CN114790121B - Fastener of heat-resistant high-strength carbon/ceramic material and preparation method thereof - Google Patents
Fastener of heat-resistant high-strength carbon/ceramic material and preparation method thereof Download PDFInfo
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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Abstract
The invention discloses a heat-resistant high-strength carbon/ceramic material fastener and a preparation method thereof, wherein the fastener comprises a substrate and a functional layer coated on the surface of the substrate; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 10-25 parts of nano silicon carbide fiber, 20-30 parts of nano boron fiber, 3-6 parts of graphene, 4-8 parts of zirconium silicide, 5-10 parts of boron carbide, 2-4 parts of tungsten carbide, 4-7 parts of titanium powder, 3-5 parts of molybdenum powder, 1-3 parts of nano silicon nitride, 8-12 parts of epoxy hyperbranched polyborosiloxane and 2-4 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is (2-3): 1. The fastener of the heat-resistant high-strength carbon/ceramic material disclosed by the invention has the advantages of good heat resistance, good mechanical property, sufficient wear resistance, excellent corrosion resistance and long service life.
Description
Technical Field
The invention relates to the technical field of fastener material preparation, in particular to a heat-resistant high-strength carbon/ceramic material fastener and a preparation method thereof.
Background
In recent years, with the development of the fields of aviation, aerospace, weapons, ships, chemical industry, energy sources and the like, the demand for fasteners working at high temperature is increasing, and the performance requirements are also increasing. The ideal fastener operating at high temperatures is required to have excellent heat resistance, mechanical properties and corrosion resistance at the same time. The heat resistance of the existing steel or iron fastener can not meet the use requirement, and the service life is shorter. It is under this circumstance that fasteners of carbon/ceramic materials have been developed, and such materials are of increasing interest for use in thermal structures such as aerospace vehicles due to their excellent high temperature specific strength and high temperature specific modulus. In order to achieve the manufacture of large complex thermal junction structures, integration with fasteners of carbon/ceramic material is an effective approach.
The existing fastening piece of the carbon/ceramic material has long preparation period, complicated equipment required in the preparation process and high cost. In addition, the fasteners of the carbon/ceramic materials on the market have the defects of low compactness, large brittleness, easy breakage, poor material performance stability, easy cracking and failure in the use process, and further improved wear resistance, durability, mechanical properties and high temperature resistance.
To solve the above problems, patent CN106830967B discloses a fastener of heat-resistant high-strength carbon/ceramic material and a method for preparing the same. The composition of the carbon/ceramic material is as follows: 30-60% of disordered carbon fiber; 10-18% of carbon black; 10-20% of silicon powder; 8-16% of molybdenum powder; 6-12% silicon carbide; 3-10% of zirconia; 10-25% of glue solution. Is prepared by high temperature firing. The invention has very good high temperature resistance and good mechanical property at high temperature, and also has good corrosion resistance and good processing property, and can greatly reduce the preparation and processing cost. However, the fastener material has the defects of insufficient friction resistance, further improved mechanical properties and further prolonged service life.
Therefore, the fastener of the heat-resistant high-strength carbon/ceramic material with good heat resistance, good mechanical property, sufficient wear resistance, excellent corrosion resistance and long service life and the preparation method thereof are developed, meet the market demand, have higher market value and application prospect, and have very important effect on promoting the development of the fastener material working under the high-temperature condition.
Disclosure of Invention
The invention mainly aims to provide a fastener of a heat-resistant high-strength carbon/ceramic material with good heat resistance, good mechanical property, sufficient wear resistance, excellent corrosion resistance and long service life and a preparation method thereof.
In order to achieve the above purpose, the invention provides a fastener of heat-resistant high-strength charcoal/ceramic material, which is characterized by comprising a substrate and a functional layer coated on the surface of the substrate; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 10-25 parts of nano silicon carbide fiber, 20-30 parts of nano boron fiber, 3-6 parts of graphene, 4-8 parts of zirconium silicide, 5-10 parts of boron carbide, 2-4 parts of tungsten carbide, 4-7 parts of titanium powder, 3-5 parts of molybdenum powder, 1-3 parts of nano silicon nitride, 8-12 parts of epoxy hyperbranched polyborosiloxane and 2-4 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is (2-3): 1.
