CN107604272A - A kind of magnesium alloy ingot and preparation method thereof - Google Patents
A kind of magnesium alloy ingot and preparation method thereof Download PDFInfo
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- CN107604272A CN107604272A CN201710847151.4A CN201710847151A CN107604272A CN 107604272 A CN107604272 A CN 107604272A CN 201710847151 A CN201710847151 A CN 201710847151A CN 107604272 A CN107604272 A CN 107604272A
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Abstract
The invention discloses a kind of magnesium alloy ingot and preparation method thereof, the magnesium alloy ingot includes the raw material of following mass percent：Carbon fibre composite 1.5 2.0%, zinc 3.8 5.0%, zirconium 0.5 0.6%, calcium 0.25 0.35%, inevitable impurity≤0.3%, surplus is magnesium.The preparation method of the magnesium alloy ingot includes smelting technology and Technology for Heating Processing, and its smelting technology includes weighing and baking material, melting, refining and standing, casting, and Technology for Heating Processing includes solution treatment and Ageing Treatment.After the magnesium alloy ingot of gained of the invention is by heat treatment, the processing characteristics of alloy cast ingot can be effectively improved, and further refinement is uniform for crystal grain in alloy cast ingot tissue, and hardness increases, overall synthetic performance has strengthened.
Description
Technical field
The invention belongs to alloy field, and in particular to a kind of magnesium alloy ingot and preparation method thereof.
Background technology
Magnesium alloy is most light structural metallic materials, and its specific strength, specific stiffness are very high, is closed than modulus of elasticity and high-strength aluminium
It is golden, steel alloy roughly the same, while there is good damping capacity.Thus this can be given full play of using magnesium alloy materials
Material effectiveness is good, weight is small, cushioning ability is strong, is easy to the characteristics of shaping, and up to now, magnesium alloy materials exist
The field such as aerospace science field and automobile making has a wide range of applications, with the development of material technology, magnesium alloy materials
Tool must have more wide application prospect and use value.
In these years as the increasingly raising of the China Auto Market level of consumption, the recoverable amount of Chinese automobile have significantly
Lifting, and magnesium alloy use can effectively reduce the total quality of automobile on automobile making material, lift the property of automobile
Can, there are energy-conserving and environment-protective, this has also enlivened the development in magnesium alloy market, in addition, in non-ferrous metal industry, magnesium alloy
It as sub-industry, played an important role, can also be carried by manufacturing industry upgrading in the evolution of Chinese manufacturing
Rise competitiveness.Magnesium alloy work industry is a kind of industry of material intensive type, and it is had a great influence by technical factor, therefore casts magnesium and close
Development of the research of technology for gold for magnesium alloy industry has great importance.
But magnesium alloy also exposes the shortcomings that more in use, for example, the hardness of magnesium alloy and plasticity compared with
Difference, the performance showed at high temperature is bad, and corrosion resistance is not also strong, and these shortcomings limit the use of magnesium alloy, are to carry
The intensity of high magnesium alloy, hardness etc. are the main contents of current magnesium alloy technical research, and the present invention is basic magnesium alloy ZK60's
On the basis of analyzed, be modified and tested, add rare earth element and carbon fiber-reinforced material, not only further refined in tissue
Portion's structure, also improve hardness of alloy etc. so that the alloy material combination property prepared is preferable.
The content of the invention
In view of object above, the invention discloses a kind of magnesium alloy ingot and preparation method thereof, by adding rare earth element
With carbon fiber-reinforced material so that hardness and mechanical performance of the magnesium alloy of preparation etc. all make moderate progress.
