CN102212727B - Authigenic quasicrystal-reinforced Mg-Zn-Y alloy and smelting method thereof - Google Patents
Authigenic quasicrystal-reinforced Mg-Zn-Y alloy and smelting method thereof Download PDFInfo
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Abstract
The invention relates to an authigenic quasicrystal-reinforced Mg-Zn-Y alloy and a smelting method thereof, and belongs to the technical field of metal material preparation. The authigenic quasicrystal-reinforced Mg-Zn-Y alloy comprises the following chemical components in percentage by weight: 3.0-10.0% of Zn, 0.5-3.0% of Y, 0.05-1.0% of Al-Ti-C and the balance of Mg and unavoidable impurities. The smelting method comprises the following steps: firstly adding commercial pure magnesium, smelting the commercial pure magnesium, then adding Zn and Mg-Y intermediate alloy, and smelting the mixture; cooling the obtained melt to 700-720 DEG C, adding the Al-Ti-C intermediate alloy, introducing ultrasonic waves into the melt; and finally carrying out ultrasonic treatment, and casting to obtain the authigenic quasicrystal-reinforced Mg-Zn-Y alloy. The authigenic quasicrystal-reinforced Mg-Zn-Y alloy obtained by the method has the advantages of high strength and high elongation; the magnesium alloy meeting use requirements can be prepared by optimally controlling the Zn/Y ratio and the mass fraction of alloying elements; and the preparation process is simple and the production cost is low, thus the method is applicable to large-scale industrial production and having good market application prospect.
Description
Technical field
The present invention relates to a kind of spontaneous accurate brilliant Mg-Zn-Y alloy and melting method thereof of strengthening, specifically, what relate to is a kind of spontaneous accurate brilliant Mg-Zn-Y of enhancing alloy that has added trace of Al-Ti-C master alloy, belongs to technical field of metal material preparation.
Background technology
The spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens not only all has the good mechanical performance in room temperature but also at high temperature, thereby causes domestic and international investigation of materials person's very big interest, and this is because it contains accurate crystalline phase I phase (Mg
3Zn
6Y
1) cause.Simultaneously, the Mg-Zn-Y alloy can be produced through traditional technologys such as casting, rolling, extruding, forgings.But under conventional curing condition, accurate crystalline phase often is reticulated structure, and is thicker, limited to the mechanical property raising, can not give full play to accurate brilliant effect.So, adopt an effective measure, change accurate crystalline phase form and make it disperse and be distributed in the magnesium alloy substrate, can obviously improve the mechanical property of magnesiumalloy.
Find that through retrieval CN718801A discloses magnesium base spherical quasi crystal master alloy and method of manufacture thereof, the chemical ingredients of this alloy is (with massfraction; The wt% meter) be: Mg 40.00～45.00%; Zn 45.50～55.00%, and Mn 0.50～4.50%, Y1.00～4.50%; Ca 0.10～1.00%, adopts microalloying and electro-pulse modification to handle the back and under the high pressure curing condition, obtains the magnesium base spherical quasi crystal master alloy.
CN 101705405A discloses magnesium base spherical quasi crystal master alloy and preparation method thereof; Adopt the method for control solidification rate to prepare five yuan of magnesium bases of Mg-Zn-Y-Mn-Cu icosahedron spherical quasi crystal master alloy; Its chemical ingredients is: Mg 55.0～65.0%, and Zn 30.0～40.0%, Y2.5～5.5%; Mn 0.1～1.5%, and Cu 0.1～0.5%.
CN 101705406 A disclose a kind of magnesium base spherical quasi crystal master alloy and preparation method thereof; Adopt the method for control solidification rate to prepare Mg-Zn-Y-C quaternary magnesium base icosahedron spherical quasi crystal master alloy; Its chemical ingredients is: Mg 55.0～65.0%; Zn 30.0～40.0%, Y2.5～5.5%, and C 0.1～0.5%.
