CN108727050B - Carbon material 3D toughened silicon carbide composite material and preparation method and application thereof - Google Patents
Carbon material 3D toughened silicon carbide composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the field of inorganic materials, and discloses a carbon material 3D toughened silicon carbide composite material and a preparation method and application thereof, wherein the carbon material 3D toughened silicon carbide composite material comprises 0.01-10 wt% of micron-sized carbon material, 0.01-10 wt% of nano-sized carbon material and 80-99 wt% of silicon carbide; the carbon material 3D toughening structure is prepared by inserting a micron-sized carbon material and a nanometer-sized carbon material into silicon carbide to form the micron-nanometer-sized carbon material 3D toughening structure. Compared with the prior art, the invention can obviously improve the toughening effect of the silicon carbide by only using a small amount of carbon material, the bonding property of the carbon material and the silicon carbide interface is good, the performance of the formed silicon carbide composite material is stable, and the silicon carbide composite ceramic prepared by the carbon material has high bending strength.
Description
Technical Field
The invention relates to the field of inorganic materials, in particular to a carbon material 3D toughened silicon carbide composite material and a preparation method and application thereof.
Background
The silicon carbide ceramic has the excellent characteristics of high-temperature strength, strong oxidation resistance, good wear resistance, good thermal stability, low thermal expansion rate, large thermal conductivity, strong chemical corrosion resistance and the like, and particularly has the characteristic that the strength of the silicon carbide ceramic is still basically unchanged at 1400 ℃, so that the silicon carbide ceramic has wide application in the fields of automobiles, mechanical and chemical engineering, environmental protection, space technology and the like, and becomes a structural material which has irreplaceable effect in various fields.
However, the silicon carbide has a brittle cracking problem, which affects the further application of the silicon carbide, so that the toughening of the silicon carbide becomes a difficult problem to be solved in the utilization process of the silicon carbide. The researchers have proposed various solutions aiming at increasing the bending strength of silicon carbide. For example, Zhenpu in "method for preparing ultra-fine grain silicon carbide ceramic by reaction sintering" (CN 105948754A), the bending strength of "silicon carbide whisker reinforced ceramic composite material and method for manufacturing the same" is increased by changing the preparation method and the grain size, and although a certain effect is obtained, the material is still silicon carbide at the end, and the brittleness characteristic is determined by the intrinsic characteristics of the material, which cannot be solved fundamentally. The introduction of mesophase or other substances with high bending strength into the silicon carbide is a better idea of toughening the silicon carbide. For example, lipiangshen, "a silicon carbide ceramic embedded with toughening material" (CN 101164973 a), teaches that the toughened silicon carbide ceramic with flaky alumina embedded in particles is low in cost and can form composite ceramic with uniform quality, and the toughening agent also comprises zirconia, boron series material, yttrium oxide, boron carbide and the like. However, such materials have the disadvantages of thermal expansion mismatch, high density, etc.
The carbon material has the obvious nanometer characteristic due to the characteristics of the carbon material, and is widely applied to the fields of aerospace, high-precision weapons, chemical machinery, sports equipment, energy, automobiles, textile, medicine and the like. For example, the carbon fiber is a special fiber with chemical composition, wherein the mass fraction of carbon-containing elements is higher than 90%, the inherent characteristic of the carbon material is a material with excellent mechanical property, and the carbon fiber has the characteristics of fatigue resistance, high temperature resistance, high modulus, high strength, electric conduction, heat conduction and the like, the density is less than 1/4 of steel, the tensile strength is 7-9 times of that of the steel, and the tensile strength reaches 2.8 GPa. The bending strength of the carbon nanotube is 14.2 GPa. Therefore, the carbon material is used as the toughening agent, and the bending strength of the silicon carbide material can be greatly improved. A device and a process for preparing carbon fiber reinforced silicon carbide composite material (CN 03138926.0) and a multi-component silicon carbide ceramic with an embedded object comprising carbon fibers, a research on preparation and fracture mechanism of a short carbon fiber toughened silicon carbide-based composite material (Zhanglong doctor thesis), a preparation method of a high-strength high-density isotropic carbon slide plate (CN 101747039A) and a preparation method of a carbon fiber reinforced carbon-silicon carbide double-matrix friction material (CN 101486588B) of Qiao guanjun all adopt carbon materials, particularly carbon fiber toughened silicon carbide, but the methods have the problems of large consumption of the carbon materials, complicated preparation process, poor interface binding property and the like and have certain defects.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a carbon material 3D toughened silicon carbide composite material and a preparation method and application thereof, only a small amount of carbon material is needed to be used, so that the toughening effect of silicon carbide can be obviously improved, the bonding property of the carbon material and the silicon carbide interface is good, the formed silicon carbide composite material has stable performance, and the silicon carbide composite ceramic prepared from the carbon material has high bending strength.
