A kind of synthesis method and application of single crystal porous square flaky tungsten nitride nanoparticles

A tungsten nitride nanotechnology and synthesis method, which is applied in chemical instruments and methods, single crystal growth, nanotechnology, etc., can solve the problems of irregular material shape and lengthy steps, and achieve regular shape, good repeatability and Stability, effects of strong localized surface plasmon resonance effects

Active Publication Date: 2022-04-15
CHINESE ACAD OF INSPECTION & QUARANTINE
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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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  • A kind of synthesis method and application of single crystal porous square flaky tungsten nitride nanoparticles
  • A kind of synthesis method and application of single crystal porous square flaky tungsten nitride nanoparticles
  • A kind of synthesis method and application of single crystal porous square flaky tungsten nitride nanoparticles

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] This embodiment provides a preparation method of single crystal porous square flaky tungsten nitride nanoparticles:

[0047] 1) Add 0.3g of sodium tungstate dihydrate and 0.1g of sodium oxalate into 25mL of deionized water, stir magnetically at a speed of 300r / min for 1.5h, add 1mL of a saturated aqueous solution of hydrochloric acid dropwise, continue stirring for 5min, turn to Put it into a 100mL reactor and keep it in a blast drying oven at 100°C for 12h. After cooling down to room temperature, transfer to a centrifuge tube, centrifuge (centrifugation speed 8000r / min, centrifugation time 7min), wash with deionized water, repeat 3 times, and keep the sample in a blast drying oven at 50°C for 12h to dry.

[0048] 2) Place the dried sample in a tube furnace, feed a mixed gas of nitrogen and ammonia (the flow rate of ammonia gas is 10mL / min, and the flow rate of nitrogen gas is 10mL / min), and the temperature is raised to 750°C and keep for 7h to get the final sample.

...

Embodiment 2

[0051] This embodiment provides a preparation method of single crystal porous square flaky tungsten nitride nanoparticles:

[0052] 1) Add 0.32g of sodium tungstate dihydrate and 0.12g of sodium oxalate into 27mL of deionized water, stir magnetically at a speed of 400r / min for 1h, add 1mL of a saturated aqueous solution of hydrochloric acid dropwise, continue stirring for 6min, and transfer to In a 100mL reactor, keep it at 110°C for 10h in a blast drying oven. After cooling down to room temperature, transfer to a centrifuge tube, centrifuge (centrifugation speed 9000r / min, centrifugation time 5min), wash with deionized water, repeat 4 times, and keep the sample in a blast drying oven at 60°C for 10h to dry.

[0053] 2) Place the dried sample in a tube furnace, feed a mixed gas of nitrogen and ammonia (the flow rate of ammonia gas is 10mL / min, and the flow rate of nitrogen gas is 15mL / min), and the temperature is raised to 760°C and keep for 6h to get the final sample.

[0054...

Embodiment 3

[0056] This embodiment provides a preparation method of single crystal porous square flaky tungsten nitride nanoparticles:

[0057] 1) Add 0.35g of sodium tungstate dihydrate and 0.13g of sodium oxalate into 30mL of deionized water, stir magnetically at a speed of 500r / min for 0.5h, add 1mL of a saturated aqueous solution of hydrochloric acid dropwise, continue stirring for 8min, turn to Put it into a 100mL reaction kettle and keep it in a blast drying oven at 120°C for 8h. After cooling down to room temperature, transfer to a centrifuge tube, centrifuge (centrifugation speed 10000r / min, centrifugation time 3min), wash with deionized water, repeat 5 times, and keep the sample in a blast drying oven at 70°C for 8h to dry.

[0058] 2) Place the dried sample in a tube furnace, feed a mixed gas of nitrogen and ammonia (the flow rate of ammonia gas is 10mL / min, and the flow rate of nitrogen gas is 20mL / min), and the temperature is raised to 770°C and keep for 5h to obtain the fina...

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Abstract

The invention relates to the field of synthesis of nanomaterials, in particular to a method for synthesizing single-crystal porous square sheet-shaped tungsten nitride nanoparticles. The method of the present invention comprises the following steps: 1) taking sodium tungstate dihydrate, sodium oxalate and saturated aqueous solution of hydrochloric acid as raw materials to carry out hydrothermal reaction to obtain hydrated tungsten oxide; the sodium tungstate dihydrate, oxalic acid The mass ratio of the saturated aqueous solution of sodium, water and hydrochloric acid is 0.3-0.4:0.1-0.15:25-35:1; the temperature of the hydrothermal reaction is 100-130°C; 2) the hydrated tungsten oxide obtained in step 1) is subjected to nitrogen Chemical treatment to obtain single crystal porous square plate-shaped tungsten nitride nanoparticles. The invention adopts a hydrothermal method to prepare single-crystal porous tungsten nitride, which is easy to operate, and the prepared single-crystal porous square sheet-shaped tungsten nitride has regular and controllable morphology, and has good repeatability and stability.

Description

technical field [0001] The invention relates to the field of synthesis of nanomaterials, in particular to a synthesis method and application of single crystal porous square plate-shaped tungsten nitride nanoparticles. Background technique [0002] As an important analytical technique, surface-enhanced Raman spectroscopy not only has the characteristics of high sensitivity, but also has the advantages of short detection time and convenient on-site detection. Process monitoring and other fields have very broad application prospects, and are one of the frontier hotspots in international research. Although surface-enhanced Raman spectroscopy has developed rapidly in recent years, there are still some problems affecting its large-scale practical detection applications. First of all, the most common Raman-enhanced substrates are based on nanomaterials such as precious metals such as gold and silver. Due to the high price and complicated preparation of the gold substrate, there i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/38C30B7/10C30B29/64G01N21/65B82Y40/00
CPCC30B29/38C30B7/10C30B29/64G01N21/658B82Y40/00
Inventor 席广成李俊芳刘大民李亚辉
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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