To achieve these goals, the technical solution adopted by the present invention is：A kind of magnesium alloy ingot, by following quality percentage
The raw material composition of ratio：Carbon fibre composite 1.5-2.0%, zinc 3.8-5.0%, zirconium 0.5-0.6%, calcium 0.25-0.35%, no
Evitable impurity≤0.3%, surplus are magnesium；Wherein, carbon fibre composite is supported rare earth element Y carbon fiber, and it is made
It is for process：
A) surface preparation is carried out to carbon nano-fiber：A certain amount of carbon nano-fiber is placed in beaker and uses deionized water
3-5 rear addition coarsening solution of cleaning is placed in 30-50KHz Ultrasound Instrument tank to be taken out after roughening 25-30min, filters off roughening
Liquid is cleaned 2-4 times with deionized water, then the carbon nano-fiber after roughening is added in sensitization-activating solution, and beaker is placed in into 30-
Shake in 50KHz Ultrasound Instrument tank and taken out after stirring 25-35min, filter off sensitization-activating solution and clean 3- with deionized water
5 times, the carbon nano-fiber of activation is placed in 70 DEG C of drying boxes is dried to constant weight afterwards, it is stand-by；Wherein, coarsening solution component is
2g/L Na and 20ml/L HF mixed solution；Sensitization-activating solution component is 0.5g/L PdCl2、60ml/L HCl、160g/L
NaCl、30g/L SnCl2Mixed solution；
B) supported rare earth element：Pretreated carbon nano-fiber is placed in the beaker for filling appropriate amount of deionized water, will
Beaker, which is placed in concussion in 30-50KHz Ultrasound Instrument tank, makes the carbon nano-fiber in beaker fully dispersed, uses HNO at room temperature3
2h is impregnated, it is neutral to take out and cleaned with deionized water to eluate, by HNO3Carbon nano-fiber after processing is impregnated in quality
Volumetric concentration is 1.2-1.5mg/mL Y (NO3)3Solution in oscillating reactions 2h, after vibration terminate after be well mixed suspended substance
System is through being filtered by vacuum, washing, the presoma of parcel yttrium nitrate is made in drying process, then in high-purity N2Protection under 300-350 DEG C
3-5h is heated, supported rare earth element Y carbon fiber is made.
Wherein, supported rare earth element Y carbon fibre composite combines the advantages of carbon fiber and rare earth oxide, both has
For enhancing of the carbon fiber to alloy, toughening effect, also possess the obstruction that rare earth element recrystallizes to alloy in fusion process and make
With so that alloy can obtain tiny globular crystal tissue, so as to refine alloy inner tissue structure, and rare-earth yttrium and magnesium zinc with
And the mutual of calcium is oozed, and alloy can be made to obtain preferable hardness.
The preparation method of above-mentioned magnesium alloy ingot includes smelting technology and Technology for Heating Processing；Wherein, the smelting technology exists
N2And SF6Carried out under the conditions of mixed gas protected, step is as follows：
(1) weighing and baking material：By material quality percentage, carbon fibre composite, magnesium ingot, zinc ingot metal, magnesium zirconium are weighed respectively
Intermediate alloy and magnesium calcium intermediate alloy；And various raw materials are placed in 230-250 DEG C of preheating furnace and preheat 6-8h；
(2) melting：Magnesium ingot after preheating is placed in melting furnace and is heated to 660-680 DEG C and is completely melt to magnesium ingot, then
740-760 DEG C is warming up to, carbon fibre composite and zinc ingot metal are added into the magnesium liquid of fusing, treats carbon fibre composite and zinc ingot metal
After being completely melt, melt temperature gos up to add preheated Mg-Zr intermediate alloy and magnesium calcium intermediate alloy during to 740-760 DEG C, stirs
Mix to being completely melt, obtain hybrid alloys melt；
(3) refine and stand：Hybrid alloys melt obtained by step (2) is warming up to 780 DEG C, skims surface scum, so
After be uniformly mixed after be incubated 15-30min, refine 3-5min at this temperature, skim surface scum after the completion of refining again, return
780 DEG C are risen to, stands 45-60min；
(4) cast：When alloy melt to be mixed is cooled to 690-700 DEG C after standing, to the steel die heated in advance
In poured into a mould, obtain alloy cast ingot；
Described Technology for Heating Processing is：
The alloy cast ingot that melting is obtained carries out 8-10h solution treatment at a temperature of 430-440 DEG C, then in 140-
20-24h Ageing Treatment is carried out in 150 DEG C of temperature.
Mixed gas N in the smelting technology2And SF6Volume ratio be 5:1.
The preheating temperature of the steel die is 260-300 DEG C.
Mass fraction shared by zirconium is 30% in the Mg-Zr intermediate alloy.
Mass fraction shared by calcium is 20% in the magnesium calcium intermediate alloy.