CN 101705407 A disclose magnesium base spherical quasi crystal master alloy and method for making thereof; Adopt the method for control solidification rate to prepare Mg-Zn-Y-Ti quaternary magnesium base icosahedron spherical quasi crystal master alloy; Its chemical ingredients is: Mg 55.00～65.0%; Zn 30.0～40.0%, and Y 2.5～5.5%, and Ti 0.1～0.5%.
Although above-mentioned patent can make magnesium base spherical quasi crystal, Zn, Y content is higher and relevant mechanical property.CN101314829 A discloses and has effectively utilized rare earth element y to strengthen Mg-Zn-Y-Zr series magnesium alloy and preparation method, and the component of this magnesium alloy materials and content thereof are: Zn is 5～30%, and Y is 0.5～5%, and Zr 0.3～0.8% forms with the Mg of surplus.
Other has domestic and international open source literature document announcement, and Zr adds in the Mg-Zn-Y alloy can crystal grain thinning, improves its mechanical property, but can not change the form of accurate crystalline phase.Therefore,, adopt the form of a kind of cost accurate crystalline phase of process reform low, easy and simple to handle, increase the quantity of accurate crystalline phase, and the mechanical property that further improves magnesiumalloy is present problem demanding prompt solution in order to give full play to accurate brilliant strengthening effect.
Summary of the invention
The objective of the invention is to deficiency, provide a kind of interpolation trace of Al-Ti-C master alloy refinement spontaneous accurate brilliant Mg-Zn-Y alloy and the preparation method of strengthening, enlarged the range of application of Mg-Zn-Y alloy to prior art.
The present invention realizes through following technical scheme:
The spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens of the present invention, its chemical ingredients quality percentage composition is: Zn 3.0～10.0%; Y0.5～3.0%; Al-Ti-C 0.05～1.0%, and surplus is Mg and unavoidable impurities.
Said unavoidable impurities is meant: Fe≤0.005%, Cu≤0.015%, Ni≤0.002%, Si≤0.01%.
The spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy of the present invention comprises melting and casting, when melt is cooled to 700～720 ℃ after melting, adds the Al-Ti-C master alloy, in melt, introduces UW, after ultrasonication, casts and processes.
The described spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy specifically comprises the steps:
(1) melting: at flux or/and under the gas shield melting condition; Pure magnesium in the time of 700～740 ℃, adds Zn and Mg-Y master alloy after in Steel Crucible, melting fully; After Zn to be added, Mg-Y master alloy melt fully; Temperature is risen to 760～780 ℃, and skimming operation after 30 minutes is left standstill in refining 5～10 minutes;
(2) casting: melt is cooled to 700～720 ℃, adds the Al-Ti-C master alloy, the UW bar that will pass through preheating inserts in the magnesium alloy fused mass and carries out ultrasonication, treat that ultrasonication finishes after, take out Steel Crucible, casting is processed.
The described Zn of step (1) adds with the form of technical pure Zn.
The described Mg-Y master alloy of step (1) adds with the form of Mg-25Y master alloy.
The described Al-Ti-C of step (2) adds with the form of Al-8Ti-2C.
Described ultrasonication frequency is 15～25kHz, and ultrasonication power is 500～2500W, and ultrasonic treatment time is 3～7 minutes.
Flux protection in the described fusion process is the compsn of Repone K, calcium chloride, bariumchloride, Calcium Fluoride (Fluorspan), Cerium II Chloride and Yttrium trichloride, and the percentage composition of chemical ingredients quality is: Repone K: 50～65%; Calcium chloride: 10～25%; Bariumchloride: 5～10%; Calcium Fluoride (Fluorspan): 1～10%; Cerium II Chloride: 3～5%; Yttrium trichloride: 3～5%.
Described gas shield is sulfur hexafluoride and carbon dioxide gas mixture or high-purity argon gas.
In described sulfur hexafluoride and the carbon dioxide gas mixture, the sulfur hexafluoride volume accounts for 0.1～0.6% of TV.
