CN113501714B - MAX phase material with high hardness and high wear resistance and preparation method thereof - Google Patents
MAX phase material with high hardness and high wear resistance and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of materials, and relates to a MAX phase material with high hardness and high wear resistance and a preparation method thereof. The present invention uses a certain proportion of lanthanide series rare earth elements to substitute Cr 2 Cr atoms in AlC obtain a MAX phase material with high hardness and high wear resistance, and the chemical formula is as follows: (Cr) 2/3 Re 1/3 ) 2 AlC（ReIs lanthanide series rare earth element), the series of compounds have two crystal structures of orthorhombic and monoclinic; obtaining a compact massive MAX phase material through vacuum pressureless sintering and vacuum hot pressing sintering; the material has high hardness (8.5 GPa) which is obviously higher than that of Cr 2 AlC (4.5 GPa) and excellent abrasion resistance, and the abrasion loss is 9.6 multiplied by 10 ‑ 5 mm ‑3 ·N ‑1 ·m ‑1 Reduced to 0.6 × 10 ‑5 mm ‑3 ·N ‑1 ·m ‑1 . The invention relates to a method for improving the hardness and the wear resistance of an MAX material by replacing M element in an MAX phase with rare earth element and further regulating and controlling the crystal structure type of the material; a series of novel MAX phase materials with high hardness and high abrasion resistance are prepared, and the types of the MAX materials are enriched.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a MAX phase material with high hardness and high wear resistance and a preparation method thereof.
Background
M n+1 AX n The phase ceramic material is a kind of transition metal carbide or nitride having a layered structure, wherein M represents a transition metal, A represents a group 13 to 16 element, and X represents C or N. Such materials have both ceramic and metallic properties and are receiving considerable attention from researchers.
Wherein, cr 2 AlC is a compound having a hexagonal structure ofP 63 /mmc) The ternary layered carbide ceramic material with the structure has the advantages of common MAX phase ceramic materials, such as high melting point, excellent chemical stability, excellent processability and the like. Studies have shown that Cr is present at high temperatures or under high sliding rate wear 2 The surface of AlC can form an oxide lubricating film, so that the friction coefficient and the abrasion loss of the material are reduced. However, compared to conventional ceramics, cr 2 AlC also has the disadvantages of common MAX ceramic materials, such as low hardness, high friction coefficient at normal temperature, large abrasion loss and the like, which limits the application of frictional abrasion in a wide temperature range.
The main methods commonly used to improve the wear resistance of MAX materials are particle strengthening and solid solution strengthening. The two methods improve the tribology performance of the material under the normal temperature condition to a certain extent by improving the mechanical properties of the material such as hardness and the like. However, the hardness of the material is still low, the wear loss is still high, and the friction and wear resistance is still not ideal. Therefore, there is a continuing need to find new ways to improve the tribological properties of MAX materials.
Disclosure of Invention
To solve the problems in the prior art, the invention provides a MAX phase material with high hardness and high wear resistance and a preparation method thereof. Substituting Cr with rare-earth elements in a certain proportion 2 Cr atoms in AlC obtain a novel MAX phase material with high hardness and high wear resistance, and the chemical formula is as follows: (Cr) 2/3 Re 1/3 ) 2 AlC。
In order to achieve the purpose, the invention adopts the following technical scheme.
A high hardness and high wear resistance MAX phase material comprising the following components:
chromium powder, lanthanide series rare earth element powder, aluminum powder and carbon powder.
Further, the mole fraction ratio of the chromium powder, the lanthanide series rare earth element powder, the aluminum powder and the carbon powder is 1.33:0.67: (1-1.5): (0.7-1).
Further, the lanthanide rare earth element powder is one of lanthanide elements.
A method for preparing a MAX phase material with high hardness and high wear resistance comprises the following steps:
step 1, weighing chromium powder, lanthanide series rare earth element powder, aluminum powder and carbon powder, packaging the raw material powder in a glove box in an argon environment in a ball milling tank, then performing ball milling and uniform mixing, and performing cold pressing to form a tablet. And then heating, sintering at high temperature under vacuum, keeping the temperature for a period of time, and cooling to room temperature along with the furnace to obtain the loose massive MAX phase material.
