CN116657012A - Mo doped with MXene phase structure 2 Molybdenum alloy of C and preparation method thereof - Google Patents
Mo doped with MXene phase structure 2 Molybdenum alloy of C and preparation method thereof Download PDFInfo
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- CN116657012A CN116657012A CN202310639759.3A CN202310639759A CN116657012A CN 116657012 A CN116657012 A CN 116657012A CN 202310639759 A CN202310639759 A CN 202310639759A CN 116657012 A CN116657012 A CN 116657012A
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- 229910001182 Mo alloy Inorganic materials 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 55
- 239000000956 alloy Substances 0.000 claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 16
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 15
- 239000011733 molybdenum Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 239000011812 mixed powder Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 24
- 238000000498 ball milling Methods 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000012300 argon atmosphere Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 3
- 230000005501 phase interface Effects 0.000 abstract description 3
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 238000011049 filling Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 239000002344 surface layer Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000691 Re alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- YUSUJSHEOICGOO-UHFFFAOYSA-N molybdenum rhenium Chemical compound [Mo].[Mo].[Re].[Re].[Re] YUSUJSHEOICGOO-UHFFFAOYSA-N 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The application discloses a Mo doped with a MXene phase structure 2 A molybdenum alloy of C and a preparation method thereof belong to the technical field of powder metallurgy. The application discloses a Mo doped with MXene phase structure 2 C molybdenum alloy adopts MXene phase structure Mo 2 Doping with C powder, said Mo being of MXene phase structure 2 Compared with other multi-element MXene phases, the particles of the C powder have less element types introduced into the molybdenum alloy, and avoid the generation of impurity phases in the sintering process of the alloy, thereby improving the mechanical properties of the alloy; furthermore, the MXene phase Mo 2 The large C-shaped carbide lamellar spacing is favorable for diffusion with a molybdenum matrix, and a phase interface with tight combination is formed, so that the toughness of the alloy is improved. The book is provided withThe application discloses the Mo doped with the MXene phase structure 2 The preparation method of the molybdenum alloy of C has simple process flow and strong controllability, and can further promote the application of the high-strength and high-toughness molybdenum alloy material.
Description
Technical Field
The application belongs to the technical field of powder metallurgy, and particularly relates to a Mo doped with MXene phase structure 2 Molybdenum alloy of C and preparation method thereof.
Background
Molybdenum is used as a rare refractory metal with high temperature resistance and has wide application in the fields of chemistry, chemical engineering, aerospace, nuclear energy and the like. The excellent characteristics of the molybdenum alloy are mainly represented by high melting point (2620 ℃), high elastic modulus, good wear resistance, good electric conduction and heat conduction properties, and excellent corrosion resistance. However, molybdenum has a body-centered cubic structure and is sensitive to C, N, O and other impurity elements, so that the molybdenum has poor plasticity and toughness and high brittleness, is difficult to carry out plastic processing, and severely limits the industrial application of the molybdenum.
The research field of molybdenum alloy at present mainly comprises Ti-Zr-Mo (TZM) alloy, molybdenum-rhenium alloy, oxide doped molybdenum alloy, multi-component molybdenum alloy and the like. These alloys have respective advantages over pure molybdenum and exhibit excellent properties in different fields of application. There are still many problems such as insignificant toughening effect, complicated preparation process, and uneven structure. Thus, there is an urgent need to research and develop new molybdenum alloys with high ductility and good toughness matching.
The MAX phase and the MXene phase of the derivative of the MAX phase of the layered ceramic developed in recent years can be used as a strengthening phase to improve the strength of the alloy and improve the toughness and the plasticity of the alloy by a unique layered structure. Studies have shown that adding a proper amount of MAX or MXene phase into a molybdenum alloy matrix to improve room temperature fracture toughness of the alloy, but adding a multi-element MXene phase still has the problems of multiple introduced element types, easy generation of impurity phase during sintering of the alloy, and reduced mechanical properties of the alloy.
