CN114807704B - Mg-containing 2 Sn and Al 3 Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases and preparation method thereof - Google Patents
Mg-containing 2 Sn and Al 3 Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases and preparation method thereof Download PDFInfo
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- CN114807704B CN114807704B CN202210293357.8A CN202210293357A CN114807704B CN 114807704 B CN114807704 B CN 114807704B CN 202210293357 A CN202210293357 A CN 202210293357A CN 114807704 B CN114807704 B CN 114807704B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 174
- 239000000956 alloy Substances 0.000 title claims abstract description 174
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 50
- 229910052718 tin Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011777 magnesium Substances 0.000 claims abstract description 95
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 41
- 238000003723 Smelting Methods 0.000 claims abstract description 34
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 34
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 31
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012535 impurity Substances 0.000 claims abstract description 28
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 230000032683 aging Effects 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims description 27
- 229910052751 metal Inorganic materials 0.000 claims description 27
- 239000002184 metal Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 15
- 238000005266 casting Methods 0.000 claims description 15
- 230000001681 protective effect Effects 0.000 claims description 15
- 239000006104 solid solution Substances 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 13
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000007670 refining Methods 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 6
- 229910001626 barium chloride Inorganic materials 0.000 claims description 6
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 4
- 239000000203 mixture Substances 0.000 claims 3
- 238000000034 method Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 229910000542 Sc alloy Inorganic materials 0.000 description 22
- 238000001816 cooling Methods 0.000 description 12
- 239000004615 ingredient Substances 0.000 description 12
- 238000005728 strengthening Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 10
- 238000004090 dissolution Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910003023 Mg-Al Inorganic materials 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 229910019743 Mg2Sn Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910019021 Mg 2 Sn Inorganic materials 0.000 description 1
- 229910000691 Re alloy Inorganic materials 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
-
- 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
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention provides a Mg-containing alloy 2 Sn and Al 3 The novel Mg-Al-Sn-Sc series alloy of Sc double heat-resistant phase and the preparation method thereof, the alloy comprises the following components in percentage by weight: 3.0-9.0wt% of aluminum Al, 3.0-7.0wt% of tin Sn, 0.1-1.0wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements, by adopting the alloy proportioning and smelting method provided by the invention and combining the step-by-step solution treatment and the step-by-step aging treatment, the distribution of alloy crystal grains and precipitated phase structure can be effectively improved, and the alloy strength under the high temperature resistant condition can be improved.
Description
Technical Field
The invention belongs to the field of nonferrous metal materials and metallurgy, and in particular relates to a metal alloy containing Mg 2 Sn and Al 3 Novel Mg-Al-Sn-Sc series alloy of Sc double heat-resistant phase and a preparation method thereof.
Background
The magnesium aluminum alloy is used as one of important magnesium alloy systems, has low density and excellent mechanical properties, is a main development object of the magnesium alloy at present, such as typical AZ91, AM61 and the like, and is already applied to the fields of automobiles, aerospace, sports equipment and the like.
The alloy depends on Mg 17 Al 12 The phase improves the room temperature strength of the alloy, but Mg 17 Al 12 The high temperature resistance of the phase is insufficient (the dissolution temperature is 437 ℃), the temperature exceeds 100 ℃ in the using process, the strengthening effect is seriously reduced, and the development of the Mg-Al alloy is seriously limited due to the poor heat resistance.
To improve the high temperature resistance of magnesium alloys, mg—sn alloys (publication No. CN201010291241.8; CN 201210334273.0) and mg—re alloys (publication No. CN201711003940.6; CN 201711003938.9) were developed successively, and it was not difficult to find that these alloy series each contain Mg2Sn phase (dissolution temperature: 561 ℃) which is excellent in heat resistance, mg—re phase (Al) 3 Y phase dissolution temperature is 567 ℃, mg 5 Gd phase dissolution temperature is 548 ℃ C.) or indissolvable XMgSn phase. The higher the solubility of the second phase in the matrix, the more excellent the high temperature strengthening effect of the alloy.
However, the alloy in the prior art has single dependence on strengthening mechanism, lacks perfect material proportion and a proper smelting method, so that the strength of the Mg-Al alloy is not high enough, and especially the strength under the condition of high temperature resistance can not meet the use requirement. Therefore, how to solve the problem of uniform grain distribution in the Mg-Al alloy smelting process, fully exert the synergistic effect of a multi-element strengthening mechanism and improve the heat resistance strength of the alloy, and the technical problem to be solved by the technicians in the field is urgent.
