CN111593221A - Preparation method of high-performance molybdenum-scandium alloy and high-performance molybdenum-scandium alloy - Google Patents
Preparation method of high-performance molybdenum-scandium alloy and high-performance molybdenum-scandium alloy Download PDFInfo
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- 229910000542 Sc alloy Inorganic materials 0.000 title claims abstract description 33
- JMFBOACKZQRCDA-UHFFFAOYSA-N molybdenum scandium Chemical compound [Sc][Mo] JMFBOACKZQRCDA-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 25
- 238000011049 filling Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 61
- 229910002804 graphite Inorganic materials 0.000 claims description 61
- 239000010439 graphite Substances 0.000 claims description 61
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium(III) oxide Inorganic materials O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 23
- 230000008569 process Effects 0.000 claims description 18
- 239000011812 mixed powder Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 238000002490 spark plasma sintering Methods 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000005275 alloying Methods 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 21
- 229910045601 alloy Inorganic materials 0.000 abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 11
- 229910001182 Mo alloy Inorganic materials 0.000 abstract description 8
- 239000011733 molybdenum Substances 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000009467 reduction Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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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
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- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a high-performance molybdenum-scandium alloy and the high-performance molybdenum-scandium alloy. The method comprises five steps of material composition design, material mixing, grinding, powder filling and pressing and sintering. Compared with other rare earth oxides, the second phase in the invention has good strengthening effect, can effectively improve the hardness of the molybdenum alloy, and simultaneously effectively reduces the friction loss of the alloy at room temperature; the method uses SPS sintering, can improve the sintering efficiency, reduce the sintering time and the sintering temperature, reduce the growth time of molybdenum crystal grains to a certain extent, and play a role in further refining the crystal grains; Mo-Sc prepared by the method of the invention2O3The hardness of the alloy is improved at room temperature. The invention prepares molybdenum with strength and high-temperature antifriction property superior to pure molybdenum alloy on the basis of SPS technologyAn alloy of scandium.
Description
Technical Field
The invention relates to the technical field of molybdenum alloy materials, in particular to a preparation method of a molybdenum-scandium alloy and a high-performance molybdenum-scandium alloy.
Background
Molybdenum is a non-renewable important strategic resource and has the characteristics of high melting point, high-temperature strength, small thermal expansion coefficient, good heat conduction and electric conduction and thermal shock resistance, thermal fatigue resistance and the like. The molybdenum product is widely applied to the fields of steel, nonferrous metal, petroleum, chemical industry, electronics, national defense, aerospace, nuclear industry and the like. However, molybdenum metal has the inherent low temperature brittleness and ductile-brittle transition characteristics of body-centered cubic metal, which limits its wider use as a structural material. The performance of the molybdenum-based material can be effectively improved through alloying, but the high temperature can promote the grain growth of the molybdenum alloy, the traditional preparation method has complex process and longer sintering time, and is difficult to obtain the molybdenum alloy with fine grains, the molybdenum alloy prepared by the method has larger brittleness and lower hardness, the doped second phase is also larger, and the performance of the alloy is further reduced.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention aims to provide a method for preparing a molybdenum-scandium alloy with high strength and good performance, and a molybdenum-scandium alloy.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of a high-performance molybdenum-scandium alloy comprises the following steps:
(1) designing the material composition: according to the mass fraction percentage, the used material comprises 97 to 99.5 percent of Mo and 0.5 percent of MoSc of 3% or more2O3；
(2) Mixing materials: mixing the components according to the material composition in the step (1) to obtain mixed powder; the microstructure of the mixed powder is nearly spherical, the average particle size is 3-5 mu m, and the Mo powder and the Sc powder2O3The mass ratio of (97-99.5) to (0.5-3.0);
(3) grinding: grinding the mixed powder obtained in the step (2) for 3-7 hours, and filling protective atmosphere;
(4) powder filling: fixing powder for forming by a set of graphite die, wherein the component of the die is graphite without other impurities, the die comprises an upper pressure head, a lower pressure head and a hollow female die with a temperature measuring hole, the upper pressure head and the lower pressure head have the same structure and are both columnar structures, the graphite female die is a sleeve-shaped hollow structure, and the side wall of the graphite female die is provided with the temperature measuring hole; inserting a lower pressure head into an inner hole of the female die, placing a graphite sheet, filling the mixed powder obtained in the step (3) into the lower pressure head in the female die, similarly placing the graphite sheet, inserting an upper pressure head into the inner hole from the upper part of the female die, and tightly pressing the mixed powder through the upper pressure head and the lower pressure head;
(5) and (3) pressure sintering: placing the die to be sintered obtained in the step (4) into a hearth of a spark plasma sintering system, and extracting air in the furnace to a vacuum state; then, adjusting a pressure system to ensure that the pressure head keeps constant pressure on the die; then, current is introduced to sinter the metal powder to obtain Mo-Sc2O3And (3) alloying.
