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Method for synthesizing carbide nano powder by solid-phase reaction

A technology of nano-powder and carbide, applied in the direction of carbide, tungsten/molybdenum carbide, etc., can solve the problems of gas pollution, etc., and achieve the effect of mild reaction pressure, lower reaction temperature and mild reaction temperature

Inactive Publication Date: 2010-11-24
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, attention should be paid to the synthesis of sulfur-sodium system, the H produced by acid treatment 2 Pollution caused by S gas

Method used

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  • Method for synthesizing carbide nano powder by solid-phase reaction
  • Method for synthesizing carbide nano powder by solid-phase reaction
  • Method for synthesizing carbide nano powder by solid-phase reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Silicon powder 1.4g, glucose 1.4g, Mg powder 1.5g and elemental iodine I 2 6g mixed, sealed in a 20mL stainless steel reaction kettle, reacted at a temperature of 120°C for 12 hours, after natural cooling, the resulting off-white powder was collected and washed with hydrochloric acid and deionized water respectively, and washed with a mixture of hydrofluoric acid and dilute nitric acid Excessive silicon powder, then the resulting product is washed with distilled water and absolute ethanol to neutral pH and then dried to obtain silicon carbide powder. The analytical spectrum of the product is as follows Figure 1-4 shown. figure 1 It is the XRD diffraction pattern of the obtained silicon carbide product, which corresponds to the standard card value (JCPDS no.29-1129). figure 2 It is a scanning electron microscope photo of the obtained silicon carbide nanowire, it can be seen that its diameter is about 65 nm, and its length is about several microns. image 3 It is a sc...

Embodiment 2

[0044] As described in Example 1, the difference is that 1.4 g of glucose is replaced by 1.4 g of maltose. Figure 5 is the XRD spectrum of the resulting product. 3C-SiC (JCPDS no.29-1129) can be calibrated as cubic crystal system.

Embodiment 3

[0046] Vanadium pentoxide (V 2 o 5 ) 0.43g, magnesium powder 0.551g, I 2 1.215g, glucose 0.14g mixed, sealed in a 20mL stainless steel reactor. The reaction time was 6 hours at 250°C. After washing, separating and drying, the XRD spectrum of the product obtained is as follows: Image 6 , can be calibrated as VC of the face-centered cubic system, which is in good agreement with the standard card (JCPDSno.65-8074). Figure 7 Its transmission electron micrograph shows that the obtained material is nanoscale. Figure 8 The photo of its high-resolution transmission electron microscope shows that its interplanar spacing is 0.204nm, which is in good agreement with the (002) plane of VC.

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Abstract

The invention relates to a method for synthesizing carbide nano powder by a solid-phase reaction, which comprises the following steps of: mixing a silicon source or a metal source, a carbon source, magnesium powder and elementary iodine according to a mol ratio of 1: (0.05-2): (1-25): (1.25-12), sealing the mixed material in an autoclave, and placing the autoclave in a drying box to perform a reaction for 6 to 48 hours at the temperature of between 100 and 500 DEG C; and washing, separating and drying the product to obtain the carbide nano powder. In the invention, glucose or maltose which universally exists in the natural world is used as the carbon source to avoid using a chlorine-containing carbon source such as carbon tetrachloride and tetrachloroethylene which have bad influences on an operation environment, and the reaction temperature and the reaction pressure are relatively mild, so that the method for synthesizing carbide nano powder by the solid-phase reaction has a potential for mass production.

Description

technical field [0001] The invention belongs to the field of preparation of transition metal carbides and silicon carbide nanopowders, and in particular relates to a method for synthesizing silicon carbide and transition metal carbides at low temperature by solid phase reaction. Background technique [0002] Silicon carbide and transition metal carbides generally have very high strength and toughness, and can be widely used as reinforcements for ceramics, metals, and polymer matrix composites (see Appl. Phys. Lett. 1995, 66, 3182.). 3C-SiC is a wide bandgap semiconductor (2.3eV), which has the advantages of high operating temperature (up to 600°C), low resistance, good thermal conductivity, and high p-n junction withstand voltage. It is a potential microwave absorbing material. It is also one of the important new semiconductor device materials (see J. Alloys Comp. 2009, 475, 506-509.). Carbides such as tungsten carbide and molybdenum carbide are good catalysts and can repla...

Claims

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Application Information

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IPC IPC(8): C01B31/30C01B31/36C01B31/34C01B32/949
Inventor 钱逸泰马小健王连成郭春丽
Owner SHANDONG UNIV
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