CN103866170A - Preparation method of rare earth magnesium alloy and sheet thereof - Google Patents
Preparation method of rare earth magnesium alloy and sheet thereof Download PDFInfo
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- CN103866170A CN103866170A CN201410065340.2A CN201410065340A CN103866170A CN 103866170 A CN103866170 A CN 103866170A CN 201410065340 A CN201410065340 A CN 201410065340A CN 103866170 A CN103866170 A CN 103866170A
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Abstract
The invention provides a rare earth magnesium alloy. The rare earth magnesium alloy is characterized by comprising the following components by mass percent: 0.5 to 4.0% of Zn, 0.1 to 2% of Gd, 0.3 to 0.9% of Zr, and the balance of Mg. The preparation method of the rare earth magnesium alloy sheet comprises the following steps of: treating a rare earth magnesium alloy ingot casting by uniform annealing; cooling with water; milling the surface; preheating a milled blank; rolling for four to eight times; melting down and heating once every two to three times after rolling; continuously rolling, wherein the total rolling reduction is 70 to 95%; annealing the sheet subjected to hot rolling; performing cold rolling for a moderate-thickness sheet subjected to hot rolling for two to four times; and then annealing the sheet subjected to cold rolling to obtain the rare earth magnesium alloy sheet. The invention also provides a preparation method of the rare earth magnesium alloy and the sheet thereof. The rare earth magnesium alloy sheet is high in plasticity and high in heat stability. Compared with hot rolling, cold rolling has the advantage that the magnesium alloy can be prevented from being oxidized into a film during heating; in addition, the prepared sheet is accurate in dimension and uniform in thickness; a thin belt which cannot be produced by hot rolling can be obtained; and mass production and application can be realized.
Description
Technical field
The invention belongs to metal material field, relate to the preparation method of a kind of magnesium-rare earth and thin plate thereof (0.4 ~ 2mm).The specifically castering action to magnesium alloy plasticity according to rare earth element adds appropriate rare earth element on traditional magnesium alloy basis, by controlling hot rolling, cold rolling and subsequent heat treatment technique subsequently, obtains the magnesium-rare earth thin plate of high-ductility, high thermal stability.
Background technology
Magnesium alloy has specific tenacity and specific rigidity is high, good casting property, electromagnetic shielding and damping capacity is excellent and the feature such as recyclable recycling, is with a wide range of applications in fields such as aerospace, the vehicles, telecommunications, opticinstrument, Technological Problems In Computer Manufacturings.Because the poor serious magnesium alloy that hindered of deformation at room temperature ability, thermostability and corrosion resisting property of magnesium and alloy is further expanded application.Because magnesium alloy has close-packed hexagonal structure, common viscous deformation at normal temperatures only limits to basal slip and the conical surface is twin, and in the time that texturing temperature exceedes 225 ℃, its cylinder and conical surface slip system start, and plastic deformation ability significantly improves.In addition, the secondary hardening phase particle in common commercialization magnesium alloy is as Mg
17al
12, MgZn
2phase fusing point is only 437 ℃, 347 ℃, and thermal stability is poor, and alligatoring and softening at high temperature easily occurs, and has reduced the barrier effect to Grain Boundary Sliding, and its working temperature is generally no more than 150 ℃.Therefore, improving magnesium alloy deformation at room temperature ability and thermostability is one of magnesium alloy Application Areas key issue urgently to be resolved hurrily.
