CN108823475A - A kind of preparation method of the magnesium titanium alloy plate of high rare-earth content - Google Patents
A kind of preparation method of the magnesium titanium alloy plate of high rare-earth content Download PDFInfo
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- CN108823475A CN108823475A CN201810966261.7A CN201810966261A CN108823475A CN 108823475 A CN108823475 A CN 108823475A CN 201810966261 A CN201810966261 A CN 201810966261A CN 108823475 A CN108823475 A CN 108823475A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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- 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
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- 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
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Abstract
The present invention relates to a kind of preparation methods of the magnesium titanium alloy plate of high rare-earth content, it is using magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy as raw material, through vacuum melting furnace melting, cast molding, Homogenization Treatments, roll forming, ageing treatment, the magnesium titanium alloy plate of high rare-earth content is made, tensile strength reaches 477MPa, and for elongation percentage up to 6.4%, this preparation method technique is advanced, data are accurately full and accurate, are the methods of the advanced magnesium titanium alloy plate for preparing high rare-earth content.
Description
Technical field
The present invention relates to a kind of preparation methods of the magnesium titanium alloy plate of high rare-earth content, belong to nonferrous materials preparation
And the technical field of application.
Background technique
Magnesium alloy is known as 21 century most potential environmentally protective engineering material, is gold most light in current engineer application
Belong to structural material, it has, and density is small, specific strength and specific stiffness are high, damping property is good, electrical and thermal conductivity performance is good, machining property
The excellent feature of energy has obvious action at product structure lightweight, reduction energy consumption, the aspect that reduces environmental pollution,
Aerospace, electronics industry, defence and military, automobile manufacturing field have obtained wide application；But the obdurability of magnesium alloy is low,
Plasticity is poor, high temperature resistance is poor, make its industrially application receive great limitation.
Alloying cooperates suitable roll forming technique and heat treatment process can effectively improve the obdurability of magnesium alloy, special
It is not that rare earth element and titanium elements significant effect are added into alloy, rare earth element has purification alloy, improvement group to magnesium alloy
The effect of mechanical property is knitted and improved, and significant precipitation strength can be generated by Homogenization Treatments and ageing treatment；Titanium tool
There are a good high temperature resistant, low temperature resistant, anti-strong acid, anti-highly basic, and is " space gold by good reputation the characteristics of high-intensitive, low-density
Belong to ".The crystal structure of titanium and magnesium is all close-packed hexagonal and has symbiosis and epibiosis, and titanium elements can be used as the heterogeneous crystalline substance in magnesium matrix
Core refines α-Mg crystal grain, thus suitable additions titanium elements can great Refining Mg Alloy tissue, effectively improve alloy property.
But titanium elements fusing point is higher to have very low intersolubility with magnesium, is difficult to be added directly into magnesium alloy.Therefore, develop a kind of high dilute
The magnesium titanium alloy plate of native content has great importance for expanding magnesium alloy application range.
Currently, the magnesium titanium alloy plate of high rare-earth content is also in conceptual phase, technology is also in scientific research.
Summary of the invention
Goal of the invention
The purpose of the present invention is being directed to background technique, with magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy
High rare-earth content is made through vacuum melting furnace melting, cast molding, Homogenization Treatments, roll forming, ageing treatment for raw material
Magnesium titanium alloy plate, to improve the mechanical property of magnesium alloy plate.
