Synthesis method and application of two-dimensional layered tungsten nitride nanoparticles

A technology of tungsten nitride nanometer synthesis method, which is applied in the direction of nitrogen-metal/silicon/boron binary compound, material excitation analysis, Raman scattering, etc., can solve the problems of irregular material shape and lengthy steps, etc. Regular appearance, good repeatability and stability, strong manipulation effect

Pending Publication Date: 2022-07-26
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above method has problems such as lengthy steps and irregular morphology of the prepared materials.

Method used

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  • Synthesis method and application of two-dimensional layered tungsten nitride nanoparticles
  • Synthesis method and application of two-dimensional layered tungsten nitride nanoparticles
  • Synthesis method and application of two-dimensional layered tungsten nitride nanoparticles

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Embodiment 1

[0043] This embodiment provides a method for preparing two-dimensional layered tungsten nitride nanoparticles:

[0044] 1) 5g of tungsten hexachloride was added to the ethanol solution of 99.5% in 300mL of ethanol solution, the rotating speed of 300r / min was magnetically stirred until the solution became pale yellow, and it was transferred into the 100mL reaction kettle at 120°C in the blast drying oven. Hold for 12h. After cooling to room temperature, it was transferred to a centrifuge tube, centrifuged (centrifugation speed 8000r / min, centrifugation time 6min), washed with deionized water, repeated 3 times, and the sample was kept in a blast drying oven at 55°C for 12h to dry.

[0045] 2) Place the dried sample in a tube furnace, feed into a mixed gas of nitrogen and ammonia (the flow rate of ammonia gas is 5mL / min, and the flow rate of nitrogen gas is 2mL / min), and the temperature is raised to 6°C / min. 720°C and kept for 8h to obtain the final sample.

[0046] The obtaine...

Embodiment 2

[0048] This embodiment provides a method for preparing two-dimensional layered tungsten nitride nanoparticles:

[0049] 4.5g of tungsten hexachloride was added to the 300mL ethanol solution with a concentration of 99.5%, the rotating speed of 280r / min was magnetically stirred until the solution became pale yellow, transferred to a 100mL reaction kettle and kept at 110°C in a blast drying oven. 10h. After cooling to room temperature, it was transferred to a centrifuge tube, centrifuged (centrifugation speed 8500 r / min, centrifugation time 4 min), washed with deionized water, repeated 3 times, and the sample was kept in a blast drying oven at 60 °C for 10 h to dry.

[0050]2) Place the dried sample in a tube furnace, feed into a mixed gas of nitrogen and ammonia (the flow rate of ammonia gas is 7mL / min, and the flow rate of nitrogen gas is 3.5mL / min), and the temperature rises at a heating rate of 1°C / min. to 700°C and kept for 6h to obtain the final sample.

[0051] The obtai...

Embodiment 3

[0053] This embodiment provides a method for preparing two-dimensional layered tungsten nitride nanoparticles:

[0054] Add 4g of tungsten hexachloride to 300mL of ethanol solution with a concentration of 99.5%, stir magnetically at a speed of 260r / min until the solution turns light yellow, transfer it to a 100mL reaction kettle and keep it in a blast drying oven at 100°C for 4h . After cooling to room temperature, it was transferred to a centrifuge tube, centrifuged (centrifugation speed 9000r / min, centrifugation time 5min), washed with deionized water, and after repeated 3 times, the samples were kept in a blast drying oven at 75°C for 7h to dry.

[0055] 2) Place the dried sample in a tube furnace, feed the mixed gas of nitrogen and ammonia (the flow rate of ammonia gas is 5mL / min, and the flow rate of nitrogen gas is 2mL / min), and heat up to 3°C / min at a heating rate. 710°C and kept for 4h to obtain the final sample.

[0056] The obtained final sample was XRD ( Figure ...

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Abstract

The invention belongs to the field of synthesis of nano materials, and discloses a synthesis method of two-dimensional layered tungsten nitride nano particles. The method comprises the following steps: (1) carrying out hydrothermal reaction by taking tungsten hexachloride and an ethanol solution as raw materials to obtain tungsten oxide; the mass ratio of the tungsten hexachloride to the ethanol solution in the reaction process is 1: (39.5-59.25); the temperature of the hydrothermal reaction is 100-140 DEG C; and 2) carrying out nitrogen treatment on the tungsten oxide obtained in the step 1) to obtain the two-dimensional layered tungsten nitride nanoparticles. The vapor deposition method is adopted for preparing the two-dimensional layered tungsten nitride, operation is easy and convenient, and the prepared two-dimensional layered tungsten nitride is regular and controllable in morphology and has good repeatability and stability.

Description

technical field [0001] The invention belongs to the field of nanomaterial synthesis, in particular to a synthesis method and application of a two-dimensional layered tungsten nitride nanoparticle. Background technique [0002] Surface-enhanced Raman scattering (SERS) is a highly sensitive and fast analytical technique, which is widely used due to its excellent advantages. Traditional SERS uses precious metals such as gold and silver as substrates. However, the development of noble metal materials is limited by the high cost of noble metal base materials, which has led to the gradual development of SERS technology research on semiconductor materials. In the preparation of semiconductor SERS substrate materials, the substrate of a single-layer sheet material is relatively easy to prepare, but it is more difficult to make the material itself a two-dimensional layered structure. When a material with a two-dimensional layered structure is placed in an optical field, the gap bet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/06G01N21/65
CPCC01B21/062G01N21/658C01P2002/72C01P2002/82C01P2004/03
Inventor 孔庆红刘大民李未希陈明毅
Owner JIANGSU UNIV
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