Disclosure of Invention
In order to overcome the defects of the prior art, the application aims to provide a Mo doped with MXene phase structure 2 The molybdenum alloy of C and the preparation method thereof are used for solving the problems that the introduced element is various when the multi-element MXene phase is added, the alloy is easy to generate impurity phase in the sintering process, and the force of the alloy is reducedTechnical problem of the chemical properties.
In order to achieve the above purpose, the application is realized by adopting the following technical scheme:
the application discloses a Mo doped with a MXene phase structure 2 The molybdenum alloy of C comprises the following components in percentage by mass: 0.6 to 3 percent of MXene phase structure Mo 2 C powder, not more than 0.1% of impurities, and the balance of Mo powder, wherein the sum of mass fractions of the components is 100%;
mo of the MXene phase structure 2 The particle size of the powder C is 20 nm-1 mu m; the grain size of the Mo powder is 2-12 mu m.
The application also discloses the Mo doped with the MXene phase structure 2 A process for producing a molybdenum alloy of C, characterized by mixing MoS 2 、Na 2 CO 3 Mixing with active carbon powder, placing into a heating furnace, heating in an oxygen-free environment for reaction to obtain reacted powder; dispersing the reacted powder in water to obtain suspension, centrifuging and drying to obtain MXene phase structure Mo 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 Mixing the powder C, and performing ball milling mixing to obtain mixed powder;
s3: carrying out hot-pressing sintering on the mixed powder to obtain the Mo doped with the MXene phase structure 2 Molybdenum alloy of C.
Further, in S1, the MoS 2 、Na 2 CO 3 And the molar ratio of the activated carbon powder is 2:4: 9-2: 5:13; the heating furnace is a tubular furnace, and the anaerobic environment is under argon atmosphere with argon flow of 20 mL/min; the technological parameters of the heating reaction are as follows: raising the temperature to 850-950 ℃ at 8 ℃/min, and then carrying out heat preservation reaction for 2-3 h.
Further, in S1, the drying is vacuum drying; the centrifugation is to repeatedly centrifuge the suspension for 3-6 times until the pH value of the centrifugate is neutral; the centrifugation is carried out in a desk centrifuge for 3-5 min, and the centrifugation speed is 3000-5000 r/min.
Further, in S2, the MXene phase structure Mo 2 Mass of C powder and Mo powderThe ratio is (0.6-3): (99.4-97).
Further, in S2, the ball-milling mixing is performed using a Y-type planetary ball mill.
Further, in S3, the mixed powder is put into a graphite mold, and then the graphite mold filled with the mixed powder is put into a vacuum hot-press sintering furnace for hot-press sintering.
Further, in S3, the hot pressed sintering process parameters are as follows: firstly heating to 1100-1200 ℃, preserving heat for 1-2 h, then axially pressing 40-45 MPa, heating to 1700 ℃ and preserving heat for 0.5-1 h, and then waiting for cooling to 1400-1500 ℃ and preserving heat and pressure for 3-4 h.
Compared with the prior art, the application has the following beneficial effects:
the application discloses a Mo doped with a MXene phase structure 2 C molybdenum alloy adopts MXene phase structure Mo 2 Doping with C powder, said Mo being of MXene phase structure 2 Compared with other multi-element MXene phases, the particles of the C powder have less element types introduced into the molybdenum alloy, and avoid the generation of impurity phases in the sintering process of the alloy, thereby improving the mechanical properties of the alloy; furthermore, the MXene phase Mo 2 The large C-shaped carbide lamellar spacing is favorable for diffusion with a molybdenum matrix, and a phase interface with tight combination is formed, so that the toughness of the alloy is improved. According to the related experimental results, the application discloses the Mo doped with MXene phase structure 2 The mechanical property of the molybdenum alloy of C is obviously improved, and compared with a pure molybdenum material, the room-temperature tensile strength of the MXene phase doped molybdenum alloy prepared by the method is improved by more than 20 percent compared with that of the pure molybdenum material, and the room-temperature elongation of the alloy reaches more than 1.7 times of that of the pure molybdenum.
