CN111471896A - Preparation method of nano hafnium oxide reinforced NiAl composite material - Google Patents
Preparation method of nano hafnium oxide reinforced NiAl composite material Download PDFInfo
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Abstract
A preparation method of a nano hafnium oxide reinforced NiAl composite material relates to a preparation method of a NiAl composite material. The invention aims to solve the problem that the existing NiAl intermetallic compound has insufficient high-temperature strength and low-temperature plasticity. The method comprises the following steps: firstly, mixing metal Ni powder, metal Al powder, metal Hf powder and cobalt chromium 15 balls; secondly, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder; thirdly, applying pressure to the uniform mixed powder; fourthly, spark plasma sintering; fifthly, cooling to obtain NiAl-HfO2A composite material. The invention solves the problems of insufficient high-temperature strength and low-temperature plasticity of NiAl intermetallic compound, and can obtain good formingNiAl-HfO with good mechanical property2The composite is greatly improved compared with pure NiAl. The invention can obtain the nano HfO2The NiAl composite material is strengthened.
Description
Technical Field
The invention relates to a preparation method of a NiAl composite material.
Background
With the development of aerospace technology, people have higher requirements on the performance of gas turbine engines, and the requirements of high thrust-weight ratio, high pressure ratio and high turbine front temperature on high-temperature structural materials are more severe. The covalent bonds in the intermetallic compound provide a strong inter-atomic bonding force compared to conventional metals, and thus the chemical bonds are quite stable. Therefore, the intermetallic compound has the advantages of high melting point, abrasion resistance, excellent oxidation resistance and the like, and is one of the most promising high-temperature structural materials between high-temperature alloy and ceramic. NiAl intermetallic compounds are considered to be promising high temperature structural materials to replace nickel-based superalloys due to low density, high melting point, high Young's modulus, large thermal conductivity, and good high temperature oxidation/corrosion resistance.
The Spark Plasma Sintering (SPS) process is a new powder metallurgy Sintering technology, in which metal powder is filled into a die made of graphite, a specific Sintering power supply and pressing pressure are applied to the sintered powder by using upper and lower punches and powered electrodes, and high-performance materials are prepared by discharge activation, thermoplastic deformation and cooling. The spark plasma sintering has the characteristic of sintering in the pressurizing process, and the plasma generated by the pulse current and the pressurizing in the sintering process are beneficial to reducing the sintering temperature of the powder. Meanwhile, the powder can be rapidly sintered and compacted due to the characteristics of low voltage and high current.
However, the NiAl intermetallic compound has the problems of insufficient high-temperature strength and low-temperature plasticity, and the structural application of the NiAl intermetallic compound is hindered.
Disclosure of Invention
The invention aims to solve the problems of insufficient high-temperature strength and low-temperature plasticity of the existing NiAl intermetallic compound, and provides a preparation method of a nano hafnium oxide reinforced NiAl composite material.
A preparation method of a nano hafnium oxide reinforced NiAl composite material comprises the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.06-0.36);
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the first step is (2.5-3.5): 1;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 300 r/min-500 r/min when the powder is mixed in the second step, and the powder mixing time is 6 h-12 h;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 5MPa to 20MPa, and the pressure maintaining time is 1min to 5 min;
fourthly, vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 500-600 ℃ at a heating rate of 50-100 ℃/min, preserving heat at 500-600 ℃ for 5-10 min, heating to 1200-1400 ℃ from 500-600 ℃ at a heating rate of 50-100 ℃/min, and preserving heat at 1200-1400 ℃ under the conditions of 30-50 MPa;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800-900 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
Furthermore, the particle size of the metal Ni powder in the step one is 10-200 μm, and the purity is more than 99.5%.
Furthermore, the grain diameter of the metal Al powder in the step one is 10-200 μm, and the purity is more than 99.9%.
Furthermore, the grain diameter of the metal Hf powder in the step one is 3-15 μm, and the purity is more than 99.9%.
Further, the diameter of the cobalt chromium 15 ball in the step one is 6mm or 8 mm.
Furthermore, the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.06-0.12).
Furthermore, the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.12-0.18).
Furthermore, the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.18-0.24).
Furthermore, the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.24-0.3).
Further, the flexural strength of the high-strength graphite mold in the third step is more than 60 MPa.
