CN107935576B - Silicon nitride combined mullite-silicon carbide ceramic composite material and preparation method thereof - Google Patents

Silicon nitride combined mullite-silicon carbide ceramic composite material and preparation method thereof Download PDF

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CN107935576B
CN107935576B CN201711279314.XA CN201711279314A CN107935576B CN 107935576 B CN107935576 B CN 107935576B CN 201711279314 A CN201711279314 A CN 201711279314A CN 107935576 B CN107935576 B CN 107935576B
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mullite
silicon carbide
silicon
composite material
ceramic composite
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CN107935576A (en
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马成良
王世界
王斌
高金星
史幸福
陈凯阳
巩志伟
詹学武
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Zhengzhou University
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Abstract

The invention discloses a silicon nitride combined mullite-silicon carbide ceramic composite material and a preparation method thereof, and the technical scheme is as follows: weighing raw materials according to 50-80wt% of mullite, 5-40wt% of silicon carbide, 5-20wt% of silicon powder and 0.5-3wt% of sintering aid, uniformly mixing, adding a bonding agent and water, wherein the using amounts of the bonding agent and the water are respectively 0.5-25wt% and 6-60wt% of the total mass of the raw materials to obtain a mixture, granulating, molding, drying, placing into a nitriding sintering furnace, and preserving heat for 3-8 hours at 1300 ℃ and 1500 ℃ to obtain the silicon nitride-mullite-silicon carbide ceramic composite material. The invention has simple process and low production cost, and the product has the advantages of excellent high temperature resistance, good thermal shock resistance stability, high strength and the like.

