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Aminothiourea-assisted low-temperature synthesis method of silicon nitride micron rod-like crystal material

A thiosemicarbazide and crystal material technology, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve the problems of poor crystal size, low material purity, difficult to repeat the reaction process, etc. The experimental device is simple and the effect of huge social and economic benefits

Inactive Publication Date: 2011-10-26
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are problems such as low material purity, poor crystallization, small crystal size generally in the nanometer range, and difficult repetition of the reaction process.

Method used

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  • Aminothiourea-assisted low-temperature synthesis method of silicon nitride micron rod-like crystal material
  • Aminothiourea-assisted low-temperature synthesis method of silicon nitride micron rod-like crystal material
  • Aminothiourea-assisted low-temperature synthesis method of silicon nitride micron rod-like crystal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 3g of thiosemicarbazide, 0.8g of silicon powder and 3g of sodium azide into a high-pressure stainless steel reactor with a volume of 30ml, and stir evenly with a glass rod; seal the reactor and place it in an oven, heat it to 250°C, and keep After continuing to heat at this temperature for 15 hours, cool naturally to room temperature, collect the product after the reaction, which is a solid powder; use dehydrated alcohol, deionized water, HNO 3 Wash with HF (v / v=3:1) mixed solution and distilled water; finally dehydrate the product with absolute ethanol, and dry it in an oven at 60°C for 2 hours. XRD, FITR, SEM and TEM tests were carried out on the prepared samples, and the results showed that the product was micron rod-shaped silicon nitride crystals.

[0037] figure 2 For the XRD collection of patterns of synthetic silicon nitride microrod crystals of embodiment 1, by figure 2 It can be seen that the obtained product is α, β mixed phase silicon nitride. No di...

Embodiment 2

[0039]The process flow of this embodiment is the same as that of Embodiment 1, the difference is that in this embodiment, the heating temperature of the reactor sealed in the oven is 180° C., and the temperature is maintained for 8 hours. The sample prepared in this embodiment can achieve the same technical effect as in Example 1.

[0040] Figure 6 The SEM morphology of silicon nitride microrod crystals synthesized in Example 2. Depend on Figure 6 It can be clearly seen that the diameter of the sample is about 0.5 μm to 1.5 μm, and its end surface presents a regular regular hexagonal cone. The surface is regular but not very smooth, the thickness is relatively uniform, and the crystal development is relatively mature.

Embodiment 3

[0042] The process flow of this embodiment is the same as that of Embodiment 1, the difference is that the heating temperature in the oven after sealing the reaction kettle is 200° C., and the temperature is kept to continue heating for 12 hours. The sample prepared in this embodiment can achieve the same technical effect as in Example 1.

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Abstract

The invention discloses an aminothiourea-assisted low-temperature synthesis method of a silicon nitride micron rod-like crystal material, which comprises the following steps of: adding aminothiourea, silicon powder and sodium azide at a weight ratio of 3:0.8:3 to a high-pressure reaction kettle and uniformly stirring with a glass stirring rod; sealing the reaction kettle, placing in an oven, heating to 180-250 DEG C, maintaining the temperature and continuing heating for 8-15 hours, then cooling to room temperature and collecting the reaction product; washing the collected product with absolute ethanol, deionized water, HNO3 and HF mixed liquid and distilled water in a proper order and dewatering the product with absolute ethanol; and drying in an oven at 60 DEG C for 2 hours to obtain the silicon nitride micron rod-like crystal. According to the invention, the prepared silicon nitride rod-like crystal has maximal diameter of 2.5 mu m, high purity and good quality, experimental equipment is simple and is easy to operate, and the synthesis method provided by the invention has low requirement on the control of growth parameters and is easy to realize industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of semiconductor material preparation, in particular to the technical field of wide bandgap semiconductor material synthesis, and specifically relates to a method for thiosemicarbazide-assisted low-temperature synthesis of silicon nitride micro-rod crystal material. Background technique [0002] Silicon nitride (Si 3 N 4 ) is an important wide bandgap semiconductor material with a bandgap width of 5.0eV at room temperature. Its unique structure and properties have attracted more and more attention. At the same time, silicon nitride is an engineering ceramic and a new type of functional material with excellent performance. It has unique mechanical, chemical, electrical, thermal and other properties, and has been widely used in many fields. It has many advantages: the linear expansion coefficient of sintered silicon nitride is relatively low; it has excellent abrasion resistance; it has high mechanical stren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/068
Inventor 赵武张志勇冯鹏飞岳刚闫军锋贠江妮
Owner NORTHWEST UNIV