Rare earth element (RE) has unique configuration of extra-nuclear electron and chemical property, in magnesium alloy, add appropriate rare earth element can strengthen Binding Forces Between Atoms on the one hand, reduce magnesium atom velocity of diffusion, there is remarkable effect to improving magnesium alloy recrystallization temperature and slowing down recrystallization process, particularly because the compound thermostability of rare earth metal and magnesium formation is high, can significantly promote mechanical property, the especially high-temperature behavior of magnesium alloy.Magnesium-rare earth has good castability, and rare earth element not only can purify alloy melt, improve alloy structure, can also be in castingprocesses remarkable crystal grain thinning, magnesium alloy solidification temperature range is narrowed, reduce microporosity and hot cracking tendency.In magnesium-rare earth melt, two important factors that affect grain refining are solute segregation and heterogeneous forming core particle.Solute segregation causes the liquid-solid interface forward position of dendritic growth to generate cold-zone, and then hinders dendritic growth and improve activation composition the motivating force of crossing the forming core particle in cold-zone; And the nucleation ability of forming core particle has determined to solidify and has started and composition is crossed the quantity of cold-zone effective nucleation.In addition, rare earth element also has good ageing strengthening effect, can separate out highly stable disperse phase particle, thereby can increase substantially hot strength and the creep resistance of magnesium alloy.Add rare earth element can change magnesium alloy axial ratio on the one hand in addition, improve magnesium alloy deformation ability.
The patent of invention that CN200910011111.1A name is called " hot rolling process of a kind of high-ductility, low-anisotropy magnesium alloy and sheet material thereof " is associated and in gold, adds 0.1 ~ 10% rare earth element at Mg-Zn, ingot casting is rolled into the thin plate of 0.1 ~ 5mm after homogenizing annealing is processed, and the thermal treatment of annealing.After rolling deformation sheet material along roll to elongation δ >=30%, along horizontal elongation δ >=36%.The sheet material of preparing has weak basal plane texture, low anisotropy (the average anisotropy factor is between 0.8 ~ 1.3).
The patent of invention that CN201210124363.7 name is called " tough deformed magnesium alloy material of a kind of high strength at high temperature and preparation method thereof " discloses on the basis of Mg-Zn-Zr adds Y(4.5 ~ 9.8%), Er(0.5 ~ 1.5%), Ho(0.3 ~ 1.0%) and other rare earth element (0.2 ~ 0.6%), after melting, casting rod, homogenizing processing and hot extrusion deformation, room temperature tensile strength reaches 340 ~ 420MPa, elongation is 5 ~ 15%, under 250 ℃ of high temperature, tensile strength can reach 310 ~ 380MPa, and elongation is 18 ~ 29%.
The patent of invention that CN200410081258.5 name is called the high plastic magnesium alloy of rare-earth yttrium " a kind of containing " hinders growing up of recrystal grain in hot extrusion process by add Rare Earth Y in ZK60 alloy, further crystal grain thinning, thus keeping improving its plasticity under alloy high strength condition.Mg-(5.0 ~ 8.5) Zn-(0.7 ~ 2.0) Y-(0.6 ~ 0.8) the Zr alloy As-extruded average grain size of this invention is 5 ~ 8 μ m, and room temperature tensile strength is 322 ~ 337 MPa, and elongation is 18 ~ 21.5%.
In above-mentioned three patents, CN200910011111.1A has improved the temperature-room type plasticity deformation performance of alloy by adding rare earth element with control hot rolling technology, and does not relate to its thermostability; Although CN201210124363.7 has obtained good room temperature, Testing Tensile Strength at Elevated Temperature by the rare earth element that adds high level, but the economy of alloy and deformation at room temperature ability still have much room for improvement, CN200410081258.5 is by adding rare earth element y crystal grain thinning, room temperature tensile strength and the plastic deformation ability of alloy are improved, and fail equally to investigate the thermostability of alloy.In sum, research and develop a kind of low cost, high-ductility, the magnesium-rare earth of good thermal stability is to expand its important topic in high-end field application.
Summary of the invention
The object of this invention is to provide a kind of magnesium-rare earth.
Another object of the present invention is to provide that a kind of plasticity is high, the preparation method of the magnesium-rare earth thin plate of Heat stability is good.
The component of described magnesium-rare earth and mass percent thereof are: Zn 0.5 ~ 4.0%, Gd 0.1 ~ 2% and Zr 0.3 ~ 0.9%, all the other are Mg.