Disclosure of Invention
In view of the above, the present invention provides a novel Mg-Al-Sn-Sc alloy and a method for manufacturing the same, comprising:
mg-containing 2 Sn and Al 3 The novel Mg-Al-Sn-Sc series alloy of the Sc double heat-resistant phase is characterized by comprising the following alloy components in percentage by weight: 3.0 to 9.0 weight percent of aluminum Al, 3.0 to 7.0 weight percent of tin Sn, 0.1 to 1.0 weight percent of scandium Sc, and the balance of magnesium Mg and uncontrollable impurity elements.
Specifically, the mass percentage of aluminum Al is 3.12% or 4.04% or 6.1% or 5.03% or 6.81% or 8.99%.
Specifically, the mass percentage of the tin Sn is 3.51% or 3.13% or 3.48% or 5.53% or 5.64% or 6.87%.
Specifically, the scandium Sc is 0.51% or 0.53% or 0.6% or 0.83% or 0.82% or 0.93% by mass.
Specifically, the alloy comprises one of the following components in percentage by weight:
3.12wt% of aluminum Al,3.51 wt% of tin Sn,0.51 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
4.04wt% of aluminum Al, 3.13wt% of tin Sn,0.53 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6.1wt% of aluminum Al,3.48 wt% of tin Sn,0.6 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
5.03 weight percent of aluminum Al,5.53 weight percent of tin Sn,0.83 weight percent of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6.81wt% of aluminum Al,5.64 wt% of tin Sn,0.82 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6 parts of combination, 8.99% by weight of aluminum Al,6.87% by weight of tin Sn,0.93% by weight of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements.
Mg-containing 2 Sn and Al 3 The preparation method of the novel Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps:
s1: raw material weighing
Raw materials are prepared according to the alloy proportion in the Mg-Al-Sn-Sc series alloy, and the raw materials comprise magnesium Mg, tin Sn, aluminum Al and intermediate alloy;
s2: preheating and charging
S2-1, placing the raw materials obtained in the step S1 and a casting mold in an environment of 300 ℃ for drying and preheating for 30min;
s2-2, raising the temperature of the smelting furnace to 300 ℃, introducing a protective gas into the furnace, and keeping the temperature for 15min;
s2-3, placing the preheated raw materials of Mg, al and intermediate alloy in the step S2-1 into a metal crucible in a smelting furnace;
s3, smelting
S3-1, raising the temperature of the smelting furnace to 710-715 ℃, and preserving heat for 10-15min;
s3-2, adding the preheated raw material Sn in the step S2, and simultaneously raising the furnace temperature to 735-750 ℃ and keeping for 5-10min;
s3-3, adding a magnesium alloy refining agent and a deslagging agent, and simultaneously stirring for the first time;
s3-4, reducing the furnace temperature to 700 ℃, stirring for the second time, and simultaneously removing waste residues on the surface of the liquid alloy;
s4, pouring
Pouring the liquid alloy finally obtained in the step S3-4 into a pouring mold which is preheated in the step S2, wherein the actual temperature of the pouring mold is higher than 150 ℃ to obtain an as-cast alloy;
s5: step-by-step solid solution treatment;
s5: and (5) step aging treatment.
Specifically, the step S5 step solid solution treatment comprises
S5-1:1 section heat preservation
Placing the as-cast alloy obtained in the step S4 at 400 ℃ and introducing argon into the environment to be protected for 4-8 hours to finish homogenization treatment;
s5-2: 2-section heat preservation
Placing the as-cast alloy obtained in the step S5-1 at 450 ℃ and introducing argon into an air-protecting environment for 12-16 hours to finish primary solution treatment;
s5-3: 3-section heat preservation
Placing the as-cast alloy obtained in the step S5-2 at 500 ℃ and introducing argon into an air-protecting environment for 2-3 hours to complete all solid solution treatment;
specifically, the step S6 step aging treatment includes:
s6-1, placing the as-cast alloy obtained in the step S5-3 in an environment of 120-140 ℃ for 10-20 hours;
s6-2, placing the as-cast alloy in an environment of 180-200 ℃ for 120-130 hours to obtain a fine and uniform Mg2Sn precipitated phase.
Specifically, the intermediate alloy is Mg-6% Sc.
Preferably, the magnesium alloy refining agent is 60% of potassium chloride, 5% of calcium fluoride, 5% of sodium chloride, 15% of calcium chloride and 15% of barium chloride;
the slag remover comprises 40% of potassium chloride, 40% of magnesium chloride, 6% of sodium chloride, 6% of calcium fluoride and 8% of barium chloride.