The application also discloses the Mo doped with the MXene phase structure 2 C molybdenum alloy preparation method adopting MoS 2 、Na 2 CO 3 And activated carbon powder for preparing MXene phase structure Mo 2 C powder, MXene phase Mo obtained 2 The large C-shaped carbide lamellar spacing is favorable for diffusion with a molybdenum matrix to form a phase interface which is tightly combined, so that the toughness of the alloy is improved; the whole preparation method has simple process flow and strong controllability, and canCan further promote the application of the high-strength and high-toughness molybdenum alloy material.
Drawings
FIG. 1 is a graph showing the hot press sintering process according to the present application.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present application, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the application in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The application discloses a Mo doped with a MXene phase structure 2 The preparation method of the molybdenum alloy of C comprises the following steps:
MoS is carried out 2 、Na 2 CO 3 And activated carbon powder at 2:4: 9-2: 5:13, placing the mixture into a tubular furnace in an argon atmosphere for heating reaction, heating to 850-950 ℃ at 8 ℃/min, preserving heat for 2-3 h, controlling Ar gas flow at 20mL/min, and obtaining reacted powder after reaction; dispersing the reacted powder in deionized water to form a suspension, centrifuging the suspension in a table centrifuge for 3-5 min at a centrifuging speed of 3000-5000r/min, and repeatedly centrifuging for 3-6 times until the pH value of the centrifugate is neutral;
s2: mo powder and MXene phase structure Mo 2 The mass ratio of the powder C is (0.6-3): (99.4-97), filling the mixture into a ball milling tank, introducing argon, putting the mixture into a planetary ball mill for ball milling and mixing, and setting the rotating speed of the ball mill to be 300-400 r/min to obtain mixed powder;
s3: filling the mixed powder into a graphite mold with an inner diameter of 30-60mm, and then placing the graphite mold filled with the mixed powder into a vacuum degree of 5 x 10 -3 Pa～1*10 -2 In a Pa vacuum hot-pressing sintering furnace, as shown in figure 1, firstly heating to 1100-1200 ℃ at a speed of 10 ℃/min, preserving heat for 1-2 h, axially pressing for 40-45 MPa, then heating to 1600-1700 ℃ at a speed of 5 ℃/min, preserving heat for 30min-1h, waiting for cooling to 1400-1500 ℃ and preserving heat for 3-4 h, unloading and cooling to room temperature along with the furnace, taking out a die, and processing a sintered body obtained after demoulding to remove 0.3-0.5 mm of a surface layer, thus obtaining the high-toughness MXene phase Mo 2 C doped molybdenum alloy.
The application will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present application and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
Mo doped with MXene phase structure 2 The preparation method of the molybdenum alloy of C comprises the following steps:
s1: moS is carried out 2 、Na 2 CO 3 And the active carbon powder is prepared according to the mole ratio of 2:4:9 ball milling and mixing, then placing the mixture into a tubular furnace in argon atmosphere for heating reaction, heating to 950 ℃ at 8 ℃/min during heating reaction, preserving heat for 2 hours, controlling Ar gas flow at 20mL/min, and obtaining reacted powder after reaction; dispersing the reacted powder in ionized water to form suspension, centrifuging in a desk centrifuge for 3min at a centrifuging speed of 5000r/min, and repeatedly centrifuging the suspension for 3 times until the pH value of the centrifugate is neutral; then vacuum drying is carried out to obtain the Mo of the MXene phase structure 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 The mass ratio of the powder C is 0.6:99.4, mixing, filling into a ball milling tank, introducing argon, putting into a planetary ball mill for ball milling and mixing, and setting the rotating speed of the ball mill to 400r/min to obtain mixed powder;
s3: filling the mixed powder into a graphite mold with an inner diameter of 60mm, and then placing the graphite mold filled with the mixed powder into a vacuum degree of 6 x 10 -3 Hot-press sintering is carried out in a Pa vacuum hot-press sintering furnace, firstly, the temperature is raised to 1200 ℃ at the speed of 10 ℃/min, the temperature is kept for 1h, the axial pressure is applied to 45MPa, then the temperature is raised to 1700 ℃ at the speed of 5 ℃/min, the temperature is kept for 1h, then the temperature is kept for 3.5h after waiting to be reduced to 1400 ℃, then the die is taken out after unloading and cooling to the room temperature along with the furnace, the surface layer of the obtained sintered body after demoulding is processed to remove 0.4mm, and the Mo doped with MXene phase structure is obtained 2 Molybdenum alloy of C.
