CN111892414A - Short carbon fiber reinforced boron carbide composite material and preparation method thereof - Google Patents
Short carbon fiber reinforced boron carbide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a short carbon fiber reinforced boron carbide composite material and a preparation method thereof. The composite material comprises the following components in percentage by volume: boron carbide 80-99 vt.%, short carbon fiber 1-20 vt.%; the preparation method comprises the following steps: weighing boron carbide powder and short carbon fibers according to the designed component proportion of the short boron carbide composite material, adding the boron carbide powder and the short carbon fibers into a deionized water solution containing polyethylene glycol, uniformly mixing, and drying to obtain mixed powder; and then the mixed powder is filled into a graphite die, and the short carbon fiber reinforced boron carbide composite material is obtained by spark plasma sintering. The preparation method disclosed by the invention is simple in preparation process, the prepared sample is high in compactness, the toughness is improved to a certain extent on the basis of keeping a certain strength, and in addition, the neutron absorption performance of the composite material can be better improved, so that the composite material can be better used in a nuclear reactor shielding layer.
Description
Technical Field
The invention relates to a boron carbide composite material and a preparation method thereof, in particular to a short carbon fiber reinforced boron carbide composite material and a preparation method thereof, belonging to the technical field of carbon fiber reinforced ceramic composite materials.
Background
Boron carbide (B)4C) Light density (2.5g/cm3), high melting point (>2400 ℃ C, a high Vickers hardness of>27GPa), stable chemical performance, low expansion coefficient (5.7 multiplied by 10 < -6 >/DEG C), high neutron absorption cross section, wide absorption spectrum, no secondary radiation pollution, and good corrosion resistance and thermal stability, thus being widely applied to nuclear reactors. The fast neutron reactor is generally adopted differently10B-enriched hot-pressed sintered boron carbide pellets as neutron absorber material because10The isotope B has high neutron absorption section, wide absorption energy spectrum and low cost, does not generate strong secondary radiation after absorbing neutrons, and is easy for post-treatment.
But the boron carbide sintering temperature is high, the densification is difficult, and the hot-pressing sintering temperature reaches the melting point of 90 percent and still has the density of more than 95 percent due to the covalent bond combination; the boron carbide has low fracture toughness and large brittleness, and the fracture toughness at normal temperature is about 2-4 MPa.m1/2During use, due to B in boron carbide10Can react with the released thermal neutrons to release gas, so that boron carbide is subjected to gas expansion, and brittle failure is more likely to occur. Therefore, the two defects of boron carbide are overcome, the toughness is enhanced, and the density of the boron carbide ceramic is improved, so that the hot spots and the difficulty of the research of the boron carbide ceramic at home and abroad are overcome.
The boron carbide toughening method comprises self toughening (phase change toughening and dispersion precipitation toughening) and composite toughening, wherein the self toughening is to obtain an internal self-generated toughening phase by sintering and heat treatment processes, and the toughening mechanism is to absorb energy through plastic deformation of the toughening phase, reduce stress concentration at the tip of a crack and prevent crack propagation. At present, boron carbide has less research reports and limited toughening potential due to complex selection of second phase elements in the aspect of self toughening. The research is more than introducing heterogeneous components, namely composite toughening, during the preparation, wherein the heterogeneous components can be continuous fibers, short fibers or whiskers, particles and metals.
