CN114853014B - MAX phase material with high hardness and M-bit middle-high entropy and preparation method and application thereof - Google Patents
MAX phase material with high hardness and M-bit middle-high entropy and preparation method and application thereof Download PDFInfo
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Abstract
The application disclosesThe high-hardness MAX phase material with high entropy in M bits and the preparation method and the application thereof are provided. The chemical expression of the MAX phase material is M 2 SnC, wherein M bits include a combination of any three or more of Ti, V, nb, zr, hf elements, and the mixed entropy of the M bits is greater than 1.1R. The preparation method of the high-hardness MAX phase material with high entropy in M bits provided by the embodiment of the application combines a series of high-hardness MAX phase materials by strictly controlling various parameter conditions of plasma discharge sintering and mutually cooperating the parameters, has low synthesis temperature and simple process, greatly improves the physical properties such as hardness and the like of the traditional 211MAX phase materials, expands the application range of the traditional MAX phase materials, and has potential application in the fields such as machinery, extreme environment materials, aerospace and the like.
Description
Technical Field
The application relates to a composite inorganic material, in particular to a high-hardness M-bit middle-high-entropy MAX phase material, and a preparation method and application for improving the MAX phase hardness, and belongs to the technical field of materials.
Background
MAX phase material is a nanometer lamellar ternary compound with molecular formula of M n+1 AX n Wherein M is a group III B, group IV B, group V B, group VI B pre-transition metal element, A is mainly a group IIIA and group IVA element, X is carbon and/or nitrogen, and n=1 to 3. The crystal of MAX phase material has hexagonal symmetry, the space group is P63/mmc, and the unit cell is M n+1 X n The units are stacked alternately with a atomic planes, n=1, 2 or 3. Because of the unique crystal structure, the ceramic material has the properties of metal and ceramic, and has excellent electric conduction, heat conduction, radiation resistance and the likeAnd therefore, are of great interest to researchers.
Whereas the hardness of MAX phase materials is generally low, especially 211 phase, generally below 5GPa. Zr currently prepared by means of hot isostatic pressing 2 SnC has a Vickers hardness of 3.9GPa and Nb under a load of 1Kg 2 The Vickers hardness of SnC is 3.8GPa, hf 2 SnC is slightly better, the hardness value is 4.5GPa, and Ti 2 The vickers hardness of SnC is only 3.5GPa as compared to the former MAX phases.
Disclosure of Invention
The application aims to report a MAX phase material with high M-bit medium and high entropy and a preparation method thereof for the first time, enrich and expand MAX phase family members, and overcome the defects of low rigidity and other mechanical properties of the existing 211-type ternary MAX phase.
It is also an object of the application to provide the use of the high-entropy MAX phase material in M bits of high hardness.
In order to achieve the purpose of the application, the technical scheme adopted by the application comprises the following steps:
the embodiment of the application provides a high-hardness MAX phase material with high entropy in M bits, wherein the chemical expression of the MAX phase material is M 2 SnC, wherein M bits include a combination of any three or four or more of Ti, V, nb, zr, hf elements, and the mixed entropy of the M bits is greater than 1.1R.
Further, the density of the high-entropy MAX phase material in the M-bit of the high hardness is 6.9-8.1 g/cm 3 The Vickers hardness is 6.5-6.75 GPa.
The embodiment of the application also provides a preparation method of the high-entropy MAX phase material in the M bits with high hardness, which comprises the following steps: mixing M and/or M-containing materials, sn and/or Sn-containing materials and C and/or C-containing materials according to the molar ratio of (2-4) to 1 to (0.9-1.2), wherein M-bit elements are mixed according to the equimolar ratio;
sintering the obtained mixture in a discharge plasma sintering device in an inert atmosphere to obtain the high-entropy MAX phase material in M bits of high hardness;
the chemical expression of the MAX phase material is M 2 SnC in which M is Ti,V, nb, zr, hf, and the mixed entropy of M bits is more than 1.1R.