Furthermore, the upper pressure head and the lower pressure head are both cylindrical structures with the diameter of 30mm and the height of 35mm, the graphite female die is of a sleeve-shaped hollow structure with the outer diameter of 60mm, the inner diameter of 30mm and the height of 50mm, temperature measuring holes with the diameter of 4mm and the depth of 5mm are formed in the middle height position of the graphite female die, and the graphite sheets are graphite wafers with the diameter of 30 mm.
Furthermore, the ball-material ratio during grinding is 10: 1, ball milling speed is 200-.
Furthermore, absolute ethyl alcohol is added in the grinding process.
Furthermore, the graphite mold and the graphite wafer have the same components and do not contain other impurities.
Further, the interior of the sintering furnace is sealed and vacuumized to the vacuum degree of less than 1.0 × 10 before sintering-1Pa, the set mechanical pressure is 30MPa, the sintering temperature is 1400-1500 ℃, the preferred temperature is 1400 ℃, and the heating and cooling rate is 110-.
Further, the sintering temperature was 1400 ℃.
The high-performance molybdenum-scandium alloy is Mo-Sc obtained by the preparation method2O3And (3) alloying.
The invention has the following beneficial effects:
(1) compared with other rare earth oxides, the second phase in the invention has good strengthening effect, can effectively improve the hardness of the molybdenum alloy, and simultaneously effectively reduces the friction loss of the alloy at room temperature.
(2) The invention uses SPS sintering, can improve sintering efficiency, reduce sintering time and sintering temperature, reduce the growth time of molybdenum crystal grains to a certain extent, and play a role in further refining the crystal grains.
(3) Mo-Sc prepared by the method of the invention2O3The hardness of the alloy is improved at room temperature.
Drawings
FIG. 1 is a flow diagram of a sintering process of the present invention;
FIG. 2 is a graph of a sintering process of the present invention;
fig. 3 is a scanning electron microscope image of example 1, example 2, example 3, example 4.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The preparation method of the high-performance molybdenum-scandium alloy is shown in figure 1, and comprises the following specific preparation steps:
(1) designing the material composition: according to the mass fraction percentage, the used material comprises 97 to 99.5 percent of Mo and 0.5 to 3 percent of Sc2O3；
(2) Mixing materials: the material according to the step (1)Material composition, mixing the components to obtain mixed powder; mo powder and Sc2O3The microstructure of the powder is spherical-like, the average size is 3-5 mu m, and the Mo powder and the Sc powder2O3The mass ratio of (97-99.5) to (0.5-3.0);
(3) grinding: mechanically grinding the mixed powder obtained in the step (2) in a mechanical grinding device for 3-7 hours, filling argon as a protective atmosphere during grinding for preventing impurities in air, and adding a little absolute ethyl alcohol during grinding to prevent the powder from adhering to the wall; the mechanical grinding process can uniformly disperse the two kinds of powder, is beneficial to subsequent sintering, and simultaneously uses argon gas for protection to avoid the powder from mixing other impurities during ball milling; the ball material ratio during grinding is 10: 1, ball milling at the speed of 200-;
(4) powder filling: in the invention, powder forming is fixed by a set of graphite die, the die comprises an upper pressure head, a lower pressure head and a hollow female die with a temperature measuring hole, the upper pressure head and the lower pressure head have the same structure and are of cylindrical structures with the diameter of 30mm and the height of 35mm, the graphite female die is of a sleeve-shaped hollow structure with the outer diameter of 60mm, the inner diameter of 30mm and the height of 50mm, and the graphite female die is provided with the temperature measuring hole with the diameter of 4mm and the depth of 5mm at the middle height position. Inserting the lower pressure head into one part of an inner hole of the female die, putting 1 to 2 graphite wafers with the diameter of 30mm to prevent the pressure head from being damaged in the sintering process, then filling the mixed powder obtained in the step (3) into the lower pressure head in the female die, putting 1 to 2 graphite wafers with the diameter of 30mm into the lower pressure head, inserting the upper pressure head into the inner hole from the upper part of the female die, and pressing the mixed metal powder tightly through the upper pressure head and the lower pressure head; the graphite mold is specially manufactured for SPS sintering, and the main component of the graphite mold is graphite without other impurities; the graphite wafer is added, so that sintering is promoted, and the phenomenon of bonding between a sintered alloy and a pressure head is prevented;