Specifically, the protective gas introduced into the furnace in the step S2-2 is 99% CO 2 With 1% SF 6 Is a mixed gas of (a) and (b).
The alloy proportion and smelting mode provided by the invention have the following beneficial effects: (1) The Mg-Al alloy has uniform alloy structure and refined crystal grains by introducing Sn and Sc elements, and simultaneously forms Al 3 Sc (dissolution temperature 569 ℃ C.) and Mg 2 A heat-resistant high-temperature phase of Sn (dissolution temperature: 561 ℃ C.), and realizes coexistence of a second phase and a precipitated phase; (2) The strength of the alloy, especially the high-temperature resistant strength, is improved by the synergistic effect of aging strengthening, fine-grain strengthening and second-phase strengthening multi-element strengthening means. The technology of the invention has good popularization value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required 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 of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a metallographic structure of an Mg-5Al-5.5Sn-0.8Sc alloy;
FIG. 2 shows the transmission structure of the precipitated phase of Mg-5Al-5.5Sn-0.8Sc alloy.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention discloses a novel Mg-Al-Sn-Sc series alloy and a manufacturing method thereof, which comprises the following steps:
mg-containing 2 Sn and Al 3 The novel Mg-Al-Sn-Sc series alloy of the Sc double heat-resistant phase comprises the following alloy components in percentage by weight: 3.0 to 9.0 weight percent of aluminum Al, 3.0 to 7.0 weight percent of tin Sn, 0.1 to 1.0 weight percent of scandium Sc, and the balance of magnesium Mg and uncontrollable impurity elements.
Specifically, the mass percentage of aluminum Al is 3.12% or 4.04% or 6.1% or 5.03% or 6.81% or 8.99%.
Specifically, the mass percentage of the tin Sn is 3.51% or 3.13% or 3.48% or 5.53% or 5.64% or 6.87%.
Specifically, the scandium Sc is 0.51% or 0.53% or 0.6% or 0.83% or 0.82% or 0.93% by mass.
Specifically, the alloy comprises one of the following components in percentage by weight:
3.12wt% of aluminum Al,3.51 wt% of tin Sn,0.51 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
4.04wt% of aluminum Al, 3.13wt% of tin Sn,0.53 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6.1wt% of aluminum Al,3.48 wt% of tin Sn,0.6 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
5.03 weight percent of aluminum Al,5.53 weight percent of tin Sn,0.83 weight percent of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6.81wt% of aluminum Al,5.64 wt% of tin Sn,0.82 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6 parts of combination, 8.99% by weight of aluminum Al,6.87% by weight of tin Sn,0.93% by weight of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements.
Mg-containing 2 Sn and Al 3 The preparation method of the novel Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps:
s1: raw material weighing
Raw materials are prepared according to the alloy proportion in the Mg-Al-Sn-Sc series alloy, and the raw materials comprise magnesium Mg, tin Sn, aluminum Al and intermediate alloy;
s2: preheating and charging
S2-1, placing the raw materials obtained in the step S1 and a casting mold in an environment of 300 ℃ for drying and preheating for 30min;
s2-2, raising the temperature of the smelting furnace to 300 ℃, introducing a protective gas into the furnace, and keeping the temperature for 15min;
s2-3, placing the preheated raw materials of Mg, al and intermediate alloy in the step S2-1 into a metal crucible in a smelting furnace;
s3, smelting
S3-1, raising the temperature of the smelting furnace to 710-715 ℃, and preserving heat for 10-15min;
s3-2, adding the preheated raw material Sn in the step S2, and simultaneously raising the furnace temperature to 735-750 ℃ and keeping for 5-10min;
s3-3, adding a magnesium alloy refining agent and a deslagging agent, and simultaneously stirring for the first time;
s3-4, reducing the furnace temperature to 700 ℃, stirring for the second time, and simultaneously removing waste residues on the surface of the liquid alloy;
s4, pouring
Pouring the liquid alloy finally obtained in the step S3-4 into a pouring mold which is preheated in the step S2, wherein the actual temperature of the pouring mold is higher than 150 ℃ to obtain an as-cast alloy;
s5: step-by-step solid solution treatment;
s5: and (5) step aging treatment.