The grain toughening is usually to prepare samples by adopting a powder sintering method, and the grain size is in a micron scale or a nanometer scale. The toughening mechanism is the energy consumption of particle induced cracking, crack deflection and crack bridging caused by the action of particles and microcracks. Grinding machineMore toughening particles (or adhesives) comprise C, Ti and ZrO2、SiC、TiB2Si, etc., as well as the limited toughening effect, such as the TiB-containing sintered body reported in patent CN 1582264A-boron carbide and the manufacturing method thereof2B of (A)4C ceramics having a fracture toughness of only 2.8MPa m1/2。
The metal toughened boron carbide is prepared by introducing high-content continuous tough metal into a boron carbide skeleton by a solution infiltration method. B prepared by the process4C-Metal is a bicontinuous phase composite structure, B4The C particles are sintered into an interconnected whole, the infiltrated metal is also a continuous whole, the integral hardness of the composite material is high, the toughness is greatly improved, and the shock resistance is not reduced, such as B reported in open abroad4The C-MgSi has an average spring index η of 8, which is not lower than that of pure sintered Boron Carbide (N Frage, Reaction-bonded Boron-Carbide/Magnesium-Silicon Composites, Applied Ceramic Technology,2014,11: 273-. The disadvantages are that the preparation process is complex, the requirement on equipment is high, and the continuous toughening metal only can adopt metal with lower melting point, so the continuous toughening metal can not be used under the high-temperature condition.
In addition, the two toughening methods do not enhance the neutron absorption performance of the enhanced boron carbide, but reduce the performance of the enhanced boron carbide.
Disclosure of Invention
The invention aims to provide a short carbon fiber reinforced boron carbide composite material with reasonable component proportion, low density, good fracture toughness, high strength and excellent neutron absorption performance aiming at the defects in the prior art.
The invention also aims to provide a rapid and direct preparation method of the short carbon fiber reinforced boron carbide composite material, which has the advantages of simple preparation process, convenient operation, low density of the prepared composite material, high hardness, good fracture toughness, high strength and excellent neutron absorption performance.
The invention relates to a short carbon fiber reinforced boron carbide composite material, which comprises the following components in percentage by mass:
boron carbide 92.5-97.5 vt%,
short carbon fibers 2.5-7.5 vt.%.
As a preferred scheme, the short carbon fiber reinforced boron carbide composite material disclosed by the invention comprises the following components in percentage by mass:
boron carbide 92.5-97.5 vt%,
short carbon fibers 2.5-7.5 vt.%.
As a further preferred embodiment; the invention relates to a short carbon fiber reinforced boron carbide composite material which comprises the following components in percentage by mass:
boron carbide 94.5-95.5 vt%,
short carbon fibers 4.5-5.5 vt.%.
As a further preferred embodiment; the invention relates to a short carbon fiber reinforced boron carbide composite material which comprises the following components in percentage by mass:
boron carbide 95 vt.%,
short carbon fibers 5 vt.%.
According to the short carbon fiber reinforced boron carbide composite material, the raw material for generating boron carbide is boron carbide powder, and the average particle size of the boron carbide powder is 1-5 mu m.
According to the short carbon fiber reinforced boron carbide composite material, the purity of boron carbide powder is 98-99.999%.
Preferably, the purity of the boron carbide is more than or equal to 99%; the others are inevitable impurities. Such as Fe, graphitic carbon, and the like.
The invention relates to a short carbon fiber reinforced boron carbide composite material, wherein the length of the short carbon fiber is 1-3 mm.
The short carbon fiber reinforced boron carbide composite material has the short carbon fiber model of T300 and the diameter of 7 microns.
The invention relates to a preparation method of a short carbon fiber reinforced boron carbide composite material, which comprises the following steps:
the first step is as follows: ingredients
Weighing boron carbide powder and short carbon fibers according to the designed component proportion of the short boron carbide composite material, adding the boron carbide powder and the short carbon fibers into a deionized water solution containing polyethylene glycol, uniformly mixing, and drying to obtain mixed powder; the short carbon fiber is degummed short carbon fiber. In industrial application, boron carbide powder and short carbon fibers can be weighed according to the designed component proportion of the short boron carbide composite material, the boron carbide powder and the short carbon fibers are added into a deionized water solution containing polyethylene glycol and uniformly mixed, the temperature of a magnetic stirrer is set to be 120 ℃, the stirring is carried out until the solution is changed into slurry, the stirring is stopped, and then the solution is placed into a drying box and dried for 12 hours, so that mixed powder is obtained.
