CN104498746A - 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 PDF

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CN104498746A
CN104498746A CN201410706153.8A CN201410706153A CN104498746A CN 104498746 A CN104498746 A CN 104498746A CN 201410706153 A CN201410706153 A CN 201410706153A CN 104498746 A CN104498746 A CN 104498746A
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master alloy
aluminium
lanthanum
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cerium
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CN104498746B (en
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李逸泰
尹建宝
胡治流
赵艳君
曾建民
许征兵
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Guangxi University
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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

The preparation method of different lanthanum cerium content Al-5Ti-1B-1 (La+Ce) master alloy grain-refining agent
Technical field
The invention belongs to aluminium applied technical field.The specifically preparation method of different lanthanum cerium content Al-5Ti-1B-1 (La+Ce) master alloy grain-refining agent.
Background technology
Fine aluminium has fusing point low (660 DEG C), little (ρ=2.7 × 10 of density 3kg/m 3), plasticity high (ψ=80%), the low (σ of intensity b=80MPa) etc. feature.The density of aluminium alloy is also very little, and after thermal treatment, intensity is high, σ b=490 ~ 588Mpa, therefore, aluminium alloy has very high specific tenacity (σ b/ ρ), be important aerospace structure material.And the heat conduction of fine aluminium and conductivity well, are only second to silver and copper.Again because the surface of aluminium very easily generates fine and close Al 2o 3oxide film, therefore, aluminium has good solidity to corrosion.Because Aluminum-aluminum alloy has excellent properties like this, therefore, be widely used in the fields such as industry, agricultural, transportation and military affairs, be also widely used as family life apparatus, sports goods and building structural materials etc.As various instrument housing, motor car engine, automobile gearbox, seagoing vessel part, Veronicastrum Herb, dental equipment, airplane spare parts, pottery and golf club etc.
Along with the fast development of Chinese national economy, the goods such as Aluminum-aluminum alloy paper tinsel, plate, band are widely applied in the national economy such as aerospace, machinofacture.But, while Aluminum-aluminum alloy development, more and more higher requirement be it is also proposed to the properties etc. of Aluminum-aluminum alloy.Grain refining is the important means obtaining premium properties aluminium alloy.The grain refining of Aluminum-aluminum alloy has very important meaning to the mechanical property and process industrial art performance that improve Aluminum-aluminum alloy.The grain refining of Aluminum-aluminum alloy can make Aluminum-aluminum alloy obtain tiny equi-axed crystal, therefore, except obtaining superior mechanical property, also can obtain good surface smoothness etc.Grain refining can be realized by different modes, and as heterogeneous nucleation, method for quick cooling, in addition, also has the stirring etc. of melt.In melt, add fining agent is most economical, the most effective thinning method.
Al-Ti-B Master alloy refiners is current widely used a kind of high-efficiency aluminum and alloy grain fining agent thereof in the world, has good in refining effect, easy to control and low cost and other advantages.Since the sixties in 20th century, Al-Ti-B master alloy is just used to refinement Aluminum-aluminum alloy always.Along with improving constantly of Al-Ti-B master alloy quality, the application in modern aluminum industry is also increasingly extensive.But also come with some shortcomings in the domestic and international quality at Al-Ti-B master alloy and production technology thereof at present:
1) second-phase in Al-Ti-B master alloy has TiB 2, TiAl 3, AlB 2, (Al, Ti) B 2deng particle, but only really play the effect of heterogeneous nucleation less than the particle of 1%, therefore, forming core potential is far from bringing into play;
2) in Al-Ti-B master alloy, foreign matter content is higher, while refinement Aluminum-aluminum alloy, also pollute Aluminum-aluminum alloy;
3) TiB in Al-Ti-B master alloy 2particle size comparatively large (as 0.5-3 μm), and it is agglomerating to be easy to gathering, thus greatly reduce Al-Ti-B master alloy grain refining efficiency; TiB 2also can with the element generation surface reactions such as Mn, Cr, Zr, cause fining agent poisoning.