Technical solution
The chemical substance material that the present invention uses is：Magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy, magnesia,
Waterglass, deionized water, argon gas, it is as follows that a combination thereof prepares dosage：With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows：
(1) solid slug material is pre-processed
1. magnesium, zinc, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy are placed on steel plate, are cut into machinery by stripping and slicing
Block, block size≤20mm × 20mm × 20mm；
2. being cleaned to magnesium, zinc, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy with dehydrated alcohol after stripping and slicing；
3. postposition preheating and drying in a vacuum drying oven is cleaned, 120 DEG C of preheating and drying temperature, vacuum degree 2Pa, drying time
40min；
(2) coating agent is prepared
Weigh magnesia 50g ± 1g, measure waterglass 10mL ± 1mL, deionized water 500mL ± 1mL, mixing hollander is added
In be stirred, after mixing evenly at milky suspension liquid, i.e. coating agent；
(3) retractable die is prepared
Retractable die makes of stainless steel material, and mold cavity is in rectangle, and mold cavity surface roughness is Ra0.08-0.16
μm；
(4) melting prepares magnesium alloy ingot
The melting of magnesium alloy ingot is carried out in vacuum melting furnace, is in mid-frequency induction heating, is vacuumized, argon gas bottom
It blows, completion during cast molding；
1. pre-processing retractable die
With washes of absolute alcohol retractable die type chamber, it is allowed to clean；
Retractable die mold cavity surface, surface coating layer thickness 0.5mm are uniformly coated with the coating agent of preparation；
Retractable die is placed in drying box and is preheated, 150 DEG C of preheating temperature, preheating time 30min；
2. opening vacuum melting furnace, clear up inside melting kettle, and cleaned with dehydrated alcohol, makes clean inside crucible
Only；
3. weighing MAG block 1396g ± 0.01g, spelter 24g ± 0.01g, titanium valve 20g ± 0.01g, magnesium gadolinium intermediate alloy block
640g ± 0.01g, magnesium yttrium intermediate alloy block 320g ± 0.01g, are placed in crucible bottom；
4. closing vacuum melting furnace, and closed；
Vacuum pump is opened, furnace air is extracted, and pressure in furnace is made to reach 2Pa；
Medium frequency induction heater is opened, is begun to warm up, 750 DEG C ± 1 DEG C of heating temperature, smelting time 60min is heated；
5. being passed through argon gas bottom blowpipe in crucible bottom, argon gas, argon gas bottom blowing speed 150cm are inputted into crucible3/ min, makes
Invariablenes pressure of liquid regulates and controls in 1 atmospheric pressure, and by outlet pipe valve in furnace；
Alloying reaction, reaction equation will occur in fusion process for magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy
It is as follows：
In formula：Mg24(Gd,Y,Zn)5：Magnesium gadolinium yttrium zinc eutectic phase
(Mg,Zn)3(Gd,Y)：Magnesium gadolinium yttrium zinc eutectic phase
α-Mg：Matrix phase
α-Ti：Matrix phase
At alloy molten solution after melting, heating temperature is down to 720 DEG C ± 1 DEG C, keeps the temperature 10min in this thermostatic；
6. casting
Close argon gas bottom blowpipe；
Open vacuum melting furnace；
Remove melting kettle inner melt surface slag；
It is directed at the retractable die cast gate of preheating, is cast, until casting is full；
7. cooling down, the retractable die for alloy molten solution of having cast is put into vacuum cooled furnace to cooling, vacuum degree 2Pa, it is cold
But 20 DEG C of temperature；
8. being opened, retractable die is opened, takes out casting, i.e. magnesium alloy ingot；
(5) Homogenization Treatments magnesium alloy ingot
The magnesium alloy ingot of preparation is placed in heat-treatment furnace and carries out Homogenization Treatments, homogenization temperature is 520 DEG C, and constant temperature is protected
The warm time is 10h, is passed through argon gas and is protected, and it is 100cm that argon gas, which is passed through speed,3/min；It is after constant temperature heat preservation, magnesium alloy ingot is fast
Speed, which is placed in 70 DEG C of warm water, carries out cooling treatment, cooling time 50s；
Magnesium gadolinium yttrium zinc eutectic phase, matrix mutually will undergo phase transition reaction during Homogenization Treatments, and reaction equation is as follows：
In formula：Mg12(Gd,Y)Zn：Long-periodic structure phase
(6) magnesium alloy plate is rolled
The rolling of magnesium alloy plate is carried out on double-roll rolling mill, is deformed in heating of plate blank, roll pressurization, material
It is completed in journey；
Adjust the distance between topping roll and bottom roll；
The double roller rotating mechanism of milling train is opened, the rotation direction of topping roll is the rotation direction of bottom roll clockwise
For counter clockwise direction, revolving speed 10r/min；
It is the slab of 16mm thickness by the magnesium alloy ingot machine cuts after Homogenization Treatments, slab is placed at 500 DEG C of heat
30min is kept the temperature in reason furnace, carries out 14 passes from right to left later, per pass rolling reduction about 10%, it will between passage
Plate, which is placed in heat-treatment furnace, keeps the temperature 8min；
Final rolling deformation total amount is 76%, and magnesium alloy plate is with a thickness of 3.8mm；
(7) magnesium alloy plate is placed in heat-treatment furnace and carries out ageing treatment, aging temp is 220 DEG C, when constant temperature is kept the temperature
Between be 58h；Then magnesium alloy plate is quickly placed into 20 DEG C of water and carries out cooling treatment, cooling time 35s, be after cooling
The magnesium titanium alloy plate of high rare-earth content；
(8) it clears up, clean magnesium titanium alloy plate
The magnesium titanium alloy plate of high rare-earth content is placed on steel plate, with the positive and negative surface of sand paper polishing and periphery, is made
Any surface finish；
Then with each portion of washes of absolute alcohol, make its cleaning；
(9) it is dried in vacuo magnesium titanium alloy plate
The magnesium titanium alloy plate of high rare-earth content is placed in a vacuum drying oven, 80 DEG C of drying temperature, vacuum degree 2Pa, is done
Dry time 10min, at final product；
(10) test, analysis and characterization
The pattern of the magnesium titanium alloy plate of the high rare-earth content of preparation, metallographic structure, mechanical property are detected, divided
Analysis, characterization；
Metallographic structure analysis is carried out with Metallographic Analysis instrument；
Tensile strength analysis is carried out with microcomputer controlled electronic universal tester；
Conclusion：The magnesium titanium alloy plate of high rare-earth content is silver gray plate, and recrystal grain distribution is equal in metallographic structure
Even, crystal grain is tiny, mainly contains α-Mg matrix phase, α-Ti matrix phase, the Luan Jing of crisscross distribution, fibrous long-periodic structure phase
Mg12(Gd, Y) Zn, strength of alloy reach 477Mpa, and elongation percentage is up to 6.4%.