Example 2
Mo doped with MXene phase structure 2 The preparation method of the molybdenum alloy of C comprises the following steps:
s1: moS is carried out 2 、Na 2 CO 3 And the active carbon powder is prepared according to the mole ratio of 2:5:13 ball milling and mixing, then placing the mixture into a tubular furnace in argon atmosphere for heating reaction, heating to 875 ℃ at 8 ℃/min during the heating reaction, preserving heat for 2.5h, controlling Ar gas flow at 20mL/min, and obtaining reacted powder after the reaction; dispersing the reacted powder in ionized water to form suspension, centrifuging in a desk centrifuge for 4min at 4000r/min, and repeatedly centrifuging the suspension for 4 times until the pH value of the centrifugate is neutral; then vacuum drying is carried out to obtain the Mo of the MXene phase structure 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 The mass ratio of the powder C is 1:99, mixing, putting into a ball milling tank, introducing argon, putting into a planetary ball mill for ball milling and mixing, and setting the rotating speed of the ball mill to be 380r/min to obtain mixed powder;
s3: filling the mixed powder into a graphite mold with an inner diameter of 40mm, and then placing the graphite mold filled with the mixed powder into a vacuum degree of 7 x 10 -3 Heating to 1180 ℃ at a speed of 10 ℃/min, preserving heat for 1.5h, axially pressing for 43MPa, heating to 1600 ℃ at a speed of 5 ℃/min, preserving heat for 1h, waiting for cooling to 1500 ℃ and preserving heat for 4h, unloading, cooling to room temperature along with the furnace, taking out a die, and processing a sintered body obtained after demoulding to remove 0.4mm of a surface layer to obtain the Mo doped MXene phase structure 2 Molybdenum alloy of C.
Example 3
Mo doped with MXene phase structure 2 The preparation method of the molybdenum alloy of C comprises the following steps:
s1: moS is carried out 2 、Na 2 CO 3 And the active carbon powder is prepared according to the mole ratio of 2:4.2:11 ball milling and mixing, then placing the mixture into a tubular furnace in argon atmosphere for heating reaction, heating to 900 ℃ at 8 ℃/min during the heating reaction, preserving heat for 2.5h, controlling Ar gas flow at 20mL/min, and obtaining reacted powder after the reaction; dispersing the reacted powder in ionized water to form suspension, centrifuging in a desk centrifuge for 5min at a centrifuging speed of 3000r/min, and repeatedly centrifuging the suspension for 4 times until the pH value of the centrifugate is neutral; along with itThen vacuum drying is carried out to obtain the Mo with the MXene phase structure 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 The mass ratio of the powder C is 1.5:98.5, mixing, filling into a ball milling tank, introducing argon, putting into a planetary ball mill for ball milling and mixing, and setting the rotating speed of the ball mill to 390r/min to obtain mixed powder;
s3: filling the mixed powder into a graphite mold with an inner diameter of 30mm, and then placing the graphite mold filled with the mixed powder into a vacuum degree of 8 x 10 -3 Heating to 1195 ℃ at a speed of 10 ℃/min, preserving heat for 1.5h, axially pressing for 44MPa, heating to 1650 ℃ at a speed of 5 ℃/min, preserving heat for 40min, waiting to cool to 1470 ℃ and preserving heat for 3.2h, unloading, cooling to room temperature along with the furnace, taking out a die, and processing a sintered body obtained after demoulding to remove 0.4mm of a surface layer to obtain the Mo doped with the MXene phase structure 2 Molybdenum alloy of C.