Component and the mass percent thereof of preferred magnesium-rare earth are: Zn 3%, Gd 2% and Zr0.6%, all the other are Mg.
The preparation method of described magnesium-rare earth thin plate is made up of following steps:
1. magnesium-rare earth ingot casting is carried out to homogenizing annealing processing for 10 ~ 48 hours 400 ~ 560 ℃ of insulations, then use water cooling, then carry out milling face;
2. the blank after milling face is incubated to 1 ~ 4 hour at 400 ~ 520 ℃, roll is preheating to 250 ~ 320 ℃ simultaneously, start the rolling of 4 ~ 8 passages, every time draught is 10 ~ 40%, after every rolling 2 ~ 3 passages, melt down and be heated to 400 ~ 520 ℃, be incubated 30 ~ 60 minutes and continue rolling, the draught of last passage is 20 ~ 40%, and total reduction is 70 ~ 95%;
3. the sheet material after hot rolling is at 0.5 ~ 24 hour after annealing of 300 ~ 400 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 2 ~ 4 roads, and every time draught is 5 ~ 20%, and total reduction is 20 ~ 55%;
5. cold rolled sheet, again after 250 ~ 500 ℃ of insulations annealing in 15 ~ 1800 seconds, obtains described magnesium-rare earth thin plate.
Compared with prior art, feature of the present invention and beneficial effect are:
1. the present invention, take Mg-Zn-Zr alloy as basic ingredient, by adding a small amount of rare earth element, utilizes semicontinuous casting technique to improve magnesium alloy ingot quality and reduces metallurgical imperfection.Carry out subsequently cold rolling moulding and obtain the magnesium-rare earth thin plate of high-temperature-room type plasticity, high thermal stability and less anisotropy by aximal deformation value hot rolling cogging, a kind of short flow process, preparation method are cheaply provided, can realize scale operation and application.Compare with hot rolling, cold rollingly can avoid the oxidation filming of magnesium alloy in heat-processed, and the product size of making is accurate, even thickness, can obtain the thin strip that hot rolling cannot be produced.
2.Zn can form MgZn with Mg
2particle, is the main strengthening phase of alloy, and Zr has the crystalline structure similar to magnesium, mainly plays crystal grain thinning in alloy.Add one side and Mg, the Zn in alloy of rare earth element form Mg-Zn-RE particle disperse, high thermal stability, suppress on the other hand the secondary phase particle MgZn of low melting point
2separate out, thereby put forward heavy alloyed thermostability (Fig. 1).In addition, adding of rare earth element is conducive to the formation of microcosmic shear zone in cold deformation process and twin generation (Fig. 2), particularly the compound interpolation of Zn and Gd has caused the appearance of microtexture segregation in tissue, when this affects annealing greatly, there is basal plane texture and be 30 in the variation of recrystallization texture
o<0001> changes (Fig. 3).
3. Static Recrystallization has occurred after short annealing and can obtain evenly tiny tissue (Fig. 4), the ductility of its sheet material is significantly enhanced.Compared with not containing the magnesium alloy of rare earth element, all increase the recrystallization temperature of magnesium-rare earth and incubation period and extend (Fig. 5), resistance to elevated temperatures has obtained enhancing.Cold rolled sheet grain-size after high temperature long term annealing does not have obvious abnormal growth yet, illustrates that rare-earth phase particle has effectively suppressed the movement (Fig. 6) of crystal boundary in annealing process.
4. through then cold rolling sheet material room temperature elongation δ >30%(Fig. 7 adding after annealing of aximal deformation value hot rolling cogging), the average anisotropy factor is between 0.9 ~ 1.1, sheet material is 0.5 hour the perfect recrystallization incubation time of 300 ℃, 3 hours perfect recrystallization time, recrystallization crystal particle dimension can reach 2 ~ 10 μ m.
Accompanying drawing explanation
Mg-1Zn-1Gd-0.3Zr alloy casting state stereoscan photograph in Fig. 1 embodiment 1.