Preferably, the ceramic matrix composite is any one of a two-dimensional C/SiC composite and a three-dimensional C/SiC composite.
Preferably, the density of the ceramic matrix composite is 2.1-2.5 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity is 12 to 25vol.%.
Preferably, the average diameter of the nano silicon carbide fiber is 300-500nm, and the length-diameter ratio is (100-200): 1; the average diameter of the nanometer boron fiber is 200-400nm, and the length-diameter ratio is (150-300): 1.
Preferably, the particle sizes of the graphene, the zirconium silicide, the boron carbide, the tungsten carbide, the titanium powder and the molybdenum powder are the same and are all 1000-1500 meshes.
Preferably, the particle size of the nano silicon nitride is 300-500nm.
Preferably, the preparation method of the epoxy hyperbranched polyborosiloxane is described in example 1 of patent CN 107868252B.
Another object of the present invention is to provide a method for preparing a fastener of heat-resistant high-strength carbon/ceramic material, characterized by comprising the steps of:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 50-70 ℃ for 10-20 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank;
and step S3, sequentially carrying out curing treatment and heat treatment on the blank manufactured in the step S2 to obtain the heat-resistant high-strength carbon/ceramic material fastener.
Preferably, in the step S2, the mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent is 1 (1-2).
Preferably, the solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
Preferably, the curing treatment specifically includes: placing the blank in a mould with the temperature of 170-190 ℃, and preserving heat for 2-3 hours at the temperature of 200-300 ℃ under the pressure of 12-18 MPa.
Preferably, the sintering is performed under an inert gas atmosphere, specifically: raising the temperature to 1200-1400 ℃ at 5-10 ℃/min, and preserving the temperature for 1-2h; then raising the temperature to 1400-1700 ℃ at 4-6 ℃/min, and preserving the temperature for 1-3h; raising the temperature to 1700-2000 ℃ at 2-5 ℃/min, preserving the heat for 1-2h, and finally cooling along with the furnace.
Preferably, the inert gas is any one of nitrogen, helium, neon and argon.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) The preparation method of the heat-resistant high-strength carbon/ceramic material fastener disclosed by the invention can be realized by adopting a conventional process, does not need special equipment or modify the existing production line, has short process flow, is convenient to operate, has small influence on environment, and is suitable for industrial production.
(2) The invention discloses a fastener of heat-resistant high-strength carbon/ceramic material, which comprises a matrix and a functional layer coated on the surface of the matrix; through the structural design, the defects of low oxidation resistance, poor ablation resistance, short service life and low quality of the traditional carbon material are effectively avoided; through formula design, the manufactured fastener has good heat resistance, good mechanical property, sufficient wear resistance, excellent corrosion resistance and long service life.
(3) The fastener of the heat-resistant high-strength carbon/ceramic material disclosed by the invention has the advantages that the compactness and the mutual permeability are high, the processing performance is good, the compactness among the components can be further improved by adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin, the interface effect is enhanced, and silicon, boron and carbon can be introduced through the epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin, so that the compactness, the heat resistance, the mechanical property, the wear resistance and the corrosion resistance are further improved, and the service life of a product is longer.
(4) The invention discloses a fastener of a heat-resistant high-strength carbon/ceramic material, which is characterized in that the functional layer is prepared from the following components in parts by weight: 10-25 parts of nano silicon carbide fiber, 20-30 parts of nano boron fiber, 3-6 parts of graphene, 4-8 parts of zirconium silicide, 5-10 parts of boron carbide, 2-4 parts of tungsten carbide, 4-7 parts of titanium powder, 3-5 parts of molybdenum powder, 1-3 parts of nano silicon nitride and 2-4 parts of nano silicon nitride. Through the synergistic effect of the components, the prepared product has the advantages of good heat resistance, excellent mechanical property, good wear resistance and long service life.
Detailed Description
The following description is presented to enable one of ordinary skill in the art to make and use the invention. The preferred embodiments in the following description are by way of example only and other obvious variations will occur to those skilled in the art.