Example 4
Mo doped with MXene phase structure 2 The preparation method of the molybdenum alloy of C comprises the following steps:
s1: moS is carried out 2 、Na 2 CO 3 And the active carbon powder is prepared according to the mole ratio of 2:4.6:10.4 ball milling and mixing, then placing the mixture into a tubular furnace in argon atmosphere for heating reaction, heating to 895 ℃ at 8 ℃/min during the heating reaction, preserving heat for 2.7h, controlling Ar gas flow at 20mL/min, and obtaining reacted powder after the reaction; dispersing the reacted powder in ionized water to form suspension, centrifuging in a desk centrifuge for 5min at a centrifuging speed of 3000r/min, and repeatedly centrifuging the suspension for 5 times until the pH value of the centrifugate is neutral; then vacuum drying is carried out to obtain the Mo of the MXene phase structure 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 The mass ratio of the powder C is 2:98, filling the mixture into a ball milling tank, introducing argon, putting the mixture into a planetary ball mill for ball milling and mixing, and setting the rotating speed of the ball mill to be 350r/min to obtain mixed powder;
s3: filling the mixed powder into a graphite mold with an inner diameter of 30mm, and then filling the graphite mold with the mixed powderWith a vacuum level of 8 x 10 -3 Heating to 1130 ℃ at a speed of 10 ℃/min, preserving heat for 2h, axially pressing for 42MPa, heating to 1650 ℃ at a speed of 5 ℃/min, preserving heat for 55min, waiting for cooling to 1450 ℃ and preserving heat for 3.8h, unloading, cooling to room temperature along with the furnace, taking out the die, processing a sintered body obtained after demoulding to remove 0.4mm of surface layer, and obtaining the Mo doped with MXene phase structure 2 Molybdenum alloy of C.
Example 5
Mo doped with MXene phase structure 2 The preparation method of the molybdenum alloy of C comprises the following steps:
s1: moS is carried out 2 、Na 2 CO 3 And the active carbon powder is prepared according to the mole ratio of 2:5:13 ball milling and mixing, then placing the mixture into a tubular furnace in argon atmosphere for heating reaction, heating to 950 ℃ at 8 ℃/min during heating reaction, preserving heat for 2 hours, controlling Ar gas flow at 20mL/min, and obtaining reacted powder after reaction; dispersing the reacted powder in ionized water to form suspension, centrifuging in a desk centrifuge for 3min at 4500r/min, and centrifuging for 6 times until the pH value of the centrifugate is neutral; then vacuum drying is carried out to obtain the Mo of the MXene phase structure 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 The mass ratio of the powder C is 3:100, mixing, putting into a ball milling tank, introducing argon, putting into a planetary ball mill, performing ball milling and mixing, and setting the rotating speed of the ball mill to be 370r/min to obtain mixed powder;
s3: filling the mixed powder into a graphite mold with an inner diameter of 60mm, and then placing the graphite mold filled with the mixed powder into a vacuum degree of 5 x 10 -3 Heating to 1150 ℃ at a speed of 10 ℃/min, preserving heat for 1.5h, axially pressing for 41MPa, heating to 1680 ℃ at a speed of 5 ℃/min, preserving heat for 20min, waiting for cooling to 1430 ℃ and preserving heat for 3.9h, unloading, cooling to room temperature along with the furnace, taking out a die, and processing a sintered body obtained after demoulding to remove 0.4mm of a surface layer to obtain the Mo doped with the MXene phase structure 2 Molybdenum alloy of C.
Will be described in detail below1 to example 5, the M.Xene-doped phase structure Mo 2 The molybdenum alloy of C was subjected to room temperature tensile test to obtain the MXene-doped phase structure Mo obtained in examples 1 to 5, respectively 2 The elongation and tensile strength of the molybdenum alloy of C are shown in table 1; as can be seen from Table 1, the MXene phase doped molybdenum alloy obtained by the application has better ductility and toughness.