Beneficial effects of the present invention：The present invention magnesium alloy ingot analyzed on the basis of basic magnesium alloy ZK60,
Modified and experiment, rare earth element and carbon fiber-reinforced material are added, then not only refined in tissue with after heat treatment by melting
Portion's structure, also improve hardness of alloy etc. so that the alloy material combination property prepared is preferable.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.In embodiment, various raw materials are all Marko's ripple
Net product.
Embodiment 1
A kind of magnesium alloy ingot, it is made up of the raw material of following mass percent：
Carbon fibre composite 1.6%, zinc 4.4%, zirconium 0.55%, calcium 0.3%, inevitable impurity≤0.3% are remaining
Measure as magnesium；Wherein, carbon fibre composite is supported rare earth element Y carbon fiber, and its preparation process is：
A) surface preparation is carried out to carbon nano-fiber：2g carbon nano-fiber is placed in beaker and cleaned with deionized water
Addition coarsening solution is placed in 45KHz Ultrasound Instrument tank and taken out after roughening 30min after 5 times, filters off coarsening solution deionized water
Cleaning 4 times, then the carbon nano-fiber after roughening is added in sensitization-activating solution, beaker is placed in 50KHz Ultrasound Instrument tank
Shake and taken out after stirring 35min, filter off sensitization-activating solution and cleaned 5 times with deionized water, afterwards by the Nano carbon fibers of activation
Dimension, which is placed in 70 DEG C of drying boxes, is dried to constant weight, stand-by；Wherein, coarsening solution component is that 2g/L Na and 20ml/L HF mixing are molten
Liquid；Sensitization-activating solution component is 0.5g/L PdCl2、60ml/L HCl、160g/L NaCl、30g/L SnCl2Mixed solution；
B) supported rare earth element：Pretreated carbon nano-fiber is placed in the beaker for filling appropriate amount of deionized water, will
Beaker, which is placed in concussion in 45KHz Ultrasound Instrument tank, makes the carbon nano-fiber in beaker fully dispersed, uses HNO at room temperature3Leaching
Stain 2h, it is neutral to take out and cleaned with deionized water to eluate, by HNO3Carbon nano-fiber after processing is impregnated in 500mL matter
Measure the Y (NO that volumetric concentration is 1.2mg/mL3)3Solution in oscillating reactions 2h, after vibration terminate after be well mixed suspension system
Through being filtered by vacuum, washing, drying process the presoma of parcel yttrium nitrate is made, then in high-purity N2Protection it is lower 300 DEG C heating 4h,
Supported rare earth element Y carbon fiber is made.
The preparation method of above-mentioned magnesium alloy ingot includes smelting technology and Technology for Heating Processing；Wherein, the smelting technology exists
N2And SF6Carried out under the conditions of mixed gas protected, step is as follows：
(1) weighing and baking material：By material quality percentage, carbon fibre composite, magnesium ingot, zinc ingot metal, magnesium zirconium are weighed respectively
Intermediate alloy and magnesium calcium intermediate alloy；And various raw materials are placed in 240 DEG C of preheating furnace and preheat 8h；
(2) melting：Magnesium ingot after preheating is placed in melting furnace and is heated to 670 DEG C and is completely melt to magnesium ingot, is then heated up
To 760 DEG C, carbon fibre composite and zinc ingot metal are added into the magnesium liquid of fusing, treats that carbon fibre composite and zinc ingot metal are completely melt
Afterwards, preheated Mg-Zr intermediate alloy and magnesium calcium intermediate alloy are added when melt temperature gos up to 760 DEG C, is stirred to completely molten
Change, obtain hybrid alloys melt；
(3) refine and stand：Hybrid alloys melt obtained by step (2) is warming up to 780 DEG C, skims surface scum, so
After be uniformly mixed after be incubated 30min, refine 5min at this temperature, skim surface scum after the completion of refining again, go up extremely
780 DEG C, stand 60min；
(4) cast：When alloy melt to be mixed is cooled to 700 DEG C after standing, to the steel die for being previously heated to 300 DEG C
In poured into a mould, obtain alloy cast ingot；
Described Technology for Heating Processing is：
The alloy cast ingot that melting obtains is carried out to 10h solution treatment at a temperature of 430 DEG C, then in 150 DEG C of temperature
Carry out 24h Ageing Treatment.