The preparation method of the epoxy hyperbranched polyborosiloxane in each embodiment of the invention is described in the embodiment 1 of the patent CN 107868252B.
Example 1
A heat-resistant high-strength carbon/ceramic fastener comprises a matrix and a functional layer coated on the surface of the matrix; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 10 parts of nano silicon carbide fiber, 20 parts of nano boron fiber, 3 parts of graphene, 4 parts of zirconium silicide, 5 parts of boron carbide, 2 parts of tungsten carbide, 4 parts of titanium powder, 3 parts of molybdenum powder, 1 part of nano silicon nitride, 8 parts of epoxy hyperbranched polyborosiloxane and 2 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is 2:1.
The ceramic matrix composite is a two-dimensional C/SiC composite; the density of the ceramic matrix composite is 2.1g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity was 12vol.%.
The average diameter of the nano silicon carbide fiber is 300nm, and the length-diameter ratio is 100:1; the average diameter of the nano boron fiber is 200nm, and the length-diameter ratio is 150:1; the particle sizes of the graphene, the zirconium silicide, the boron carbide, the tungsten carbide, the titanium powder and the molybdenum powder are the same and are all 1000 meshes; the particle size of the nano silicon nitride is 300nm.
A preparation method of a heat-resistant high-strength carbon/ceramic material fastener comprises the following steps:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 50 ℃ for 10 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank;
and step S3, sequentially carrying out curing treatment and heat treatment on the blank manufactured in the step S2 to obtain the heat-resistant high-strength carbon/ceramic material fastener.
The mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent in the step S2 is 1:1; the solvent is dimethyl sulfoxide; the curing treatment specifically comprises the following steps: placing the blank in a mould with the temperature of 170 ℃ and preserving heat for 2 hours at the temperature of 200 ℃ under 12 MPa.
The sintering is carried out in an inert gas atmosphere, specifically: firstly, raising the temperature to 1200 ℃ at 5 ℃/min, and preserving the temperature for 1h; then raising the temperature to 1400 ℃ at 4 ℃/min, and preserving the heat for 1h; raising the temperature to 1700 ℃ at 2 ℃/min, preserving the heat for 1 hour, and finally cooling along with a furnace; the inert gas is nitrogen.
Example 2
A heat-resistant high-strength carbon/ceramic fastener comprises a matrix and a functional layer coated on the surface of the matrix; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 15 parts of nano silicon carbide fiber, 22 parts of nano boron fiber, 4 parts of graphene, 5 parts of zirconium silicide, 6 parts of boron carbide, 2.5 parts of tungsten carbide, 5 parts of titanium powder, 3.5 parts of molybdenum powder, 1.5 parts of nano silicon nitride, 9 parts of epoxy hyperbranched polyborosiloxane and 2.5 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is 2.2:1.
The ceramic matrix composite is a three-dimensional C/SiC composite; the density of the ceramic matrix composite is 2.3g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity is 15vol.%; the average diameter of the nano silicon carbide fiber is 350nm, and the length-diameter ratio is 130:1; the average diameter of the nano boron fiber is 250nm, and the length-diameter ratio is 180:1.
The particle sizes of the graphene, the zirconium silicide, the boron carbide, the tungsten carbide, the titanium powder and the molybdenum powder are the same and are 1100 meshes; the particle size of the nano silicon nitride is 350nm.
A preparation method of a heat-resistant high-strength carbon/ceramic material fastener comprises the following steps:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 55 ℃ for 12 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank;
and step S3, sequentially carrying out curing treatment and heat treatment on the blank manufactured in the step S2 to obtain the heat-resistant high-strength carbon/ceramic material fastener.
The mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent in the step S2 is 1:1.2; the solvent is N, N-dimethylformamide.
The curing treatment specifically comprises the following steps: the blank is placed in a mould with the temperature of 175 ℃ and is kept at 13MPa and 220 ℃ for 2.3 hours.
The sintering is carried out in an inert gas atmosphere, specifically: firstly, raising the temperature to 1250 ℃ at a speed of 6 ℃/min, and preserving the temperature for 1.2h; then raising the temperature to 1500 ℃ at a speed of 4.5 ℃/min, and preserving the temperature for 1.5 hours; raising the temperature to 1800 ℃ at 3 ℃/min, preserving the heat for 1.2h, and finally cooling along with a furnace; the inert gas is helium.
