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Method for preparing graphene oxide wrapped silicon nitride composite powder

A technology of composite powder and graphene, which is applied in the field of graphene toughened and reinforced ceramic composite materials, can solve the problems of difficult batch production, complicated process, high equipment requirements, etc., and achieve the advantages of convenient industrial production, simple operation and less time-consuming Effect

Inactive Publication Date: 2018-01-12
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing methods commonly used for surface oxidation are concentrated sulfuric acid, nitric acid, acidic potassium permanganate solution, and hypochlorous acid solution as oxidants. Although they are efficient, they have low controllability and cause pollution to the environment. It is not easy to produce in batches, and the equipment requires high technology. more complicated process
At present, the reported modification method adopts toluene as a solvent, nitrogen is a protective gas, and carries out a liquid phase reaction (see CN105884377A); although the effect is improved like this, there are problems such as cost and environmental protection in industrialized production
It is also reported that using ethanol as a solvent and using a ball milling process to use a silane coupling agent to graft and modify nanoparticle powders, this method is more complicated and inefficient.
So far, no graphene oxide-coated Si 3 N 4 particle reports

Method used

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  • Method for preparing graphene oxide wrapped silicon nitride composite powder
  • Method for preparing graphene oxide wrapped silicon nitride composite powder
  • Method for preparing graphene oxide wrapped silicon nitride composite powder

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Graphene oxide coated silicon nitride (Si 3 N 4 @GO) preparation method of composite powder, the steps are as follows:

[0044] (1) Weigh the raw material Si with an average particle size of 100nm 3 N 4 Add 200 mL of 15% hydrogen peroxide solution to 2 g of powder, stir magnetically, raise the temperature to 70° C., and react for 15 min. Cool to room temperature, centrifuge, wash with distilled water 2 to 3 times, place in a drying oven at 200°C for 6 hours at high temperature, and obtain surface oxidized Si 3 N 4 Powder.

[0045] (2) Prepare 3-aminopropyltrimethoxysilane (KH540) silane coupling agent solution: the amount of silane coupling agent is 0.05g, dropwise into 50mL absolute ethanol:distilled water=1:1 volume ratio solution, Ultrasonic hydrolysis for 30min for later use.

[0046] (3) get the surface oxidized Si prepared by step (1) 3 N 4 2g of powder, placed in 200mL of absolute ethanol: distilled water = 1:1 volume ratio solution and ultrasonically st...

Embodiment 2

[0051] Graphene oxide coated silicon nitride (Si 3 N 4 @GO) preparation method of composite powder, the steps are as follows:

[0052] (1) Weigh the raw material Si with an average particle size of 200nm 3 N 4 Add 200 mL of 20% hydrogen peroxide solution to 2 g of powder, stir magnetically, raise the temperature to 80° C., and react for 20 min. Cool to room temperature, centrifuge, wash with distilled water 2 to 3 times, place in a drying oven at 220°C for 8 hours at high temperature, and obtain surface oxidized Si 3 N 4 Powder.

[0053] (2) Prepare 3-aminopropyltriethoxysilane (KH-550) silane coupling agent solution, the amount of silane coupling agent is 0.1g, drop into 80mL absolute ethanol:distilled water=1:1 volume ratio solution, ultrasonically hydrolyzed for 40 min for later use.

[0054] (3) get the surface oxidized Si prepared by step (1) 3 N 4 2g of powder, placed in 200mL of absolute ethanol: distilled water = 1:1 volume ratio of the solution ultrasonically s...

Embodiment 3

[0059] Graphene oxide coated silicon nitride (Si 3 N 4 @GO) preparation method of composite powder, the steps are as follows:

[0060] (1) Weigh the raw material Si with an average particle size of 200nm 3 N 4 Add 200mL of 30% hydrogen peroxide solution to 2g of powder, stir magnetically, raise the temperature to 90°C, and react for 30min. Cool to room temperature, centrifuge, wash with distilled water 2 to 3 times, and place in a drying oven at 250°C for 10 hours to obtain surface oxidized Si 3 N 4 Powder.

[0061] (2) Prepare N-2 (aminoethyl) 3-aminopropyltriethoxysilane (KH910) silane coupling agent solution, the amount of silane coupling agent is 0.2g, drop into 100mL absolute ethanol: distilled water = In a solution with a volume ratio of 1:1, ultrasonically hydrolyze for 50 minutes for later use.

[0062] (3) get the surface oxidized Si prepared by step (1) 3 N 4 Powder 2g, placed in 300mL of absolute ethanol: distilled water = 1:1 volume ratio of the solution u...

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Abstract

The invention relates to a method for preparing graphene oxide wrapped silicon nitride composite powder. The method comprises the following steps: performing high-temperature surface oxidation on Si3N4 powder in hydrogen peroxide, putting a coupling agent hydrolysis solution into a surface oxidized Si3N4 suspension, and performing grafting modification treatment on the surface of Si3N4; and preparing a graphene oxide water dispersion, putting the Si3N4 suspension into the graphene oxide water dispersion, performing ultrasonic treatment, leaving to stand till wrapped particles completely settledown, removing supernate, and drying, thereby obtaining the graphene oxide wrapped silicon nitride composite powder. The graphene oxide wrapped silicon nitride composite powder prepared by using themethod is good in wrapping completeness, simple and convenient in process and high in efficiency. Application spaces of silicon nitride and graphene oxide are expanded, and after the graphene oxide wrapped silicon nitride composite powder is applied to a ceramic material, the mechanical properties of the ceramic material can be remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of graphene toughened and reinforced ceramic composite materials, and in particular relates to a preparation method of graphene oxide-coated silicon nitride composite powder. Background technique [0002] At present, graphene toughened and reinforced ceramic nanocomposites have achieved effects that cannot be achieved by traditional reinforcement phase materials, see CN106007680A. However, graphene is a new two-dimensional honeycomb carbonaceous material, and its unique structure makes its sheets have strong attraction. Therefore, the dispersion of graphene in the ceramic matrix is ​​the key to the preparation of high-performance ceramic matrix composites. Traditional physical dispersion methods such as mechanical methods and ultrasonic dispersion methods cannot fundamentally eliminate the attraction between the sheets. The chemical dispersion method is complicated in process and introduces some impurities...

Claims

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Application Information

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IPC IPC(8): C04B35/78C04B35/63
Inventor 许崇海张文亮陈照强衣明东肖光春
Owner QILU UNIV OF TECH
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