Beneficial effect
There is apparent advance compared with the background technology, the present invention, be in magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium
Between alloy be raw material, through vacuum melting furnace melting, argon gas protection, cast molding, Homogenization Treatments, roll forming, ageing treatment,
The magnesium titanium alloy plate of high rare-earth content is made, tensile strength reaches 477MPa, and for elongation percentage up to 6.4%, this preparation method technique is first
Into data are accurately full and accurate, are the methods of the advanced magnesium titanium alloy plate for preparing high rare-earth content.
Detailed description of the invention
Fig. 1, the magnesium titanium alloy plate rolling state diagram of high rare-earth content；
Fig. 2, the magnesium titanium alloy plate cross section metallographic structure figure of high rare-earth content；
Fig. 3, the magnesium titanium alloy plate stretch stress-strain curve diagram of high rare-earth content；
As shown in the figure, list of numerals is as follows：
1, double-roll rolling mill footstock, 2, topping roll heating rotating mechanism, 3, topping roll, 4, magnesium alloy plate, 5, bottom roll, 6,
Bottom roll heats rotating mechanism, 7, double-roll rolling mill pedestal, 8, double roller space regulator, 9, roll work light, and 10, double roller rolls
Electromechanical source indicator light, 11, roll rotation controller, 12, double-roll rolling mill power switch, 13, double-roll rolling mill electric cabinet.
Specific embodiment
The present invention will be further described below with reference to the accompanying drawings：
It is the magnesium titanium alloy plate rolling state diagram of high rare-earth content shown in Fig. 1, each portion position will be correctly arranged according to quantity,
Sequentially operate.
Preparing the magnitude of chemical substance used is determined by pre-set range, with millimeter, milliliter, centimetre3For
Measurement unit.
The rolling of magnesium alloy plate is carried out on double-roll rolling mill, is deformed in heating of plate blank, roll pressurization, material
It is completed in journey；
Double-roll rolling mill be it is vertical, the upper right quarter of double-roll rolling mill pedestal 7 is double-roll rolling mill electric cabinet 13, double-roll rolling mill electric cabinet
13 are equipped with double roller space regulator 8, roll work light 9, double-roll rolling mill power supply indicator 10, roll rotation controller
11, double-roll rolling mill power switch 12；It is that bottom roll heats rotating mechanism 6, bottom roll heating in the upper left quarter of double-roll rolling mill pedestal 1
Rotating mechanism 6 couples bottom roll 5；Topping roll is equipped in 1 lower part of double-roll rolling mill footstock and heats rotating mechanism 2, and topping roll heating turns
Motivation structure 2 couples topping roll 3；It is magnesium alloy plate 4 between topping roll 3 and bottom roll 5；The rolling direction of magnesium alloy plate 4 is
From right to left.
It is the magnesium titanium alloy plate cross section metallographic structure figure of high rare-earth content shown in Fig. 2, as shown in the figure, recrystallization is brilliant
Grain is evenly distributed, and crystal grain is tiny, mainly contains α-Mg matrix phase, α-Ti matrix phase, the Luan Jing of crisscross distribution, fibrous long period
Structure phase Mg12(Gd,Y)Zn。
It is the tensile stress strain curve figure of the magnesium titanium alloy plate of high rare-earth content shown in Fig. 3, it is as shown in the figure, high dilute
The tensile strength of the magnesium titanium alloy plate of native content is up to 477MPa, and elongation is up to 6.4%.