4), during Al-Ti-B master alloy refinement Aluminum-aluminum alloy, thinning effect is unstable.Therefore, the quality product controlling aluminum products is difficult to.
Therefore, develop, develop efficient, stable, the clean Al-Ti-B Master alloy refiners of a new generation, become the current urgent problem of people.
Adding of rare earth, effectively can make up the deficiency of above Al-Ti-B Master alloy refiners, therefore, develop the Al-Ti-B-RE master alloy grain-refining agent that a new generation is efficient, clean, stable, there is wide market application foreground.
Summary of the invention
The present invention provides the preparation method of different lanthanum cerium content Al-5Ti-1B-1 (La+Ce) master alloy grain-refining agent in order to overcome the deficiencies in the prior art.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
The preparation method of different lanthanum cerium content Al-5Ti-1B-1 (La+Ce) master alloy grain-refining agent, operation steps is as follows:
1. be respectively according to RE and Al mass percent: 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): the ratio of 80%Al is produced by vacuum arc fumace and obtained 20%Ce: 80%Al respectively, 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 master alloy.
2., according to generation mass percent: 5%Ti, 1%B, 1% (La+Ce), all the other are the quality of Al, weigh potassium fluotitanate K respectively 2tiF 6, potassium fluoborate KBF 4and commercial-purity aluminium, and by potassium fluotitanate K 2tiF 6, potassium fluoborate KBF 4powder mixes.
3. clear up used tool in 6# plumbago crucible and experimentation, and prepare coating, be coated in by coating on used tool, coating is wanted evenly, and described coating is 20%ZnO+7%Na 2siO 39H 2o+73%H 2o.
4. opening power, set well formula resistance furnace used temperature required to 800 DEG C and chamber type electric resistance furnace to temperature required to 350 DEG C.
5. plumbago crucible is put into pit furnace to run; Experiment outfit is put into box-type furnace run, instrument is dried.
6., after plumbago crucible is dried, put into previously prepd aluminium ingot.After pit furnace runs for some time, after aluminium block feels like jelly fusing, add insulating covering agent, to prevent aluminium ingot to be oxidized, described insulating covering agent is 50%NaCl+50%KCl.
7. after aluminium ingot melts completely, with graphite bell jar by step 2) K that mixes 2tiF 6, KBF 4in powder press-in aluminium liquid, reaction 20min, period stirs once every 10min, all will add insulating covering agent, be oxidized to prevent molten aluminium after each stirring.
8.20min after, by step 1) 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 master alloy add in melt, reaction 30min.Period stirs once every 10min, all will add insulating covering agent after each stirring.
9. when the last 10min of whole reaction, add refining agent, refining agent will be added to bottom melt, stirs, adds insulating covering agent, and leave standstill, described refining agent is C 2cl 6.
10. after having reacted, skim, liquation is poured in ready mould (Φ 18mm), cast molding, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 100%Ce, 100%La, 20%La+80%Ce, 40%La+60%Ce, 60%La+8%Ce or 80%La+20%Ce.
The present invention be applicable to Different L a/Ce ratio, different Ti/B ratio series and different rare earth ratio.
Beneficial effect of the present invention:
Second phase particles TiB in Al-Ti-B-(La+Ce) the master alloy grain-refining agent of the best lanthanum cerium percentage composition prepared by the present invention 2, TiAl 3, Ti 2al 20la and Ti 2al 20ce is tiny and be uniformly dispersed, and makes it meet the service requirements of thin plate or foil; Al-Ti-B-(La+Ce) the master alloy grain-refining agent of the best lanthanum cerium percentage composition prepared by the present invention to be better than under same condition both at home and abroad Al-Ti-B master alloy grain-refining agent to the grain refining capability of technical pure Aluminum-aluminum alloy.