Preferably, the mole fraction ratio of the chromium powder, the lanthanide rare earth element powder, the aluminum powder and the carbon powder in the step 1 is 1.33 (1-1.5): (0.6-1).
Preferably, the lanthanide rare earth element powder in step 1 is one of lanthanide elements.
Preferably, the ball milling speed in the step 1 is 100-400rpm/min; the ball milling time is 5-15h; the heating rate is 5-20 ℃/min; the high-temperature sintering temperature under vacuum is 1100-1700 ℃; the heat preservation time is 0.5-5h.
Preferably, the ball milling speed in the step 2 is 100-500rpm/min, and the ball milling time is 10-20h. The heating rate is 5-40 ℃/min, and the pressure condition is 10-50Mpa; the high-temperature hot pressing temperature is 1000-1600 ℃; the heat preservation time is 2-10h.
Compared with the prior art, the invention has the beneficial effects of.
1. By substituting Cr with rare earth elements in appropriate proportions 2 Cr atoms in the AlC MAX phase obtain MAX phase materials with high hardness and high wear resistance. The method is provided for replacing M element in MAX phase by rare earth element, thereby changing the original crystal structure type of the material to improve the hardness and wear resistance of MAX material.
2. Synthesize (Cr) 2/3 Re 1/3 ) 2 AlC phase, whereinReIs one of lanthanide rare earth elements, having an orthogonal (Cmcm) And monoclinic (C)2/c) Two crystal structures; the metal carbide layer and the aluminum atom layer are alternately arranged along a certain crystal axis, wherein the metal carbide layer is formed by alternately and periodically arranging 2 Cr atoms and 1 rare earth metal atom, the atoms in the metal carbide layer are bonded by stronger covalent bonds, and the metal carbide layer and the aluminum atom layer are bonded by weaker metal bonds, so that a layered structure is formed. The successful preparation of the novel MAX material widens the category of the known MAX phase.
Drawings
FIG. 1 shows example 1 (Cr) 2/3 Gd 1/3 ) 2 XRD pattern of AlC phase.
FIG. 2 shows example 1 (Cr) 2/3 Gd 1/3 ) 2 TEM images of the AlC phase. (a) Is (Cr) 2/3 Gd 1/3 ) 2 Electron diffraction pattern of selected area of AlC phase; (b) Is (Cr) 2/3 Gd 1/3 ) 2 A corresponding high angle annular dark field image of the AlC phase.
FIG. 3 shows example 2 (Cr) 2/3 Dy 1/3 ) 2 XRD pattern of AlC phase.
FIG. 4 shows example 2 (Cr) 2/3 Dy 1/3 ) 2 TEM images of the AlC phase. (a) Is (Cr) 2/3 Dy 1/3 ) 2 A selected area electron diffraction pattern of the AlC phase; (b) Is (Cr) 2/3 Dy 1/3 ) 2 A corresponding high angle annular dark field image of the AlC phase.
FIG. 5 shows example 3 (Cr) 2/3 Er 1/3 ) 2 XRD pattern of AlC phase.
FIG. 6 shows example 3 (Cr) 2/3 Er 1/3 ) 2 TEM images of AlC phase. (a) Is (Cr) 2/3 Er 1/3 ) 2 Electron diffraction pattern of selected area of AlC phase; (b) Is (Cr) 2/3 Er 1/3 ) 2 A corresponding high angle annular dark field image of the AlC phase.
FIG. 7 shows example 3 (Cr) 2/3 Er 1/3 ) 2 AlC phase and Cr 2 Abrasion amount of AlC carbide is shown in a graph.
FIG. 8 shows (Cr) 2/3 Re 1/3 ) 2 AlC phase (a)Re= Gd, tb, dy, ho, er, tm, lu) and Cr 2 Vickers hardness values of AlC carbides are plotted versus time.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A high hardness and high wear resistance MAX phase material comprising the following components:
chromium powder, lanthanide series rare earth element powder, aluminum powder and carbon powder.
Further, the mole fraction ratio of the chromium powder, the lanthanide series rare earth element powder, the aluminum powder and the carbon powder is 1.33:0.67: (1-1.5): (0.7-1).