Description

Silicon nitride combined mullite-silicon carbide ceramic composite material and preparation method thereof
Technical Field
The invention relates to the field of ceramic material preparation, in particular to a silicon nitride combined mullite-silicon carbide ceramic composite material and a preparation method thereof.
Background
Silicon carbide and silicon nitride are compounds with extremely strong covalent bonds, have similar physicochemical properties, have the advantages of high strength, high hardness, high corrosion resistance, high thermal conductivity, low expansion coefficient and the like, and are widely applied to industries such as metallurgy, building materials, electronics, machinery and the like. The mullite material has the advantages of good high-temperature mechanical property, lower thermal expansion coefficient and thermal conductivity, excellent high-temperature creep resistance, chemical stability and the like, is widely applied to the fields of refractory materials, ceramic materials, electronic packaging materials and the like, but has poor thermal shock resistance. Therefore, the silicon carbide is added into the mullite-based material, and the silicon nitride combined mullite-silicon carbide ceramic composite material is prepared through a nitridation reaction, so that the mechanical property of the mullite-based material can be obviously improved.
At present, some researches on silicon nitride combined mullite-silicon carbide ceramic composite materials have been carried out, for example, Zyong (influence of adding silicon nitride on properties of mullite-silicon carbide materials [ J ], Shandong metallurgy, 2016, 38 (6): 56-59) uses mullite and andalusite as main raw materials, and silicon nitride and silicon carbide are added to prepare the silicon nitride-mullite-silicon carbide composite materials, but the silicon nitride-mullite-silicon carbide composite materials have the advantages of complex preparation process, high production cost and poor oxidation resistance. The invention discloses a porous mullite-silicon carbide composite ceramic material and a preparation method thereof (CN 103553583A), wherein aluminum hydroxide, silica, silicon dioxide, silicon powder, carbon powder and magnesium carbonate are used as raw materials, and the porous mullite-silicon carbide composite ceramic material prepared by the method has the advantages but the defects of complex preparation process and low compressive strength. The invention relates to a Chinese patent 'silicon nitride and silicon carbide complex phase porous ceramic and a preparation method thereof' (CN 104150940A). Si, SiC and sintering aid are used as raw materials, and the silicon nitride and silicon carbide complex phase porous ceramic prepared by wet grinding, drying, sieving and molding has the advantages, but the defect is that the preparation process is complex.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a silicon nitride combined mullite-silicon carbide ceramic composite material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a silicon nitride combined mullite-silicon carbide ceramic composite material comprises a composite material, a bonding agent and water, wherein the composite material consists of the following raw materials in percentage by mass: 50-80wt% of mullite, 5-40wt% of silicon carbide, 5-20wt% of silicon powder and 0.5-3wt% of sintering aid.
The mullite, the silicon carbide and the silicon powder are all powder, the particle size of the fine powder is less than or equal to 0.1mm, and the mass ratio of the binding agent and the water in the silicon nitride combined mullite-silicon carbide ceramic composite material is as follows: 0.5-25wt% of binding agent and 6-60wt% of water.
The sintering aid is yttrium oxide, and Y in the yttrium oxide2O3The content is more than or equal to 99 percent, and the grain diameter is less than or equal to 0.074 mm.
The binding agent is one or a mixture of more of water glass, pulp waste liquid, dextrin and polyvinyl alcohol.
The preparation method of the silicon nitride combined mullite-silicon carbide ceramic composite material comprises the following steps:
step 1, weighing the components according to the formula of claim 1;
step 2, placing the weighed mullite, silicon carbide, silicon powder and sintering aid into a mixer, and mixing for 2-8 hours to obtain mixed powder;
step 3, mixing the weighed binding agent and water to form a mixed solution, adding the mixed solution into the mixed powder obtained in the step 2, and mixing the materials for 1-3 hours to obtain a mixed material;
step 4, placing the mixture obtained in the step 3 into a granulator for granulation to obtain particles with the particle size of 0.5-2 mm;
step 5, placing the particles obtained in the step 4 into a hydraulic press for molding treatment, wherein the molding pressure is 30-100MPa, and obtaining a blank body;
and 6, drying the blank obtained in the step 5 in a drying box at 70-120 ℃ for 4-24 hours, placing the dried blank in a nitriding sintering furnace, nitriding and sintering the blank at 1300-1500 ℃, keeping the temperature for 3-8 hours, and cooling the blank to room temperature along with the furnace in a nitrogen atmosphere to obtain the silicon nitride combined mullite-silicon carbide ceramic composite material.
Preferably: and the mixer in the step 2 is a planetary mixer or a drum mixer.
Preferably: the granulation mode in the step 4 is spray granulation or extrusion granulation.
Preferably: the method for introducing nitrogen in the step 6 is a flow method or a static method.
The invention has the following beneficial effects:
the silicon nitride combined mullite-silicon carbide ceramic composite material is prepared by taking mullite, silicon carbide and silicon powder as main raw materials through a nitridation reaction, has the advantages of simple production process, excellent mechanical property of a product, good thermal shock resistance stability and the like, and has wide economic and social values. The bulk density of the product is 1.70-1.89g/cm3The porosity is 35-41%, the normal temperature compressive strength is 70-100MPa, and the material can be used as kiln furniture materials of high temperature kilns and the like.
Detailed Description
The invention will be further described with reference to specific examples:
the mullite, silicon carbide and silicon powder used in the following examples are all powders, the particle size of the fine powder is less than or equal to 0.1mm, and Y in yttrium oxide2O3The content is more than or equal to 99 percent, and the grain diameter is less than or equal to 0.074 mm.