Accompanying drawing explanation
Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent XRD material phase analysis figure of Fig. 1 to be lanthanum cerium percentage composition be 0%wt La (100%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent XRD material phase analysis figure of Fig. 2 to be lanthanum cerium percentage composition be 100%wt La (0%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent XRD material phase analysis figure of Fig. 3 to be lanthanum cerium percentage composition be 20%wt La (80%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent XRD material phase analysis figure of Fig. 4 to be lanthanum cerium percentage composition be 40%wt La (60%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent XRD material phase analysis figure of Fig. 5 to be lanthanum cerium percentage composition be 60%wt La (40%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent XRD material phase analysis figure of Fig. 6 to be lanthanum cerium percentage composition be 80%wt La (20%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy SEM micro-organization chart of Fig. 7 to be lanthanum cerium percentage composition be 0%wt La (100%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy SEM micro-organization chart of Fig. 8 to be lanthanum cerium percentage composition be 100%wt La (0%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy SEM micro-organization chart of Fig. 9 to be lanthanum cerium percentage composition be 20%wt La (80%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy SEM micro-organization chart of Figure 10 to be lanthanum cerium percentage composition be 40%wt La (60%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy SEM micro-organization chart of Figure 11 to be lanthanum cerium percentage composition be 60%wt La (40%wt Ce).
Al-5Ti-1B-1 (La+Ce) the master alloy SEM micro-organization chart of Figure 12 to be lanthanum cerium percentage composition be 80%wt La (20%wt Ce).
Figure 13 is the Al-5Ti-1B master alloy SEM micro-organization chart that certain company domestic produces.
Figure 14 is the Al-5Ti-1B master alloy SEM micro-organization chart that import KBM company produces.
Figure 15 is for making the Al-5Ti-1B master alloy of Al-5Ti-1B-1 (La+Ce) master alloy and certain company domestic and the production of import KBM company by oneself 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 the Al-5Ti-1B master alloy of certain company domestic production is to the thinning effect figure after commercial-purity aluminium refinement; Hj is that the Al-5Ti-1B master alloy of import KBM company production is to the thinning effect figure after commercial-purity aluminium refinement; 0 is commercial-purity aluminium design sketch.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1. produce Al-20 (La+Ce) master alloy according to the ratio of 20%wt RE (100%wt Ce), 80%wt Al by vacuum arc fumace;
2., according to generation mass percent: 5%Ti, 1%B, 1% (La+Ce), all the other are the quality of Al, weigh potassium fluotitanate (K 2tiF 6), potassium fluoborate (KBF 4) and commercial-purity aluminium, and by K 2tiF 6, KBF 4powder mixes;
3. clear up used tool in 6# plumbago crucible and experimentation, and prepare coating (20%ZnO+7%Na 2siO 39H 2o+73%H 2o).Be coated in by coating on used tool, coating is wanted evenly;
4. opening power, set well formula resistance furnace used temperature required to 800 DEG C and chamber type electric resistance furnace to temperature required to 350 DEG C;
5. plumbago crucible is put into pit furnace, make it run; Experiment outfit is put into box-type furnace, makes it run, dry to make instrument;
6., after plumbago crucible is dried, put into previously prepd aluminium ingot.After for some time, after aluminium block feels like jelly fusing, add insulating covering agent (50%wt NaCl+50%wt KCl), be oxidized to prevent aluminium ingot;
7., after aluminium ingot melts completely, use graphite bell jar will to weigh up and the K mixed 2tiF 6, KBF 4in powder press-in aluminium liquid, reaction 20min, period stirs once every 10min, all will add insulating covering agent, be oxidized to prevent molten aluminium after each stirring;
After 8.20min, be that Al-20 (La+Ce) master alloy of 0%wt La (100%wt Ce) adds in melt by homemade lanthanum cerium percentage composition, reaction 30min.Period stirs once every 10min, all will add insulating covering agent after each stirring.
9., when the last 10min of whole reaction, add refining agent (C 2cl 6), refining agent will be added to bottom melt, stirs, adds insulating covering agent, leaves standstill;
10. after having reacted, skim, liquation is poured in ready mould (Φ 18mm), cast molding, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 0%wt La (100%wt Ce).Its XRD material phase analysis figure and SEM micro-organization chart are respectively Fig. 1, Fig. 7.