Specifically, the step S5 step solid solution treatment comprises
S5-1:1 section heat preservation
Placing the as-cast alloy obtained in the step S4 at 400 ℃ and introducing argon into the environment to be protected for 4-8 hours to finish homogenization treatment;
s5-2: 2-section heat preservation
Placing the as-cast alloy obtained in the step S5-1 at 450 ℃ and introducing argon into an air-protecting environment for 12-16 hours to finish primary solution treatment;
s5-3: 3-section heat preservation
Placing the as-cast alloy obtained in the step S5-2 at 500 ℃ and introducing argon into an air-protecting environment for 2-3 hours to complete all solid solution treatment;
specifically, the step S6 step aging treatment includes:
s6-1, placing the as-cast alloy obtained in the step S5-3 in an environment of 120-140 ℃ for 10-20 hours;
s6-2, placing the as-cast alloy in an environment of 180-200 ℃ for 120-130 hours to obtain fine and uniform Mg 2 And Sn precipitates.
Specifically, the intermediate alloy is Mg-6% Sc.
Preferably, the magnesium alloy refining agent is 60% of potassium chloride, 5% of calcium fluoride, 5% of sodium chloride, 15% of calcium chloride and 15% of barium chloride;
the slag remover comprises 40% of potassium chloride, 40% of magnesium chloride, 6% of sodium chloride, 6% of calcium fluoride and 8% of barium chloride.
Specifically, the protective gas introduced into the furnace in the step S2-2 is 99% CO 2 With 1% SF 6 Is a mixed gas of (a) and (b).
For further explanation of the inventive arrangements, the invention provides 6 specific embodiments.
Example 1:
the alloy component ingredients are prepared from the following components in percentage by mass: 3.12% of Al,3.51% of Sn,0.51% of Sc and the balance of magnesium (Mg) and uncontrollable impurity elements, and the alloy smelting and performance testing operations are as follows:
raw materials, namely high-purity Mg, high-purity Sn and high-purity Al, are weighed according to the corresponding alloy proportion in the Mg-Al-Sn-Sc series alloy, and the Mg-6% Sc intermediate alloy and a casting die are dried and preheated for 30min at 300 ℃; after the temperature of a smelting furnace is raised to 300 ℃, shielding gas (the shielding atmosphere is 99 percent CO2 plus 1 percent SF6 mixed gas) is introduced into the furnace for about 15 minutes, then high-purity Mg, high-purity Al and Mg-6 percent Sc intermediate alloy ingredients are put into a metal crucible of the smelting furnace, the furnace temperature is raised to 710 ℃, the temperature is kept for 15 minutes, pure Sn is added into an alloy melt after metal is melted, the furnace temperature is raised to 735 ℃ and the temperature is kept for 8 minutes, and then a proper amount of magnesium alloy refining agent and covering agent are added for primary stirring; cooling the furnace temperature to 700 ℃ after stirring, stirring for the second time, and simultaneously removing waste residues on the surface of the alloy; and pouring the liquid alloy into a metal mold, preheating the metal mold to 300 ℃, and naturally cooling after casting to obtain the as-cast alloy. Homogenizing and solution treating an as-cast Mg-Al-Sn-Sc alloy, wherein the as-cast Mg-Al-Sn-Sc alloy is subjected to heat preservation at 400 ℃ for 4 hours, at 450 ℃ for 12 hours and at 500 ℃ for 2 hours under Ar gas protection, homogenizing and solution treating are completed, then the alloy is cooled in water to obtain a step-by-step aging treatment of the Mg-Al-Sn-Sc alloy after solution treatment, and the alloy after solution treatment is subjected to aging treatment and is kept in an environment at 120 ℃ for 20 hours; the alloy was then placed in an environment at 190 ℃ for 120 hours. The alloy has a tensile strength of 220.3MPa at room temperature and 201.9MPa at 180 ℃.