Further, the lanthanide rare earth element powder is one of lanthanide elements.
A method for preparing a MAX phase material with high hardness and high wear resistance comprises the following steps:
step 1, weighing chromium powder, lanthanide series rare earth element powder, aluminum powder and carbon powder, packaging the raw material powder in a glove box in an argon environment in a ball milling tank, then performing ball milling and uniform mixing, and performing cold pressing to form a tablet. And then heating, sintering at high temperature under vacuum, keeping the temperature for a period of time, and cooling to room temperature along with the furnace to obtain the loose massive MAX phase material.
Preferably, the mole fraction ratio of the chromium powder, the lanthanide rare earth element powder, the aluminum powder and the carbon powder in the step 1 is 1.33 (1-1.5): (0.6-1).
Preferably, the lanthanide rare earth element powder in step 1 is one of lanthanide elements.
Preferably, the rotation speed of the ball mill in the step 1 is 100-400rpm/min; the ball milling time is 5-15h; the heating rate is 5-20 ℃/min; the high-temperature sintering temperature under vacuum is 1100-1700 ℃; the heat preservation time is 0.5-5h.
Preferably, the ball milling speed in the step 2 is 100-500rpm/min, and the ball milling time is 10-20h. The heating rate is 5-40 ℃/min, and the pressure condition is 10-50Mpa; the high-temperature hot pressing temperature is 1000-1600 ℃; the heat preservation time is 2-10h.
Example 1.
Four elements with corresponding mass are weighed and respectively comprise chromium powder (Cr, 6.43 g), gadolinium powder (Gd, 9.80 g), aluminum powder (Al, 2.76 g) and carbon powder (C, 1.01 g). And (3) in a glove box, packaging into a ball milling tank in an argon environment, performing ball milling at the rotating speed of 100rpm/min for 10 hours, and performing cold pressing to form the tablet after the powder is uniformly mixed. Placing in a vacuum sintering furnace, heating to 1400 deg.C at a heating rate of 5 deg.C/min, and maintaining for 2 hr to obtain loose block (Cr) 2/3 Gd 1/3 ) 2 AlC phase material.
After vacuum sintering (Cr) 2/3 Gd 1/3 ) 2 Grinding the surface of AlC phase material with grinder and abrasive paper, pulverizing into fine particles with mortar, packaging in a glove box under argon atmosphere, ball-milling at 300rpm/min for 10 hr to obtain a particle size of 30
Fine powder on the left and right sides. In the form of powder (Cr) 2/3 Gd 1/3 ) 2 Placing AlC phase in graphite mold, heating to 1300 deg.C at a heating rate of 20 deg.C/min in vacuum hot-pressing furnace, maintaining at 30MPa for 5 hr, and cooling to room temperature to obtain compact block (Cr phase) 2/3 Gd 1/3 ) 2 AlC phase material. Warp beamMeasurement, bulk (Cr) 2/3 Gd 1/3 ) 2 The vickers hardness value of AlC is 8.39GPa.
Example 2.
Four elements with corresponding mass are weighed and respectively comprise chromium powder (Cr, 6.25 g), rare earth dysprosium powder (Dy, 9.84 g), aluminum powder (Al, 2.93 g) and carbon powder (C, 0.98 g). Packaging into a ball milling tank in a glove box under argon atmosphere, ball milling at 200rpm/min for 5h, and cold pressing to obtain the final product. Placing in a vacuum sintering furnace, heating to 1500 ℃ at a heating rate of 15 ℃/min, and preserving heat for 1 hour to obtain a loose block (Cr) 2/3 Dy 1/3 ) 2 AlC phase material. Block body (Cr) 2/3 Dy 1/3 ) 2 Crushing AlC phase material in mortar, ball milling in a ball milling pot in a glove box under argon atmosphere to obtain fine powder, loading into a graphite grinding tool, heating to 1400 deg.C at 30 deg.C/min in a vacuum sintering furnace, and holding at 40Mpa for 3 hr to obtain compact block (Cr) material 2/3 Dy 1/3 ) 2 An AlC phase material. Block shape (Cr) 2/3 Dy 1/3 ) 2 The vickers hardness value of AlC was 8.34GPa.