Claims (2)
1. a kind of preparation method of the magnesium titanium alloy plate of high rare-earth content, it is characterised in that：The chemical substance material used is：
Magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy, magnesia, waterglass, deionized water, argon gas, a combination thereof prepare dosage
It is as follows：With gram, milliliter, centimetre3For measurement unit
Preparation method is as follows：
(1) solid slug material is pre-processed
1. magnesium, zinc, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy are placed on steel plate, block blocking with mechanical cutting by stripping and slicing
Body size≤20mm × 20mm × 20mm；
2. being cleaned to magnesium, zinc, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy with dehydrated alcohol after stripping and slicing；
3. postposition preheating and drying in a vacuum drying oven is cleaned, 120 DEG C of preheating and drying temperature, vacuum degree 2Pa, drying time
40min；
(2) coating agent is prepared
Weigh magnesia 50g ± 1g, measure waterglass 10mL ± 1mL, deionized water 500mL ± 1mL, be added in mixing hollander into
Row stirring, after mixing evenly at milky suspension liquid, i.e. coating agent；
(3) retractable die is prepared
Retractable die makes of stainless steel material, and mold cavity is in rectangle, and mold cavity surface roughness is Ra0.08-0.16 μm；
(4) melting prepares magnesium alloy ingot
The melting of magnesium alloy ingot is carried out in vacuum melting furnace, is in mid-frequency induction heating, is vacuumized, argon gas bottom blowing, pours
It is completed during type casting moulding；
1. pre-processing retractable die
With washes of absolute alcohol retractable die type chamber, it is allowed to clean；
Retractable die mold cavity surface, surface coating layer thickness 0.5mm are uniformly coated with the coating agent of preparation；
Retractable die is placed in drying box and is preheated, 150 DEG C of preheating temperature, preheating time 30min；
2. opening vacuum melting furnace, clear up inside melting kettle, and cleaned with dehydrated alcohol, makes clean inside crucible；
3. weigh MAG block 1396g ± 0.01g, spelter 24g ± 0.01g, titanium valve 20g ± 0.01g, magnesium gadolinium intermediate alloy block 640g ±
0.01g, magnesium yttrium intermediate alloy block 320g ± 0.01g, are placed in crucible bottom；
4. closing vacuum melting furnace, and closed；
Vacuum pump is opened, furnace air is extracted, and pressure in furnace is made to reach 2Pa；
Medium frequency induction heater is opened, is begun to warm up, 750 DEG C ± 1 DEG C of heating temperature, smelting time 60min is heated；
5. being passed through argon gas bottom blowpipe in crucible bottom, argon gas, argon gas bottom blowing speed 150cm are inputted into crucible3/ min, makes in furnace
Invariablenes pressure of liquid regulates and controls in 1 atmospheric pressure, and by outlet pipe valve；
Alloying reaction will occur in fusion process for magnesium, zinc, titanium, magnesium yttrium intermediate alloy, magnesium gadolinium intermediate alloy, and reaction equation is such as
Under：
In formula：Mg24(Gd,Y,Zn)5：Magnesium gadolinium yttrium zinc eutectic phase
(Mg,Zn)3(Gd,Y)：Magnesium gadolinium yttrium zinc eutectic phase
α-Mg：Matrix phase
α-Ti：Matrix phase
At alloy molten solution after melting, heating temperature is down to 720 DEG C ± 1 DEG C, keeps the temperature 10min in this thermostatic；
6. casting
Close argon gas bottom blowpipe；
Open vacuum melting furnace；
Remove melting kettle inner melt surface slag；
It is directed at the retractable die cast gate of preheating, is cast, until casting is full；
7. cooling down, the retractable die for alloy molten solution of having cast is put into vacuum cooled furnace to cooling, vacuum degree 2Pa, cooling temperature
20 DEG C of degree；
8. being opened, retractable die is opened, takes out casting, i.e. magnesium alloy ingot；
(5) Homogenization Treatments magnesium alloy ingot
The magnesium alloy ingot of preparation is placed in heat-treatment furnace and carries out Homogenization Treatments, homogenization temperature is 520 DEG C, when constant temperature is kept the temperature
Between be 10h, be passed through argon gas and protected, argon gas be passed through speed be 100cm3/min；After constant temperature heat preservation, magnesium alloy ingot is quickly set
Carry out cooling treatment in 70 DEG C of warm water, cooling time 50s；
Magnesium gadolinium yttrium zinc eutectic phase, matrix mutually will undergo phase transition reaction during Homogenization Treatments, and reaction equation is as follows：
In formula：Mg12(Gd,Y)Zn：Long-periodic structure phase