The second step is that: vacuum sintering
And (2) putting the mixed powder into a graphite die, and performing spark plasma sintering, wherein the sintering process parameters are as follows:
the vacuum degree is 1-10Pa, the pressure of 30-50MPa is applied to the powder in the die, the temperature is raised to 1800-plus-one 2100 ℃ at the temperature raising rate of 80-120 ℃/min, the temperature is preserved for 10-30min, the temperature is lowered to 500-plus-one 800 ℃ at the rate of 80-120 ℃/min, and then the product is cooled to the room temperature along with the furnace to obtain the finished product.
The invention relates to a preparation method of a short carbon fiber reinforced boron carbide composite material, wherein the degummed short carbon fiber is obtained by the following steps:
placing the carbon fiber into a vacuum furnace, sintering at 800-950 ℃, preferably 900 ℃ for 1-3, preferably 2 hours, ultrasonically cleaning to remove residues on the surface of the fiber, cleaning the fiber with deionized water, and then placing the fiber into a drying box for drying; then cutting into short carbon fibers; and obtaining the degummed carbon fiber.
The invention relates to a preparation method of a short carbon fiber reinforced boron carbide composite material, which comprises the following steps of in the first step, the mass fraction of polyethylene glycol is 0.4-0.6%, the temperature of a magnetic stirrer is 120 ℃, and the rotating speed is 100 r/min.
In the second step, in the stage of temperature rise and heat preservation of discharge plasma equipment, the current 320-4000A and the voltage 4-7V are applied, and the current parameter on-off is selected from one of 9ms-1ms, 8ms-2ms, 6ms-4ms and 5ms-5 ms.
The invention relates to a preparation method of a short carbon fiber reinforced boron carbide composite material, in the second step, the optimized sintering technological parameters are as follows:
the vacuum degree is 1-6Pa, the pressure of 40-50MPa is applied to the powder in the die, the temperature is raised to 1900-2000 ℃ at the heating rate of 90-110 ℃ per minute, the temperature is kept for 15-25 mm, and then the temperature is lowered to 500-600 ℃ at the heating rate of 90-110 ℃ per minute.
The method for preparing the short carbon fiber-containing reinforced boron carbide composite material has the working principle that:
the short carbon fiber in proper amount may be used as one kind of common toughening and reinforcing material, and has bearing strength, crack propagation resistance, energy consumption and toughness. Meanwhile, in the preparation process, a proper amount of boron carbide can promote a proper amount of short carbon fibers to perform proper amount of graphitization conversion, and the graphitized carbon material has a high neutron reflection section and a low thermal neutron absorption section and is an excellent nuclear reflection material. According to the invention, a proper amount of short carbon fibers are added into a proper amount of boron carbide, so that the short carbon fibers are partially graphitized, the toughness of the boron carbide can be promoted, the collision frequency of thermal neutrons and the boron carbide can be promoted, and the neutron absorption efficiency of the boron carbide is improved.
The invention adopts the discharge plasma technology to sinter and form the boron carbide/carbon fiber composite material, the sintering process integrates the discharge plasma activation and the resistance heating into a whole, and large pulse current (10) is generated among powder particles3-104A) And the spontaneous heating effect generated by the discharge among the powder particles is effectively utilized. The boron carbide powder which is difficult to sinter is rapidly bonded together, and meanwhile, the micro-scale short carbon fiber can promote the compactness of the boron carbide powder, so that the boron carbide/short carbon fiber composite material with higher compactness is obtained.
In conclusion, the preparation process is simple, and the prepared composite material is low in density, high in hardness and good in fracture toughness and can be used as a shielding layer for absorbing thermal neutrons in a nuclear reactor. Meanwhile, the optimized process provided by the invention has the advantage that the product performance is remarkably improved under the synergistic effect of all parameters.
Description of the drawings:
FIG. 1 is a micrograph of a boron carbide/short carbon fiber composite material prepared in example 2 of the present invention after polishing.
As can be seen from the appearance in the attached figure 1, the short carbon fibers are uniformly distributed in the boron carbide phase, so that the strength and the toughness of the boron carbide can be well improved.