Example 1
Weighing the mixed raw materials in percentage by mass: 79.5wt% of mullite, 10wt% of silicon carbide, 10wt% of silicon powder and 0.5wt% of sintering aid, placing the weighed mixed raw materials into a drum type mixer, mixing for 4 hours, adding a mixed solution of bonding agent dextrin and water, wherein the mass percentages of the mixed raw materials are respectively 4wt% and 15wt% of the total mass of the mixed raw materials, continuing mixing for 1 hour to obtain a mixed material, placing the obtained mixed material into an extrusion type granulator for granulation, the particle size of the particles is 0.5-2mm, placing the manufactured particles into a hydraulic press for molding, the molding pressure is 50MPa to obtain a green body, drying the obtained green body for 12 hours at 120 ℃, placing the dried green body into a nitriding sintering furnace, introducing nitrogen into the furnace in a static mode, and performing nitriding sintering at 1450 ℃ for 4 hours to obtain the silicon nitride-combined mullite-silicon carbide ceramic composite material.
Through detection, the performance indexes of the silicon nitride and mullite-silicon carbide combined ceramic composite material prepared by the embodiment are as follows: bulk density 1.79g/cm3Porosity of 40.2%, and room-temperature compressive strength of 88 MPa.
Example 2
Weighing the mixed raw materials in percentage by mass: 79.5wt% of mullite, 10wt% of silicon carbide, 10wt% of silicon powder and 0.5wt% of sintering aid, placing the weighed mixed raw materials into a drum type mixer, mixing for 4 hours, adding a mixed liquid of a binding agent polyvinyl alcohol and water, wherein the mass percentages of the mixed liquid are respectively 1wt% and 50wt% of the total mass of the mixed raw materials, continuing mixing for 1 hour to obtain a mixed material, placing the obtained mixed material into a spray granulator for granulation, the particle size of the particles is 0.5-1mm, placing the prepared particles into a hydraulic press for molding, the molding pressure is 50MPa to obtain a green body, drying the obtained green body for 24 hours at 120 ℃, placing the dried green body into a nitriding sintering furnace, introducing nitrogen into the furnace in a dynamic mode, and conducting nitriding and sintering at 1450 ℃ for 4 hours to obtain the silicon nitride-combined mullite-silicon carbide ceramic composite material.
Through detection, the performance indexes of the silicon nitride and mullite-silicon carbide combined ceramic composite material prepared by the embodiment are as follows: bulk density 1.81g/cm3Porosity 38.2%, and room-temperature compressive strength 90 MPa.
Example 3
Weighing the mixed raw materials in percentage by mass: 74wt% of mullite, 15wt% of silicon carbide, 10wt% of silicon powder and 1wt% of sintering aid, placing the weighed mixed raw materials into a drum type mixer, mixing for 4 hours, adding mixed liquid of binding agent dextrin and water, the mass percentages of the mixed raw materials are respectively 4wt% and 15wt% of the total mass of the mixed raw materials, continuing mixing for 1 hour to obtain a mixture, placing the obtained mixture into an extrusion type granulator for granulation, wherein the particle size of the particles is 0.5-2mm, placing the prepared particles into a hydraulic press for molding, wherein the molding pressure is 50MPa, obtaining a green body, drying the obtained green body at 120 ℃ for 12 hours, placing the green body into a nitriding sintering furnace, introducing nitrogen in a static method, and carrying out nitriding sintering at 1440 ℃ for 4 hours to obtain the silicon nitride-combined mullite-silicon carbide ceramic composite material.
Through detection, the performance indexes of the silicon nitride and mullite-silicon carbide combined ceramic composite material prepared by the embodiment are as follows: bulk density 1.83g/cm3Porosity 35.9%, and room-temperature compressive strength 90 MPa.
Example 4
Weighing the mixed raw materials in percentage by mass: 68wt% of mullite, 20wt% of silicon carbide, 10wt% of silicon powder and 2wt% of sintering aid, placing the weighed mixed raw materials into a drum type mixer, mixing for 4 hours, adding mixed liquid of binding agent dextrin and water, the mass percentages of the mixed raw materials are respectively 4wt% and 15wt% of the total mass of the mixed raw materials, continuing mixing for 1 hour to obtain a mixture, placing the obtained mixture into an extrusion type granulator for granulation, wherein the particle size of the particles is 0.5-2mm, placing the prepared particles into a hydraulic press for molding, wherein the molding pressure is 50MPa, obtaining a green body, drying the obtained green body for 24 hours at 120 ℃, placing the green body into a nitriding sintering furnace, introducing nitrogen in a dynamic method, and carrying out nitriding sintering at 1420 ℃ for 4 hours to obtain the silicon nitride-combined mullite-silicon carbide ceramic composite material.
Through detection, the performance indexes of the silicon nitride and mullite-silicon carbide combined ceramic composite material prepared by the embodiment are as follows: bulk density 1.84g/cm3Porosity 35.1%, and room-temperature compressive strength 94 MP.
Example 5
Weighing the mixed raw materials in percentage by mass: 57wt% of mullite, 25wt% of silicon carbide, 15wt% of silicon powder and 3wt% of sintering aid, placing the weighed mixed raw materials into a drum type mixer, mixing for 4 hours, adding a mixed solution of binding agent dextrin and water, wherein the mass percentages of the mixed raw materials are respectively 4wt% and 50wt% of the total mass of the mixed raw materials, continuing mixing for 1 hour to obtain a mixed material, placing the obtained mixed material into a spray granulator for granulation, the particle size of the particles is 0.5-1mm, placing the prepared particles into a hydraulic press for molding, the molding pressure is 50MPa to obtain a green body, drying the obtained green body for 24 hours at 120 ℃, placing the green body into a nitriding sintering furnace, introducing nitrogen into the furnace in a dynamic mode, and carrying out nitriding sintering at 1420 ℃ for 4 hours to obtain the silicon nitride-combined mullite-silicon carbide ceramic composite material.
Through detection, the performance indexes of the silicon nitride and mullite-silicon carbide combined ceramic composite material prepared by the embodiment are as follows: bulk density 1.85g/cm3Porosity of 34.8%, and room-temperature compressive strength of 94 MP.