Example 3
A heat-resistant high-strength carbon/ceramic fastener comprises a matrix and a functional layer coated on the surface of the matrix; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 18 parts of nano silicon carbide fiber, 25 parts of nano boron fiber, 4.5 parts of graphene, 6 parts of zirconium silicide, 7.5 parts of boron carbide, 3 parts of tungsten carbide, 5.5 parts of titanium powder, 4 parts of molybdenum powder, 2 parts of nano silicon nitride, 10 parts of epoxy hyperbranched polyborosiloxane and 3 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is (2-3): 1.
The ceramic matrix compositeThe material is a two-dimensional C/SiC composite material; the density of the ceramic matrix composite is 2.3g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity is 19vol.%; the average diameter of the nano silicon carbide fiber is 400nm, and the length-diameter ratio is 150:1; the average diameter of the nano boron fiber is 300nm, and the length-diameter ratio is 220:1.
The particle sizes of the graphene, the zirconium silicide, the boron carbide, the tungsten carbide, the titanium powder and the molybdenum powder are the same and are 1300 meshes; the grain diameter of the nano silicon nitride is 400nm.
A preparation method of a heat-resistant high-strength carbon/ceramic material fastener comprises the following steps:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 60 ℃ for 15 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank;
and step S3, sequentially carrying out curing treatment and heat treatment on the blank manufactured in the step S2 to obtain the heat-resistant high-strength carbon/ceramic material fastener.
The mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent in the step S2 is 1:1.5; the solvent is N-methyl pyrrolidone.
The curing treatment specifically comprises the following steps: the blank is placed in a mould with the temperature of 180 ℃ and is kept at 15MPa and 250 ℃ for 2.5 hours.
The sintering is carried out in an inert gas atmosphere, specifically: firstly, raising the temperature to 1300 ℃ at 7 ℃/min, and preserving the temperature for 1.5h; then raising the temperature to 1550 ℃ at 5 ℃/min, and preserving the heat for 2 hours; raising the temperature to 1850 ℃ at 3.5 ℃/min, preserving the heat for 1.5 hours, and finally cooling along with a furnace; the inert gas is neon.
Example 4
A heat-resistant high-strength carbon/ceramic fastener comprises a matrix and a functional layer coated on the surface of the matrix; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 23 parts of nano silicon carbide fiber, 28 parts of nano boron fiber, 5.5 parts of graphene, 7 parts of zirconium silicide, 9 parts of boron carbide, 3.5 parts of tungsten carbide, 6.5 parts of titanium powder, 4.5 parts of molybdenum powder, 2.5 parts of nano silicon nitride, 11 parts of epoxy hyperbranched polyborosiloxane and 3.5 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is 2.8:1.
The ceramic matrix composite is a three-dimensional C/SiC composite; the density of the ceramic matrix composite is 2.4g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity was 23vol.%.
The average diameter of the nano silicon carbide fiber is 450nm, and the length-diameter ratio is 190:1; the average diameter of the nano boron fiber is 350nm, and the length-diameter ratio is 280:1; the particle sizes of the graphene, the zirconium silicide, the boron carbide, the tungsten carbide, the titanium powder and the molybdenum powder are the same and are 1400 meshes; the particle size of the nano silicon nitride is 450nm.
A preparation method of a heat-resistant high-strength carbon/ceramic material fastener comprises the following steps:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 65 ℃ for 18 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank;
step S3, sequentially performing curing treatment and heat treatment on the blank manufactured in the step S2 to obtain a heat-resistant high-strength carbon/ceramic material fastener; the mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent is 1:1.8; the solvent is dimethyl sulfoxide.
The curing treatment specifically comprises the following steps: the blank was placed in a mold at 185℃and incubated at 16MPa and 280℃for 2.8 hours.