The invention has the following beneficial effects:
the invention discloses a preparation method of a nano hafnium dioxide reinforced NiAl composite material, which prepares NiAl-HfO by spark plasma sintering2The composite solves the problems of insufficient high-temperature strength and low-temperature plasticity of NiAl intermetallic compound, and can obtain NiAl-HfO with good forming and excellent mechanical property2A complex;
secondly, the room-temperature compressive yield strength of pure NiAl is 958MPa, the compressive ultimate deformation is 24.6%, the compressive strength is 2084MPa, the microhardness is 315HV, and the compressive yield strength is 108MPa at 1200 ℃; the NiAl-HfO prepared by the invention2The room-temperature compressive yield strength of the composite is 1050-1550 MPa, the compressive ultimate deformation is 15.5-27%, the compressive strength is 2000-3200 MPa, the microhardness is 350-550 HV, and the compressive yield strength is 130-500 MPa at 1200 ℃, so that the NiAl-HfO prepared by the invention2The mechanical property of the composite material is greatly improved compared with that of pure NiAl, and the problem of the existing NiAl intermetallic compound is solvedInsufficient high temperature strength and low temperature plasticity.
The nano HfO can be obtained by the embodiment2A preparation method of a reinforced NiAl composite material.
Drawings
FIG. 1 shows NiAl-HfO prepared in the first example2Macroscopic view of the composite removal surface scale;
FIG. 2 shows NiAl-HfO prepared in the first example2A microstructure map of the complex;
FIG. 3 shows the NiAl-HfO prepared in example V2A microstructure map of the complex;
FIG. 4 shows NiAl-HfO prepared in example V2XRD pattern of the complex;
FIG. 5 shows the NiAl-HfO prepared in example V2TEM images of the composites.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of a nano hafnium dioxide reinforced NiAl composite material, which is completed by the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.06-0.36);
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the first step is (2.5-3.5): 1;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 300 r/min-500 r/min when the powder is mixed in the second step, and the powder mixing time is 6 h-12 h;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 5MPa to 20MPa, and the pressure maintaining time is 1min to 5 min;
fourthly, vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 500-600 ℃ at a heating rate of 50-100 ℃/min, preserving heat at 500-600 ℃ for 5-10 min, heating to 1200-1400 ℃ from 500-600 ℃ at a heating rate of 50-100 ℃/min, and preserving heat at 1200-1400 ℃ under the conditions of 30-50 MPa;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800-900 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
In the second step of the embodiment, the roller ball mill is used, so that the energy consumption of low-energy ball milling is low, and impurities are not easy to introduce;
in the fourth step of the embodiment, a temperature step is formed at 500-600 ℃ to avoid the segregation of the material due to the liquefaction of Al caused by too high temperature rise rate;
in the fifth step of the embodiment, the pressure is released at 800-900 ℃ to avoid microcracks inside the material;
in the fifth step of the present embodiment, the diffusion pump is turned off after the temperature is reduced to 400 ℃, so as to avoid the surface oxidation of the material.
The embodiment has the following beneficial effects:
the embodiment of the invention discloses a preparation method of a nano hafnium oxide reinforced NiAl composite material, which is used for preparing NiAl-HfO through spark plasma sintering2The composite solves the problems of insufficient high-temperature strength and low-temperature plasticity of NiAl intermetallic compound, and can obtain NiAl-HfO with good forming and excellent mechanical property2A complex;
secondly, the room-temperature compressive yield strength of pure NiAl is 958MPa, the compressive ultimate deformation is 24.6 percent, the compressive strength is 2084MPa, and the microhardness is 2084MPa315HV, a compressive yield strength of 108MPa at 1200 ℃; the NiAl-HfO prepared by the invention2The room-temperature compressive yield strength of the composite is 1050-1550 MPa, the compressive ultimate deformation is 15.5-27%, the compressive strength is 2000-3200 MPa, the microhardness is 350-550 HV, and the compressive yield strength is 130-500 MPa at 1200 ℃, so that the NiAl-HfO prepared by the embodiment2The mechanical property of the composite material is greatly improved compared with that of pure NiAl, and the problems of insufficient high-temperature strength and low-temperature plasticity of the existing NiAl intermetallic compound are solved.