In some embodiments, the preparation method specifically includes: placing the mixture in a discharge plasma sintering device in an inert atmosphere for one-time pressureless sintering treatment to obtain a MAX phase material; wherein the temperature of the one-time pressureless sintering treatment is 1100-1400 ℃ and the time is 5-15 min.
In some embodiments, the preparation method specifically includes:
pickling the MAX phase material for 24-48 hours; the method comprises the steps of,
and placing the MAX phase material subjected to acid washing in a discharge plasma sintering device in an inert atmosphere for secondary sintering treatment to obtain the MAX phase block material with high hardness, wherein the temperature of the secondary sintering treatment is 1350-1550 ℃, the pressure is 30-50 MPa, and the pressure maintaining time is 5-15 min.
The embodiment of the application also provides application of the high-hardness M-bit middle-high-entropy MAX phase material in the fields of machinery, extreme environment materials or aerospace and the like.
Compared with the prior art, the application has at least the following advantages:
(1) The preparation method of the high-hardness MAX phase material with high entropy in M bits provided by the embodiment of the application is characterized in that various parameter conditions of plasma discharge sintering are strictly controlled, the parameters are mutually cooperated and matched to synthesize a series of high-hardness MAX phase materials, the synthesis temperature is low, the process is simple, and the MAX phase material system is greatly enriched;
(2) The high-hardness MAX phase material with high entropy in M bits solves the common situation that 211MAX phase material has low hardness, greatly improves the physical properties such as the hardness of the traditional 211MAX phase material, expands the application range of the traditional 211MAX phase material, and has potential application in the fields such as machinery, extreme environment materials, aerospace and the like.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 shows a high hardness MAX phase (TiVNb) in example 1 of the present application 2 XRD pattern of SnC material;
FIG. 2 is a high hardness MAX phase (TiVNbZr) in example 2 of the application 2 XRD pattern of SnC material;
FIG. 3 is a high hardness MAX phase (TiVNbZrHf) in example 3 of the present application 2 XRD pattern of SnC material;
FIG. 4 is a high hardness MAX phase (TiVNbZrHf) in example 3 of the present application 2 STEM diagram of SnC material;
FIG. 5 shows the high hardness MAX phase (TiVNb) in example 1 of the application 2 The test result diagram of the vickers hardness indentation of the SnC material under the load of 1 Kg.
Detailed Description
In view of the defects of the prior art, the inventor tries to synthesize a series of MAX phase materials with high hardness by strictly controlling various parameter conditions of plasma discharge sintering and mutually cooperating and mutually matching the parameters.
The M-bit is used as a key position in a MAX phase crystal structure, and a metal bond between an M atom and an A atom endows the MAX phase with good metal characteristics such as electric conduction, heat conduction and the like, and an ionic bond between the M atom and an X atom determines certain strength and hardness of the MAX phase, so that the M-bit atom is very important. The inventor designs that three or more elements are solid-dissolved through M-bit to prepare a novel high-hardness MAX phase material with higher mixed entropy, and utilizes solid-solution strengthening to realize the improvement of the mechanical property of the MAX phase material.
The technical scheme, the implementation process, the principle and the like are further explained as follows.
One aspect of the embodiment of the application provides a high-hardness MAX phase material with M bits and high entropy, wherein the chemical expression of the MAX phase material is M 2 SnC, wherein M bits include a combination of any three or more of five elements (i.e., three or more) such as Ti, V, nb, zr, hf, and the mixed entropy of M bits is greater than 1.1R.
Further, M bits of the high-entropy MAX phase material in M bits of high hardness are in solid solution with equal molar ratios of three or more elements.
Further, the MAX phase material with high entropy in M bits of high hardness is in a crystalline state and has a hexagonal lattice structure; and the unit cells of the high-entropy MAX phase material in the M bits of high hardness are formed by alternately stacking M-C units and Sn units.
Further, the density of the MAX phase material with high entropy in M bits of high hardness is between 6.9 and 8.1g/cm 3 The surface of the block material is smooth and the mirror surface is smooth.
Further, the Vickers hardness of the high-entropy MAX phase material in the M bits of the high hardness is 6.5-6.75GPa, which is 1.6 times of that of the ternary MAX phase material with the conventional 211 structure.