Example 2:
the alloy component ingredients are prepared from the following components in percentage by mass: 4.04% of Al,3.31% of Sn,0.53% of Sc, and the balance of magnesium (Mg) and uncontrollable impurity elements, and the alloy smelting and performance testing operations are as follows:
raw materials, namely high-purity Mg, high-purity Sn and high-purity Al, are weighed according to the corresponding alloy proportion in the Mg-Al-Sn-Sc series alloy, and the Mg-6% Sc intermediate alloy and a casting die are dried and preheated for 30min at 300 ℃; after the temperature of the smelting furnace is raised to 300 ℃, the furnace is filled withProtective gas (protective atmosphere of 99% CO) 2 +1％SF 6 Mixed gas), then placing high-purity Mg, high-purity Al and Mg-6% Sc intermediate alloy ingredients into a metal crucible of a smelting furnace, then heating the furnace to 710 ℃, preserving heat for 15 minutes, adding pure Sn into an alloy melt after metal is melted, heating the furnace to 740 ℃ and preserving heat for 5 minutes, adding a proper amount of magnesium alloy refining agent and slag remover, and stirring for the first time; cooling the furnace temperature to 700 ℃ after stirring, stirring for the second time, and simultaneously removing waste residues on the surface of the alloy; and pouring the liquid alloy into a metal mold, preheating the metal mold to 300 ℃, and naturally cooling after casting to obtain the as-cast alloy. Homogenizing and solution treating an as-cast Mg-Al-Sn-Sc alloy, wherein the as-cast Mg-Al-Sn-Sc alloy is subjected to homogenization and solution treatment at 400 ℃ for 4.5 hours and at 450 ℃ for 12 hours under Ar gas protection, the as-cast Mg-Al-Sn-Sc alloy is subjected to homogenization and solution treatment at 500 ℃ for 2 hours, then the alloy is cooled in water to obtain a solid-dissolved Mg-Al-Sn-Sc alloy, the solid-solution treated alloy is subjected to aging treatment step by step, and the solid-solution treated alloy is kept in an environment of 120 ℃ for 10 hours; the alloy was then placed in an environment at 180 ℃ for 140 hours. The alloy has a tensile strength of 227.6MPa at room temperature and 205.1MPa at 180 ℃.
Example 3:
the alloy component ingredients are prepared from the following components in percentage by mass: 6.10% of Al,3.48% of Sn,0.60% of Sc and the balance of magnesium (Mg) and uncontrollable impurity elements, and the alloy smelting and performance testing operations are as follows:
raw materials, namely high-purity Mg, high-purity Sn and high-purity Al, are weighed according to the corresponding alloy proportion in the Mg-Al-Sn-Sc series alloy, and the Mg-6% Sc intermediate alloy and a casting die are dried and preheated for 30min at 300 ℃; after the temperature of the smelting furnace is raised to 300 ℃, protective gas (the protective atmosphere is 99 percent CO) is introduced into the furnace 2 +1％SF 6 Mixed gas), then placing high-purity Mg, high-purity Al and Mg-6% Sc intermediate alloy ingredients into a metal crucible of a smelting furnace, then heating the furnace to 713 ℃, preserving heat for 15 minutes, adding pure Sn into an alloy melt after metal is melted, heating the furnace to 740 ℃ and preserving heat for 10 minutes, adding a proper amount of magnesium alloy refining agent and slag remover, and stirring for the first time; cooling the furnace temperature to the temperature after stirringStirring for the second time at 700 ℃ and simultaneously removing waste residues on the surface of the alloy; and pouring the liquid alloy into a metal mold, preheating the metal mold to 300 ℃, and naturally cooling after casting to obtain the as-cast alloy. Homogenizing and solution treating an as-cast Mg-Al-Sn-Sc alloy, wherein the as-cast Mg-Al-Sn-Sc alloy is subjected to heat preservation at 400 ℃ for 5 hours, at 450 ℃ for 14 hours and at 500 ℃ for 2 hours under Ar gas protection, homogenizing and solution treating are completed, then the alloy is cooled in water to obtain a step-by-step aging treatment of the Mg-Al-Sn-Sc alloy after solution treatment, and the alloy after solution treatment is subjected to aging treatment and is kept in an environment at 130 ℃ for 10 hours; the alloy was then placed in an environment at 190 ℃ for 120 hours. The alloy has a tensile strength of 234.6MPa at room temperature and 214.4MPa at 180 ℃.