The technical scheme is as follows: the invention provides a carbon material 3D toughened silicon carbide composite material which comprises 0.01-10 wt% of micron-sized carbon material, 0.01-10 wt% of nanometer-sized carbon material and 80-99 wt% of silicon carbide.
Preferably, the micron-sized carbon material has at least one dimension on the micron or submicron scale.
Preferably, the micron-sized carbon material is any one or a combination of the following: carbon fiber, carbon nano tube, graphene, carbon microsphere and carbon foam.
Preferably, the nano-sized carbon material has at least its largest dimension in the order of microns.
Preferably, the nano-sized carbon material is any one or a combination of the following: carbon nanotubes, graphene, carbon microspheres, carbon foam, porous carbon.
The invention also provides a preparation method of the carbon material 3D toughening silicon carbide composite material, which is prepared by inserting the micron-sized carbon material and the nanometer-sized carbon material into silicon carbide to form a micron-nanometer-sized carbon material 3D toughening structure.
Further, before the micron-sized carbon material and the nanometer-sized carbon material are introduced into the silicon carbide, the micron-sized carbon material and the nanometer-sized carbon material are subjected to moistening pretreatment.
Preferably, the intervention is any one or a combination of the following: ball milling, presetting, magnetic stirring, ultrasonic dispersion and three-dimensional material mixing.
Preferably, if the intervening manner is ball milling, the ball milling manner is dry ball milling and/or wet ball milling; the ball-material ratio during ball milling is 2-8: 1, the mixed material accounts for 1/3-4/5 of the volume of the ball milling tank, the ball milling speed is 150-500 r/min, and the ball milling time is 0.5-48 h.
Preferably, if the ball milling mode is wet ball milling, absolute ethyl alcohol is further added as a dispersion medium during the wet ball milling.
The invention also provides application of the carbon material 3D toughened silicon carbide composite material in ceramics.
The invention also provides a method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material, wherein the silicon carbide composite ceramic is prepared by drying, sieving, molding and sintering the carbon material 3D toughened silicon carbide composite material; the drying conditions were: drying at 100-180 ℃ for 6-8 h; the sintering conditions are as follows: and (3) the sintering pressure is 30-140 MPa, the temperature is raised to 1600-2050 ℃ at the temperature rise rate of 10-80 ℃/min, and the temperature is preserved for 0.5-3 h and then the mixture is naturally cooled.
Preferably, the sintering method is any one of the following: reaction sintering, pressureless sintering, hot pressing sintering or hot isostatic pressing sintering, cold isostatic pressing sintering, spark plasma sintering and vacuum high-temperature sintering.
Has the advantages that: in the invention, a proper amount of micron-sized carbon material and nanometer-sized carbon material are inserted into the silicon carbide to form a 3D toughening structure formed by the micron-sized carbon material and the nanometer-sized carbon material together in the silicon carbide, and in the fracture process, when cracks are expanded to the vicinity of the nanometer carbon material, the nanometer-sized carbon is pulled out or debonded; when the crack propagates near the micron-sized carbon material, the crack will deflect or slip. In the crack transfer process, a large amount of energy is absorbed through the micro-and nano-sized cooperative pulling-out, bridging, 3D structure strengthening and the like, so that the toughening of the silicon carbide in the internal three-dimensional range is realized, the use amount of carbon materials is reduced, and the bending strength of the silicon carbide can be greatly improved; the silicon carbide composite ceramic prepared from the silicon carbide composite material has high bending strength, solves the problem of brittleness of ceramic materials, and expands the application of carbon materials and the composite materials thereof in the aspects of special functional materials and the like.
Drawings
Fig. 1 is a schematic structural view of a carbon material 3D toughened silicon carbide composite material in embodiments 1 to 6.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
the embodiment provides a carbon material 3D toughened silicon carbide composite material, which comprises 5wt% of carbon fibers with the length of 1.0 mm, 3wt% of carbon nanotubes and 92wt% of silicon carbide (D50 =0.6 um).