Example 3.
Four elements with corresponding mass are weighed, namely chromium powder (Cr, 6.27 g), rare earth erbium powder (Er, 10.16 g), aluminum powder (Al, 2.70 g) and carbon powder (C, 0.87 g). Packaging into a ball milling tank under argon atmosphere, ball milling at 200rpm/min for 5h, and cold pressing into tablets. Placing in a vacuum sintering furnace, heating to 1500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1 hour to obtain a loose block (Cr) 2/3 Er 1/3 ) 2 An AlC phase material. Block body (Cr) 2/3 Er 1/3 ) 2 Ball milling AlC phase material in argon protective atmosphere into fine powder, heating to 1500 deg.C at 30 deg.C/min in a vacuum sintering furnace, and maintaining at 40Mpa for 2 hr to obtain compact block (Cr) 2/3 Er 1/3 ) 2 An AlC phase material. Measured as bulk (Cr) 2/3 Er 1/3 ) 2 AlC has high Vickers hardness of 9.34GPa and excellent wear resistance (low abrasion loss of 0.6 x 10) -5 mm -3 ·N -1 ·m -1 ）。
Comparative example 1.
Cr 2 The preparation process of AlC is the same as that of example 1, except that rare earth elements are not added as in example 1. Obtained Cr 2 AlC has a low hardness (4.5 GPa) and poor wear resistance (9.6X 10 wear loss) -5 mm -3 ·N -1 ·m -1 ）。
By X-ray and transmission electron microscope examination (as shown in FIG. 1-FIG. 6), (Cr) 2/3 Re 1/3 ) 2 The main phase of the AlC material is an orthorhombic symmetrical structure, contains a small amount of monoclinic structures and has an atomic-level layered structure: the selected area electron diffraction image presents a diffraction pattern in which two crystal structures coexist (as shown in fig. 2 (a), fig. 4 (a) and fig. 6 (a)); high resolution atomic image display (Cr) 2/3 Re 1/3 ) 2 The AlC material is composed ofReThe Cr-C layer and the Al atomic layer ofcThe shafts are stacked alternately; in the Cr-C layer, due to the differenceReAre heterogeneous atoms, resulting in bonding differences slightly protruding fromReA C-plane (e.g., FIG. 2 (b), FIG. 4 (b), and FIG. 6 (b)), and two adjacent Cr-C planesReThe atoms are arranged in different relative positions and are orthogonalCmcm) And monoclinic (C2/c) Two structures are provided.
The series of compounds have excellent wear resistance (as shown in figure 7) and Cr with a hexagonal structure without rare earth 2 Comparison of AlC Compound with (Cr) 2/3 Er 1/3 ) 2 The abrasion loss of the AlC material is 9.6 multiplied by 10 -5 mm -3 ·N -1 ·m -1 Reduced to 0.6 × 10 -5 mm -3 ·N -1 ·m -1 (see fig. 7).
The series of compounds have high hardness and are synthesized according to different rare earth elements (Cr) 2/3 Re 1/3 ) 2 The average microhardness of the compact block sintered by hot pressing of AlC phase is 8.5GPa (as shown in figure 8), which is obviously higher than that of the Cr with hexagonal structure without rare earth elements 2 AlC compound (4.5 GPa) (see fig. 8).
The above-described embodiments are preferable embodiments of the present invention, but the above-described embodiments are not limited to the above exemplary embodiments. Various modifications, changes, simplifications and adaptations may be made by those skilled in the art without departing from the spirit and principles of the invention and are intended to be included within the scope and spirit of the invention.