(6) magnesium alloy plate is rolled
The rolling of magnesium alloy plate is carried out on double-roll rolling mill, is in heating of plate blank, roll pressurization, material deformation process
It completes；
Adjust the distance between topping roll and bottom roll；
The double roller rotating mechanism of milling train is opened, the rotation direction of topping roll is that clockwise, the rotation direction of bottom roll is inverse
Clockwise, revolving speed 10r/min；
It is the slab of 16mm thickness by the magnesium alloy ingot machine cuts after Homogenization Treatments, slab is placed in 500 DEG C of heat-treatment furnace
Middle heat preservation 30min carries out 14 passes from right to left, per pass rolling reduction about 10% later, by plate between passage
It is placed in heat-treatment furnace and keeps the temperature 8min；
Final rolling deformation total amount is 76%, and magnesium alloy plate is with a thickness of 3.8mm；
(7) magnesium alloy plate is placed in heat-treatment furnace and carries out ageing treatment, aging temp is 220 DEG C, and constant temperature soaking time is
58h；Then magnesium alloy plate is quickly placed into 20 DEG C of water and carries out cooling treatment, cooling time, 35s, was high dilute after cooling
The magnesium titanium alloy plate of native content；
(8) it clears up, clean magnesium titanium alloy plate
The magnesium titanium alloy plate of high rare-earth content is placed on steel plate, with the positive and negative surface of sand paper polishing and periphery, makes surface
It is bright and clean；
Then with each portion of washes of absolute alcohol, make its cleaning；
(9) it is dried in vacuo magnesium titanium alloy plate
The magnesium titanium alloy plate of high rare-earth content is placed in a vacuum drying oven, 80 DEG C of drying temperature, vacuum degree 2Pa, when dry
Between 10min, at final product；
(10) test, analysis and characterization
The pattern of the magnesium titanium alloy plate of the high rare-earth content of preparation, metallographic structure, mechanical property are detected, analyzed, table
Sign；
Metallographic structure analysis is carried out with Metallographic Analysis instrument；
Tensile strength analysis is carried out with microcomputer controlled electronic universal tester；
Conclusion：The magnesium titanium alloy plate of high rare-earth content is silver gray plate, and recrystal grain is evenly distributed in metallographic structure, brilliant
Grain is tiny, mainly contains α-Mg matrix phase, α-Ti matrix phase, the Luan Jing of crisscross distribution, fibrous long-periodic structure phase Mg12(Gd,
Y) Zn, strength of alloy reach 477Mpa, and elongation percentage is up to 6.4%.
2. a kind of preparation method of the magnesium titanium alloy plate of high rare-earth content according to claim 1, it is characterised in that：Magnesium
The rolling of sheet alloy is carried out on double-roll rolling mill, is completed in heating of plate blank, roll pressurization, material deformation process
's；
Double-roll rolling mill be it is vertical, the upper right quarter of double-roll rolling mill pedestal 7 is double-roll rolling mill electric cabinet 13, on double-roll rolling mill electric cabinet 13
Equipped with double roller space regulator 8, roll work light 9, double-roll rolling mill power supply indicator 10, roll rotation controller 11, double
Roller mill power switch 12；It is that bottom roll heats rotating mechanism 6, bottom roll heating rotation in the upper left quarter of double-roll rolling mill pedestal 1
Mechanism 6 couples bottom roll 5；Topping roll is equipped in 1 lower part of double-roll rolling mill footstock and heats rotating mechanism 2, and topping roll heats rotating machine
Structure 2 couples topping roll 3；It is magnesium alloy plate 4 between topping roll 3 and bottom roll 5；The rolling direction of magnesium alloy plate 4 is by the right side
To the left.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113881879A (en) * | 2021-09-27 | 2022-01-04 | 中北大学 | Preparation method of magnesium-zinc alloy plate |
| CN117344166A (en) * | 2023-12-05 | 2024-01-05 | 成都先进金属材料产业技术研究院股份有限公司 | High-homogeneity titanium alloy cast ingot and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113881879A (en) * | 2021-09-27 | 2022-01-04 | 中北大学 | Preparation method of magnesium-zinc alloy plate |
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| CN117344166B (en) * | 2023-12-05 | 2024-03-08 | 成都先进金属材料产业技术研究院股份有限公司 | High-homogeneity titanium alloy cast ingot and preparation method thereof |
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Application publication date: 20181116 |