The preparation method of the carbon material 3D toughened silicon carbide composite material comprises the following steps:
adding 5 parts by mass of carbon fiber subjected to moistening pretreatment, 3 parts by mass of carbon nano tubes subjected to moistening pretreatment and 92 parts by mass of silicon carbide micro powder into a ball milling tank, adding silicon carbide grinding balls according to a ball-to-material ratio of 4:1, wherein the material ratio accounts for 2/3 of the volume of the ball milling tank, the ball milling speed is 400 r/min, the ball milling time is 0.5 h, and obtaining the carbon material 3D toughened silicon carbide composite material after ball milling.
The method of the above-mentioned moistening pretreatment of the carbon fiber and the carbon nanotube is the same as the method of the surface modification of the carbon fiber described in the patent with the application number of 201710228574.8, and is not repeated herein.
The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material comprises the following steps:
placing the carbon material 3D toughened silicon carbide composite material into a graphite mold, placing the graphite mold into a sintering furnace, keeping the pressure in the furnace to be less than 120 Pa, heating to 1750 ℃ at a speed of 10 ℃/min, then preserving the heat for 1.5 h, and naturally cooling to obtain the toughened silicon carbide composite ceramic, wherein the bending strength is 610 Mpa (20 ℃), and the volume density is more than 95% of the theoretical density.
Embodiment 2:
the embodiment provides a carbon material 3D toughened silicon carbide composite material, which comprises carbon fibers with a length of 0.5 mm by 1wt%, carbon nanotubes with a length of 0.5 mm by 0.5wt% and silicon carbide (D50 =1.2 um) with a length of 98.5 wt%.
The preparation method of the carbon material 3D toughened silicon carbide composite material comprises the following steps:
adding 1 part by mass of carbon fiber subjected to moistening pretreatment, 0.5 part of carbon nano tube subjected to moistening pretreatment and 98.5 parts of silicon carbide micro powder into a ball milling tank, adding silicon carbide grinding balls according to a ball-to-material ratio of 2:1, taking absolute ethyl alcohol as a dispersion medium, wherein the material ratio accounts for 2/3 of the volume of the ball milling tank, the ball milling speed is 500 r/min, the ball milling time is 6 hours, and obtaining the carbon material 3D toughened silicon carbide composite material after ball milling.
The method of the above-mentioned moistening pretreatment of the carbon fiber and the carbon nanotube is the same as the method of the surface modification of the carbon fiber described in the patent with the application number of 201710228574.8, and is not repeated herein.
The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material comprises the following steps:
placing the carbon material 3D toughened silicon carbide composite material into a rotary evaporator, drying at the temperature of 100 ℃ and 120 ℃ for 8h, grinding, sieving with a 100-mesh sieve, placing the undersize into a graphite mold, placing into a discharge plasma sintering furnace, heating to 1600 ℃ at the speed of 50 ℃/min, then preserving heat for 0.5 h, wherein the sintering pressure is 80 MPa, and naturally cooling to obtain the toughened silicon carbide composite ceramic, wherein the bending strength is 597 MPa (20 ℃), and the volume density is more than 95% of the theoretical density.
Embodiment 3:
the embodiment provides a carbon material 3D toughened silicon carbide composite material, which comprises 3wt% of carbon nanotubes with the length of 100 um, 10wt% of porous carbon mainly containing mesopores, and 87wt% of silicon carbide (D50 =0.9 um).
The preparation method of the carbon material 3D toughened silicon carbide composite material comprises the following steps:
adding 3 parts by mass of carbon nano tubes subjected to moistening pretreatment, 10 parts by mass of porous carbon subjected to moistening pretreatment and mainly containing mesopores and 87 parts by mass of silicon carbide micro powder into a ball milling tank, adding silicon carbide grinding balls according to a ball-to-material ratio of 8:1, taking absolute ethyl alcohol as a dispersion medium, wherein the material ratio accounts for 2/5 in the volume of the ball milling tank, the ball milling speed is 400 r/min, the ball milling time is 12 hours, and obtaining the carbon material 3D toughened silicon carbide composite material after ball milling.
The method for the moistening pretreatment of the carbon nanotubes and the porous carbon is the same as the method for the surface modification of the carbon fibers described in the patent application No. 201710228574.8, and is not repeated herein.