The nano HfO can be obtained by the embodiment2A preparation method of a reinforced NiAl composite material.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the particle size of the metal Ni powder in the first step is 10-200 mu m, and the purity is more than 99.5%. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the grain diameter of the metal Al powder in the step one is 10-200 mu m, and the purity is more than 99.9%. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the particle size of the metal Hf powder in the first step is 3-15 microns, and the purity is more than 99.9%. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the diameter of the cobalt chromium 15 ball in the step one is 6mm or 8 mm. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.06-0.12). The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.12-0.18). The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.18-0.24). The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.24-0.3). The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa. The other steps are the same as those in the first to ninth embodiments.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, methods and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
The first embodiment is as follows: the preparation method of the nano hafnium oxide reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1: 0.06;
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the step one is 3: 1;
the particle size of the metal Ni powder in the first step is 10-15 μm, and the purity is more than 99.5%;
the grain diameter of the metal Al powder in the step one is 10-15 μm, and the purity is more than 99.9%;
the particle size of the metal Hf powder in the step one is 10-15 microns, and the purity is more than 99.9%;
the diameter of the cobalt chromium 15 ball in the step one is 6 mm;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 400r/min when powder is mixed in the second step, and the powder mixing time is 12 hours;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 10MPa, and the pressure maintaining time is 1 min;
the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa;
vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 600 ℃ at the heating rate of 50 ℃/min, preserving heat at 600 ℃ for 10min, heating to 1400 ℃ from 600 ℃ at the heating rate of 50 ℃/min, and preserving heat at 1400 ℃ and under the pressure of 50MPa for 30 min;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
EXAMPLE one NiAl-HfO preparation2The room-temperature compressive yield strength of the composite material is 1055MPa, the compressive ultimate deformation is 26.7%, the compressive strength is 2539MPa, and the microhardness is 358 HV; the compressive yield strength is 122MPa at 1200 ℃.
FIG. 1 shows NiAl-HfO prepared in the first example2Macroscopical composite descalingA drawing;
as can be seen from FIG. 1, NiAl-HfO prepared in the first example2The composite block has high surface smoothness, good size precision and no macroscopic holes, and the sintering process is reasonable.
FIG. 2 shows NiAl-HfO prepared in the first example2A microstructure map of the complex;
as can be seen from FIG. 2, NiAl-HfO prepared in the first example2The compound has no obvious segregation of elements and good sintering quality, the gray matrix is NiAl, and the bright white particles are HfO2，HfO2The particles are distributed in the NiAl matrix more uniformly, and HfO is generated according to the dislocation bypass mechanism2Spherical HFO which can block dislocation movement to increase material strength and is distributed in matrix2Can effectively prevent or reduce the crack propagation in the matrix and play a role in delaying the material fracture.
Example two: the preparation method of the nano hafnium oxide reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1: 0.12;
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the step one is 3: 1;
the particle size of the metal Ni powder in the first step is 10-15 μm, and the purity is more than 99.5%;
the grain diameter of the metal Al powder in the step one is 10-15 μm, and the purity is more than 99.9%;
the particle size of the metal Hf powder in the step one is 10-15 microns, and the purity is more than 99.9%;
the diameter of the cobalt chromium 15 ball in the step one is 6 mm;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 400r/min when powder is mixed in the second step, and the powder mixing time is 12 hours;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 10MPa, and the pressure maintaining time is 1 min;
the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa;
vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 600 ℃ at the heating rate of 50 ℃/min, preserving heat at 600 ℃ for 10min, heating to 1400 ℃ from 600 ℃ at the heating rate of 50 ℃/min, and preserving heat at 1400 ℃ and under the pressure of 50MPa for 30 min;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
Example two NiAl-HfO preparation2The room-temperature compressive yield strength of the composite material is 1134MPa, the compressive ultimate deformation is 26.8 percent, the compressive strength is 2642MPa, and the microhardness is 379 HV; the compressive yield strength is 139MPa at 1200 ℃.
Example three: the preparation method of the nano hafnium oxide reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1: 0.18;
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the step one is 3: 1;
the particle size of the metal Ni powder in the first step is 10-15 μm, and the purity is more than 99.5%;
the grain diameter of the metal Al powder in the step one is 10-15 μm, and the purity is more than 99.9%;
the particle size of the metal Hf powder in the step one is 10-15 microns, and the purity is more than 99.9%;
the diameter of the cobalt chromium 15 ball in the step one is 6 mm;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 400r/min when powder is mixed in the second step, and the powder mixing time is 12 hours;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 10MPa, and the pressure maintaining time is 1 min;
the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa;
vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 600 ℃ at the heating rate of 50 ℃/min, preserving heat at 600 ℃ for 10min, heating to 1400 ℃ from 600 ℃ at the heating rate of 50 ℃/min, and preserving heat at 1400 ℃ and under the pressure of 50MPa for 30 min;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
Example III preparation of NiAl-HfO2The room-temperature compressive yield strength of the composite material is 1210MPa, and the compression limit deformationThe content is 26.9 percent, the compressive strength is 2785MPa, and the microhardness is 418 HV; the compressive yield strength is 178MPa at 1200 ℃.