Embodiment 2
A kind of magnesium alloy ingot, it is made up of the raw material of following mass percent：
Carbon fibre composite 2.0%, zinc 4.8%, zirconium 0.55%, calcium 0.35%, inevitable impurity≤0.3%,
Surplus is magnesium；Wherein, carbon fibre composite is supported rare earth element Y carbon fiber, and its preparation process is：
A) surface preparation is carried out to carbon nano-fiber：2g carbon nano-fiber is placed in beaker and cleaned with deionized water
Addition coarsening solution is placed in 50KHz Ultrasound Instrument tank and taken out after roughening 30min after 5 times, filters off coarsening solution deionized water
Cleaning 4 times, then the carbon nano-fiber after roughening is added in sensitization-activating solution, beaker is placed in 50KHz Ultrasound Instrument tank
Shake and taken out after stirring 35min, filter off sensitization-activating solution and cleaned 5 times with deionized water, afterwards by the Nano carbon fibers of activation
Dimension, which is placed in 70 DEG C of drying boxes, is dried to constant weight, stand-by；Wherein, coarsening solution component is that 2g/L Na and 20ml/L HF mixing are molten
Liquid；Sensitization-activating solution component is 0.5g/L PdCl2、60ml/L HCl、160g/L NaCl、30g/L SnCl2Mixed solution；
B) supported rare earth element：Pretreated carbon nano-fiber is placed in the beaker for filling appropriate amount of deionized water, will
Beaker, which is placed in concussion in 50KHz Ultrasound Instrument tank, makes the carbon nano-fiber in beaker fully dispersed, uses HNO at room temperature3Leaching
Stain 2h, it is neutral to take out and cleaned with deionized water to eluate, by HNO3Carbon nano-fiber after processing is impregnated in 500mL matter
Measure the Y (NO that volumetric concentration is 1.5mg/mL3)3Solution in oscillating reactions 2h, after vibration terminate after be well mixed suspension system
Through being filtered by vacuum, washing, drying process the presoma of parcel yttrium nitrate is made, then in high-purity N2Protection it is lower 300 DEG C heating 5h,
Supported rare earth element Y carbon fiber is made.
The preparation method of above-mentioned magnesium alloy ingot includes smelting technology and Technology for Heating Processing；Wherein, the smelting technology exists
N2And SF6Carried out under the conditions of mixed gas protected, step is as follows：
(1) weighing and baking material：By material quality percentage, carbon fibre composite, magnesium ingot, zinc ingot metal, magnesium zirconium are weighed respectively
Intermediate alloy and magnesium calcium intermediate alloy；And various raw materials are placed in 240 DEG C of preheating furnace and preheat 8h；
(2) melting：Magnesium ingot after preheating is placed in melting furnace and is heated to 680 DEG C and is completely melt to magnesium ingot, is then heated up
To 760 DEG C, carbon fibre composite and zinc ingot metal are added into the magnesium liquid of fusing, treats that carbon fibre composite and zinc ingot metal are completely melt
Afterwards, preheated Mg-Zr intermediate alloy and magnesium calcium intermediate alloy are added when melt temperature gos up to 760 DEG C, is stirred to completely molten
Change, obtain hybrid alloys melt；
(3) refine and stand：Hybrid alloys melt obtained by step (2) is warming up to 780 DEG C, skims surface scum, so
After be uniformly mixed after be incubated 30min, refine 5min at this temperature, skim surface scum after the completion of refining again, go up extremely
780 DEG C, stand 60min；
(4) cast：When alloy melt to be mixed is cooled to 700 DEG C after standing, to the steel die for being previously heated to 300 DEG C
In poured into a mould, obtain alloy cast ingot；
Described Technology for Heating Processing is：
The alloy cast ingot that melting obtains is carried out to 10h solution treatment at a temperature of 430 DEG C, then in 150 DEG C of temperature
Carry out 24h Ageing Treatment.
