CN107628818B - Preparation method of carbon fiber powder reinforced molybdenum disilicide-based composite material - Google Patents
Preparation method of carbon fiber powder reinforced molybdenum disilicide-based composite material Download PDFInfo
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- CN107628818B CN107628818B CN201710764465.8A CN201710764465A CN107628818B CN 107628818 B CN107628818 B CN 107628818B CN 201710764465 A CN201710764465 A CN 201710764465A CN 107628818 B CN107628818 B CN 107628818B
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Abstract
The invention belongs to the field of preparation of molybdenum disilicide based composite materials, and discloses a preparation method of a carbon fiber powder reinforced molybdenum disilicide based composite material. Dispersing liquid phenolic resin in absolute ethyl alcohol; mixing MoSi2Adding 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 molybdenum disilicide based composite material. The invention has the advantages of simple process, convenient operation and the like, and C/MoSi2Simultaneously has the advantages of carbon fiber and molybdenum disilicide, and overcomes MoSi2And the brittleness is higher.
Description
Technical Field
The invention belongs to the field of preparation of molybdenum disilicide based composite materials, and particularly relates to a preparation method of a carbon fiber powder reinforced molybdenum disilicide 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. Molybdenum disilicide (MoSi)2) The intermetallic compound has excellent performance, high melting point and moderate densityThe high-temperature structural material has good electric and heat conducting properties, is a high-temperature structural material with high application value, and is widely applied to the aerospace field, the transportation, the chemical industry, the mechanical transportation and other directions. But MoSi2The material has obvious brittle-ductile transition characteristics, the transition temperature is about 800-1000 ℃, namely, the material is hard and brittle at room temperature and soft and plastic at high temperature. Therefore, MoSi is to be further improved2The mechanical properties of (2). The main methods for improving molybdenum disilicide based composite materials at present are particle reinforcement based on the micro-alloying theory and whisker reinforcement based on the fiber reinforcement theory. Particle dispersion toughening needs to ensure that the reinforcement and the matrix can not generate violent chemical reaction to obtain a clean interface, so that the strength reduction of a phase interface and a crystal boundary is avoided, and the toughness of the material is improved. The length-diameter ratio of the fiber and the whisker is large, the diameter size is small, and the occurrence of microcracks can be effectively reduced, so that the reinforcing effect of the fiber and the whisker is better than that of the particle reinforcing effect in terms of strength. The toughness of the alloy is enhanced by adopting an alloy or solution mode, namely, A atoms are used for replacing B atoms in crystal lattices without changing the crystal structure, only the properties are changed, and Mo-Mo are combined by metal bonds, so that the alloy is alloyed in MoSi2The toughening agent is widely applied to toughening. In general, many molybdenum atoms are used instead of Mo atoms, and the mechanical properties of the Mo atoms can be changed by changing the strength of the bond between the Mo atoms due to the difference in atomic number and atomic size.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon fiber powder reinforced molybdenum disilicide based composite material, which has the advantages of simple process, convenient operation and the like, and C/MoSi2Meanwhile, the carbon fiber and the molybdenum disilicide have the advantages of carbon fiber and molybdenum disilicide, and the toughness and the bending strength of the molybdenum disilicide are correspondingly improved while the conductivity is further improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a carbon fiber reinforced molybdenum disilicide 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 MoSi2The mass ratio of the powder to the absolute ethyl alcohol is (0.5-1.2) to 1, and MoSi is added2Adding the powder into the solution obtained in the step (1), and uniformly stirring at 40-60 ℃;
(3) carbon fiber powder and MoSi2Adding carbon fiber 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 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 molybdenum disilicide based composite material.
Preferably, the solid content of the liquid phenolic resin is more than or equal to 50 wt%.
Preferably, the MoSi2The 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 reinforced molybdenum disilicide based composite material, which has the advantages of simple process, convenient operation and the like. The carbon fiber powder is used for reinforcing the molybdenum disilicide, so that the molybdenum disilicide has excellent performances of both the carbon fiber and the molybdenum disilicide, the conductivity of the molybdenum disilicide is further improved by adding the carbon fiber, the defect of high brittleness of the molybdenum disilicide is overcome, and the toughness and the bending strength of the molybdenum disilicide are improved. The carbon fiber reinforced molybdenum disilicide based composite material is expected to be widely applied to the aspect of cathode coatings of aluminum electrolytic cells.
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 molybdenum disilicide 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 MoSi2The mass ratio of the powder (with an average diameter of 5 μm) to the absolute ethyl alcohol is 1: 1, and MoSi is added2Adding the powder into the solution obtained in the step (1), heating at 50 ℃, and uniformly stirring;
(3) according to the carbon fiber powder (with the length of 45 mu m) and MoSi2Adding 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 the 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 reinforced molybdenum disilicide based composite material.
The fracture toughness of the carbon fiber reinforced molybdenum disilicide-based composite material prepared in the embodiment is 4.8 MPa-m1/2The bending strength is 347 MPa.
Example 2
A preparation method of a carbon fiber powder reinforced molybdenum disilicide 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 MoSi2Powder (average diameter)5 μm) and absolute ethyl alcohol in a mass ratio of 0.5: 1, adding MoSi2Adding the powder into the solution obtained in the step (1), and heating and stirring the solution uniformly at 40 ℃;
(3) according to the carbon fiber powder (the length is 30 mu m) and MoSi2Adding 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 oven, and drying at 60 ℃; after granulation and 80-mesh sieve sieving, placing the powder particles in a mould, and pressing under 250 MPa to form a blank;
(5) and (3) 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 the heat for 1 hour at the temperature of 1650 ℃ in vacuum to increase densification, and naturally cooling to obtain the carbon fiber reinforced molybdenum disilicide-based composite material.
The fracture toughness of the carbon fiber reinforced molybdenum disilicide-based composite material prepared in the embodiment is 4.5 MPa.m1/2The bending strength is 315 MPa.
Example 3
A preparation method of a carbon fiber powder reinforced molybdenum disilicide 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 MoSi2The mass ratio of the powder (average diameter of 5 μm) to the absolute ethyl alcohol is 1.2: 1, and MoSi is added2Adding the powder into the solution obtained in the step (1), and heating and stirring the solution uniformly at 60 ℃;
(3) according to the carbon fiber powder (length is 50 mu m) and MoSi2Adding 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 the heat for 3 hours at the temperature of 1550 ℃ in vacuum to increase densification, and naturally cooling to obtain the carbon fiber reinforced molybdenum disilicide based composite material.
The fracture toughness of the carbon fiber reinforced molybdenum disilicide-based composite material prepared in the embodiment is 3.8 MPa-m1/2The bending strength is 300 MPa.
Claims (8)
1. A preparation method of a carbon fiber reinforced molybdenum disilicide 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 MoSi2The mass ratio of the powder to the absolute ethyl alcohol is (0.5-1.2) to 1, and MoSi is added2Adding the powder into the solution obtained in the step (1), and uniformly stirring at 40-60 ℃;
(3) carbon fiber powder and MoSi2Adding carbon fiber 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 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 molybdenum disilicide 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: the MoSi is2The 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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