The application adopts M bits to realize the solid solution of three or more elements, and has the following principle: the crystal structure of the MAX phase influences the hardness of the material to a certain extent, and the MAX phase material with high hardness has multiple components in M site and does not contain solute solvent atoms, so that a large amount of lattice distortion is caused, the lattice distortion increases the resistance of dislocation movement, slip is difficult to carry out, and the hardness of the 211MAX phase is greatly improved.
The preparation method of the MAX phase material with high entropy in M bits and high hardness provided by the other aspect of the embodiment of the application comprises a discharge plasma sintering method, and specifically comprises the following steps:
mixing M and/or M-containing materials, sn and/or Sn-containing materials and C and/or C-containing materials according to the molar ratio of (2-4) to 1 to (0.9-1.2), wherein M-bit elements are mixed according to the equimolar ratio;
sintering the obtained mixture in a discharge plasma sintering device in an inert atmosphere to obtain the high-entropy MAX phase material in M bits of high hardness;
the chemical expression of the MAX phase material is M 2 SnC, wherein M bits comprise any three or more combinations of five elements such as Ti, V, nb, zr, hf, and the mixed entropy of the M bits is greater than 1.1R.
In some embodiments, the MAX phase material may be directly obtained from a sintering process at a temperature of 1350-1550 ℃, a pressure of 30-50 MPa, and a dwell time of 5-15 min.
In other embodiments, the preparation method specifically includes: placing the mixture in a discharge plasma sintering device in an inert atmosphere for one-time pressureless sintering treatment to obtain a MAX phase material; wherein the temperature of the one-time pressureless sintering treatment is 1100-1400 ℃ and the time is 5-15 min.
Further, in some embodiments, the preparation method further specifically includes:
pickling the MAX phase material for 24-48 hours; the method comprises the steps of,
and placing the MAX phase material subjected to acid washing in a discharge plasma sintering device in an inert atmosphere for secondary sintering treatment to obtain the MAX phase material with high hardness, wherein the temperature of the secondary sintering treatment is 1350-1550 ℃, the pressure is 30-50 MPa, and the pressure maintaining time is 5-15 min.
Further, the preparation method comprises the following steps: and (3) pickling the MAX phase material for 24-48 hours by adopting dilute hydrochloric acid, drying at 50 ℃ for 1-2 hours, and sieving with a 400-mesh sieve.
Further, the M-containing material includes an alloy containing M, and is not limited thereto, and there is no requirement for its particle size.
Further, the Sn-containing material includes an alloy containing Sn, and is not limited thereto, and there is no requirement on its particle size.
Further, the C-containing material includes an alloy containing C, and is not limited thereto, and there is no requirement for its particle size.
In some more specific embodiments, the preparation method of the MAX phase material with high entropy in M bits of high hardness specifically may include the following steps:
1) Mixing M and/or M-containing materials, sn and/or Sn-containing materials and C and/or C-containing materials according to the molar ratio of (2-4) to 1 to (0.9-1.2), wherein M-bit elements are mixed according to the equimolar ratio;
2) Die mounting and sample filling: assembling the pressure head and the sleeve, weighing a certain amount of mixed powder, filling the powder into a die, and compacting; placing the powder material in a discharge plasma sintering furnace in an inert atmosphere for pressureless sintering to obtain high-hardness MAX phase powder material; wherein the synthesis temperature in the step 2) is 1100-1400 ℃, and the heat preservation time in the step 2) is 5-15 min.
3) Grinding MAX phase powder fully, pickling for 24-48 h, and sieving;
4) And (3) the processed MAX phase powder is filled into a graphite mold, and the MAX phase block material with high hardness is prepared by sintering in an inert atmosphere through a plasma discharge technology.
Wherein the densification temperature in the step 4) is 1350-1550 ℃.
Wherein the pressure in the step 4) is 30-50 MPa.
Wherein the heat preservation time in the step 4) is 5-15 min.