Above-mentioned chemical reagent and gas are the commercially available prod, the mass content of described pure magnesium >=99.90%; The mass content of described industrial-purity zinc >=99.90%; The purity of sulfur hexafluoride >=99.9%; The purity of carbonic acid gas＞99.995%; High-purity argon gas purity＞99.999%, nitrogen content＜5ppm, oxygen level＜2ppm, hydrogen richness＜1ppm, total carbon content (with methanometer)＜2ppm, moisture content＜4ppm.
Inherent mechanism of the present invention is: the massfraction of the formation of accurate crystalline phase and content and Zn, Y and Zn/Y are than relevant; Massfraction and Zn/Y ratio through control Zn, Y; And consider that the Al in the Al-Ti-C master alloy will consume a part of Y; Make in the alloy volumn concentration of accurate crystalline phase reach maximum, thereby improve the mechanical property of alloy effectively.The Al-Ti-C master alloy is by α-Al and tiny TiC and the Al of a large amount of disperse
4C
3Granulometric composition, Al generates HMP Al mutually with Y when the Al-Ti-C master alloy joins in the magnesium alloy fused mass
2Y, and TiC, Al
4C
3And Al
2Y all can be used as the heterogeneous crystallization nuclei of matrix α-Mg, refinement magnesiumalloy crystal grain.The adding of Al-Ti-C master alloy has changed the surface tension of magnesium alloy fused mass, and grain refining in addition makes accurate crystalline phase form be transformed into particulate state or corynebacterium by thick reticulated structure.The Al atom enters into the Mg lattice, has reduced Zn and the solid solubility of Y atom in the Mg lattice, makes Zn and the rising of Y atom content in the magnesium alloy fused mass, has increased the quantity of accurate crystalline phase in process of setting subsequently.Magnesium alloy fused mass is carried out ultrasonication, can make the heterogeneous crystallization nuclei disperse more of matrix α-Mg, grain refining effect strengthens.The increase of the refinement of matrix Mg, accurate brilliant quantity and the change of accurate crystalline form attitude can obviously improve the mechanical property of alloy.
Trace of Al among the present invention-Ti-C master alloy has joined in the Mg-Zn-Y alloy not only refinement crystal grain has changed accurate crystalline phase form, and can increase the volumn concentration of accurate crystalline phase, and this will help the raising of alloy mechanical property.
Beneficial effect of the present invention is following:
Alloy of the present invention has good intensity and elongation, its tensile strength sigma
b=170～260MPa, elongation δ=10～16%.Can be according to the demands of different of different application occasion to material property; Massfraction through optimal control Zn/Y ratio and alloying element; Prepare the magnesiumalloy that satisfies request for utilization, its preparation technology is simple, low production cost; Can carry out large-scale industrial production, have good market application prospect.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Comparative Examples 1
A kind of spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens, the percentage composition of chemical ingredients quality is: 3.0%Zn, 0.5%Y, impurity element Fe≤0.005%, Cu≤0.015%, Ni≤0.002%, Si≤0.01%, surplus is Mg.
Melting method:, under the flux protection melting condition, in the electrical crucible Steel Crucible, add pure magnesium according to mentioned component configuration alloy; Spread a small amount of insulating covering agent simultaneously in the Steel Crucible bottom, after pure magnesium melts fully, in the time of 720 ± 10 ℃; Add technical pure Zn and Mg-25Y master alloy, after technical pure Zn to be added, Mg-25Y master alloy melt fully, temperature is risen to 770 ± 10 ℃; Skimming operation after 30 minutes is left standstill in refining 10 minutes; Melt is cooled to 710 ± 5 ℃, and casting is processed.
The quality percentage composition of flux is: Repone K 60%, calcium chloride 18%, bariumchloride 5%, Calcium Fluoride (Fluorspan) 8%, Cerium II Chloride 4% and Yttrium trichloride 5%.