(5) and (3) pressure sintering: placing the die to be sintered obtained in the step (4) into a hearth of a spark plasma sintering system, and extracting air in the furnace to a vacuum state, thereby preventing molybdenum powder from being oxidized in the sintering process during sintering on one hand, and on the other hand, being capable of preventing molybdenum powder from being oxidized in the sintering process during sinteringCan promote the elimination of gas generated in the sintering process and the proceeding of the sintering densification process. Then, adjusting a pressure system to enable a pressure head to keep constant pressure on the die to promote powder forming, then introducing current to sinter the metal powder, wherein the sintering process curve is shown in figure 2, and Mo-Sc is obtained2O3Sealing the interior of the sintering furnace before sintering, and vacuumizing until the vacuum degree is less than 1.0 × 10- 1Pa, the set mechanical pressure is 30MPa, the sintering temperature is 1400-1500 ℃, the preferred temperature is 1400 ℃, and the heating and cooling rate is 110-. In the sintering process, the influence of elements in the air, particularly oxygen elements, on the sintering can be avoided by a smaller vacuum degree, and higher sintering performance can be ensured by higher sintering pressure and lower sintering temperature.
The invention can rapidly sinter by a Spark Plasma Sintering (SPS) method, avoids molybdenum crystal grain growth during sintering, can prepare the molybdenum scandium alloy at a lower sintering temperature, and has fine spherical Sc during sintering2O3Can effectively organize the grain boundary migration of molybdenum grains, refine the grains, purify the grain boundary, block the dislocation movement and play a role in pinning, and the Sc2O3The grains have less tendency to concentrate stress in interaction with dislocations, reducing the likelihood of cracking of the alloy at the grain boundaries.
In this description, the friction and wear test is given in the following examples, and the test procedure is as follows: for an alumina ball with a grinding ball of 6.5mm, a reciprocating type friction and wear form is adopted to carry out a friction and wear experiment on the alloy, and the experimental process conditions are as follows: the test load was 10N, the single stroke 5mm, the rubbing time 30min, and the experiment was carried out at room temperature.
Example 1
The molybdenum-scandium alloy of the embodiment comprises the following chemical components in percentage by mass: mo: 99.5% of Sc2O3：0.5％。
Firstly, pretreating Mo powder and Sc2O3The powder is mixed according to the mass ratio of 99.5: proportioning according to the proportion of 0.5. Mixing in a planetary ball mill at a ball material ratio of 10: 1, grinding for 5 hr, adding a little anhydrous ethanol during grinding to prevent powder from stickingA wall;
secondly, making a graphite mold, filling 1-2 graphite wafers with the diameter of 30mm, and processing the well processed Mo-Sc2O3The alloy powder is put into a graphite female die from bottom to top, 1-2 graphite wafers with the diameter of 30mm are filled in the graphite female die, and then the graphite female die is tightly pressed by an upper pressing head and a lower pressing head to prevent the powder from leaking;
thirdly, sintering, placing the graphite mold to be sintered in a hearth of a spark plasma sintering system, and vacuumizing to be not higher than 1.0 × 10-1Pa, then introducing direct current pulse current to Mo-Sc2O3The alloy powder is sintered and bonded, and the sintering process comprises the following steps: the axial pressure of the upper pressure head and the lower pressure head on the iron base and the metal powder is 30 MPa; the heating rate is as follows: 110 ℃/min from the room temperature region to 900 ℃, and 125 ℃/min from 900 ℃ to the sintering temperature; the heat preservation time is 6 min; the cooling rate is: the temperature reduction rate of the interval from the sintering temperature to 600 ℃ is 115 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and after cooling, the molybdenum-scandium alloy is successfully prepared, and the hardness of the alloy is better.