The optical microstructure photo of Mg-1Zn-1Gd-0.3Zr alloy after cold rolling in Fig. 2 embodiment 1.
In Fig. 3 embodiment 1 Mg-1Zn-1Gd-0.3Zr alloy cold rolling after 300 ℃ of annealing (0002) face marcotexture after 30 seconds again.
In Fig. 4 embodiment 2 Mg-1Zn-2Gd-0.6Zr alloy cold rolling after the optical microstructure's photo after 1 minute 400 ℃ of annealing again.
Recrystallize kinetic curve in Mg-3Zn-2Gd-0.6Zr alloy annealing process in Fig. 5 embodiment 6.
300 ℃ of annealing of Mg-1Zn-1Gd-0.3Zr alloy cold rolled sheet 30 seconds in Fig. 6 embodiment 1, then be warming up to 400 ℃, optical microstructure's photo of annealing after 24 hours.
The cold rolling tensile mechanical properties curve after 1800 seconds 420 ℃ of annealing again of Mg-3Zn-2Gd-0.6Zr alloy in Fig. 7 embodiment 6.
Embodiment
Content in conjunction with technical solution of the present invention provides following examples, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The square ingot casting that the thickness that the present embodiment adopts semi-continuous casting method to produce is 100mm, the mass percent of alloying constituent is: Zn 1%, Gd 1%, Zr 0.3%, all the other are Mg;
1. alloy side's ingot homogenizing 48h at 400 ℃ of temperature, then uses water cooling;
2. the blank after milling face is incubated to 4 hours at 400 ℃; Roll is preheating to 250 ℃ simultaneously, starts 6 passage rollings, every time draught is 30%.After the 2nd and the 4th passage, melt down and be heated to 400 ℃ of insulations and continue rolling after 30 minutes again, last reduction in pass is 40%, and total reduction is 90%;
3. the sheet material after hot rolling is in 2 hours anneal of 300 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 4 passages, and every time draught is 15%, and total reduction is 52%;
5. cold rolled sheet is again in 30 seconds anneal of 300 ℃ of insulations;
Embodiment 2
The square ingot casting that the thickness that the present embodiment adopts semi-continuous casting method to produce is 100mm, the mass percent of alloying constituent is: Zn 1%, Gd 2%, Zr 0.6%, all the other are Mg;
1. alloy side's ingot homogenizing 24h at 450 ℃ of temperature, then uses water cooling;
2. the blank after milling face is incubated to 2 hours at 450 ℃; Roll is preheating to 280 ℃ simultaneously, starts 6 passage rollings, every time draught is 35%.After the 2nd and the 4th passage, melt down and be heated to 450 ℃ of insulations and continue rolling after 45 minutes again, last reduction in pass is 30%, and total reduction is 94%;
3. the sheet material after hot rolling is in 12 hours anneal of 350 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 3 passages, and every time draught is 15%, and total reduction is 40%;
5. cold rolled sheet is again in 1 minute anneal of 400 ℃ of insulations;
Embodiment 3
The square ingot casting that the thickness that the present embodiment adopts semi-continuous casting method to produce is 100mm, the mass percent of alloying constituent is: Zn 2%, Gd 2%, Zr 0.3%, all the other are Mg.
