CN107512921B - Preparation method of carbon fiber powder reinforced silicon nitride-based composite material - Google Patents

Preparation method of carbon fiber powder reinforced silicon nitride-based composite material Download PDF

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CN107512921B
CN107512921B CN201710762676.8A CN201710762676A CN107512921B CN 107512921 B CN107512921 B CN 107512921B CN 201710762676 A CN201710762676 A CN 201710762676A CN 107512921 B CN107512921 B CN 107512921B
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powder
carbon fiber
silicon nitride
composite material
based composite
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CN107512921A (en
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孙卫康
董会娜
张东生
姚栋嘉
牛利伟
吴恒
刘喜宗
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Gongyi Van Research Yihui Composite Material Co Ltd
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63472—Condensation polymers of aldehydes or ketones
    • C04B35/63476—Phenol-formaldehyde condensation polymers
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention belongs to the field of preparation of silicon nitride-based composite materials, and discloses a preparation method of a carbon fiber powder reinforced silicon nitride-based composite material. Dispersing liquid phenolic resin in absolute ethyl alcohol; mixing Si3N4Adding the powder into the obtained solution, and uniformly stirring at 40-60 ℃; adding carbon fiber powder into the obtained solution, and continuously stirring at 60-80 ℃ until the slurry is viscous and cannot be stirred; drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank; and coating the blank with the mixed powder of the silicon powder and the titanium powder, placing the blank in a graphite crucible, and reacting for 1-3 hours at the temperature of 1550-1650 ℃ in vacuum to obtain the carbon fiber reinforced silicon nitride-based composite material. The invention has the advantages of simple process, convenient operation, C/Si3N4Has the advantages of both carbon fiber and silicon nitride, and overcomes Si3N4The brittleness is higher and the like.