Example 4:
the alloy component ingredients are prepared from the following components in percentage by mass: 5.03% of Al,5.53% of Sn,0.83% of Sc and the balance of magnesium (Mg) and uncontrollable impurity elements, and the alloy smelting and performance testing operations are as follows:
raw materials, namely high-purity Mg, high-purity Sn and high-purity Al, are weighed according to the corresponding alloy proportion in the Mg-Al-Sn-Sc series alloy, and the Mg-6% Sc intermediate alloy and a casting die are dried and preheated for 30min at 300 ℃; after the temperature of the smelting furnace is raised to 300 ℃, protective gas (the protective atmosphere is 99 percent CO) is introduced into the furnace 2 +1％SF 6 Mixed gas), then placing high-purity Mg, high-purity Al and Mg-6% Sc intermediate alloy ingredients into a metal crucible of a smelting furnace, then heating the furnace to 713 ℃, preserving heat for 10 minutes, adding pure Sn into the alloy melt after metal is melted, heating the furnace to 740 ℃ and preserving heat for 10 minutes, adding a proper amount of magnesium alloy refining agent and slag remover, and stirring for the first time; cooling the furnace temperature to 700 ℃ after stirring, stirring for the second time, and simultaneously removing waste residues on the surface of the alloy; and pouring the liquid alloy into a metal mold, preheating the metal mold to 300 ℃, and naturally cooling after casting to obtain the as-cast alloy. Homogenizing and solution treating cast Mg-Al-Sn-Sc alloy, under Ar gas protection, preserving the cast Mg-Al-Sn-Sc alloy at 400 ℃ for 7 hours, preserving the cast Mg-Al-Sn-Sc alloy at 450 ℃ for 14 hours, preserving the cast Mg-Al-Sn-Sc alloy at 500 ℃ for 2.5 hours to complete homogenizing and solution treatment, and then carrying out alloy treatmentCooling the obtained Mg-Al-Sn-Sc alloy subjected to solid solution in water, performing step-by-step aging treatment, and performing aging treatment on the alloy subjected to solid solution treatment, wherein the alloy is kept in an environment of 130 ℃ for 20 hours; the alloy was then left to stand in an environment of 200 ℃ for 120 hours. The alloy has a tensile strength at room temperature of 233.6MPa and a tensile strength at 180 ℃ of 221.4MPa.
Example 5:
the alloy component ingredients are prepared from the following components in percentage by mass: 6.81% of Al,5.64% of Sn,0.82% of Sc, and the balance of magnesium (Mg) and uncontrollable impurity elements, and the alloy smelting and performance testing operations are as follows:
raw materials, namely high-purity Mg, high-purity Sn and high-purity Al, are weighed according to the corresponding alloy proportion in the Mg-Al-Sn-Sc series alloy, and the Mg-6% Sc intermediate alloy and a casting die are dried and preheated for 30min at 300 ℃; after the temperature of the smelting furnace is raised to 300 ℃, protective gas (the protective atmosphere is 99 percent CO) is introduced into the furnace 2 +1％SF 6 Mixed gas), then placing high-purity Mg, high-purity Al and Mg-6% Sc intermediate alloy ingredients into a metal crucible of a smelting furnace, then heating the furnace to 713 ℃, preserving heat for 15 minutes, adding pure Sn into the alloy melt after metal is melted, heating the furnace to 745 ℃ and preserving heat for 10 minutes, adding a proper amount of magnesium alloy refining agent and slag remover, and stirring for the first time; cooling the furnace temperature to 700 ℃ after stirring, stirring for the second time, and simultaneously removing waste residues on the surface of the alloy; and pouring the liquid alloy into a metal mold, preheating the metal mold to 300 ℃, and naturally cooling after casting to obtain the as-cast alloy. Homogenizing and solution treating an as-cast Mg-Al-Sn-Sc alloy, wherein the as-cast Mg-Al-Sn-Sc alloy is subjected to heat preservation at 400 ℃ for 8 hours, at 450 ℃ for 15 hours and at 500 ℃ for 2.5 hours under Ar gas protection, then the alloy is cooled in water to obtain a solid-dissolved Mg-Al-Sn-Sc alloy, the solid-solution treated alloy is subjected to step aging treatment, and the solid-solution treated alloy is kept in a 130 ℃ environment for 15 hours; the alloy was then placed in an environment at 180 ℃ for 130 hours. The alloy has a tensile strength of 243.9MPa at room temperature and 230.5MPa at 180 ℃.