The specific implementation mode is as follows:
the invention is further illustrated with reference to the following figures and examples:
example 1:
97.5 vt.% of boron carbide powder with the particle size of about 3.5 mu m and 2.5 vt.% of short carbon fiber are weighed, the boron carbide powder and the short carbon fiber are uniformly mixed and dried under a magnetic stirrer to obtain mixed powder of B4C and the short carbon fiber, the purity of the boron carbide powder is more than 99%, and the boron carbide powder contains trace Fe or graphite carbon; the short carbon fibers were T300 type with a diameter of 7 μm.
Pouring the mixed powder into a graphite die with the diameter of 40mm, separating the die and the powder by graphite paper, sending the powder into discharge plasma sintering equipment (FCT D25/3) for sintering, continuously pressurizing to 45MPa under the conditions of vacuum degree of 1Pa, prepressing of 8MPa and current parameter on-off of 8ms-2ms, and heating to 2000 ℃ at the heating rate of 100 ℃/min. Keeping the temperature for 20min, cooling to 500 ℃ at a cooling speed of 100 ℃/min, and then cooling to room temperature;
and taking the mold out of the spark plasma sintering furnace, removing the mold, taking out a sample, and processing to obtain the boron carbide/short carbon fiber composite material.
The density and porosity of the composite material were determined by drainage. The bending strength of the test sample is evaluated by adopting a three-point bending experiment, the fracture toughness of the composite material is tested by adopting a ceramic material single-edge notched beam bending method (SENB), and the main performance results are shown in Table 1.
Example 2:
weighing 95 vt.% boron carbide powder with the particle size of about 3.5 mu m and 5 vt.% short carbon fiber, uniformly mixing the boron carbide powder and the short carbon fiber in a magnetic stirrer, and drying to obtain mixed powder of B4C and the short carbon fiber, wherein the purity of the boron carbide powder is more than 99%, and the boron carbide powder contains trace Fe or graphite carbon; the short carbon fibers were T300 type with a diameter of 7 μm.
Pouring the mixed powder into a graphite die with the diameter of 40mm, separating the die and the powder by graphite paper, sending the powder into discharge plasma sintering equipment (FCT D25/3) for sintering, continuously pressurizing to 45MPa under the conditions of vacuum degree of 1Pa, prepressing of 8MPa and current parameter on-off of 8ms-2ms, and heating to 2000 ℃ at the heating rate of 100 ℃/min. Keeping the temperature for 20min, cooling to 500 ℃ at a cooling speed of 100 ℃/min, and then cooling to room temperature;
and taking the mold out of the spark plasma sintering furnace, removing the mold, taking out a sample, and processing to obtain the boron carbide/short carbon fiber composite material.
The density and porosity of the composite material were determined by drainage. The bending strength of the test sample is evaluated by adopting a three-point bending experiment, the fracture toughness of the composite material is tested by adopting a ceramic material single-edge notched beam bending method (SENB), and the main performance results are shown in Table 1.
Example 3:
weighing 92.5 vt.% of boron carbide powder with the particle size of about 3.5 mu m and 7.5 vt.% of short carbon fiber, uniformly mixing the boron carbide powder and the short carbon fiber under a magnetic stirrer, and drying to obtain mixed powder of B4C and the short carbon fiber, wherein the purity of the boron carbide powder is more than 99%, and the boron carbide powder contains trace Fe or graphite carbon; the short carbon fibers were T300 type with a diameter of 7 μm.
Pouring the mixed powder into a graphite die with the diameter of 40mm, separating the die and the powder by graphite paper, sending the powder into discharge plasma sintering equipment (FCT D25/3) for sintering, continuously pressurizing to 45MPa under the conditions of vacuum degree of 1Pa, prepressing of 8MPa and current parameter on-off of 8ms-2ms, and heating to 2000 ℃ at the heating rate of 100 ℃/min. Keeping the temperature for 20min, cooling to 500 ℃ at a cooling speed of 100 ℃/min, and then cooling to room temperature;
and taking the mold out of the spark plasma sintering furnace, removing the mold, taking out a sample, and processing to obtain the boron carbide/short carbon fiber composite material.