After testing, the technical parameter of magnesium alloy ingot produced by the present invention is as follows：
Claims (6)
1. a kind of magnesium alloy ingot, it is characterised in that be made up of the raw material of following mass percent：Carbon fibre composite 1.5-
2.0%, zinc 3.8-5.0%, zirconium 0.5-0.6%, calcium 0.25-0.35%, inevitable impurity≤0.3%, surplus is magnesium；Its
In, carbon fibre composite is supported rare earth element Y carbon fiber, and its preparation process is：
A) surface preparation is carried out to carbon nano-fiber：A certain amount of carbon nano-fiber is placed in beaker and cleaned with deionized water
Addition coarsening solution is placed in 30-50KHz Ultrasound Instrument tank and taken out after roughening 25-30min after 3-5 times, filters off coarsening solution and uses
Deionized water is cleaned 2-4 times, then the carbon nano-fiber after roughening is added in sensitization-activating solution, and beaker is placed in into 30-50KHz
Ultrasound Instrument tank in shake and taken out after stirring 25-35min, filter off sensitization-activating solution and simultaneously cleaned 3-5 times with deionized water,
The carbon nano-fiber of activation is placed in 70 DEG C of drying boxes afterwards and is dried to constant weight, it is stand-by；Wherein, coarsening solution component is 2g/L
Na and 20ml/L HF mixed solution；Sensitization-activating solution component is 0.5g/L PdCl2、60ml/L HCl、160g/L NaCl、
30g/L SnCl2Mixed solution；
B) supported rare earth element：Pretreated carbon nano-fiber is placed in the beaker for filling appropriate amount of deionized water, by beaker
Being placed in concussion in 30-50KHz Ultrasound Instrument tank makes the carbon nano-fiber in beaker fully dispersed, uses HNO at room temperature3Dipping
2h, it is neutral to take out and cleaned with deionized water to eluate, by HNO3Carbon nano-fiber after processing is impregnated in quality volume
Concentration is 1.2-1.5mg/mL Y (NO3)3Solution in oscillating reactions 2h, after vibration terminate after be well mixed suspension system warp
The presoma for wrapping up yttrium nitrate is made in vacuum filtration, washing, drying process, then in high-purity N2Protection under 300-350 DEG C heating
3-5h, supported rare earth element Y carbon fiber is made.
2. the preparation method of a kind of magnesium alloy ingot described in claim 1, it is characterised in that the preparation method includes melting
Technique and Technology for Heating Processing；Wherein, the smelting technology is in N2And SF6Carried out under the conditions of mixed gas protected, step is as follows：
(1) weighing and baking material：By material quality percentage, weigh respectively carbon fibre composite, magnesium ingot, zinc ingot metal, among magnesium zirconium
Alloy and magnesium calcium intermediate alloy；And various raw materials are placed in 230-250 DEG C of preheating furnace and preheat 6-8h；
(2) melting：Magnesium ingot after preheating is placed in melting furnace and is heated to 660-680 DEG C and is completely melt to magnesium ingot, is then heated up
To 740-760 DEG C, carbon fibre composite and zinc ingot metal are added into the magnesium liquid of fusing, treats that carbon fibre composite and zinc ingot metal are complete
After fusing, melt temperature gos up to add preheated Mg-Zr intermediate alloy and magnesium calcium intermediate alloy during to 740-760 DEG C, and stirring is extremely
It is completely melt, obtains hybrid alloys melt；
(3) refine and stand：Hybrid alloys melt obtained by step (2) is warming up to 780 DEG C, surface scum is skimmed, then stirs
Mix and be incubated 15-30min after being well mixed, refine 3-5min at this temperature, skim surface scum after the completion of refining again, go up extremely
780 DEG C, stand 45-60min；
(4) cast：When alloy melt to be mixed is cooled to 690-700 DEG C after standing, enter into the steel die heated in advance
Row cast, obtains alloy cast ingot；
Described Technology for Heating Processing is：
The alloy cast ingot that melting is obtained carries out 8-10h solution treatment at a temperature of 430-440 DEG C, then at 140-150 DEG C
20-24h Ageing Treatment is carried out in temperature.
A kind of 3. preparation method of magnesium alloy ingot according to claim 2, it is characterised in that：Mixed in the smelting technology
Close gas N2And SF6Volume ratio be 5:1.
A kind of 4. preparation method of magnesium alloy ingot according to claim 2, it is characterised in that：The steel die it is pre-
Hot temperature is 260-300 DEG C.
A kind of 5. preparation method of magnesium alloy ingot according to claim 2, it is characterised in that：The Mg-Zr intermediate alloy
Mass fraction shared by middle zirconium is 30%.
A kind of 6. preparation method of magnesium alloy ingot according to claim 2, it is characterised in that：The magnesium calcium intermediate alloy
Mass fraction shared by middle calcium is 20%.
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