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Method for synthesizing silicon nitride nano material under low temperature by solvent hot reaction

A technology of solvothermal reaction and nanomaterials, applied in the direction of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of high reaction temperature and inability to obtain crystalline Si

Inactive Publication Date: 2008-03-05
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Aiming at the deficiencies of the prior art, the present invention proposes a method for preparing silicon nitride nanomaterials at a relatively low temperature (200-300° C.) by using solvothermal reaction, so as to overcome the high reaction temperature and the inability of low temperature in the prior art. Obtain crystalline Si 3 N 4 Drawbacks of Nanomaterials

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  • Method for synthesizing silicon nitride nano material under low temperature by solvent hot reaction
  • Method for synthesizing silicon nitride nano material under low temperature by solvent hot reaction
  • Method for synthesizing silicon nitride nano material under low temperature by solvent hot reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Prepare β-Si by reacting sodium azide, magnesium powder and silicon tetrachloride 3 N 4 Nanorod-based silicon nitride powder

[0024] Take 1g of sodium azide, 0.5g of magnesium powder and 10mL of silicon tetrachloride, put them into a special stainless steel 18mL reaction kettle, use nitrogen to remove the air in the kettle, seal it and place it in a resistance crucible boiler, and make three groups at 200°C ±5°C, 250°C±5°C, 300°C±5°C for 10 hours; after stopping heating, cool the reactor to room temperature naturally; Separation and drying, that is obtained as β-Si 3 N 4 Nanorod-based silicon nitride powder products. Vacuum-dried at 50°C for 6 hours to obtain an off-white powder product.

[0025] Cu Kα rays (wavelength The scanning step speed is 0.08° / sec) as the diffraction light source for X-ray diffraction analysis of the product.

[0026] Fig. 1 is the X-ray diffraction spectrum of the product prepared by reacting sodium azide, magnesium powder a...

Embodiment 2

[0027] Example 2: Preparation of α-Si by reacting sodium azide, iron powder and silicon tetrachloride 3 N 4 Nanowire based silicon nitride powder

[0028] SiCl was added in a molar ratio of 5.8:1:0.58 4 , NaN 3 Mixed with iron powder, sealed in an autoclave, and reacted at 250 ° C for 10 hours; the product was pickled, washed with water, centrifuged and dried to obtain α-Si 3 N 4 Nanowire-based silicon nitride powder. The results are shown in Figure 2.

[0029] Figure 2 shows the α-Si prepared by using metal iron powder as reducing agent at 250°C 3 N 4 X-ray diffraction spectrum (XRD) of the nanowire-dominated silicon nitride product. It can be seen from the figure that the sample is α-Si 3 N 4 and β-Si 3 N 4 mixed phase.

Embodiment 3

[0030] Example 3: Comparison of the effects of various metal additives on the experiment (as shown in Figure 9)

[0031] It is found that only metal magnesium powder, calcium particles and aluminum powder can generate β-Si at low temperature 3 N 4 It has a promoting effect, especially magnesium powder has the best effect; metal iron powder, sodium and nickel powder have the effect of producing α-Si at low temperature. 3 N 4 There is a promoting effect.

[0032] The morphology and particle size of the product were observed using H700 transmission electron microscope (TEM) and JSM-6700F scanning electron microscope (SEM):

[0033] It can be seen from Fig. 3, the SEM photo of the product, that the nanowire micrographs with different contrasts show that the nanorods are uniform in thickness and 100-800 nm in diameter. Figure 4 is the Si prepared in Mode 2 3 N 4 SEM photo of nanowires, with diameters of 30-125 nanometers and lengths of tens of micrometers. FIG. 5 is a TEM ph...

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Abstract

The present invention is low temperature thermal reaction process in solvent to synthesize nanometer silicon nitride material. The process includes the following steps: mixing SiCl4, NaN3 and Mg powder in the molar ratio of 2.8-5.8 to 1 to 0.8-2.7, or mixing SiCl4, NaN3 and Fe powder in the molar ratio of 5.8-6.0 to 1 to 0.58-0.60; reacting in a sealed autoclave at 200-300 deg.c for 10 hr; acid washing and water washing the product, centrifugally separating and drying to obtain 1D nanometer silicon nitride material. The process can produce nanometer beta-Si3N4 rod of 100-800 nm diameter, nanometer beta-Si3N4 line of 30-125 nm diameter, and nanometer alpha-Si3N4 line of 50-165 nm diameter. The process has low reaction temperature and good product form, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of silicon nitride nanomaterial preparation, in particular to a low-temperature synthesis of Si by solvothermal reaction. 3 N 4 methods for nanomaterials. Background technique [0002] Netherlands "Materials Science" (JOURNAL OF MATERIALS SCIENCE 33(24): 5803-5810 DEC 1998) reported elongated β-Si 3 N 4 The particles have the property of inhibiting the brittleness of ceramics, and are a kind of reinforcing and toughening agent for ceramic materials with excellent performance. JOURNAL OF THE AMERICAN CERAMIC SOCIETY 81 (10): 2661-26691998 reported that polycrystalline silicon nitride was used as raw material to add 2-3% aluminum powder and 6-10% yttrium oxide in a nitrogen atmosphere Prepare β-Si by heating to 1900°C 3 N 4 whiskers. British "Materials Research Bulletin" (MATERIALS RESEARCH BULLETIN 37 (8): 1481-1485 JULY 2002) reported that silicon powder, α-Si 3 N 4 as raw material, Y 2 O 3 Prepar...

Claims

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Application Information

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IPC IPC(8): C01B31/36B82B3/00
Inventor 钱逸泰郭春丽邢政徐立强
Owner SHANDONG UNIV
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