The density and porosity of the composite material were determined by drainage. The bending strength of the test sample is evaluated by adopting a three-point bending experiment, the fracture toughness of the composite material is tested by adopting a ceramic material single-edge notched beam bending method (SENB), and the main performance results are shown in Table 1.
TABLE 1
As can be seen from the data in Table 1, the boron carbide/short carbon fiber composite material prepared by the invention has higher room temperature strength than pure boron carbideThe fracture toughness is greatly improved to 7.33 MPa.m but is reduced to be within an acceptable range1/2. The density is close to 100%; can be used as a shielding layer in a nuclear reactor.
Claims (9)
1. A short carbon fiber reinforced boron carbide composite material is characterized in that: the composite material comprises the following components in percentage by volume:
boron carbide 80-99 vt%,
short carbon fibers 1-20 vt.%.
2. The short carbon fiber reinforced boron carbide composite material of claim 1, wherein: the composite material comprises the following components in percentage by volume:
boron carbide 80-99 vt%,
short carbon fibers 1-20 vt.%.
3. The short carbon fiber reinforced boron carbide composite material of claim 1, wherein: the composite material comprises the following components in percentage by volume:
boron carbide 94.5-95.5 vt%,
short carbon fibers 4.5-5.5 vt.%.
4. The short carbon fiber reinforced boron carbide composite material of claim 3, wherein: the composite material comprises the following components in percentage by volume:
boron carbide 95 vt.%,
short carbon fibers 5 vt.%.
5. The short carbon fiber reinforced boron carbide composite material of claim 1, wherein: the raw material for generating boron carbide is boron carbide powder, the average particle size of the boron carbide powder is 1-5 mu m, and the length of the short carbon fiber is 1-3 mm.
6. The short carbon fiber reinforced boron carbide composite material of claim 5, wherein: the purity of the boron carbide powder is 98-99.9%, the type of the short carbon fiber is T300, and the diameter of the carbon fiber is 7 μm.
7. A preparation method of a short carbon fiber reinforced boron carbide composite material is characterized in that; the method comprises the following steps:
first step of mixing
Weighing boron carbide powder and short carbon fibers according to the designed component proportion of the short boron carbide composite material, adding the boron carbide powder and the short carbon fibers into a deionized water solution containing polyethylene glycol, uniformly mixing, and drying to obtain mixed powder; the short carbon fiber is degummed short carbon fiber;
second step sintering
And (2) putting the mixed powder into a graphite die, and performing spark plasma sintering, wherein the sintering process parameters are as follows:
the vacuum degree is 1-10Pa, the pressure of 30-50MPa is applied to the powder in the die, the temperature is raised to 1800-plus-one 2100 ℃ at the temperature raising rate of 80-120 ℃/min, the temperature is preserved for 10-30min, the temperature is lowered to 500-plus-one 800 ℃ at the rate of 80-120 ℃/min, and then the product is cooled to the room temperature along with the furnace to obtain the finished product.
8. The method of preparing a short carbon fiber reinforced boron carbide composite material according to claim 7, wherein; the degummed short carbon fiber is obtained by the following method:
placing the carbon fiber into a vacuum furnace, sintering at 800-950 ℃, preferably 900 ℃ for 1-3, preferably 2 hours, ultrasonically cleaning to remove residues on the surface of the fiber, cleaning the fiber with deionized water, and then placing the fiber into a drying box for drying; and then cutting the carbon fiber into short carbon fiber to obtain the degummed carbon fiber.
9. The method for preparing a short carbon fiber reinforced boron carbide composite material according to claim 7, wherein the method comprises the following steps: in the second step, in the temperature rising and heat preservation stage of the discharge plasma equipment, the applied current is 320-4000A, the voltage is 4-7V, and the current parameter on-off is selected from one of 9ms-1ms, 8ms-2ms, 6ms-4ms and 5ms-5 ms.
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