CN104498746B - Method for preparing Al-5Ti-1B-1(La+Ce) intermediate alloy grain refiner having different content of lanthanum and cerium - Google Patents
Method for preparing Al-5Ti-1B-1(La+Ce) intermediate alloy grain refiner having different content of lanthanum and cerium Download PDFInfo
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Abstract
The invention discloses a method for preparing an Al-5Ti-1B-1RE intermediate alloy grain refiner having different content of lanthanum and cerium. The Al-5Ti-1B-1RE intermediate alloy grain refiner is prepared by a fluorine salt reaction method. La and Ce are added into an Al-Ti-B intermediate alloy to generate compounds of Al, Ti, La and Ce, namely, Ti2Al20La and Ti2Al20Ce. By designing Al-Ti-B-(La+Ce) intermediate alloys having different percentage content of lanthanum and cerium, the Al-Ti-B-(La+Ce) intermediate alloy grain refiner having optimal percentage content of lanthanum and cerium is sought. The method has the beneficial effects that second phase particles TiB2, TiAl3, Ti2Al20La and Ti2Al20Ce in the Al-Ti-B-(La+Ce) intermediate alloy grain refiner having optimal percentage content of lanthanum and cerium are fine and uniformly dispersed and meet the usage requirements of sheets or foils; the Al-Ti-B-(La+Ce) intermediate alloy grain refiner having optimal percentage content of lanthanum and cerium, which is prepared by the method, has better grain refining capacity on industrial pure aluminum and alloys thereof than that of the Al-Ti-B intermediate alloy grain refiner at home and abroad under the same conditions.
Description
Technical field
The invention belongs to aluminium applied technical field.Specifically different lanthanum cerium content al-5ti-1b-1 (la+ce) intermediate alloys
The preparation method of grain refiner.
Background technology
Fine aluminium has fusing point low (660 DEG C), little (ρ=2.7 × 10 of density3kg/m3), plasticity height (ψ=80%), low intensity
(σb=80mpa) the features such as.The density of aluminium alloy also very little, after heat treatment, intensity is high, σb=490～588mpa, therefore, aluminium closes
Gold utensil has very high specific strength (σb/ ρ), it is important aerospace structure material.And, the heat conduction of fine aluminium and electric conductivity are good
Good, it is only second to silver and copper.Again because the surface of aluminium easily generates the al of densification2o3Oxide-film, therefore, aluminium has good anti-corrosion
Property.Because aluminium and its alloy have such excellent properties, therefore, it is widely used in industry, agricultural, transportation and military affairs
In field, also it is widely used as family life apparatus, sports goods and building structural materials etc..As various instrument and meter housings,
Automobile engine, automobile gearbox, seagoing vessel part, fishing rod, dental equipment, airplane spare parts, pottery and golf clubs etc..
With the fast development of Chinese national economy, the product such as aluminium and its Alloy Foil, plate, band is in Aero-Space, machinery system
Make etc. in national economy and have been obtained for extensively applying.However, while aluminium and its alloy development, each to aluminium and its alloy
Item performance etc. it is also proposed higher and higher requirement.Crystal grain refinement is the important means obtaining premium properties aluminium alloy.Aluminium and its
The crystal grain refinement of alloy has very important meaning to raising aluminium and its mechanical property of alloy and process industrial art performance.Aluminium and
The crystal grain refinement of its alloy can make aluminium and its alloy obtain tiny equi-axed crystal, therefore, except obtaining superior mechanicalness
Can be outer, also can obtain good surface smoothness etc..Crystal grain refinement can be realized by way of different, such as non-homogeneous shape
Core, method for quick cooling, additionally, also stirring of melt etc..Adding fining agent in melt is most economical, maximally effective refinement side
Method.
Al-ti-b Master alloy refiners are a kind of current widely used in the world high-efficiency aluminum and its alloy grain refinement
Agent, has good in refining effect, easy to control and low cost and other advantages.Since the sixties in 20th century, al-ti-b intermediate alloy is with regard to one
Directly it is used for refining aluminium and its alloy.With the continuous improvement of al-ti-b intermediate alloy quality, the application in modern aluminum industry
Also increasingly extensive.But still have several drawbacks in terms of the quality and its production technology of al-ti-b intermediate alloy both at home and abroad at present:
1) second in al-ti-b intermediate alloy mutually has tib2, tial3, alb2, (al, ti) b2Deng particle, but, only
Particle less than 1% really plays the effect of heterogeneous nucleation, and therefore, forming core potential is far from bringing into play；
2) in al-ti-b intermediate alloy, impurity content is higher, refine aluminium and its also pollute while alloy aluminium and its
Alloy；
3) tib in al-ti-b intermediate alloy2Particle size larger (as 0.5-3 μm), and it is easy to assemble agglomerating, thus
Greatly reduce al-ti-b intermediate alloy grain refining efficiency；tib2Also with elements such as mn, cr, zr, interfacial reaction can occur, lead to thin
Agent is poisoned.