1. alloy side's ingot homogenizing 10h at 520 ℃ of temperature, then uses water cooling;
2. the blank after milling face is incubated to 1 hour at 500 ℃; Roll is preheating to 300 ℃ simultaneously, starts 4 passage rollings, every time draught is 40%.After the 2nd passage, melt down and be heated to 500 ℃ of insulations and continue rolling after 45 minutes again, last reduction in pass is 20%, and total reduction is 85%;
3. the sheet material after hot rolling is in 1 hour anneal of 400 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 4 passages, and every time draught is 10%, and total reduction is 35%;
5. cold rolled sheet is again in 60 seconds anneal of 450 ℃ of insulations;
Embodiment 4
The square ingot casting that the thickness that the present embodiment adopts semi-continuous casting method to produce is 100mm, the mass percent of alloying constituent is: Zn 2.0%, Gd 1.0%, Zr 0.6%, all the other are Mg;
1. alloy side's ingot homogenizing 24h at 460 ℃ of temperature, then uses water cooling;
2. the blank after milling face is incubated to 2 hours at 460 ℃; Roll is preheating to 280 ℃ simultaneously, starts 6 passage rollings, every time draught is 20%.After the 2nd and the 4th passage, melt down and be heated to 460 ℃ of insulations and continue rolling after 30 minutes again, last reduction in pass is 30%, and total reduction is 90%;
3. the sheet material after hot rolling is in 24 hours anneal of 300 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 2 passages, and every time draught is 10%, and total reduction is 20%;
5. cold rolled sheet is again in 120 seconds anneal of 450 ℃ of insulations;
Embodiment 5
The square ingot casting that the thickness that the present embodiment adopts semi-continuous casting method to produce is 100mm, the mass percent of alloying constituent is: Zn 3.0%, Gd 1.0%, Zr 0.6%, all the other are Mg;
1. alloy side's ingot homogenizing 16h at 420 ℃ of temperature, then uses water cooling;
2. the blank after milling face is incubated to 2 hours at 460 ℃; Roll is preheating to 250 ℃ simultaneously, starts 6 passage rollings, every time draught is 15%.After the 2nd and the 4th passage, melt down and be heated to 460 ℃ of insulations and continue rolling after 60 minutes again, last reduction in pass is 20%, and total reduction is 78%;
3. the sheet material after hot rolling is in 12 hours anneal of 350 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 4 passages, and every time draught is 8%, and total reduction is 30%;
5. cold rolled sheet is again in 360 seconds anneal of 400 ℃ of insulations;
Embodiment 6
The square ingot casting that the thickness that the present embodiment adopts semi-continuous casting method to produce is 100mm, the mass percent of alloying constituent is: Zn 3.0%, Gd 2.0%, Zr 0.6%, all the other are Mg;
1. alloy side's ingot homogenizing 24h at 460 ℃ of temperature, then uses water cooling;
2. the blank after milling face is incubated to 2 hours at 460 ℃; Roll is preheating to 300 ℃ simultaneously, starts 8 passage rollings, every time draught is 15%.2nd, after the 4th and the 6th passage, melt down and be heated to 460 ℃ of insulations and continue rolling after 60 minutes again, last reduction in pass is 30%, and total reduction is 74%;
3. the sheet material after hot rolling is in 10 hours anneal of 380 ℃ of insulations;
4. the plate of moderate thickness after hot rolling is at room temperature cold rolling through 3 passages, and every time draught is 12%, and total reduction is 33%;
5. cold rolled sheet is again in 1800 seconds anneal of 420 ℃ of insulations;
The test result of table 1 embodiment
Claims (3)
1. a magnesium-rare earth, is characterized in that component and mass percent thereof are: Zn 0.5 ~ 4.0%, Gd 0.1 ~ 2% and Zr 0.3 ~ 0.9%, all the other are Mg.
2. magnesium-rare earth according to claim 1, is characterized in that component and mass percent thereof are: Zn 3%, Gd 2% and Zr0.6%, all the other are Mg.