The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material comprises the following steps:
placing the carbon material 3D toughened silicon carbide composite material into a rotary evaporator, drying at 180 ℃ for 8h, pouring the dried material into an alloy mold, pressing the material into a shape by adopting a cold isostatic press, wherein the pressure is 40Mpa, the pressure maintaining time is 0.5 h, preparing a biscuit, placing the biscuit in a vacuum high-temperature sintering furnace, embedding the biscuit with silicon powder, heating to 1850 ℃ at the speed of 80 ℃/min under the vacuum degree of 60 Pa, preserving the heat for 3h, and naturally cooling to obtain the toughened silicon carbide composite ceramic, wherein the free silicon content is less than 3 percent, the bending strength is 347 Mpa (20 ℃), and the volume density is more than 90 percent of the theoretical density.
Embodiment 4:
the embodiment provides a carbon material 3D toughened silicon carbide composite material, which comprises 10wt% of carbon nanotubes with the length of 100 um, 10wt% of porous carbon mainly containing mesopores, and 80wt% of silicon carbide (D50 =1.0 um).
The preparation method of the carbon material 3D toughened silicon carbide composite material comprises the following steps:
taking 10 parts by mass of a carbon nano tube subjected to moistening pretreatment, 10 parts of porous carbon subjected to moistening pretreatment and mainly containing mesopores, and 80 parts of silicon carbide micro powder (D50 =1.0 um), adding the silicon carbide micro powder into a ball milling tank, adding silicon carbide grinding balls according to the ball-to-material ratio of 8:1, taking absolute ethyl alcohol as a dispersion medium, wherein the material ratio accounts for 4/5 of the volume of the ball milling tank, the ball milling speed is 200 r/min, the ball milling time is 36 h, and obtaining the carbon material 3D toughened silicon carbide composite material after ball milling.
The method for the moistening pretreatment of the carbon nanotubes and the porous carbon is the same as the method for the surface modification of the carbon fibers described in the patent application No. 201710228574.8, and is not repeated herein.
The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material comprises the following steps:
placing the carbon material 3D toughened silicon carbide composite material into a rotary evaporator, drying at 180 ℃ for 6 h, pouring the dried material into an alloy mold, pressing the material into a shape by adopting a cold isostatic press, wherein the pressure is 30 Mpa, the pressure maintaining time is 1.0 h, preparing a biscuit, placing the biscuit in a vacuum high-temperature sintering furnace, embedding the biscuit with silicon powder, heating to 1700 ℃ at a speed of 80 ℃/min under a vacuum degree of 30 Pa, and naturally cooling for 3h to obtain the toughened silicon carbide composite ceramic, wherein the free silicon content is less than 5%, the bending strength is 320 Mpa (20 ℃), and the volume density is more than 92% of the theoretical density.
Embodiment 5:
the embodiment provides a carbon material 3D toughened silicon carbide composite material, which comprises 1.5wt% of carbon nanotubes with the length of 100 um, 7wt% of porous carbon mainly containing mesopores, and 91.5wt% of silicon carbide (D50 =0.4 um).
The preparation method of the carbon material 3D toughened silicon carbide composite material comprises the following steps:
adding 1.5 parts by mass of a carbon nano tube subjected to moistening pretreatment, 7 parts of porous carbon mainly containing mesopores and 91.5 parts of silicon carbide micro powder into a ball milling tank, adding silicon carbide grinding balls according to a ball-to-material ratio of 8:1, taking absolute ethyl alcohol as a dispersion medium, wherein the material ratio accounts for 2/5 of the volume of the ball milling tank, the ball milling speed is 150 r/min, the ball milling time is 2 hours, and obtaining the carbon material 3D toughened silicon carbide composite material after ball milling.
The method for the moistening pretreatment of the carbon nanotubes and the porous carbon is the same as the method for the surface modification of the carbon fibers described in the patent application No. 201710228574.8, and is not repeated herein.
The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material comprises the following steps:
placing the carbon material 3D toughened silicon carbide composite material into a rotary evaporator, drying at 140 ℃ for 8h, placing the material into a vacuum high-temperature sintering furnace, pressing the material into a shape by adopting a cold isostatic press, wherein the pressure is 140Mpa, the temperature is increased to 2000 ℃ at 80 ℃/min under the vacuum degree of 60 Pa, the temperature is kept for 3h, and the material is naturally cooled to obtain the toughened silicon carbide composite ceramic, the bending strength is 615 Mpa (20 ℃), and the volume density is more than 98% of the theoretical density.
Embodiment 6:
the embodiment provides a carbon material 3D toughened silicon carbide composite material, which comprises 0.05wt% of carbon nanotubes with the length of 100 um, 0.95wt% of porous carbon mainly containing mesopores, and 99.0wt% of silicon carbide (D50 =0.6 um).