The sintering is carried out in an inert gas atmosphere, specifically: raising the temperature to 1350 ℃ at 9 ℃/min, and preserving the temperature for 1.8 hours; then raising the temperature to 1650 ℃ at 5.5 ℃/min, and preserving the temperature for 2.5 hours; heating to 1950deg.C at 4.5 deg.C/min, maintaining the temperature for 1.8 hr, and cooling with furnace; the inert gas is argon.
Example 5
A heat-resistant high-strength carbon/ceramic fastener comprises a matrix and a functional layer coated on the surface of the matrix; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 25 parts of nano silicon carbide fiber, 30 parts of nano boron fiber, 6 parts of graphene, 8 parts of zirconium silicide, 10 parts of boron carbide, 4 parts of tungsten carbide, 7 parts of titanium powder, 5 parts of molybdenum powder, 3 parts of nano silicon nitride, 12 parts of epoxy hyperbranched polyborosiloxane and 4 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is 3:1.
The ceramic matrix composite is a three-dimensional C/SiC composite; the density of the ceramic matrix composite is 2.5g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity is 25vol.%; the average diameter of the nano silicon carbide fiber is 500nm, and the length-diameter ratio is 200:1; the average diameter of the nano boron fiber is 400nm, and the length-diameter ratio is 300:1.
The particle sizes of the graphene, the zirconium silicide, the boron carbide, the tungsten carbide, the titanium powder and the molybdenum powder are the same and are 1500 meshes; the particle size of the nano silicon nitride is 500nm.
The preparation method of the heat-resistant high-strength carbon/ceramic material fastener is characterized by comprising the following steps of:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 70 ℃ for 20 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank;
and step S3, sequentially carrying out curing treatment and heat treatment on the blank manufactured in the step S2 to obtain the heat-resistant high-strength carbon/ceramic material fastener.
The mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent in the step S2 is 1:2; the solvent is dimethyl sulfoxide.
The curing treatment specifically comprises the following steps: placing the blank in a mould with the temperature of 190 ℃, and preserving heat for 3 hours at the temperature of 18MPa and 300 ℃; the sintering is carried out in an inert gas atmosphere, specifically: firstly, heating to 1400 ℃ at 10 ℃/min, and preserving heat for 2 hours; then raising the temperature to 1700 ℃ at the speed of 6 ℃/min, and preserving the heat for 3 hours; heating to 2000 deg.c at 5 deg.c/min, maintaining for 2 hr, and cooling with furnace; the inert gas is nitrogen.
Comparative example 1
The invention provides a heat-resistant high-strength carbon/ceramic material fastener, which is similar to the embodiment 1 in formula and preparation method, except that nano silicon carbide fibers are used for replacing nano boron fibers, and zirconium silicide is not added.
Comparative example 2
The invention provides a heat-resistant high-strength carbon/ceramic material fastener, which is similar to the formula and the preparation method of the fastener in example 1, except that hydroxypropyl-beta-cyclodextrin is used for replacing epoxy hyperbranched polyborosiloxane, and tungsten carbide is not added.
In order to further illustrate the beneficial technical effects of the heat-resistant high-strength carbon/ceramic material fastener prepared by the embodiments of the invention, the heat-resistant high-strength carbon/ceramic material fastener prepared by the embodiments is subjected to relevant performance test according to the current national standard in China, the linear wear rate is tested by adopting an MM-1000 friction tester, and the test conditions are as follows: inertia of 3.8kgf cm s 2 Specific pressure 100N/cm 2 The linear velocity was 25m/s and the test results are shown in Table 1.