This Comparative Examples alloy at room temperature tensile strength and elongation are respectively 153MPa and 7.6%.
Embodiment 1
The spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens of the present invention, the percentage composition of chemical ingredients quality is: 3.0%Zn, 0.5%Y, 0.10%Al-Ti-C, impurity element Fe≤0.005%, Cu≤0.015%, Ni≤0.002%, Si≤0.01%, surplus is Mg.
Melting method:, under the flux protection melting condition, in the electrical crucible Steel Crucible, add pure magnesium according to mentioned component configuration alloy; Spread a small amount of insulating covering agent simultaneously in the Steel Crucible bottom, after pure magnesium melts fully, in the time of 720 ± 10 ℃; Add technical pure Zn and Mg-25Y master alloy, after technical pure Zn to be added, Mg-25Y master alloy melt fully, temperature is risen to 770 ± 10 ℃; Skimming operation after 30 minutes is left standstill in refining 10 minutes; Melt is cooled to 710 ± 5 ℃, adds the Al-8Ti-2C master alloy, in melt, introduce UW subsequently; The UW bar (600 ℃ of preheating temperatures) that will pass through preheating inserts in the magnesium alloy fused mass and carries out ultrasonication; After treating that ultrasonication finishes, take out Steel Crucible, casting is processed.
The ultrasonication frequency is 20kHz, and ultrasonication power is 1000W, and ultrasonic treatment time is 5 minutes.
The quality percentage composition of flux is: Repone K 60%, calcium chloride 18%, bariumchloride 5%, Calcium Fluoride (Fluorspan) 8%, Cerium II Chloride 4% and Yttrium trichloride 5%.
The room temperature tensile strength and the elongation of present embodiment are respectively 175MPa and 10.4%, have improved 14.4% and 36.8% respectively than the tensile strength and the elongation of Comparative Examples.
Embodiment 2
The spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens of the present invention, the percentage composition of chemical ingredients quality is: 5.0%Zn, 1.2%Y, 0.14%Al-Ti-C, impurity element Fe≤0.005%, Cu≤0.015%, Ni≤0.002%, Si≤0.01%, surplus is Mg.
Melting method: adopt flux and high-purity argon gas to carry out the melting protection; The ultrasonication frequency is 20kHz; Ultrasonication power is 1500W, and ultrasonic treatment time is 7 minutes, all the other steps such as embodiment 1; Present embodiment alloy at room temperature tensile strength and elongation are respectively 225MPa and 12.7%, have improved 47.1% and 67.1% respectively than the tensile strength and the elongation of Comparative Examples.
Embodiment 3
The spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens of the present invention, the percentage composition of chemical ingredients quality is: 7.0%Zn, 1.75%Y, 0.25%Al-Ti-C, impurity element Fe≤0.005%, Cu≤0.015%, Ni≤0.002%,, Si≤0.01%, surplus is Mg.
Melting method: adopt high-purity argon gas to carry out the melting protection; The ultrasonication frequency is 20kHz; Ultrasonication power is 2500W, and ultrasonic treatment time is 3 minutes, all the other steps such as embodiment 1; Present embodiment alloy at room temperature tensile strength and elongation are respectively 243MPa and 16.0%, have improved 58.9% and 110.5% respectively than the tensile strength and the elongation of Comparative Examples.
Embodiment 4
The spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens of the present invention, the percentage composition of chemical ingredients quality is: 9.5%Zn, 2.3%Y, 1.0%Al-Ti-C, impurity element Fe≤0.005%, Cu≤0.015%, Ni≤0.002%, Si≤0.01%, surplus is Mg.
Melting method: adopt sulfur hexafluoride and carbon dioxide gas mixture (sulfur hexafluoride volume account for TV 0.5%) to carry out melting protection; The ultrasonication frequency is 20kHz; Ultrasonication power is 2000W, and ultrasonic treatment time is 4 minutes, all the other steps such as embodiment 1; Present embodiment alloy at room temperature tensile strength and elongation are respectively 260MPa and 10.7%, have improved 69.9% and 40.8% respectively than the tensile strength and the elongation of Comparative Examples.