Example four: the preparation method of the nano hafnium oxide reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1: 0.24;
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the step one is 3: 1;
the particle size of the metal Ni powder in the first step is 10-15 μm, and the purity is more than 99.5%;
the grain diameter of the metal Al powder in the step one is 10-15 μm, and the purity is more than 99.9%;
the particle size of the metal Hf powder in the step one is 10-15 microns, and the purity is more than 99.9%;
the diameter of the cobalt chromium 15 ball in the step one is 6 mm;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 400r/min when powder is mixed in the second step, and the powder mixing time is 12 hours;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 10MPa, and the pressure maintaining time is 1 min;
the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa;
vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 600 ℃ at the heating rate of 50 ℃/min, preserving heat at 600 ℃ for 10min, heating to 1400 ℃ from 600 ℃ at the heating rate of 50 ℃/min, and preserving heat at 1400 ℃ and under the pressure of 50MPa for 30 min;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
Example four NiAl-HfO preparation2The room-temperature compressive yield strength of the composite material is 1306MPa, the compressive ultimate deformation is 26.8 percent, the compressive strength is 2945MPa, and the microhardness is 456 HV; the compressive yield strength is 295MPa at 1200 ℃.
Example five: the preparation method of the nano hafnium oxide reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1: 0.3;
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the step one is 3: 1;
the particle size of the metal Ni powder in the first step is 10-15 μm, and the purity is more than 99.5%;
the grain diameter of the metal Al powder in the step one is 10-15 μm, and the purity is more than 99.9%;
the particle size of the metal Hf powder in the step one is 10-15 microns, and the purity is more than 99.9%;
the diameter of the cobalt chromium 15 ball in the step one is 6 mm;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 400r/min when powder is mixed in the second step, and the powder mixing time is 12 hours;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 10MPa, and the pressure maintaining time is 1 min;
the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa;
vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 600 ℃ at the heating rate of 50 ℃/min, preserving heat at 600 ℃ for 10min, heating to 1400 ℃ from 600 ℃ at the heating rate of 50 ℃/min, and preserving heat at 1400 ℃ and under the pressure of 50MPa for 30 min;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
EXAMPLE five NiAl-HfO prepared2The room-temperature compressive yield strength of the composite material is 1410MPa, the compressive ultimate deformation is 26.6%, the compressive strength is 3169MPa, and the microhardness is 503 HV; the compressive yield strength is 422MPa at 1200 ℃.
FIG. 3 shows the NiAl-HfO prepared in example V2A microstructure map of the complex;
as can be seen from FIG. 3, NiAl-HfO prepared in example V2The composite has no obvious element segregation and good sintering quality, the gray matrix is NiAl, the bright white particles are HfO2, HfO2 particles are more uniformly distributed in the NiAl matrix compared with the first example, the number of HfO2 particles is also obviously increased, the HfO2 can better obstruct dislocation motion according to a dislocation bypass mechanism, so that the strength of the material is increased, and the spherical HFO2 distributed in the matrix can effectively prevent or reduce crack propagation in the matrixAnd the function of delaying the material fracture is realized.
FIG. 4 shows NiAl-HfO prepared in example V2XRD pattern of the complex;
as can be seen from FIG. 4, NiAl-HfO prepared in example V2The main composition phases of the compound are NiAl and HfO2Original element powders Ni, Al and Hf and intermediate phase Al generated by solid phase transformation during sintering3Ni and Al3Ni2None of which is present in the final product, indicating that the sintering process reaction is complete.
FIG. 5 shows the NiAl-HfO prepared in example V2A TEM image of the composite;
as can be seen from FIG. 5, NiAl-HfO prepared in example V2HfO in composites2The particle size is nanometer, and the average size is measured to be 85nm, and the second phase of the nanometer can block dislocation motion to improve the strength of the material.
