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

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

Inactive Publication Date: 2009-11-18
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

Method used

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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
Comparison scheme
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; open the reactor and remove unreacted SiCl 4 , the resulting product was washed with acid and water, centrifuged and dried to obtain 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] figure 1 It is the...

Embodiment 2

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

[0028] The SiCl 4 , NaN 3 Mix with iron powder, seal in an autoclave, and react at 250°C for 10 hours; the product is pickled, washed with water, centrifuged and dried to obtain α-Si 3 N 4 Nanowire-based silicon nitride powder. see results figure 2 .

[0029] figure 2 α-Si prepared at 250°C with metal iron powder as reducing agent 3 N 4 X-ray diffraction spectrum (XRD) of the nanowire-based 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] Embodiment 3: compare the impact of various metal additives on experiment (as Figure 9 shown)

[0031] It was found that only metal magnesium powder, calcium particles and aluminum powder are effective for the formation of β-Si at low temperature 3 N 4 It has a promoting effect, among which magnesium powder has the best effect; metal iron powder, sodium and nickel powder can form α-Si at low temperature 3 N 4 There is a promotional effect.

[0032] Use H700 type transmission electron microscope (TEM) and JSM-6700F type scanning electron microscope (SEM) to observe the morphology and particle size of product:

[0033] From the SEM photo of the product image 3 It can be seen that the micrographs of nanowires with different contrasts show that the nanorods are uniform in thickness and have a diameter of 100-800 nm. Figure 4 is the Si prepared by way 2 3 N 4 SEM photos of nanowires, with a diameter of 30-125 nanometers and a length of tens of microns. Figure 5 ...

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Abstract

The invention discloses a method for synthesizing silicon nitride nanometer material at low temperature by using solvothermal reaction, which is to mix SiCl4, NaN3 and magnesium powder according to the molar ratio of 2.8-5.8:1:0.8-2.7, or use iron powder as the reducing agent. The agent is mixed with SiCl4, NaN3 and iron powder in a molar ratio of 5.8-6.0:1:0.58-0.60, sealed in an autoclave, and reacted at 200°C-300°C for 10 hours ± 0.5 hours; the product is pickled, washed, Centrifugal separation and drying to obtain silicon nitride one-dimensional nanomaterials. The diameter of the β-Si3N4 nanorods prepared by the method of the invention is about 100 nanometers to 800 nanometers, the diameter of the nanowires is 30 nanometers to 125 nanometers; the diameter of the α-Si3N4 nanometer wires is 50 nanometers to 165 nanometers. The reaction temperature of the method of the invention is low, the obtained product has good appearance, and is suitable for large-scale 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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Patent Type & Authority Patents(China)
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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