Preparation method of multi-dimensional pure-phase W18O49

A pure-phase, multi-dimensional technology, applied in nanotechnology for materials and surface science, tungsten oxide/tungsten hydroxide, nanotechnology, etc., can solve the problem of material morphology, poor crystallinity, low product purity, sintering High temperature and other problems, to achieve the effect of controllable shape and size, high purity and good crystallinity

Inactive Publication Date: 2015-11-11
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The solid-phase synthesis method has higher sintering temperature, longer holding time, and lower product purity
Prepared...

Method used

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  • Preparation method of multi-dimensional pure-phase W18O49
  • Preparation method of multi-dimensional pure-phase W18O49
  • Preparation method of multi-dimensional pure-phase W18O49

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) 0.7852g of analytically pure WCl 6 Add it to 40mL of absolute ethanol to prepare a solution, and seal it with plastic wrap in time to avoid contact with air.

[0033] 2) Stir the solution with a magnetic stirrer for 30 minutes. After the solution gradually changes from yellow to blue, perform ultrasonic (60 Hz) treatment for 30 minutes to obtain a uniformly mixed solution;

[0034] 3) Pour the uniformly mixed solution into a 100mL autoclave lined with polytetrafluoroethylene, and the volume filling ratio is controlled at 40%; feed 30min of N into the autoclave 2 To reduce the oxygen in the reactor, then put the sealed reactor into a homogeneous reactor, and react at 160°C for 24 hours.

[0035] 4) After the reaction is completed, cool down to room temperature with the furnace, centrifuge and wash the final reactant with absolute ethanol for 3 times, put the centrifuged material in a vacuum oven and dry at 40°C for 12 hours to obtain a multidimensional pure phase W ...

Embodiment 2

[0039] 1) 0.5968g of analytically pure WCl 6 Add it to 50mL of isopropanol to prepare a solution, and seal it with plastic wrap in time to avoid contact with air.

[0040] 2) Stir the solution with a magnetic stirrer for 20 minutes. After the solution gradually changes from yellow to blue, perform ultrasonic (60 Hz) treatment for 40 minutes to obtain a uniformly mixed solution;

[0041] 3) Pour the homogeneously mixed solution into a 100 mL polytetrafluoroethylene-lined autoclave, keeping the volume filling ratio at 50%. Introduce 20min of N into the reactor 2 To reduce the oxygen in the reactor, then put the sealed reactor into a homogeneous reactor, and react at 170°C for 6h.

[0042] 4) After the reaction is completed, cool down to room temperature with the furnace, and centrifuge and wash the final reactant with absolute ethanol for 5 times. The centrifuged material was dried in a vacuum oven at 60°C for 3 hours to obtain a multidimensional pure phase W 18 o 49 .

[...

Embodiment 3

[0045] 1) 0.8328g of analytically pure WCl 6 Add it to the mixture of absolute ethanol and isopropanol to prepare a solution, and seal it with plastic wrap in time to avoid contact with air. Wherein, in the mixture of absolute ethanol and isopropanol, the volume ratio of absolute ethanol:isopropanol=1:1, and each of absolute ethanol and isopropanol is 20 mL.

[0046] 2) Stir the solution with a magnetic stirrer for 40 minutes. After the solution gradually changes from yellow to blue, perform ultrasonic (60 Hz) treatment for 40 minutes to obtain a uniformly mixed solution;

[0047] 3) Pour the homogeneously mixed solution into a 100 mL polytetrafluoroethylene-lined autoclave, keeping the volume filling ratio at 40%. Introduce 20min of N into the reactor 2 To reduce the oxygen in the reactor, then put the sealed reactor into a homogeneous reactor, and react at 160°C for 18h.

[0048] 4) After the reaction is completed, cool down to room temperature with the furnace, and centr...

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Abstract

The invention discloses a preparation method of multi-dimensional pure-phase W18O49. The preparation method comprises the steps of placing analytically pure WCl6 into alcohol to prepare a solution; stirring the solution until the solution turns from yellow to blue, and then, carrying out ultrasonic treatment to obtain a uniformly-mixed solution; pouring the uniformly-mixed solution into a high-pressure reaction kettle, and then, introducing N2 to the reaction kettle; and then, placing the high-pressure reaction kettle into a homogeneous reactor, reacting at the temperature of 120-200 DEG C, then, separating and drying to obtain the multi-dimensional pure-phase W18O49. The preparation method is simple, low in raw material component and relatively low in raw material cost, both the reaction temperature and time are controlled within the relatively wide range, and the multi-dimensional pure-phase W18O49 is not needed to be subjected to later-period crystallization treatment, so that defects of grain growth, roughening or curling and the like possibly caused in the later-period heat treatment process are avoided to a certain extent. The W18O49 prepared by using the preparation method is various in shape such as a sea urchin shape assembled by using nanowires, a flower shape assembled by using sheets and a flower or sphere shape assembled by using wires.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, in particular to a multidimensional pure phase W 18 o 49 method of preparation. Background technique [0002] Tungsten oxide has a variety of existing forms and crystal structures, including the stoichiometric ratio of WO 3 and non-stoichiometric W 18 o 49 (WO 2.72 ), W 5 o 14 (WO 2.8 ), W 24 o 68 (WO 2.83 ) and W 20 o 58 (WO 2.9 ), its general chemical formula is WO 3-x (x=0~1). non-stoichiometric WO 3-x The color is yellow-green depending on the oxygen content. It is an important multifunctional n-type wide bandgap (2.5-3.6eV) semiconductor. It exhibits many unique properties and has potential applications. For example, due to tungsten oxide Due to its electrochromic, photochromic and aerochromic properties, it can be widely used in the fields of flat panel displays, smart windows and various sensors. . [0003] where W 18 o 49 Has the largest number of oxy...

Claims

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Application Information

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IPC IPC(8): C01G41/02B82Y30/00
Inventor 黄剑锋海国娟介燕妮曹丽云李嘉胤吴建鹏孔新刚卢靖张博
Owner SHAANXI UNIV OF SCI & TECH
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