3. the preparation method of magnesium-rare earth thin plate claimed in claim 1, is characterized in that being made up of following steps:
1) magnesium-rare earth ingot casting is carried out to homogenizing annealing processing for 10 ~ 48 hours 400 ~ 560 ℃ of insulations, then use water cooling, then carry out milling face;
2) blank after milling face is incubated to 1 ~ 4 hour at 400 ~ 520 ℃, roll is preheating to 250 ~ 320 ℃ simultaneously, start the rolling of 4 ~ 8 passages, every time draught is 10 ~ 40%, after every rolling 2 ~ 3 passages, melt down and be heated to 400 ~ 520 ℃, be incubated 30 ~ 60 minutes and continue rolling, the draught of last passage is 20 ~ 40%, and total reduction is 70 ~ 95%;
3) sheet material after hot rolling is at 0.5 ~ 24 hour after annealing of 300 ~ 400 ℃ of insulations;
4) plate of moderate thickness after hot rolling is at room temperature cold rolling through 2 ~ 4 roads, and every time draught is 5 ~ 20%, and total reduction is 20 ~ 55%;
5) cold rolled sheet, again after 250 ~ 500 ℃ of insulations annealing in 15 ~ 1800 seconds, obtains described magnesium-rare earth thin plate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607466A (en) * | 2015-01-14 | 2015-05-13 | 大连理工大学 | Hot rolling machining method for high indoor temperature plastic magnesium alloy plate |
| CN107338379A (en) * | 2017-07-12 | 2017-11-10 | 北京科技大学 | A kind of magnesium Tin-zinc-aluminium manganese wrought magnesium alloy and preparation method thereof |
| CN109468560A (en) * | 2019-01-15 | 2019-03-15 | 吉林大学 | Second phase homogenization regulation preparation method in a kind of high aluminium content casting magnesium alloy plate |
| CN109680172A (en) * | 2019-03-08 | 2019-04-26 | 吉林大学 | One kind having weak texture high-strength plasticity low-alloy content magnesium alloy preparation method |
| CN110066951A (en) * | 2019-05-21 | 2019-07-30 | 重庆大学 | A kind of super-high-plasticity magnesium alloy and its deformation material preparation method |
| CN113070455A (en) * | 2021-03-19 | 2021-07-06 | 合肥诺瓦新材料科技有限公司 | High-performance LPSO (Long period fiber reinforced SO) type magnesium alloy plate prepared by double-roller casting and rolling and method thereof |
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| CN1851020A (en) * | 2006-05-25 | 2006-10-25 | 上海交通大学 | Authigenic quasicrystal reinforced high plastic deformation magnesium alloy |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104607466A (en) * | 2015-01-14 | 2015-05-13 | 大连理工大学 | Hot rolling machining method for high indoor temperature plastic magnesium alloy plate |
| CN107338379A (en) * | 2017-07-12 | 2017-11-10 | 北京科技大学 | A kind of magnesium Tin-zinc-aluminium manganese wrought magnesium alloy and preparation method thereof |
| CN107338379B (en) * | 2017-07-12 | 2019-02-15 | 北京科技大学 | A kind of magnesium-tin-zinc-aluminium-manganese wrought magnesium alloy and preparation method thereof |
| CN109468560A (en) * | 2019-01-15 | 2019-03-15 | 吉林大学 | Second phase homogenization regulation preparation method in a kind of high aluminium content casting magnesium alloy plate |
| CN109680172A (en) * | 2019-03-08 | 2019-04-26 | 吉林大学 | One kind having weak texture high-strength plasticity low-alloy content magnesium alloy preparation method |
| CN110066951A (en) * | 2019-05-21 | 2019-07-30 | 重庆大学 | A kind of super-high-plasticity magnesium alloy and its deformation material preparation method |
| CN110066951B (en) * | 2019-05-21 | 2021-03-02 | 重庆大学 | Ultrahigh-plasticity magnesium alloy and preparation method of wrought material thereof |
| CN113070455A (en) * | 2021-03-19 | 2021-07-06 | 合肥诺瓦新材料科技有限公司 | High-performance LPSO (Long period fiber reinforced SO) type magnesium alloy plate prepared by double-roller casting and rolling and method thereof |
| CN113070455B (en) * | 2021-03-19 | 2023-09-12 | 合肥诺瓦新材料科技有限公司 | Double-roller casting and rolling method for preparing high-performance LPSO (low-pressure-sensitive adhesive) magnesium alloy plate and method thereof |
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