Example six: nano HfO2The preparation method of the reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1: 0.36;
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the step one is 3: 1;
the particle size of the metal Ni powder in the first step is 10-15 μm, and the purity is more than 99.5%;
the grain diameter of the metal Al powder in the step one is 10-15 μm, and the purity is more than 99.9%;
the particle size of the metal Hf powder in the step one is 10-15 microns, and the purity is more than 99.9%;
the diameter of the cobalt chromium 15 ball in the step one is 6 mm;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 400r/min when powder is mixed in the second step, and the powder mixing time is 12 hours;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 10MPa, and the pressure maintaining time is 1 min;
the breaking strength of the high-strength graphite mould in the third step is more than 60 MPa;
vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 600 ℃ at the heating rate of 50 ℃/min, preserving heat at 600 ℃ for 10min, heating to 1400 ℃ from 600 ℃ at the heating rate of 50 ℃/min, and preserving heat at 1400 ℃ and under the pressure of 50MPa for 30 min;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
Example six NiAl-HfO preparation2The room-temperature compressive yield strength of the composite material is 1509MPa, the compressive ultimate deformation is 15.9%, the compressive strength is 2088MPa, and the microhardness is 542 HV; the compressive yield strength is 472MPa at 1200 ℃.
Claims (10)
1. A preparation method of a nano hafnium oxide reinforced NiAl composite material is characterized in that the preparation method of the nano hafnium oxide reinforced NiAl composite material is completed according to the following steps:
firstly, weighing metal Ni powder, metal Al powder and metal Hf powder in a vacuum glove box to obtain mixed metal powder; putting the mixed metal powder into a powder mixing barrel, and adding a cobalt-chromium 15 ball;
the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the first step is 2.175:1 (0.06-0.36);
the mass ratio of the cobalt-chromium 15 balls to the mixed metal powder in the first step is (2.5-3.5): 1;
taking the powder mixing barrel out of the vacuum glove box, introducing oxygen into the powder mixing barrel, and putting the powder mixing barrel on a roller ball mill for mixing powder to obtain uniform mixed powder;
the rotating speed of the roller ball mill is 300 r/min-500 r/min when the powder is mixed in the second step, and the powder mixing time is 6 h-12 h;
the molar ratio of the oxygen to the metal Hf powder in the powder mixing barrel in the step two is 1: 1;
thirdly, transferring the uniform mixed powder into a high-strength graphite die, applying pressure to the uniform mixed powder and maintaining the pressure, and finally placing the high-strength graphite die into a discharge plasma sintering furnace;
the pressure in the third step is 5MPa to 20MPa, and the pressure maintaining time is 1min to 5 min;
fourthly, vacuumizing the discharge plasma sintering furnace, electrifying for heating, heating to 500-600 ℃ at a heating rate of 50-100 ℃/min, preserving heat at 500-600 ℃ for 5-10 min, heating to 1200-1400 ℃ from 500-600 ℃ at a heating rate of 50-100 ℃/min, and preserving heat at 1200-1400 ℃ under the conditions of 30-50 MPa;
fifthly, closing the power supply of the discharge plasma sintering furnace, relieving pressure when the temperature is reduced to 800-900 ℃, closing the diffusion pump when the temperature is reduced to below 400 ℃, naturally cooling to below 80 ℃, taking out the high-strength graphite mold, and obtaining the NiAl-HfO2A composite material.
2. The method for preparing nano hafnium oxide reinforced NiAl composite material according to claim 1, wherein the grain size of the metal Ni powder in the first step is 10 μm-200 μm, and the purity is more than 99.5%.
3. The method for preparing nano hafnium oxide reinforced NiAl composite material according to claim 1, wherein the grain size of the metal Al powder in the first step is 10 μm-200 μm, and the purity is higher than 99.9%.
4. The method as claimed in claim 1, wherein the particle size of the metal Hf powder in the first step is 3-15 μm, and the purity is greater than 99.9%.
5. The method for preparing a nano hafnium oxide reinforced NiAl composite material according to claim 1, wherein the diameter of the cobalt chromium 15 ball in the step one is 6mm or 8 mm.
6. The method for preparing a nano hafnium oxide reinforced NiAl composite material as claimed in claim 1, wherein the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.06-0.12).
7. The method for preparing a nano hafnium oxide reinforced NiAl composite material as claimed in claim 1, wherein the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.12-0.18).