Further, more preferably, the preparation method of the MAX phase material with high entropy in M bits of high hardness specifically further comprises the following steps:
a) Mixing M and/or M-containing materials, A and/or A-containing materials and X and/or X-containing materials according to the molar ratio of (2-4) to 1 to (0.9-1.2), wherein M-site elements are in an equimolar ratio, grinding for 30min under the condition of alcohol medium, mixing uniformly, and then drying in a vacuum drying oven for 24h;
b) Cleaning a furnace chamber;
c) Die mounting and sample filling: assembling the pressure head and the sleeve, weighing a certain amount of mixed powder, filling the powder into a die, and compacting; placing the powder in a discharge plasma sintering furnace in inert atmosphere for pressureless sintering to obtain M-bit medium-high entropy MAX phase powder;
d) Fully grinding the powder in an agate mortar, pickling for 24-48 h by dilute hydrochloric acid, drying for 1-2 h in a blast drying oven at 50 ℃, and sieving the dried powder with a 400-mesh sieve;
e) And (3) putting the treated powder into a graphite mold, and sintering in an inert atmosphere through a plasma discharge technology to prepare a compact mass of MAX phase with high entropy in M positions.
Another aspect of the embodiment of the application also provides a potential application prospect of any of the high-hardness MAX phase materials with high entropy in M bits in the fields of machinery, extreme environment materials or aerospace and the like.
In summary, the preparation method of the high-hardness MAX phase material provided by the embodiment of the application combines all parameters of the plasma discharge sintering by strictly controlling all parameter conditions, and the parameters are mutually cooperated to synthesize a series of high-hardness MAX phase material, and the preparation method has the advantages of low synthesis temperature and simple process, and can greatly enrich the MAX phase material system. The Vickers hardness of the high-hardness MAX phase material prepared by the application is 6.5-6.75GPa, which is 1.6 times of that of the ternary MAX phase material with a conventional 211 structure. Solves the general situation that 211MAX phase material has lower hardness, greatly improves the hardness of MAX phase material, and has potential application in the fields of machinery, extreme environment materials, aerospace and the like.
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further elucidated below with reference to the specific embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the present application, and the experimental conditions and setting parameters thereof should not be construed as limiting the basic technical scheme of the present application. And the scope of the present application is not limited to the following examples. In addition, the technical features of the embodiments of the present application described below may be combined with each other as long as they do not collide with each other.
Unless otherwise indicated, the starting materials and reagents in the examples of the application were all purchased commercially.
A high hardness MAX phase material of the following examples was prepared, characterized and tested according to the following methods:
crystal structure:
using a Bruker D8 advanced X-ray diffractometer (XRD) from Germany, using Cu K α And (3) rays, wherein the detection angle is set to be 10-70 degrees, and the step size is 0.01. And analyzing the microstructure and elemental composition of the material using high resolution STEM large angle annular dark field imaging (HRSTEM-HAADF) techniques with a spectrometer (FEI titanium 3 60-300, usa).
Density determination
The method comprises the steps of weighing the mass by using an electronic balance with the precision of 0.0001g according to the Archimedes law and the bulk material density by a drainage method, measuring the mass of the mass in the air by using the balance, measuring the mass of a sample in ethanol, and calculating the density according to a formula.
Hardness test
With a Wilson VH3300 Vickers hardness tester, a loading load of 1Kg, a dwell time of 10s, a separation distance of 200mm, 10 test points per sample were measured and then averaged.
Example 1: in this embodiment, a high-hardness MAX phase with high entropy in M bits is (TiVNb) 2 SnC bulk material. This (TiVNb) 2 The preparation method of the SnC block material comprises the following steps:
(1) Weighing M powder (Ti+V+Nb), sn powder and carbon powder according to the proportion of 2:1:0.9, wherein Ti, V and Nb are in equimolar proportion, the mixing entropy of M position is 1.11R, and grinding and mixing the materials in alcohol to obtain a mixture.
(2) Assembling the pressure head and the sleeve, weighing a proper amount of mixed powder, filling the mixed powder into a die, and compacting; placing the powder in a discharge plasma sintering furnace in an inert atmosphere, and performing pressureless sintering for 5min at 1100 ℃ to obtain the powder.