Claims (6)
1. the spontaneous accurate brilliant Mg-Zn-Y alloy that strengthens is characterized in that the percentage composition of chemical ingredients quality is: Zn3.0 ~ 9.50%; Y 0.5 ~ 1.75%; Al-Ti-C 0.05 ~ 1.0%, and surplus is Mg and unavoidable impurities;
The described spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy comprises melting and casting, when melt is cooled to 700 ~ 720 ℃ after the melting, adds the Al-Ti-C master alloy, in melt, introduces UW, after ultrasonication, casts and processes;
Flux in the described fusion process is the compsn of Repone K, calcium chloride, bariumchloride, Calcium Fluoride (Fluorspan), Cerium II Chloride and Yttrium trichloride.
2. the spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy according to claim 1, it is characterized in that: described Al-Ti-C master alloy adds with the form of Al-8Ti-2C.
3. the spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy according to claim 1, it is characterized in that: described ultrasonication frequency is 15 ~ 25kHz.
4. the spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy according to claim 1, it is characterized in that: described ultrasonication power is 500 ~ 2500W.
5. the spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy according to claim 1, it is characterized in that: described ultrasonic treatment time is 3 ~ 7 minutes.
6. the spontaneous accurate brilliant melting method that strengthens the Mg-Zn-Y alloy according to claim 1, it is characterized in that: the percentage composition of described flux chemical ingredients quality is: Repone K: 50 ~ 65%; Calcium chloride: 10 ~ 25%; Bariumchloride: 5 ~ 10%; Calcium Fluoride (Fluorspan): 1 ~ 10%; Cerium II Chloride: 3 ~ 5%; Yttrium trichloride: 3 ~ 5%.
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| CN102851523A (en) * | 2012-08-22 | 2013-01-02 | 淄博宏泰防腐有限公司 | Refining flux for smelting of WE43 magnesium alloy, and preparation and usage method thereof |
| CN103215468B (en) * | 2013-04-19 | 2015-01-14 | 扬州峰明金属制品有限公司 | Rear-earth magnesium alloy smelting agent and preparation method thereof |
| CN105256262B (en) * | 2015-10-29 | 2017-08-11 | 东北大学 | The method that Mg Zn y alloy aging hardening effects are improved by preset twin |
| US10799947B2 (en) * | 2018-12-28 | 2020-10-13 | North University Of China | Method of semi-solid indirect squeeze casting for magnesium-based composite material |
| CN109852857B (en) * | 2019-03-29 | 2021-08-06 | 上海交通大学 | High-strength-toughness heat-resistant Mg-Y alloy suitable for gravity casting and preparation method thereof |
| CN109868402B (en) * | 2019-03-29 | 2021-08-17 | 上海交通大学 | High-strength-toughness heat-resistant die-casting Mg-Y alloy and preparation method thereof |
| CN113106277B (en) * | 2021-04-10 | 2022-03-01 | 中北大学 | Preparation method of magnesium-zinc-yttrium quasicrystal and titanium carbide synergistically reinforced magnesium matrix composite |
| CN115838878A (en) * | 2022-12-06 | 2023-03-24 | 上海云铸三维科技有限公司 | Covering flux for magnesium-lithium-aluminum-zinc-yttrium alloy, preparation method of covering flux and smelting method of magnesium-lithium-aluminum-zinc-yttrium alloy |
| CN115896573B (en) * | 2022-12-23 | 2023-09-01 | 深圳市鑫申新材料科技有限公司 | High-strength high-heat-conductivity die-casting magnesium alloy and preparation method and application thereof |
| CN116732402B (en) * | 2023-08-11 | 2023-11-07 | 上海交通大学内蒙古研究院 | Nanoparticle refined magnesium-yttrium intermediate alloy and preparation method thereof |
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