Claims (3)

1. A silicon nitride combined mullite-silicon carbide ceramic composite material is characterized in that: the silicon nitride combined mullite-silicon carbide ceramic composite material comprises a composite material, a bonding agent and water, wherein the composite material is prepared from the following raw materials in percentage by mass: 50-80wt% of mullite, 5-40wt% of silicon carbide, 5-20wt% of silicon powder and 0.5-3wt% of sintering aid;
the mullite, the silicon carbide and the silicon powder are all powder, the particle size of the fine powder is less than or equal to 0.1mm, and the mass ratio of the binding agent and the water in the silicon nitride combined mullite-silicon carbide ceramic composite material is as follows: 0.5-25wt% of binding agent and 6-60wt% of water;
the sintering aid is yttrium oxide, and Y in the yttrium oxide2O3The content is more than or equal to 99 percent, and the grain diameter is less than or equal to 0.074 mm;
the binding agent is one or a mixture of more of water glass, pulp waste liquid, dextrin and polyvinyl alcohol;
the preparation method comprises the following steps:
step 1, weighing the components according to the formula of claim 1;
step 2, placing the weighed mullite, silicon carbide, silicon powder and sintering aid into a mixer, and mixing for 2-8 hours to obtain mixed powder;
step 3, mixing the weighed binding agent and water to form a mixed solution, adding the mixed solution into the mixed powder obtained in the step 2, and mixing the materials for 1-3 hours to obtain a mixed material;
step 4, placing the mixture obtained in the step 3 into a granulator for granulation to obtain particles with the particle size of 0.5-2 mm;
step 5, placing the particles obtained in the step 4 into a hydraulic press for molding treatment, wherein the molding pressure is 30-100MPa, and obtaining a blank body;
step 6, placing the blank obtained in the step 5 in a drying oven at 70-120 ℃ for drying for 4-24 hours, placing the dried blank in a nitriding sintering furnace, carrying out nitriding reaction sintering at 1300-1500 ℃, keeping the temperature for 3-8 hours, and cooling the blank to room temperature along with the furnace in a nitrogen atmosphere to obtain the silicon nitride combined mullite-silicon carbide ceramic composite material;
the granulation mode in the step 4 is spray granulation or extrusion granulation.
2. A silicon nitride bonded mullite-silicon carbide ceramic composite as claimed in claim 1 wherein: and the mixer in the step 2 is a planetary mixer or a drum mixer.
3. A silicon nitride bonded mullite-silicon carbide ceramic composite as claimed in claim 1 wherein: the method for introducing nitrogen in the step 6 is a flow method or a static method.
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CN108675780B (en) * 2018-06-11 2021-08-24 郑州大学 Metal composite mullite-silicon carbide ceramic composite material and preparation method thereof
CN113998986B (en) * 2021-11-01 2022-08-26 中冶武汉冶金建筑研究院有限公司 High-strength wear-resistant low-porosity clay brick based on waste mullite silicon carbide brick and preparation method thereof
CN115594492A (en) * 2022-09-27 2023-01-13 郑州荣盛窑炉耐火材料有限公司（Cn） Semi-light carbon-nitrogen composite refractory brick for rotary kiln of garbage incinerator and preparation method thereof

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