8. The method for preparing a nano hafnium oxide reinforced NiAl composite material as claimed in claim 1, wherein the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.18-0.24).
9. The method for preparing a nano hafnium oxide reinforced NiAl composite material as claimed in claim 1, wherein the mass ratio of the metal Ni powder, the metal Al powder and the metal Hf powder in the step one is 2.175:1 (0.24-0.3).
10. The method for preparing a nano hafnium oxide reinforced NiAl composite material according to claim 1, wherein the flexural strength of the high-strength graphite mold in the third step is greater than 60 MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112458351A (en) * | 2020-10-22 | 2021-03-09 | 中国人民解放军陆军装甲兵学院 | High compressive strength nickel-cobalt-based high temperature alloy |
| CN113909475A (en) * | 2021-10-11 | 2022-01-11 | 哈尔滨工业大学 | Preparation method of in-situ synthesized three-dimensional network structure reinforced compound |
| CN114042912A (en) * | 2021-11-12 | 2022-02-15 | 哈尔滨工业大学 | Method for finely controlling mechanical properties of NiAl-based composite material through powder particle size |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04136135A (en) * | 1990-09-28 | 1992-05-11 | Toshiba Corp | High corrosion resistant and wear resistant material and its manufacture |
| CN1775988A (en) * | 2005-12-01 | 2006-05-24 | 哈尔滨工业大学 | In-situ self-generated reinforced Ni3Al composite and method for preparing same |
| CN102876926A (en) * | 2012-09-27 | 2013-01-16 | 辽宁工程技术大学 | Laser sintering synthesis method of ceramic-particle-reinforced nickel-aluminum-based composite |
| CN105463226A (en) * | 2015-12-28 | 2016-04-06 | 黄河水利职业技术学院 | Modified NiAl-based self-lubricating material and preparation method thereof |
| CN109468494A (en) * | 2019-01-04 | 2019-03-15 | 青岛市资源化学与新材料研究中心 | A kind of wear-resistant netted Cr3C2Enhance the preparation method of NiAl alloy epitaxy |
-
2020
- 2020-05-14 CN CN202010410126.1A patent/CN111471896B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04136135A (en) * | 1990-09-28 | 1992-05-11 | Toshiba Corp | High corrosion resistant and wear resistant material and its manufacture |
| CN1775988A (en) * | 2005-12-01 | 2006-05-24 | 哈尔滨工业大学 | In-situ self-generated reinforced Ni3Al composite and method for preparing same |
| CN102876926A (en) * | 2012-09-27 | 2013-01-16 | 辽宁工程技术大学 | Laser sintering synthesis method of ceramic-particle-reinforced nickel-aluminum-based composite |
| CN105463226A (en) * | 2015-12-28 | 2016-04-06 | 黄河水利职业技术学院 | Modified NiAl-based self-lubricating material and preparation method thereof |
| CN109468494A (en) * | 2019-01-04 | 2019-03-15 | 青岛市资源化学与新材料研究中心 | A kind of wear-resistant netted Cr3C2Enhance the preparation method of NiAl alloy epitaxy |
Non-Patent Citations (1)
| Title |
|---|
| 黄臻瀚: "粉末热压烧结NiAl高温变形及动态再结晶行为演化研究", 《中国优秀硕士学位论全文数据库 工程科技Ⅰ辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112458351A (en) * | 2020-10-22 | 2021-03-09 | 中国人民解放军陆军装甲兵学院 | High compressive strength nickel-cobalt-based high temperature alloy |
| CN112458351B (en) * | 2020-10-22 | 2021-10-15 | 中国人民解放军陆军装甲兵学院 | High compressive strength nickel-cobalt-based high temperature alloy |
| CN113909475A (en) * | 2021-10-11 | 2022-01-11 | 哈尔滨工业大学 | Preparation method of in-situ synthesized three-dimensional network structure reinforced compound |
| CN113909475B (en) * | 2021-10-11 | 2022-08-02 | 哈尔滨工业大学 | Preparation method of in-situ synthesized three-dimensional network structure reinforced compound |
| CN114042912A (en) * | 2021-11-12 | 2022-02-15 | 哈尔滨工业大学 | Method for finely controlling mechanical properties of NiAl-based composite material through powder particle size |
| CN114042912B (en) * | 2021-11-12 | 2022-07-29 | 哈尔滨工业大学 | Method for finely controlling mechanical properties of NiAl-based composite material through powder particle size |
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