4), when al-ti-b intermediate alloy refines aluminium and its alloy, thinning effect is unstable.Accordingly, it is difficult to control aluminum products
Product quality.
Therefore, develop, develop efficient, stable, clean al-ti-b Master alloy refiners of new generation, it has also become people
Current urgent problem.
The addition of rare earth, can effectively make up the deficiency of above al-ti-b Master alloy refiners, therefore, develop
Go out efficient, clean, the stable al-ti-b-re intermediate alloy grain refiner of a new generation, there is wide market application foreground.
Content of the invention
The present invention closes to overcome the deficiencies in the prior art to provide in the middle of different lanthanums cerium content al-5ti-1b-1 (la+ce)
The preparation method of golden grain refiner.
The technical scheme is that
The preparation method of different lanthanum cerium content al-5ti-1b-1 (la+ce) intermediate alloy grain refiners, operating procedure is such as
Under:
1. be respectively as follows: 20%ce: 80%al according to re and al mass percent, 20%la: 80%al, (4%la+16%
Ce): 80%al, (8%la+12%ce): 80%al, (12%la+8%ce): 80%al, (16%la+4%ce): 80%al
Ratio produced by vacuum arc furnace ignition respectively obtain 20%ce: 80%al, 20%la: 80%al, (4%la+16%ce):
80%al, (8%la+12%ce): 80%al, (12%la+8%ce): 80%al, (16%la+4%ce): in the middle of 80%al
Alloy.
2., according to generating mass percent: 5%ti, 1%b, 1% (la+ce), remaining is the quality of al, weighs fluorine respectively
Metatitanic acid kalium2tif6, potassium fluoborate kbf4And commercial-purity aluminium, and by potassium fluotitanate k2tif6, potassium fluoborate kbf4Powder mixing is all
Even.
3. clear up used tool in 6# graphite crucible and experimentation, and prepare coating, coating is coated in used tool
On, coating will uniformly, and described coating is 20%zno+7%na2sio3·9h2O+73%h2o.
4. turn on the power, temperature required to 800 DEG C of well formula resistance furnace used by setting and chamber type electric resistance furnace arrive to temperature required
350℃.
5. graphite crucible is put in shaft furnace and run；Experiment outfit is put into batch-type furnace run, so that instrument is dried.
6., after graphite crucible drying, put into preprepared aluminium ingot.After shaft furnace runs a period of time, treat that aluminium block is sent out
After soft heat, add coverture, to prevent aluminium ingot from aoxidizing, described coverture is 50%nacl+50%kcl.
7. after aluminium ingot is completely melt, with graphite bell jar by step 2) k that mixes2tif6、kbf4Powder is pressed into aluminium liquid
In, react 20min, period stirs once every 10min, after stirring every time, coverture will be added, to prevent aluminum melt from aoxidizing.
After 8.20min, by step 1) be obtained 20%ce: 80%al, 20%la: 80%al, (4%la+16%ce):
80%al, (8%la+12%ce): 80%al, (12%la+8%ce): 80%al or (16%la+4%ce): in 80%al
Between alloy add melt in, react 30min.Period stirs once every 10min, will add coverture after stirring every time.
9., in the last 10min of whole reaction, add refining agent, refining agent will be added to melt bottom, stirring, add and cover
Agent, standing, described refining agent is c2cl6.
10. after the completion of reacting, skim, liquation is poured in ready mould (φ 18mm), cast molding, thus be obtained
The al- of 100%ce, 100%la, 20%la+80%ce, 40%la+60%ce, 60%la+8%ce or 80%la+20%ce
5ti-1b-1 (la+ce) intermediate alloy grain refiner.
The present invention is applied to different la/ce ratios, the serial and different rare earth ratio of ratio of different ti/b.