Example 2
The molybdenum-scandium alloy of the embodiment comprises the following chemical components in percentage by mass: mo: 99% of Sc2O3：1.0％。
Firstly, pretreating Mo powder and Sc2O3The powder is prepared from the following components in percentage by mass 99: 1, proportioning. Mixing the materials in a ball mill according to the ball material ratio of 10: 1, grinding for 5 hours, and adding a little absolute ethyl alcohol during grinding to prevent the powder from sticking to the wall;
secondly, making a graphite mold, filling 1-2 graphite wafers with the diameter of 30mm, and processing the well processed Mo-Sc2O3The alloy powder is put into a graphite female die from bottom to top, 1-2 graphite wafers with the diameter of 30mm are filled in the graphite female die, and then the graphite female die is tightly pressed by an upper pressing head and a lower pressing head to prevent the powder from leaking;
thirdly, sintering, placing the graphite mold to be sintered in a hearth of a spark plasma sintering system, and vacuumizing to be not higher than 1.0 × 10-1Pa, then introducing direct current pulse current to Mo-Sc2O3The alloy powder is sintered and bonded, and the sintering process comprises the following steps: of iron-based and metal powders with upper and lower indentersThe axial pressure is 30 MPa; the heating rate is as follows: 110 ℃/min from the room temperature region to 900 ℃, and 125 ℃/min from 900 ℃ to the sintering temperature; the heat preservation time is 6 min; the cooling rate is: the temperature reduction rate of the interval from the sintering temperature to 600 ℃ is 115 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and after cooling, the molybdenum-scandium alloy is successfully prepared, and the hardness of the alloy is better.
Example 3
The molybdenum-scandium alloy of the embodiment comprises the following chemical components in percentage by mass: mo: 98.5% of Sc2O3：1.5％。
Firstly, pretreating Mo powder and Sc2O3The powder is mixed according to the mass ratio of 98.5: 1.5. Mixing the materials in a ball mill according to the ball material ratio of 10: 1, grinding for 5 hours, and adding a little absolute ethyl alcohol during grinding to prevent the powder from sticking to the wall;
secondly, making a graphite mold, filling 1-2 graphite wafers with the diameter of 30mm, and processing the well processed Mo-Sc2O3The alloy powder is put into a graphite female die from bottom to top, 1-2 graphite wafers with the diameter of 30mm are filled in the graphite female die, and then the graphite female die is tightly pressed by an upper pressing head and a lower pressing head to prevent the powder from leaking;
thirdly, sintering, placing the graphite mold to be sintered in a hearth of a spark plasma sintering system, and vacuumizing to be not higher than 1.0 × 10-1Pa, then introducing direct current pulse current to Mo-Sc2O3The alloy powder is sintered and bonded, and the sintering process comprises the following steps: the axial pressure of the upper pressure head and the lower pressure head on the iron base and the metal powder is 30 MPa; the heating rate is as follows: 110 ℃/min from the room temperature region to 900 ℃, and 125 ℃/min from 900 ℃ to the sintering temperature; the heat preservation time is 6 min; the cooling rate is: the temperature reduction rate of the interval from the sintering temperature to 600 ℃ is 115 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and after cooling, the molybdenum-scandium alloy is successfully prepared, and the hardness of the alloy is better.
Example 4
The molybdenum-scandium alloy of the embodiment comprises the following chemical components in percentage by mass: mo: 97% of Sc2O3：3.0％。
Firstly, pretreating Mo powder and Sc2O3Powder ofAccording to the mass ratio of 97: 3, proportioning. Mixing the materials in a ball mill according to the ball material ratio of 10: 1, grinding for 5 hours, and adding a little absolute ethyl alcohol during grinding to prevent the powder from sticking to the wall;
secondly, making a graphite mold, filling 1-2 graphite wafers with the diameter of 30mm, and processing the well processed Mo-Sc2O3The alloy powder is put into a graphite female die from bottom to top, 1-2 graphite wafers with the diameter of 30mm are filled in the graphite female die, and then the graphite female die is tightly pressed by an upper pressing head and a lower pressing head to prevent the powder from leaking;
thirdly, sintering, placing the graphite mold to be sintered in a hearth of a spark plasma sintering system, and vacuumizing to be not higher than 1.0 × 10-1Pa, then introducing direct current pulse current to Mo-Sc2O3The alloy powder is sintered and bonded, and the sintering process comprises the following steps: the axial pressure of the upper pressure head and the lower pressure head on the iron base and the metal powder is 30 MPa; the heating rate is as follows: 110 ℃/min from the room temperature region to 900 ℃, and 125 ℃/min from 900 ℃ to the sintering temperature; the heat preservation time is 6 min; the cooling rate is: the temperature reduction rate of the interval from the sintering temperature to 600 ℃ is 115 ℃/min, and the interval from 600 ℃ to room temperature is cooled along with the furnace; and after cooling, the molybdenum-scandium alloy is successfully prepared, and the hardness of the alloy is better.
