or tungsten oxide nanowire with large specific surface area
  • Preparation method of cation-modified molybdenum oxide or tungsten oxide nanowire with large specific surface area
  • Preparation method of cation-modified molybdenum oxide or tungsten oxide nanowire with large specific surface area

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Experimental program
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Embodiment 1

[0038] Dissolve 0.16 mmol of ferric nitrate and 2 mmol of ammonium molybdate (molar ratio 0.08:1) in 70 mL of deionized water at the same time, then titrate with nitric acid until the pH of the solution is 1.0, and pour it into a 100 mL stainless steel self-pressurized reaction kettle after stabilization , After sealing, react at 160°C for 4h. After the reaction is completed, the sample is centrifuged, washed, and air-dried to obtain a molybdenum oxide nanowire sample.

[0039] Figure 1 is the X-ray diffraction spectrum of the nanowires obtained by the above reaction. It can be seen that the molybdenum oxide nanowire crystal form under the action of ferric iron belongs to the orthorhombic crystal system (JCPDS# 35-0609), and the crystallinity is low, along the [ 110] direction of growth.

[0040] Figure 6 (a) and (b) are the scanning and transmission photos of the product, respectively. It can be seen that the molybdenum oxide nanowires form a network structure with a diame...

Embodiment 2

[0043] Dissolve 0.6 mmol of chromium acetate and 3 mmol of sodium tungstate (molar ratio 0.2:1) in 110 mL of deionized water at the same time, then titrate with hydrochloric acid until the pH of the solution is 2.0, and pour it into a 150 ml stainless steel self-pressurized reaction kettle after stabilization , and react at 180°C for 12 h after sealing. After the reaction is completed, the sample is centrifuged, washed, and air-dried to obtain a tungsten oxide nanowire sample.

[0044] Figure 2 is the X-ray diffraction spectrum of the nanowires obtained by the above reaction. It can be seen from the figure that the crystal form of tungsten oxide nanowires obtained under the action of trivalent chromium belongs to the hexagonal crystal system (JCPDS# 35-1001), and the crystallinity is low, growing along the [001] direction.

[0045] Figure 7 (a) and (b) are the scanning and transmission photos of the product, respectively. It can be seen that the tungsten oxide nanowires are...

Embodiment 3

[0050] Dissolve 0.35 mmol of copper acetate and 3.5 mmol of sodium molybdate (molar ratio 0.1:1) in 100 ml of deionized water at the same time, then titrate with sulfuric acid until the pH of the solution is 1.5, and pour it into a 150 mL stainless steel self-pressurized reaction kettle after stabilization , and react at 200°C for 10 h after sealing. After the reaction is completed, the sample is centrifuged, washed, and air-dried to obtain a tungsten oxide nanowire sample.

[0051] Figure 3 is the X-ray diffraction spectrum of the nanowires obtained by the above reaction. It can be seen that the molybdenum oxide nanowire crystal form obtained under the action of divalent copper still belongs to the orthorhombic crystal system (JCPDS# 35-0609), and the crystallinity is low , growing along the [110] direction.

[0052] Figure 8 (a) and (b) are the scanning and transmission pictures of the obtained nanowires, respectively, with a diameter of 3-8 nm, a length of nanowires grea...

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Abstract

The invention discloses a preparation method of a cation-modified molybdenum oxide or tungsten oxide nanowire with a large specific surface area. The preparation method comprises the following steps of: dissolving inorganic cations and a molybdenum source or tungsten source in deionized water, stirring solution, simultaneously regulating the pH value of the solution to be above an isoelectric point of molybdenum oxide or tungsten oxide by using protonic acid, then transferring into a self-pressure reaction kettle, reacting for 1-30 hours at a constant temperature of 100-240 DEG C after sealing, separating out solid products after the reaction is ended, washing, and drying to obtain the cation-modified molybdenum oxide or tungsten oxide nanowire with the large specific surface area. The cation-modified molybdenum oxide or tungsten oxide nanowire has the characteristics that the diameter is small, the distribution is narrow (3-10nm), the length-diameter ratio is more than 250, the porouseffect is achieved, the specific surface area is not smaller than 200m<2> / g, the degree of crystallinity is lower and the surface hydroxyl groups are rich and the like.

Description

technical field [0001] The invention belongs to the preparation technology of one-dimensional nanometer materials, in particular to a method for preparing molybdenum oxide or tungsten nanowires with large specific surface area induced by inorganic cations. Background technique [0002] As two important transition metal oxides, molybdenum oxide and tungsten oxide have similar physical and chemical properties. They can not only be used as functional materials in sensing, photochromic and photocatalytic fields, but also can be used as excellent catalytic materials in traditional thermal catalysis. Therefore, it has received extensive attention from researchers at home and abroad. One-dimensional molybdenum oxide and tungsten oxide nanomaterials mainly include nanorods and nanowires, and nanowires have a larger aspect ratio, which is useful for studying the radial size and dimension of one-dimensional materials in optical, electrical, and sensing properties. function is of grea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02C01G39/02B82Y40/00
CPCB82Y40/00C01G39/02C01G41/02C01P2002/72C01P2002/82C01P2004/02C01P2004/04C01P2004/16C01P2006/12
Inventor 吕宝亮王会香曹英王连成
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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