Beneficial effects of the present invention:
In al-ti-b- (la+ce) the intermediate alloy grain refiner of optimal lanthanum cerium percentage composition prepared by the present invention
Secondary phase particle tib2、tial3、ti2al20La and ti2al20Ce tiny and be uniformly dispersed so as to meet thin plate or foil using will
Ask；Al-ti-b- (la+ce) the intermediate alloy grain refiner of the optimal lanthanum cerium percentage composition prepared by the present invention is better than same bar
The grain refining capability to commercial-purity aluminium and its alloy for the domestic and international al-ti-b intermediate alloy grain refiner under part.
Brief description
Fig. 1 is that al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 0%wt la (100%wt ce) is brilliant
Grain fining agent xrd material phase analysis figure.
Fig. 2 is that al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 100%wt la (0%wt ce) is brilliant
Grain fining agent xrd material phase analysis figure.
Fig. 3 is that al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 20%wt la (80%wt ce) is brilliant
Grain fining agent xrd material phase analysis figure.
Fig. 4 is that al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 40%wt la (60%wt ce) is brilliant
Grain fining agent xrd material phase analysis figure.
Fig. 5 is that al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 60%wt la (40%wt ce) is brilliant
Grain fining agent xrd material phase analysis figure.
Fig. 6 is that al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 80%wt la (20%wt ce) is brilliant
Grain fining agent xrd material phase analysis figure.
Fig. 7 is al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 0%wt la (100%wt ce)
Sem micro-organization chart.
Fig. 8 is al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 100%wt la (0%wt ce)
Sem micro-organization chart.
Fig. 9 is al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 20%wt la (80%wt ce)
Sem micro-organization chart.
Figure 10 is al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 40%wt la (60%wt ce)
Sem micro-organization chart.
Figure 11 is al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 60%wt la (40%wt ce)
Sem micro-organization chart.
Figure 12 is al-5ti-1b-1 (la+ce) intermediate alloy that lanthanum cerium percentage composition is 80%wt la (20%wt ce)
Sem micro-organization chart.
Figure 13 is the al-5ti-1b intermediate alloy sem micro-organization chart that certain company domestic produces.
Figure 14 is the al-5ti-1b intermediate alloy sem micro-organization chart that import kbm company produces.
Figure 15 is self-control al-5ti-1b-1 (la+ce) intermediate alloy and certain company domestic and import kbm company produces
Al-5ti-1b intermediate alloy is to the thinning effect comparison diagram after commercial-purity aluminium refinement.
In figure, h1-h6 is respectively b1-b6 to the thinning effect figure after commercial-purity aluminium refinement；Hg is that certain company domestic produces
Al-5ti-1b intermediate alloy to commercial-purity aluminium refinement after thinning effect figure；Hj is the al-5ti- that import kbm company produces
1b intermediate alloy is to the thinning effect figure after commercial-purity aluminium refinement；0 is commercial-purity aluminium design sketch.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
1. according to the ratio of 20%wt re (100%wt ce), 80%wt al, al-20 (la is produced by vacuum arc furnace ignition
+ ce) intermediate alloy；
2., according to generating mass percent: 5%ti, 1%b, 1% (la+ce), remaining is the quality of al, weighs fluotitanic acid
Potassium (k2tif6), potassium fluoborate (kbf4) and commercial-purity aluminium, and by k2tif6、kbf4Powder mixes；
3. clear up used tool in 6# graphite crucible and experimentation, and prepare coating (20%zno+7%na2sio3·
9h2O+73%h2o).Coating is coated on used tool, coating will be uniformly；
4. turn on the power, temperature required to 800 DEG C of well formula resistance furnace used by setting and chamber type electric resistance furnace arrive to temperature required
350℃；
5. graphite crucible is put in shaft furnace so as to run；Experiment outfit is put in batch-type furnace so as to transport
OK, so that instrument is dried；
6., after graphite crucible drying, put into preprepared aluminium ingot.After a period of time, after aluminium block feels like jelly fusing,
Add coverture (50%wt nacl+50%wt kcl), to prevent aluminium ingot from aoxidizing；
7. after aluminium ingot is completely melt, the k that will have been weighed up and mix using graphite bell jar2tif6、kbf4Powder
In press-in aluminium liquid, react 20min, period stirs once every 10min, after stirring every time, coverture will be added, to prevent aluminium
Melt oxidation；
After 8.20min, in the al-20 (la+ce) that homemade lanthanum cerium percentage composition is 0%wt la (100%wt ce)
Between alloy add melt in, react 30min.Period stirs once every 10min, will add coverture after stirring every time.