TABLE 1
| Project | Flexural Strength | Fracture toughness | Linear wear rate |
| Unit (B) | MPa | MPa·m 1/2 | μm/surface/times |
| Example 1 | 352 | 16.5 | 0.75 |
| Example 2 | 364 | 17.1 | 0.72 |
| Example 3 | 370 | 17.5 | 0.70 |
| Example 4 | 378 | 18.3 | 0.66 |
| Example 5 | 383 | 18.7 | 0.64 |
| Comparative example 1 | 305 | 15.3 | 0.98 |
| Comparative example 2 | 313 | 15.7 | 1.08 |
As can be seen from Table 1, the fasteners of the heat resistant high strength carbon/ceramic materials disclosed in the examples of the present invention have more excellent mechanical properties, abrasion resistance and toughness than the comparative example products, which are the result of the synergistic effect of the components and raw materials.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. The fastener of the heat-resistant high-strength carbon/ceramic material is characterized by comprising a matrix and a functional layer coated on the surface of the matrix; the matrix is made of a ceramic matrix composite material; the functional layer is prepared from the following components in parts by weight: 10-25 parts of nano silicon carbide fiber, 20-30 parts of nano boron fiber, 3-6 parts of graphene, 4-8 parts of zirconium silicide, 5-10 parts of boron carbide, 2-4 parts of tungsten carbide, 4-7 parts of titanium powder, 3-5 parts of molybdenum powder, 1-3 parts of nano silicon nitride, 8-12 parts of epoxy hyperbranched polyborosiloxane and 2-4 parts of hydroxypropyl-beta-cyclodextrin; the mass ratio of the matrix to the functional layer is (2-3) 1;
the preparation method of the heat-resistant high-strength carbon/ceramic material fastener comprises the following steps:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 50-70 ℃ for 10-20 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank; the ceramic matrix composite is any one of a two-dimensional C/SiC composite and a three-dimensional C/SiC composite;
step S3, sequentially performing curing treatment and heat treatment on the blank manufactured in the step S2 to obtain a heat-resistant high-strength carbon/ceramic material fastener; the heat treatment is carried out under the inert gas atmosphere, and specifically comprises the following steps: raising the temperature to 1200-1400 ℃ at 5-10 ℃/min, and preserving the temperature for 1-2h; then raising the temperature to 1400-1700 ℃ at 4-6 ℃/min, and preserving the temperature for 1-3h; raising the temperature to 1700-2000 ℃ at 2-5 ℃/min, preserving the heat for 1-2h, and finally cooling along with a furnace; the inert gas is any one of nitrogen, helium, neon and argon.
2. The heat resistant high strength carbon/ceramic material fastener of claim 1 wherein the ceramic matrix composite has a density of 2.1 to 2.5g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The open porosity is 12 to 25vol.%.
3. The fastener of heat-resistant high-strength carbon/ceramic material according to claim 1, wherein the particle sizes of the graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder and molybdenum powder are the same and are all 1000-1500 meshes.
4. A method of making a fastener of the heat resistant high strength carbon/ceramic material of claim 1, comprising the steps of:
step S1, mixing nano silicon carbide fibers, nano boron fibers, graphene, zirconium silicide, boron carbide, tungsten carbide, titanium powder, molybdenum powder and nano silicon nitride to prepare a mixed intermediate;
s2, adding epoxy hyperbranched polyborosiloxane and hydroxypropyl-beta-cyclodextrin into a solvent to form a mixed solution; immersing the ceramic matrix composite material into the mixed solution at 50-70 ℃ for 10-20 hours, taking out, coating the surface of the ceramic matrix composite material with the mixed intermediate material prepared in the step S1, and preparing a blank; the ceramic matrix composite is any one of a two-dimensional C/SiC composite and a three-dimensional C/SiC composite; the mass ratio of the epoxy hyperbranched polyborosiloxane to the solvent is 1 (1-2); the solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone;
step S3, sequentially performing curing treatment and heat treatment on the blank manufactured in the step S2 to obtain a heat-resistant high-strength carbon/ceramic material fastener; the heat treatment is carried out under the inert gas atmosphere, and specifically comprises the following steps: raising the temperature to 1200-1400 ℃ at 5-10 ℃/min, and preserving the temperature for 1-2h; then raising the temperature to 1400-1700 ℃ at 4-6 ℃/min, and preserving the temperature for 1-3h; raising the temperature to 1700-2000 ℃ at 2-5 ℃/min, preserving the heat for 1-2h, and finally cooling along with a furnace; the inert gas is any one of nitrogen, helium, neon and argon.
5. The method for producing a heat resistant high strength char/ceramic material fastener according to claim 4, wherein the curing treatment specifically comprises: placing the blank in a mould with the temperature of 170-190 ℃, and preserving heat for 2-3 hours at the temperature of 200-300 ℃ under the pressure of 12-18 MPa.
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