The sem images of examples 1, 2, 3, and 4 are shown in fig. 3, and the relevant parameters are shown in the following table.
TABLE 1 conditions of the respective implementation parameters
| Average grain size/. mu.m | Relative density/% | Vickers hardness/HV | Coefficient of friction at room temperature | |
| Example 1 | 2.23 | 96.7 | 349.7 | 0.434 |
| Example 2 | 1.68 | 97 | 358.9 | 0.327 |
| Example 3 | 1.72 | 97.3 | 360.6 | 0.318 |
| Example 4 | 2.56 | 97.5 | 374.1 | 0.490 |
In summary, the method for preparing a high performance molybdenum-scandium alloy according to the present invention prepares a molybdenum-scandium alloy having better strength and better high temperature wear reduction than the pure molybdenum alloy based on SPS technology, and the examples of the present invention are merely to describe the preferred embodiments of the present invention, and do not limit the concept and scope of the present invention, and various modifications and improvements made to the technical solutions of the present invention by the engineers in the art without departing from the design concept of the present invention shall fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of a high-performance molybdenum-scandium alloy comprises the following steps:
(1) designing the material composition: according to the mass fraction percentage, the used material comprises 97 to 99.5 percent of Mo and 0.5 to 3 percent of Sc2O3；
(2) Mixing materials: mixing the components according to the material composition in the step (1) to obtain mixed powder; the microstructure of the mixed powder is nearly spherical, the average particle size is 3-5 mu m, and the mass ratio of the Mo powder to the Sc2O3 is (97-99.5): 0.5-3.0;
(3) grinding: grinding the mixed powder obtained in the step (2) for 3-7 hours, and filling protective atmosphere;
(4) powder filling: fixing powder for forming by a set of graphite die, wherein the component of the die is graphite without other impurities, the die comprises an upper pressure head, a lower pressure head and a hollow female die with a temperature measuring hole, the upper pressure head and the lower pressure head have the same structure and are both columnar structures, the graphite female die is a sleeve-shaped hollow structure, and the side wall of the graphite female die is provided with the temperature measuring hole; inserting a lower pressure head into an inner hole of the female die, placing a graphite sheet, filling the mixed powder obtained in the step (3) into the lower pressure head in the female die, similarly placing the graphite sheet, inserting an upper pressure head into the inner hole from the upper part of the female die, and tightly pressing the mixed powder through the upper pressure head and the lower pressure head;
(5) and (3) pressure sintering: placing the die to be sintered obtained in the step (4) into a hearth of a spark plasma sintering system, and extracting air in the furnace to a vacuum state; then, adjusting a pressure system to ensure that the pressure head keeps constant pressure on the die; then, current is introduced to sinter the metal powder to obtain Mo-Sc2O3And (3) alloying.
2. The preparation method of the high-performance molybdenum-scandium alloy according to claim 1, wherein the upper pressure head and the lower pressure head are both cylindrical structures with a diameter of 30mm and a height of 35mm, the graphite female die is a sleeve-shaped hollow structure with an outer diameter of 60mm, an inner diameter of 30mm and a height of 50mm, a temperature measuring hole with a diameter of 4mm and a depth of 5mm is formed in the middle height position of the graphite female die, and the graphite sheet is a graphite wafer with a diameter of 30 mm.
3. The method for preparing the high-performance molybdenum-scandium alloy according to claim 1, wherein a ball-to-feed ratio during grinding is 10: 1, ball milling speed is 200-.
4. The method for preparing a high-performance molybdenum-scandium alloy according to claim 1, wherein absolute ethyl alcohol is added during the grinding process.
5. The method for preparing a high-performance molybdenum-scandium alloy according to claim 1, wherein the graphite mold and the graphite wafer are the same in composition and do not contain other impurities.
6. The method for preparing the high-performance molybdenum-scandium alloy according to claim 1, wherein an interior of the sintering furnace is closed and vacuumized to a degree of vacuum of less than 1.0 × 10 before sintering-1Pa, the set mechanical pressure is 30MPa, the sintering temperature is 1400-1500 ℃, the preferred temperature is 1400 ℃, and the heating and cooling rate is 110-.
7. The method for producing a high performance molybdenum scandium alloy according to claim 1, wherein the sintering temperature is 1400 ℃.
8. A high performance molybdenum scandium alloy, characterized in that it is Mo-Sc obtained by the method according to any one of claims 1 to 72O3And (3) alloying.
Priority Applications (1)
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