9., in the last 10min of whole reaction, add refining agent (c2cl6), refining agent will be added to melt bottom, stirring, plus
Enter coverture, standing；
10. after the completion of reacting, skim, liquation is poured in ready mould (φ 18mm), cast molding, thus be obtained
Al-5ti-1b-1 (la+ce) the intermediate alloy grain refiner of 0%wt la (100%wt ce).Its xrd material phase analysis figure and
Sem micro-organization chart is respectively Fig. 1, Fig. 7.
Embodiment 2
1. according to the ratio of 20%wt re (i.e. 100%wt la), 80%wt al, al-20 is produced by vacuum arc furnace ignition
(la+ce) intermediate alloy；
2. following steps are with step 2～step 10 in embodiment 1, thus the al- of 100%wt la (0%wt ce) is obtained
5ti-1b-1 (la+ce) intermediate alloy grain refiner.Its xrd material phase analysis figure and sem micro-organization chart are respectively Fig. 2, figure
8.
Embodiment 3
1. pass through vacuum arc furnace ignition system according to the ratio of 20%wt re (20%wt la+80%wt ce), 80%wt al
Take al-20 (la+ce) intermediate alloy；
2. following steps are with step 2～step 10 in embodiment 1, thus the al- of 20%wt la (80%wt ce) is obtained
5ti-1b-1 (la+ce) intermediate alloy grain refiner.Its xrd material phase analysis figure and sem micro-organization chart are respectively Fig. 3, figure
9.
Embodiment 4
1. according to the ratio of 20%re (40%wt la+60%wt ce), 80%al, al-20 is produced by vacuum arc furnace ignition
(la+ce) intermediate alloy；
2. following steps are with step 2～step 10 in embodiment 1, thus the al- of 40%wt la (60%wtce) is obtained
5ti-1b-1 (la+ce) intermediate alloy grain refiner.Its xrd material phase analysis figure and sem micro-organization chart are respectively Fig. 4, figure
10.
Embodiment 5
1. pass through vacuum arc furnace ignition system according to the ratio of 20%wt re (60%wt la+40%wt ce), 80%wt al
Take al-20 (la+ce) intermediate alloy；
2. following steps are with step 2～step 10 in embodiment 1, thus the al- of 60%wt la (40%wt ce) is obtained
5ti-1b-1 (la+ce) intermediate alloy grain refiner.Its xrd material phase analysis figure and sem micro-organization chart are respectively Fig. 5, figure
11.
Embodiment 6
1. pass through vacuum arc furnace ignition system according to the ratio of 20%wt re (80%wt la+20%wt ce), 80%wt al
Take al-20 (la+ce) intermediate alloy；
2. following steps are with step 2～step 10 in embodiment 1, thus the al- of 80%wt la+20%wt ce is obtained
Its xrd material phase analysis figure of 5ti-1b-1 (la+ce) intermediate alloy grain refiner and sem micro-organization chart are respectively Fig. 6, figure
12.
Commercial-purity aluminium is refined: by al-5ti-1b-1 (la+ce) intermediate alloy of different for self-control lanthanum cerium percentage compositions, state
The al-5ti-1b intermediate alloy that certain company interior and import kbm company produce at a temperature of 800 DEG C, by the 0.2% of aluminum melt quality
It is added in the 350g commercial-purity aluminium melt weighing up, be incubated 10min, refining, skim, be poured in mould；Grind away, corrosion, see
Examine thinning effect.
By contrast, find: the part self-control thinning effect to commercial-purity aluminium for al-5ti-1b-1 (la+ce) intermediate alloy
The thinning effect to commercial-purity aluminium for the al-5ti-1b intermediate alloy producing better than certain company domestic and import kbm company.As Figure 15
Shown.