Description

Preparation method of carbon fiber powder reinforced silicon nitride-based composite material
Technical Field
The invention belongs to the field of preparation of silicon nitride-based composite materials, and particularly relates to a preparation method of a carbon fiber powder reinforced silicon nitride-based composite material.
Background
The carbon fiber has a series of excellent performances such as low density, high specific strength, high specific modulus, high temperature resistance and the like, and one of important applications of the carbon fiber is used as a reinforcement of a composite material for bearing load. Silicon nitride has the advantages of high strength, high temperature resistance, oxidation resistance, corrosion resistance, thermal shock resistance, low thermal expansion coefficient and the like, is widely applied to thermal structural materials, is also widely applied to substrates of wave-transmitting materials and high-temperature-resistant wave-absorbing materials due to low dielectric constant and low electromagnetic loss, still has the common defect of large brittleness of ceramic materials, namely the weakness of the brittleness, and ensures that the reliability in application cannot be guaranteed, so the toughness is improved, and the reliability is improved all the time, which is an important research on silicon nitride ceramicsAnd (4) direction. At present, Si3N4The ceramic toughening approaches mainly comprise particle toughening, fiber or whisker toughening and ZrO2Phase change toughened, columnar b-Si3N4And the self-toughening of the crystal grains is five types, wherein the bridging fiber which is based on a bridging toughening mechanism in fiber or whisker toughening generates a force for closing cracks on a matrix, and the toughness of the material is improved by consuming the work done by external load. The visible crystal whisker or fiber can greatly improve Si3N4But its practical application is limited due to the complicated dispersion process of whiskers or fibers, difficulty in sintering densification and compatibility with the matrix.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon fiber powder reinforced silicon nitride-based composite material, which has the advantages of simple process, convenient operation and the like, and C/Si3N4Meanwhile, the composite material has the advantages of carbon fiber and silicon nitride, the toughness of the composite material is further improved, and the bending strength is correspondingly improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a carbon fiber powder reinforced silicon nitride-based composite material comprises the following steps:
(1) dispersing the liquid phenolic resin in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 5-12 wt%;
(2) according to Si3N4The mass ratio of the powder to the absolute ethyl alcohol is (0.5-1.2) to 1, and Si is added3N4Adding the powder into the solution obtained in the step (1), and uniformly stirring at 40-60 ℃;
(3) carbon fiber powder and Si3N4Adding the powder into the solution obtained in the step (2) according to the mass ratio of (0.1-0.2) to 1, and continuously stirring at the temperature of 60-80 ℃ until the slurry is viscous and cannot be stirred;
(4) drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank body;
(5) and coating the blank with the silicon/titanium powder mixed powder, placing the blank in a graphite crucible, and reacting for 1-3 hours at the temperature of 1550-1650 ℃ in vacuum to obtain the carbon fiber powder reinforced silicon nitride-based composite material.
Preferably, the solid content of the liquid phenolic resin is more than or equal to 50 wt%.
Preferably, said Si is3N4The average diameter of the powder was 5 μm.
Preferably, the length of the carbon fiber powder is 30-50 μm.
Preferably, the drying temperature is 60-80 ℃.
Preferably, the powder is sieved by a sieve of 60-100 meshes.
Preferably, the pressure of the compression molding is controlled to be 150-250 MPa.
Preferably, the mass ratio of the silicon powder to the titanium powder is (1.8-2.5) to 1.
The invention provides a preparation method of a carbon fiber powder reinforced silicon nitride-based composite material, which has the advantages of simple process, convenience in operation and the like. The carbon fiber powder is used for reinforcing the silicon nitride, so that the silicon nitride has excellent performances of both carbon fiber and molybdenum disilicide, the interface bonding state of the fiber and the silicon nitride is well improved by adding the phenolic resin, the defect of high brittleness of the silicon nitride is overcome by the good toughening effect of the carbon fiber powder, and the toughness and the bending strength of the composite material are improved; meanwhile, pyrolytic carbon generated by decomposition of the phenolic resin at high temperature also prevents carbon fiber from reacting with silicon nitride in the subsequent sintering process, so that the carbon fiber reinforced silicon nitride-based composite material has wider and wider application in the aspect of thermal structural materials.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of a carbon fiber powder reinforced silicon nitride-based composite material comprises the following steps:
(1) dispersing liquid phenolic resin (solid content is 50 wt%) in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 8 wt%;
(2) according to Si3N4The mass ratio of the powder (average diameter of 5 μm) to the absolute ethyl alcohol is 1: 1, and Si is added3N4Adding the powder into the solution obtained in the step (1), heating at 50 ℃, and uniformly stirring;
(3) carbon fiber powder (45 μm in length) and Si3N4Adding carbon fiber powder into the solution obtained in the step (2) according to the mass ratio of the powder of 0.15: 1, and continuously stirring at 70 ℃ until the slurry is viscous and cannot be stirred;
(4) placing the slurry in a drying oven, and drying at 70 ℃; after granulation and 60-mesh sieve, placing the powder particles in a mould, and pressing and forming under 200 MPa to obtain a blank;
(5) coating a blank with mixed powder of silicon powder and titanium powder (the mass ratio of Si to Ti is 2.4: 1), placing the blank in a graphite crucible, keeping the temperature for 2 hours at 1600 ℃ in vacuum to increase densification, and naturally cooling to obtain the carbon fiber powder reinforced silicon nitride based composite material (C/Si for short)3N4Composite materials).
C/Si obtained in this example3N4The composite material has a flexural strength of 420 MPa and a fracture toughness of 4.1 MPa-m1/2。
Example 2
A preparation method of a carbon fiber powder reinforced silicon nitride-based composite material comprises the following steps:
(1) dispersing liquid phenolic resin (solid content is 50 wt%) in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 6 wt%;
(2) according to Si3N4The mass ratio of the powder (average diameter of 5 μm) to the absolute ethyl alcohol is 0.5: 1, and Si is added3N4Adding the powder into the solution obtained in the step (1), and heating and stirring the solution uniformly at 40 ℃;
(3) carbon fiber powder (length of 30 μm) and Si3N4Adding carbon fiber powder into the solution obtained in the step (2) according to the mass ratio of the powder of 0.1: 1, and continuously stirring at 60 ℃ until the slurry is viscous and cannot be stirred;
(4) placing the slurry in a drying box, and drying at 60 ℃; after granulation and 80-mesh sieve sieving, placing the powder particles in a mould, and pressing under 250MPa to form a blank;
(5) coating the blank with mixed powder of silicon powder and titanium powder (the mass ratio of Si to Ti is 2: 1), placing the blank in a graphite crucible, preserving heat for 1 h at the temperature of 1650 ℃ in vacuum to increase densification, and naturally cooling to obtain the carbon fiber powder reinforced silicon nitride-based composite material.
C/Si obtained in this example3N4The composite material has a bending strength of 500 MPa and a fracture toughness of 3.6 MPa-m1/2。
Example 3
A preparation method of a carbon fiber powder reinforced silicon nitride-based composite material comprises the following steps:
(1) dispersing liquid phenolic resin (solid content is 50 wt%) in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 10 wt%;
(2) according to Si3N4The mass ratio of the powder (average diameter of 5 μm) to the absolute ethyl alcohol is 1.2: 1, and Si is added3N4Adding the powder into the solution obtained in the step (1), and heating and stirring the solution uniformly at 60 ℃;
(3) carbon fiber powder (length 50 μm) and Si3N4Adding carbon fiber powder into the solution obtained in the step (2) according to the mass ratio of the powder of 0.2: 1, and continuously stirring at 80 ℃ until the slurry is viscous and cannot be stirred;
(4) placing the slurry in a drying oven, and drying at 80 ℃; after granulation and 100-mesh sieve, placing the powder particles in a mould, and pressing under 150 MPa to form a blank;
(5) coating the blank with mixed powder of silicon powder and titanium powder (the mass ratio of Si to Ti is 1.8: 1), placing the blank in a graphite crucible, preserving heat for 3 hours at the temperature of 1550 ℃ in vacuum to increase densification, and naturally cooling to obtain the carbon fiber powder reinforced silicon nitride based composite material.
C/Si obtained in this example3N4The bending strength of the composite material is 350 MPa, and the fracture toughness is 5.8 MPa.m1/2。