Example 6:
the alloy component ingredients are prepared from the following components in percentage by mass: 8.99% of Al,6.87% of Sn,0.93% of Sc, and the balance of magnesium (Mg) and uncontrollable impurity elements, and the alloy smelting and performance testing operations are as follows:
raw materials, namely high-purity Mg, high-purity Sn and high-purity Al, are weighed according to the corresponding alloy proportion in the Mg-Al-Sn-Sc series alloy, and the Mg-6% Sc intermediate alloy and a casting die are dried and preheated for 30min at 300 ℃; after the temperature of the smelting furnace is raised to 300 ℃, protective gas (the protective atmosphere is 99 percent CO) is introduced into the furnace 2 +1％SF 6 Mixed gas), then placing high-purity Mg, high-purity Al and Mg-6% Sc intermediate alloy ingredients into a metal crucible of a smelting furnace, then heating the furnace to 713 ℃, preserving heat for 15 minutes, adding pure Sn into the alloy melt after metal is melted, heating the furnace to 745 ℃ and preserving heat for 10 minutes, adding a proper amount of magnesium alloy refining agent and slag remover, and stirring for the first time; cooling the furnace temperature to 700 ℃ after stirring, stirring for the second time, and simultaneously removing waste residues on the surface of the alloy; and pouring the liquid alloy into a metal mold, preheating the metal mold to 300 ℃, and naturally cooling after casting to obtain the as-cast alloy. Homogenizing and solution treating an as-cast Mg-Al-Sn-Sc alloy, wherein the as-cast Mg-Al-Sn-Sc alloy is subjected to heat preservation at 400 ℃ for 8 hours, at 450 ℃ for 16 hours and at 500 ℃ for 3 hours under Ar gas protection, homogenizing and solution treating are completed, then the alloy is cooled in water to obtain a step-by-step aging treatment of the Mg-Al-Sn-Sc alloy after solution treatment, and the alloy after solution treatment is subjected to aging treatment and is kept in an environment at 140 ℃ for 20 hours; the alloy was then placed in an environment of 200 ℃ for 130 hours. The alloy has a tensile strength of 251.9MPa at room temperature and 240.1MPa at 180 ℃.
The following table is summarized for the main process parameters in the above examples:
in the scheme of the invention, from the angle of content proportioning and the influence of two angles of process parameters on alloy performance, the method performs multi-azimuth research and research to find out the natural law and finally recommends one or more combinationsPut into practical production. Wherein, FIG. 1 is a metallographic structure of the Mg-5Al-5.5Sn-0.8Sc alloy, and FIG. 2 is a transmission structure of a precipitated phase of the Mg-5Al-5.5Sn-0.8Sc alloy. As can be seen from the drawings and the summary of the embodiments, the Mg-Al alloy has uniform structure and refined crystal grains by introducing Sn and Sc elements, and simultaneously forms Al 3 Sc (dissolution temperature 569 ℃ C.) and Mg 2 The heat-resistant high-temperature phase of Sn (dissolution temperature: 561 ℃ C.) realizes coexistence of the second phase and the precipitated phase. The strength of the alloy, especially the high-temperature resistant strength, is improved by the synergistic effect of aging strengthening, fine-grain strengthening and second-phase strengthening multi-element strengthening means.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many forms may be made by those having ordinary skill in the art without departing from the spirit of the present invention and the scope of the claims, which are to be protected by the present invention.
Claims (8)
1. Mg-containing 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps:
the alloy comprises the following components in percentage by weight: 3.0 to 9.0 weight percent of aluminum Al, 3.0 to 7.0 weight percent of tin Sn, 0.1 to 1.0 weight percent of scandium Sc, and the balance of magnesium Mg and uncontrollable impurity elements;
the preparation method comprises the following steps:
s1: raw material weighing
Raw materials are prepared according to the alloy proportion in the Mg-Al-Sn-Sc series alloy, and the raw materials comprise magnesium Mg, tin Sn, aluminum Al and intermediate alloy;
s2: preheating and charging
S2-1, placing the raw materials obtained in the step S1 and a casting mold in an environment of 300 ℃ for drying and preheating for 30min;
s2-2, raising the temperature of the smelting furnace to 300 ℃, introducing a protective gas into the furnace, and keeping the temperature for 15min;
s2-3, placing the preheated raw materials of Mg, al and intermediate alloy in the step S2-1 into a metal crucible in a smelting furnace;
s3, smelting
S3-1, raising the temperature of the smelting furnace to 710-715 ℃, and preserving heat for 10-15min;
s3-2, adding the preheated raw material Sn in the step S2, and simultaneously raising the furnace temperature to 735-750 ℃ and keeping for 5-10min;
s3-3, adding a magnesium alloy refining agent and a deslagging agent, and simultaneously stirring for the first time;
s3-4, reducing the furnace temperature to 700 ℃, stirring for the second time, and simultaneously removing waste residues on the surface of the liquid alloy;
s4, pouring
Pouring the liquid alloy finally obtained in the step S3-4 into a pouring mold which is preheated in the step S2, wherein the actual temperature of the pouring mold is higher than 150 ℃ to obtain an as-cast alloy;
s5: step-by-step solid solution treatment;
s5-1:1 section heat preservation
Placing the as-cast alloy obtained in the step S4 at 400 ℃ and introducing argon into the environment to be protected for 4-8 hours to finish homogenization treatment;
s5-2: 2-section heat preservation
Placing the as-cast alloy obtained in the step S5-1 at 450 ℃ and introducing argon into an air-protecting environment for 12-16 hours to finish primary solution treatment;
s5-3: 3-section heat preservation
Placing the as-cast alloy obtained in the step S5-2 at 500 ℃ and introducing argon into an air-protecting environment for 2-3 hours to complete all solid solution treatment;
s6: step aging treatment
S6-1, placing the as-cast alloy obtained in the step S5-3 in an environment of 120-140 ℃ for 10-20 hours;
s6-2, placing the as-cast alloy in an environment of 180-200 ℃ for 120-130 hours to obtain fine and uniform Mg 2 And Sn precipitates.