Claims (3)
1. MAX phase material with high hardness and high abrasion resistance, characterized in that the MAX phase material is a layered material with chemical formula of (Cr) 2/3 Re 1/3 ) 2 AlC；
The preparation method of the MAX phase material with high hardness and high wear resistance comprises the following steps:
step 1, weighing chromium powder, lanthanide series rare earth element powder, aluminum powder and carbon powder, packaging the raw material powder in a glove box in an argon environment in a ball milling tank, then performing ball milling and mixing uniformly, performing ball milling at the ball milling rotation speed of 100-400rpm/min for 5-15h, and performing cold pressing to form a sheet; heating at the heating rate of 5-20 ℃/min, sintering at high temperature under vacuum at 1100-1700 ℃, keeping the temperature for 0.5-5h, and cooling to room temperature along with the furnace to obtain loose massive MAX phase material;
2, grinding and polishing the surface of the obtained loose massive MAX phase material by using a grinder and abrasive paper in sequence, then primarily crushing the loose massive MAX phase material into small particles by using a mortar, further packaging the small particles in a glove box in an argon environment in a ball milling tank, wherein the ball milling speed is 100-500rpm/min, the ball milling time is 10-20h, the ball milling is carried out to obtain fine powder with the particle size of 10-50 microns, the fine powder is placed in a graphite mold, the temperature is increased to 1000-1600 ℃ at the temperature rise rate of 5-40 ℃/min, and the temperature is kept for 2-10h under the pressure of 10-50MPa to obtain a compact massive MAX phase material;
the mole fraction ratio of the chromium powder, the lanthanide series rare earth element powder, the aluminum powder and the carbon powder in the step 1 is 1.33 (1-1.5): (0.6-1);
the MAX phase material with high hardness and high wear resistance is a material prepared by substituting Cr with lanthanide rare earth elements in a certain proportion 2 Cr atoms in AlC; the material has two crystal structures of orthorhombic crystal structure and monoclinic crystal structure, and the metal carbide layer and the aluminum atom layer are arranged along the metal carbide layercThe axes are stacked alternately, wherein the metal carbide layer is formed by alternately, orderly and periodically arranging 2 chromium atoms and one rare earth atom;
the lanthanide rare earth element powder is one of lanthanide elements.
2. A method for preparing MAX phase materials with high hardness and high wear resistance is characterized by comprising the following steps:
step 1, weighing chromium powder, lanthanide series rare earth element powder, aluminum powder and carbon powder, packaging the raw material powder in a glove box in an argon environment in a ball milling tank, then performing ball milling and mixing uniformly, performing ball milling at the rotating speed of 100-400rpm/min for 5-15h, and performing cold pressing to form tablets; heating at the heating rate of 5-20 ℃/min, sintering at the high temperature of 1100-1700 ℃ under vacuum for 0.5-5h, and cooling to room temperature along with the furnace to obtain loose massive MAX phase material;
2, grinding and polishing the surface of the obtained loose massive MAX phase material by using a grinder and abrasive paper in sequence, then primarily crushing the loose massive MAX phase material into small particles by using a mortar, further packaging the small particles in a glove box in an argon environment in a ball milling tank, wherein the ball milling speed is 100-500rpm/min, the ball milling time is 10-20h, the ball milling is carried out to obtain fine powder with the particle size of 10-50 microns, the fine powder is placed in a graphite mold, the temperature is increased to 1000-1600 ℃ at the temperature rise rate of 5-40 ℃/min, and the temperature is kept for 2-10h under the pressure of 10-50MPa to obtain a compact massive MAX phase material;
the mole fraction ratio of the chromium powder, the lanthanide series rare earth element powder, the aluminum powder and the carbon powder in the step 1 is 1.33 (1-1.5): (0.6-1).
3. A method of preparation of a MAX phase material with high hardness and high wear resistance as claimed in claim 2 wherein the lanthanide rare earth element powder in step 1 is one of the lanthanide elements.
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| CN103451462B (en) * | 2013-08-01 | 2016-01-20 | 西安交通大学 | A kind of rare earth improves block Cr 7c 3the method of anti-erosion performance |
| CN103468991B (en) * | 2013-08-01 | 2015-07-01 | 西安交通大学 | Method for increasing oxidation resistance and high-temperature mechanical performance of Cr23C6 compound |
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| CN108793167B (en) * | 2018-07-19 | 2022-02-25 | 陕西科技大学 | Method for preparing layered MXenes material by utilizing ternary MAX material |
| CN111549248B (en) * | 2020-06-12 | 2021-04-06 | 陕西科技大学 | Preparation method of M-site ternary solid solution type MAX phase material |
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