Claims (1)
1. different lanthanum cerium content al-5ti-1b-1 (la+ce) intermediate alloy grain refiners preparation method it is characterised in that:
Method operating procedure is as follows:
1) be respectively as follows: 20%ce: 80%al according to re and al mass percent, 20%la: 80%al, (4%la+16%ce):
80%al, (8%la+12%ce): 80%al, (12%la+8%ce): 80%al, the ratio of (16%la+4%ce): 80%al
Example is produced by vacuum arc furnace ignition and to be respectively obtained 20%ce: 80%al, 20%la: 80%al, (4%la+16%ce): 80%
Al, (8%la+12%ce): 80%al, (12%la+8%ce): 80%al, (16%la+4%ce): 80%al intermediate alloy；
2) according to generating mass percent: 5%ti, 1%b, 1% (la+ce), remaining is the quality of al, weighs fluotitanic acid respectively
Kalium2tif6, potassium fluoborate kbf4And commercial-purity aluminium, and by potassium fluotitanate k2tif6, potassium fluoborate kbf4Powder mixes；
3) clear up used tool in 6# graphite crucible and experimentation, and prepare coating, coating is coated on used tool, apply
Layer will uniformly, and described coating is 20%zno+7%na2sio3·9h2O+73%h2o；
4) turn on the power, temperature required to 800 DEG C of well formula resistance furnace used by setting and chamber type electric resistance furnace are to temperature required to 350
℃；
5) graphite crucible is put in well formula resistance furnace and run；Experiment outfit is put into chamber type electric resistance furnace run, so that work
Tool is dried；
6) after graphite crucible drying, put into preprepared aluminium ingot, after well formula resistance furnace runs a period of time, treat that aluminium block is sent out
After soft heat, add coverture, to prevent aluminium ingot from aoxidizing, described coverture is 50%nacl+50%kcl；
7) after aluminium ingot is completely melt, with graphite bell jar by step 2) k that mixes2tif6、kbf4In powder press-in aluminium liquid,
Reaction 20min, period stirs once every 10min, will add coverture after stirring every time, to prevent aluminum melt from aoxidizing；
8) after 20min, by step 1) be obtained 20%ce: 80%al, 20%la: 80%al, (4%la+16%ce): 80%
Al, (8%la+12%ce): 80%al, (12%la+8%ce): 80%al or (16%la+4%ce): 80%al intermediate alloy
Add in melt, react 30min, period stirs once every 10min, after stirring every time, coverture will be added；
9) in the last 10min of whole reaction, add refining agent, refining agent will be added to melt bottom, stirring, add coverture,
Standing, described refining agent is c2cl6；
10) after the completion of reacting, skim, liquation is poured in ready mould φ 18mm, cast molding, thus be obtained 100%
The al-5ti- of ce, 100%la, 20%la+80%ce, 40%la+60%ce, 60%la+40%ce or 80%la+20%ce
1b-1 (la+ce) intermediate alloy grain refiner.
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| CN104946920B (en) * | 2015-06-17 | 2017-01-11 | 广东省材料与加工研究所 | Preparation method of grain refiner |
| CN104946938A (en) * | 2015-07-08 | 2015-09-30 | 济南大学 | Preparation method of Al-Ti-B-Y intermediate alloy and application thereof |
| CN105463223B (en) * | 2015-12-01 | 2017-05-31 | 湖南金联星特种材料股份有限公司 | A kind of preparation method of Al B RE intermediate alloys |
| CN105648251A (en) * | 2016-02-01 | 2016-06-08 | 东南大学 | Preparation method of aluminum, lanthanum and boron grain refiner used for cast aluminum alloy |
| CN106111917A (en) * | 2016-06-24 | 2016-11-16 | 芜湖黄燕实业有限公司 | High intensity wheel hub and preparation method thereof |
| CN106048273B (en) * | 2016-07-04 | 2018-09-21 | 东南大学 | A kind of aluminium silicon lanthanum boron quaternary intermediate alloy and preparation method thereof |
| CN106893912A (en) * | 2017-02-27 | 2017-06-27 | 广东省材料与加工研究所 | A kind of magnesium alloy grain refining agent and preparation method thereof |
| CN107299240B (en) * | 2017-05-17 | 2019-04-05 | 东北大学秦皇岛分校 | A method of improving al-ti-b refiner structure property |
| CN111560544B (en) * | 2020-05-25 | 2021-07-27 | 湖南西瑞尔新材料科技有限公司 | Preparation method of anode aluminum alloy for air battery and air battery |
| CN113293316A (en) * | 2021-04-16 | 2021-08-24 | 中国科学院金属研究所 | Method for efficiently improving refining capacity of Al-5Ti-1B intermediate alloy |
| CN113388747A (en) * | 2021-04-29 | 2021-09-14 | 百色市广百金属材料有限公司 | Novel aluminum-zirconium-rare earth ternary aluminum alloy additive and preparation method thereof |
| CN117107104A (en) * | 2023-05-30 | 2023-11-24 | 秦皇岛峰越科技有限公司 | Preparation method of aluminum lanthanum boron titanium grain refiner |
| CN117210724B (en) * | 2023-09-13 | 2024-04-02 | 山东迈奥晶新材料有限公司 | Al-MB for reducing transition group element content in aluminum alloys 6 Alloy and preparation method thereof |
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