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Preparation method for scale-controllable silicon nitride nano wire short-wavelength light emitting material

A silicon nitride nanometer and short-wavelength technology, applied in chemical instruments and methods, nitrogen compounds, nanotechnology, etc., can solve the problems of inapplicability to industrial production, difficulty in precise control of the scale, and low yield of nanowires, etc., and achieve uniform scale The effect of controllability, convenient operation and simple process

Inactive Publication Date: 2012-01-25
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the silicon nitride nanowires prepared by the above methods have the following deficiencies or defects: (1) The diameter of the silicon nitride nanowires prepared by the direct silicon powder nitridation method and the silicon oxide carbothermal reduction method is large, and the scale is difficult to be accurate control; (2) organic precursor pyrolysis method, self-propagating high-temperature synthesis method and other methods have oxidation phenomenon during the synthesis process, the yield of nanowires is low, the purity is low, and there are many lattice defects; (3) microwave plasma heating Although high-yield and high-purity silicon nitride nanowires can be produced by the laser ablation method, the cost is high and the process is complicated, which cannot be applied to industrial production.

Method used

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  • Preparation method for scale-controllable silicon nitride nano wire short-wavelength light emitting material
  • Preparation method for scale-controllable silicon nitride nano wire short-wavelength light emitting material
  • Preparation method for scale-controllable silicon nitride nano wire short-wavelength light emitting material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Put nano silicon powder (with a grain size of 35nm) into a stainless steel heat preservation tank and immerse it in liquid nitrogen to keep the liquid level stable. The pretreatment time is 12 hours; transfer the heat preservation tank to a vacuum glove box and place it for 12 hours. Collect the prepared nano silicon powder. Put the prepared nano silicon powder in the corundum ark, put it into a vertical high temperature tube furnace, and pass a mixed gas of nitrogen and ammonia as the nitriding gas. The volume ratio of nitrogen and ammonia is 10:0, and the atmosphere The flow rate is 500 ml / min, the temperature is increased to 1300°C at a temperature increase rate of 10°C / min, the temperature is kept for 6 hours, and then cooled to room temperature. The silicon nitride nanowires are collected. The diameter of the silicon nitride nanowires is 40nm and the length is 20μm.

[0034] by figure 1 It can be seen that, in this embodiment, after the nano silicon powder is pretrea...

Embodiment 2

[0037] Put nano silicon powder (grain size of 30nm) into a stainless steel heat preservation tank and immerse it in liquid nitrogen to keep the liquid level stable. The pretreatment time is 60 hours; transfer the heat preservation tank to a vacuum glove box and place it for 18 hours. Collect the prepared nano silicon powder. Place the prepared nano silicon powder in a corundum ark, put it into a vertical high-temperature tube furnace, and pass a mixed gas of nitrogen and ammonia as the nitriding gas. The volume ratio of nitrogen to ammonia is 5:5. The flow rate is 200 ml / min, the temperature is increased to 1400°C at a heating rate of 8°C / min, the temperature is kept for 4 hours, and then cooled to room temperature. The silicon nitride nanowires are collected. The diameter of the silicon nitride nanowires is 33nm and the length is 15μm.

[0038] by figure 2 It can be seen that the main phase of the final product obtained in this example is α-Si 3 N 4 .

Embodiment 3

[0040] Put nano silicon powder (grain size of 20nm) into a stainless steel heat preservation tank and immerse it in liquid nitrogen to keep the liquid level stable. The pretreatment time is 80 hours; transfer the heat preservation tank to a vacuum glove box and place it for 24 hours. Collect the prepared nano silicon powder. Put the prepared nano silicon powder in the corundum ark, put it into a vertical high-temperature tube furnace, and pass a mixed gas of nitrogen and ammonia as the nitriding gas. The volume ratio of nitrogen to ammonia is 4:6. The flow rate is 500 ml / min, the temperature is increased to 1300°C at a heating rate of 5°C / min, the temperature is kept for 10 hours, and then cooled to room temperature. The silicon nitride nanowires are collected. The diameter of the silicon nitride nanowires is 25nm and the length is 45μm.

[0041] by image 3 It can be seen that the final product obtained in this embodiment is a silicon nitride nanowire.

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Abstract

The invention relates to a preparation method for a silicon nitride nano wire short-wavelength light emitting material with high purity and even and controllable scale, which comprises the steps of: using market nano silicon powder with the purity being 99.999 percent and the grain size being 10-100nm as a raw material and treating the nano silicon powder in liquid nitrogen for 1-100 hours to obtain nano silicon powder with nitrogen-passivated surfaces; and conducting subsequent nitriding treatment to obtain single-phase high-purity silicon nitride nano wires with the diameter being 10-160nm and the length being 5-80mum, wherein the nitriding temperature is controlled to be 1000 DEG C to 1500 DEG C, the nitriding gas is mixed gas of nitrogen and ammonia, the gas flow rate is controlled to be 100-1000ml / min, and heat preservation for nitriding is conducted for 1-24 hours. The preparation method has the advantages that the process is simple, the cost is low, the repeatability is good, the prepared silicon nitride nano wires have excellent performances of high purity, single phase, even and controllable scale, short-wavelength light emission and the like, and the preparation method can be widely used in the field of photo-electronic information and nano techniques.

Description

Technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing a scale-controllable silicon nitride nanowire short-wavelength luminescent material. The prepared scale-controllable silicon nitride nanowire short-wavelength luminescent material can be applied to The fields of optoelectronic information and nanotechnology. Background technique [0002] In recent years, my country’s optoelectronic information technology industry has developed rapidly, and has played an extremely important role in the modernization of the national economy and national defense. It has placed more stringent and urgent requirements on semiconductor laser materials, the key materials for optical storage and optical communications. Nitride nanowire semiconductor materials, such as silicon nitride, gallium nitride, and aluminum nitride nanowires are the third generation semiconductor materials after silicon and gallium arsenide, and a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B82Y40/00C01B21/068
Inventor 陈斐王志浩沈强王传彬张联盟
Owner WUHAN UNIV OF TECH
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