Claims (8)

1. A preparation method of a carbon fiber powder reinforced silicon nitride-based composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) dispersing the liquid phenolic resin in absolute ethyl alcohol, and ensuring that the content of the liquid phenolic resin in the dispersion liquid is 5-12 wt%;
(2) according to Si3N4The mass ratio of the powder to the absolute ethyl alcohol is (0.5-1.2) to 1, and Si is added3N4Adding the powder into the solution obtained in the step (1), and uniformly stirring at 40-60 ℃;
(3) carbon fiber powder and Si3N4Adding the powder into the solution obtained in the step (2) according to the mass ratio of (0.1-0.2) to 1, and continuously stirring at the temperature of 60-80 ℃ until the slurry is viscous and cannot be stirred;
(4) drying the slurry, granulating and sieving, putting the obtained granular powder into a mould, and performing compression molding to obtain a blank body;
(5) and coating the blank with the mixed powder of the silicon powder and the titanium powder, placing the blank in a graphite crucible, and reacting for 1-3 hours at the temperature of 1550-1650 ℃ in vacuum to obtain the carbon fiber reinforced silicon nitride-based composite material.
2. The method of claim 1, wherein: the solid content of the liquid phenolic resin is more than or equal to 50 wt%.
3. The method of claim 1, wherein: said Si3N4The average diameter of the powder was 5 μm.
4. The method of claim 1, wherein: the length of the carbon fiber powder is 30-50 mu m.
5. The method of claim 1, wherein: the drying temperature is 60-80 ℃.
6. The method of claim 1, wherein: sieving the powder by a sieve of 60-100 meshes.
7. The method of claim 1, wherein: the pressure of the pressing forming is controlled to be 150-250 MPa.
8. The method of claim 1, wherein: the mass ratio of the silicon powder to the titanium powder is (1.8-2.5) to 1.
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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101224989A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 Two-dimensional fiber cloth reinforced composite material and preparation method thereof
CN105130438A (en) * 2015-08-21 2015-12-09 上海工程技术大学 Method for preparing boron carbide ceramic composite material based on reaction sintering

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101224989A (en) * 2008-01-29 2008-07-23 中国人民解放军国防科学技术大学 Two-dimensional fiber cloth reinforced composite material and preparation method thereof
CN105130438A (en) * 2015-08-21 2015-12-09 上海工程技术大学 Method for preparing boron carbide ceramic composite material based on reaction sintering

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