(3) Grinding the powder in a mortar, filling into a beaker, adding a proper amount of diluted hydrochloric acid, pickling for 24h, drying at 50 ℃ for 1h, and sieving with a 400-mesh sieve.
(4) Putting the treated powder into a graphite mold, and maintaining the temperature at 1350 deg.C and 50MPa for 10min in inert atmosphere by plasma discharge technique to obtain (TiVNb) 2 The density of the compact block product of SnC is 6.922g/cm 3 The hardness value was 6.51GPa.
Detection of bulk product (TiVNb) by X-ray diffraction Spectroscopy (XRD) 2 SnC, its XRD pattern is shown in figure 1. The product was subjected to a vickers indentation test under a load of 1Kg, and the result is shown in fig. 5.
Example 2: in this embodiment, the MAX phase with high entropy in M bits of high hardness is (TiVNbZr) 2 SnC bulk material. This (TiVNbZr) 2 The preparation method of the SnC block material comprises the following steps:
(1) Weighing M powder (Ti+V+Nb+Zr), sn powder and carbon powder in the ratio of 4:1:1.2, wherein Ti, V, nb, zr is equal molar ratio, mixing entropy of M site is 1.25R, and grinding and mixing the materials to obtain a mixture.
(2) Assembling the pressure head and the sleeve, weighing a proper amount of mixed powder, filling the mixed powder into a die, and compacting; placing in an inert atmosphere in a discharge plasma sintering furnace, and pressureless sintering at 1400 ℃ for 15min to obtain (TiVNbZr) 2 SnC powder.
(3) Grinding the powder in a mortar, filling into a beaker, adding a proper amount of diluted hydrochloric acid, pickling for 48h, drying at 50 ℃ for 2h, and sieving with a 400-mesh sieve.
(4) Putting the treated powder into a graphite mold, and maintaining the temperature for 15min at 1550 ℃ and 30MPa in an inert atmosphere by a plasma discharge technology to obtain (TiVNbZr) 2 The density of the compact block product of SnC is 7.017g/cm 3 The hardness value was 6.75GPa.
Detection of bulk products (TiVNbZr) by X-ray diffraction Spectrometry (XRD) 2 SnC, its XRD pattern is shown in FIG. 2.
Example 3: in this embodiment, a high-entropy MAX phase in M bits of high hardness is (TiVNbZrHf) 2 SnC bulk material.
This (TiVNbZrHf) 2 The preparation method of the SnC block material comprises the following steps:
(1) Weighing M powder (Ti+V+Nb+Zr+Hf), sn powder and carbon powder in the ratio of 4:1:1, wherein Ti, V, nb, zr, hf is equal molar ratio, the mixing entropy of M position is 1.56R, and grinding and mixing the materials to obtain a mixture.
(2) Assembling the pressure head and the sleeve, weighing a proper amount of mixed powder, filling the mixed powder into a die, and compacting; placing in a discharge plasma sintering furnace in inert atmosphere, and pressureless sintering at 1300 ℃ for 10min to obtain (TiVNbZrHf) 2 SnC powder.
(3) Grinding the powder in mortar, loading into beaker, adding appropriate amount of diluted hydrochloric acid, pickling for 30 hr, drying at 50deg.C for 1 hr, and sieving.
(4) Putting the treated powder into a graphite mold, and maintaining the temperature at 1450 deg.C and 40MPa for 10min in inert atmosphere by plasma discharge technique to obtain (TiVNbZrHf) 2 The density of the compact block product of SnC is 8.009g/cm 3 The hardness value was 6.53GPa.
Detection of bulk product (TiVNbZrHf) by X-ray diffraction Spectrometry (XRD) 2 SnC, whose XRD pattern is shown in FIG. 3, and whose STEM pattern is shown in FIG. 4, is observed by a Scanning Electron Microscope (SEM).
Example 4: in this embodiment, a high-hardness MAX phase with high entropy in M bits is (VNbZr) 2 SnC bulk material. This (VNbZr) 2 The preparation method of the SnC block material comprises the following steps:
(1) Weighing M powder (V+Nb+Zr), sn powder and carbon powder in the ratio of 3:1:1, wherein Ti, V, nb, zr, hf is equal molar ratio, mixing entropy of M site is 1.13R, and grinding and mixing the materials to obtain a mixture.