The preparation method of the carbon material 3D toughened silicon carbide composite material comprises the following steps:
taking 0.05 part by mass of carbon nano tubes subjected to moistening pretreatment, 0.95 part by mass of graphene subjected to moistening pretreatment and 99.0 parts by mass of silicon carbide micro powder, adding the silicon carbide micro powder into a ball milling tank, adding silicon carbide grinding balls according to a ball-to-material ratio of 4:1, taking absolute ethyl alcohol as a dispersion medium, wherein the material ratio accounts for 1/3 of the volume of the ball milling tank, the ball milling speed is 250 r/min, the ball milling time is 48 hours, and obtaining the carbon material 3D toughened silicon carbide composite material after the ball milling is finished.
The method for the moistening pretreatment of the carbon nanotubes and the graphene is the same as the method for the surface modification of the carbon fibers described in the patent with the application number of 201710228574.8, and is not repeated herein.
The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material comprises the following steps:
the carbon material 3D toughened silicon carbide composite material is placed into a rotary evaporator to be dried for 8h at the temperature of 100 ℃ and 140 ℃, placed into a sintering furnace, heated to 2050 ℃ at the speed of 80 ℃/min, and naturally cooled after being kept for 3h to obtain the toughened silicon carbide composite ceramic, the bending strength is 245 Mpa (20 ℃), and the volume density is more than 92% of the theoretical density.
A schematic structural view of the carbon material 3D toughened silicon carbide composite material in embodiments 1 to 6 is shown in fig. 1 (a and b in the drawing represent only one example of a carbon material).
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. The carbon material 3D toughened silicon carbide composite material is characterized by comprising 0.01-10 wt% of a carbon material A, 0.01-10 wt% of a carbon material B and 80-99 wt% of silicon carbide;
the carbon material A has at least one dimension in micron or submicron level; the carbon material A is any one or combination of the following materials: carbon fiber, graphene, carbon microspheres, carbon foam;
the carbon material B has at least the largest dimension in the micrometer scale; the carbon material B is a carbon nano tube.
2. The preparation method of the carbon material 3D toughened silicon carbide composite material as claimed in claim 1, characterized in that the carbon material is prepared by interposing a carbon material A and a carbon material B into silicon carbide to form a micron-nanometer sized carbon material 3D toughened structure.
3. The method for preparing the carbon material 3D toughened silicon carbide composite material according to claim 2, wherein the carbon material A and the carbon material B are subjected to moistening pretreatment before being introduced into the silicon carbide.
4. The preparation method of the carbon material 3D toughened silicon carbide composite material according to claim 2 or 3, characterized in that the intervention mode is any one or combination of the following:
ball milling, magnetic stirring, ultrasonic dispersion and three-dimensional material mixing.
5. The method for preparing the carbon material 3D toughened silicon carbide composite material according to claim 2 or 3, wherein if the intervening manner is ball milling, the ball milling manner is dry ball milling and/or wet ball milling; the ball-material ratio during ball milling is 2-8: 1, the mixed material accounts for 1/3-4/5 of the volume of the ball milling tank, the ball milling speed is 150-500 r/min, and the ball milling time is 0.5-48 h.
6. The method for preparing the carbon material 3D toughened silicon carbide composite material according to claim 5, wherein if the ball milling is wet ball milling, absolute ethyl alcohol is further added as a dispersion medium during the wet ball milling.
7. Use of the carbon material 3D toughened silicon carbide composite material according to claim 1 in ceramics.
8. The method for preparing the silicon carbide composite ceramic by using the carbon material 3D toughened silicon carbide composite material as claimed in claim 1, wherein the carbon material 3D toughened silicon carbide composite material is dried, sieved, molded and sintered to prepare the silicon carbide composite ceramic;
the drying conditions were: drying at 100-180 ℃ for 6-8 h;
the sintering conditions are as follows: and (3) the sintering pressure is 30-140 MPa, the temperature is raised to 1600-2050 ℃ at the temperature rise rate of 10-80 ℃/min, and the temperature is preserved for 0.5-3 h and then the mixture is naturally cooled.
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| CN113896559B (en) * | 2021-11-19 | 2023-04-28 | 山东建筑大学 | Silicon carbide/carbon nano tube composite material and preparation method thereof |
| CN115196967A (en) * | 2022-07-05 | 2022-10-18 | 烟台哈尔滨工程大学研究院 | Method for preparing nano powder modified silicon carbide composite ceramic by spark plasma sintering |
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