Compared with pure molybdenum material, the MXene phase doped molybdenum alloy prepared by the method has the advantages that the room temperature tensile strength of the material is improved by more than 20 percent compared with that of the pure molybdenum material, and the room temperature elongation of the alloy is more than 1.7 times of that of the pure molybdenum.
Table 1: elongation and tensile Strength
The above is only for illustrating the technical idea of the present application, and the protection scope of the present application is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present application falls within the protection scope of the claims of the present application.
Claims (8)
1. Mo doped with MXene phase structure 2 The molybdenum alloy of C is characterized by comprising the following components in percentage by mass: 0.6 to 3 percent of MXene phase structure Mo 2 C powder, not more than 0.1% of impurities, and the balance of Mo powder, wherein the sum of mass fractions of the components is 100%;
mo of the MXene phase structure 2 The particle size of the powder C is 20 nm-1 mu m; the grain size of the Mo powder is 2-12 mu m.
2. A doped MXene phase structure Mo as defined in claim 1 2 The preparation method of the molybdenum alloy is characterized by comprising the following steps:
s1: moS is carried out 2 、Na 2 CO 3 Mixing with active carbon powder, placing into a heating furnace, heating in an oxygen-free environment for reaction to obtain reacted powder; after the reactionDispersing the powder in water to obtain suspension, centrifuging and drying to obtain MXene phase structure Mo 2 C, powder;
s2: mo powder and MXene phase structure Mo 2 Mixing the powder C, and performing ball milling mixing to obtain mixed powder;
s3: carrying out hot-pressing sintering on the mixed powder to obtain the Mo doped with the MXene phase structure 2 Molybdenum alloy of C.
3. An MXene phase structure Mo doped according to claim 2 2 A method for producing a molybdenum alloy of C, characterized in that in S1, the MoS 2 、Na 2 CO 3 And the molar ratio of the activated carbon powder is 2:4: 9-2: 5:13; the heating furnace is a tubular furnace, and the anaerobic environment is under argon atmosphere with argon flow of 20 mL/min; the technological parameters of the heating reaction are as follows: raising the temperature to 850-950 ℃ at 8 ℃/min, and then carrying out heat preservation reaction for 2-3 h.
4. An MXene phase structure Mo doped according to claim 2 2 The preparation method of the molybdenum alloy is characterized in that in S1, the drying is vacuum drying; the centrifugation is to repeatedly centrifuge the suspension for 3-6 times until the pH value of the centrifugate is neutral; the centrifugation is carried out in a desk centrifuge for 3-5 min, and the centrifugation speed is 3000-5000 r/min.
5. An MXene phase structure Mo doped according to claim 2 2 A process for producing a molybdenum alloy of C, characterized in that in S2, mo is in the MXene phase structure 2 The mass ratio of the C powder to the Mo powder is (0.6-3): (99.4-97).
6. An MXene phase structure Mo doped according to claim 2 2 The preparation method of the molybdenum alloy is characterized in that in S2, the ball milling and mixing are performed by using a Y-type planetary ball mill.
7. An MXene phase structure Mo doped according to claim 2 2 Molybdenum of CThe preparation method of the alloy is characterized in that in S3, the mixed powder is placed into a graphite mold, and then the graphite mold filled with the mixed powder is placed into a vacuum hot-press sintering furnace for hot-press sintering.
8. An MXene phase structure Mo doped according to claim 2 2 The preparation method of the molybdenum alloy is characterized in that in S3, the hot-pressed sintering process parameters are as follows: firstly heating to 1100-1200 ℃, preserving heat for 1-2 h, then axially pressing 40-45 MPa, heating to 1700 ℃ and preserving heat for 0.5-1 h, and then waiting for cooling to 1400-1500 ℃ and preserving heat and pressure for 3-4 h.
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