(2) Assembling the pressure head and the sleeve, weighing a proper amount of mixed powder, filling the mixed powder into a die, and compacting; placing in a discharge plasma sintering furnace in inert atmosphere, and pressureless sintering at 1350 ℃ for 10min to obtain (VNbZr) 2 SnC powder.
(3) Grinding the powder in a mortar, filling into a beaker, adding a proper amount of diluted hydrochloric acid, pickling for 40h, drying at 50 ℃ for 1.5h, and sieving with a 400-mesh sieve.
(4) Putting the treated powder into a graphite mold, and maintaining the temperature at 1400 deg.C and 35MPa for 5min in inert atmosphere by plasma discharge technique to obtain (VNbZr) 2 The density of the compact block product of SnC is 6.974g/cm 3 The hardness value was 6.61GPa.
Example 5: in this embodiment, a high-entropy MAX phase in M bits of high hardness is (NbZrHf) 2 SnC bulk material. This (NbZrHf) 2 The preparation method of the SnC block material comprises the following steps:
(1) Weighing M powder (Nb+Zr+Hf), sn powder and carbon powder in the ratio of 2.5:1:1, wherein Nb, zr and Hf are in equimolar ratio, the mixing entropy of M site is 1.12R, and grinding and mixing the materials to obtain a mixture.
(2) Assembling the pressure head and the sleeve, weighing a proper amount of mixed powder, filling the mixed powder into a die, and compacting; placing in a discharge plasma sintering furnace in inert atmosphere, and pressureless sintering at 1380deg.C for 10min to obtain (NbZrHf) 2 SnC powder.
(3) Grinding the powder in a mortar, filling into a beaker, adding a proper amount of diluted hydrochloric acid, pickling for 40h, drying at 50 ℃ for 1.5h, and sieving with a 400-mesh sieve.
(4) Putting the treated powder into a graphite mold, and maintaining the temperature at 1400 deg.C and 35MPa for 5min in inert atmosphere by plasma discharge technique to obtain (NbZrHf) 2 The density of the compact block product of SnC is 6.977g/cm 3 The hardness value was 6.71GPa.
Example 6: in this embodiment, a high-entropy MAX phase in M bits of high hardness is (TiNbZrHf) 2 SnC bulk material. The (TiNbZrHf) 2 The preparation method of the SnC block material comprises the following steps:
(1) Weighing M powder (Ti+Nb+Zr+Hf), sn powder and carbon powder in the ratio of 4:1:1, wherein Ti, nb, zr, hf is equal molar ratio, mixing entropy of M site is 1.45R, and grinding and mixing the materials to obtain a mixture.
(2) Assembling the pressure head and the sleeve, weighing a proper amount of mixed powder, filling the mixed powder into a die, and compacting; placing in a discharge plasma sintering furnace in inert atmosphere, and pressureless sintering at 1340 ℃ for 8min to obtain (TiNbZrHf) 2 SnC powder.
(3) Grinding the powder in mortar, loading into beaker, adding appropriate amount of diluted hydrochloric acid, pickling for 30 hr, drying at 50deg.C for 1 hr, and sieving.
(4) Putting the treated powder into a graphite mold, and preserving the temperature for 10min under the conditions of 1420 ℃ and 40MPa in an inert atmosphere by a plasma discharge technology to obtain (TiNbZrHf) 2 The density of the compact block product of SnC is 7.954g/cm 3 The hardness value was 6.68GPa.
In addition, the inventor also replaces the corresponding raw materials and process conditions in the previous examples 1-6 with other raw materials and process conditions described in the specification, and the results show that the MAX phase material with high entropy in M bits with high hardness can be obtained.
Comparative example 1
The present comparative example is different from example 1 in that step (1) is: weighing M powder (Ti), sn powder and carbon powder according to the proportion of 2:1:0.9, grinding and mixing the materials in alcohol to prepare a block.