2. A Mg-containing product according to claim 1 2 Sn and Al 3 Preparation method of Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phasesIs characterized in that: the mass percentage of the aluminum Al is 3.12 percent or 4.04 percent or 6.1 percent or 5.03 percent or 6.81 percent or 8.99 percent.
3. A Mg-containing product according to claim 1 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps: the mass percentage of the tin Sn is 3.51 percent or 3.13 percent or 3.48 percent or 5.53 percent or 5.64 percent or 6.87 percent.
4. A Mg-containing product according to claim 1 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps: the scandium Sc is 0.51% or 0.53% or 0.6% or 0.83% or 0.82% or 0.93% by mass.
5. A Mg-containing product according to claim 1 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with the Sc double heat-resistant phases is characterized by comprising the following alloy components in percentage by weight:
3.12wt% of aluminum Al,3.51 wt% of tin Sn,0.51 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
4.04wt% of aluminum Al, 3.13wt% of tin Sn,0.53 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6.1wt% of aluminum Al,3.48 wt% of tin Sn,0.6 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
5.03 weight percent of aluminum Al,5.53 weight percent of tin Sn,0.83 weight percent of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6.81wt% of aluminum Al,5.64 wt% of tin Sn,0.82 wt% of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements;
6 parts of combination, 8.99% by weight of aluminum Al,6.87% by weight of tin Sn,0.93% by weight of scandium Sc and the balance of magnesium Mg and uncontrollable impurity elements.
6. The Mg-containing composition according to claim 1 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps: the intermediate alloy is Mg-6% Sc.
7. The Mg-containing composition according to claim 1 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps:
the magnesium alloy refining agent is 60% of potassium chloride, 5% of calcium fluoride, 5% of sodium chloride, 15% of calcium chloride and 15% of barium chloride;
the slag remover comprises 40% of potassium chloride, 40% of magnesium chloride, 6% of sodium chloride, 6% of calcium fluoride and 8% of barium chloride.
8. The Mg-containing composition according to claim 1 2 Sn and Al 3 The preparation method of the Mg-Al-Sn-Sc series alloy with Sc double heat-resistant phases is characterized by comprising the following steps: the protective gas introduced into the furnace in the step S2-2 is 99 percent CO 2 With 1% SF 6 Is a mixed gas of (a) and (b).
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| WO2007107286A2 (en) * | 2006-03-18 | 2007-09-27 | Acrostak Corp. Bvi | Magnesium-based alloy with improved combination of mechanical and corrosion characteristics |
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| WO2006095999A1 (en) * | 2005-03-08 | 2006-09-14 | Dong-Hyun Bae | Mg alloys containing misch metal, manufacturing method of wrought mg alloys containing misch metal, and wrought mg alloys thereby |
| KR101133775B1 (en) * | 2009-09-21 | 2012-08-24 | 한국생산기술연구원 | Magnesium mother alloy, manufacturing method thereof, Metal alloy using the same, and Metal alloy manufacturing method thereof |
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| WO2007107286A2 (en) * | 2006-03-18 | 2007-09-27 | Acrostak Corp. Bvi | Magnesium-based alloy with improved combination of mechanical and corrosion characteristics |
| CN109161752A (en) * | 2018-10-17 | 2019-01-08 | 上海海洋大学 | A kind of heat-resistant creep-resistant magnesium alloy and preparation method thereof |
| CN110029250A (en) * | 2019-04-03 | 2019-07-19 | 宁波合力模具科技股份有限公司 | High-elongation birmastic and its compression casting preparation method |
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