The test results show that: the density of the finally obtained MAX phase material is 5.92g/cm 3 The hardness value was 3.51GPa.
Comparative example 2
The present comparative example is different from example 1 in that step (1) is: weighing M powder (Nb), sn powder and carbon powder according to the proportion of 2:1:0.9, grinding and mixing the materials in alcohol, and preparing a block.
The test results show that: the density of the MAX phase material finally obtained is 6.01g/cm 3 The hardness value was 3.64GPa.
Comparative example 3
The present comparative example is different from example 1 in that step (1) is: weighing M powder (Ti+Nb), sn powder and carbon powder according to the proportion of 2:1:0.9, grinding and mixing the materials in alcohol to prepare a block.
The test results show that: the density of the MAX phase material finally obtained is 6.32g/cm 3 The hardness value was 3.76GPa.
The various aspects, embodiments, features and examples of the application are to be considered in all respects as illustrative and not intended to limit the application, the scope of which is defined solely by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed application.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the present application.
Throughout this disclosure, where a composition is described as having, comprising, or including a particular component, or where a process is described as having, comprising, or including a particular process step, it is contemplated that the composition of the teachings of the present application also consist essentially of, or consist of, the recited component, and that the process of the teachings of the present application also consist essentially of, or consist of, the recited process step.
It should be understood that the order of steps or order in which a particular action is performed is not critical, as long as the present teachings remain operable. Furthermore, two or more steps or actions may be performed simultaneously.
While the application has been described with reference to an illustrative embodiment, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the application. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the application without departing from the scope thereof. Therefore, it is intended that the application not be limited to the particular embodiment disclosed for carrying out this application, but that the application will include all embodiments falling within the scope of the appended claims.
Claims (7)
1. A MAX phase material with high entropy in M bits and high hardness is characterized in that: the chemical expression of the MAX phase material is M 2 SnC, wherein M bits include a combination of any three or four or more of the Ti, V, nb, zr, hf elements, and the mixed entropy of the M bits is greater than 1.1R;
the MAX phase material with high entropy in M bits of high hardness is in a crystal state and has six phasesSquare lattice structure, its unit cell is formed by alternately stacking M-C unit and Sn unit; the density of the high-entropy MAX phase material in the M bits of high hardness is 6.9-8.1 g/cm 3 The Vickers hardness is 6.5-6.75 GPa.
2. The method for preparing the MAX phase material with high entropy in M bits of high hardness according to claim 1, comprising:
mixing M and/or M-containing materials, sn and/or Sn-containing materials and C and/or C-containing materials according to the molar ratio of (2-4) 1 (0.9-1.2), wherein M-site elements are mixed according to the equimolar ratio;
and sintering the obtained mixture in a discharge plasma sintering device in an inert atmosphere to obtain the high-entropy MAX phase material in M bits of high hardness.
3. The preparation method according to claim 2, characterized by comprising the following steps: placing the mixture in a discharge plasma sintering device in an inert atmosphere for one-time pressureless sintering treatment to obtain a MAX phase material; the temperature of the one-time pressureless sintering treatment is 1100-1400 ℃ and the time is 5-15 min.
4. A method of preparation according to claim 3, characterized in that it comprises in particular:
pickling the MAX phase material for 24-48 hours; the method comprises the steps of,
and placing the pickled MAX phase material in discharge plasma sintering equipment in inert atmosphere for secondary sintering treatment to obtain the high-hardness MAX phase material, wherein the temperature of the secondary sintering treatment is 1350-1550 ℃, the pressure is 30-50 MPa, and the pressure maintaining time is 5-15 min.
5. The preparation method according to claim 4, characterized by comprising: and (3) carrying out acid washing on the MAX phase material for 24-48 hours by adopting dilute hydrochloric acid, and then drying.
6. The preparation method according to claim 2, characterized in that: the M-containing material comprises an alloy containing M; and/or the Sn-containing material comprises an alloy containing Sn; and/or the C-containing material comprises a C-containing alloy.
7. Use of the high-hardness M-bit medium high-entropy MAX-phase material according to claim 1 in the mechanical, extreme environmental or aerospace fields.
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