Embodiment 2
1. produce Al-20 (La+Ce) master alloy according to the ratio of 20%wt RE (i.e. 100%wt La), 80%wt Al by vacuum arc fumace;
2. following steps are with step 2 ~ step 10 in embodiment 1, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 100%wt La (0%wt Ce).Its XRD material phase analysis figure and SEM micro-organization chart are respectively Fig. 2, Fig. 8.
Embodiment 3
1. produce Al-20 (La+Ce) master alloy according to the ratio of 20%wt RE (20%wt La+80%wt Ce), 80%wt Al by vacuum arc fumace;
2. following steps are with step 2 ~ step 10 in embodiment 1, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 20%wt La (80%wt Ce).Its XRD material phase analysis figure and SEM micro-organization chart are respectively Fig. 3, Fig. 9.
Embodiment 4
1. produce Al-20 (La+Ce) master alloy according to the ratio of 20%RE (40%wt La+60%wt Ce), 80%Al by vacuum arc fumace;
2. following steps are with step 2 ~ step 10 in embodiment 1, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 40%wt La (60%wtCe).Its XRD material phase analysis figure and SEM micro-organization chart are respectively Fig. 4, Figure 10.
Embodiment 5
1. produce Al-20 (La+Ce) master alloy according to the ratio of 20%wt RE (60%wt La+40%wt Ce), 80%wt Al by vacuum arc fumace;
2. following steps are with step 2 ~ step 10 in embodiment 1, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 60%wt La (40%wt Ce).Its XRD material phase analysis figure and SEM micro-organization chart are respectively Fig. 5, Figure 11.
Embodiment 6
1. produce Al-20 (La+Ce) master alloy according to the ratio of 20%wt RE (80%wt La+20%wt Ce), 80%wt Al by vacuum arc fumace;
2. following steps are with step 2 ~ step 10 in embodiment 1, thus its XRD material phase analysis figure of Al-5Ti-1B-1 (La+Ce) master alloy grain-refining agent of obtained 80%wt La+20%wt Ce and SEM micro-organization chart are respectively Fig. 6, Figure 12.
To commercial-purity aluminium refinement: Al-5Ti-1B master alloy Al-5Ti-1B-1 (La+Ce) master alloy of the different lanthanum cerium percentage composition of self-control, certain company domestic and import KBM company produced is at 800 DEG C of temperature, add to by 0.2% of molten aluminium quality in the 350g commercial-purity aluminium melt weighed up, insulation 10min, refining, skim, be poured in mould; Grind away, corrosion, observes thinning effect.
By contrast, find: part is made the thinning effect of Al-5Ti-1B-1 (La+Ce) master alloy to commercial-purity aluminium by oneself and is better than the Al-5Ti-1B master alloy of certain company domestic and the production of import KBM company to the thinning effect of commercial-purity aluminium.As shown in figure 15.

Claims (1)

1. the preparation method of different lanthanum cerium content Al-5Ti-1B-1 (La+Ce) master alloy grain-refining agent, is characterized in that: method operation steps is as follows:
1) be respectively according to RE and Al mass percent: 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): the ratio of 80%Al is produced by vacuum arc fumace and obtained 20%Ce: 80%Al respectively, 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 master alloy,
2) according to generation mass percent: 5%Ti, 1%B, 1% (La+Ce), all the other are the quality of Al, weigh potassium fluotitanate K respectively 2tiF 6, potassium fluoborate KBF 4and commercial-purity aluminium, and by potassium fluotitanate K 2tiF 6, potassium fluoborate KBF 4powder mixes;
3) clear up used tool in 6# plumbago crucible and experimentation, and prepare coating, be coated in by coating on used tool, coating is wanted evenly, and described coating is 20%ZnO+7%Na 2siO 39H 2o+73%H 2o;
4) opening power, set well formula resistance furnace used temperature required to 800 DEG C and chamber type electric resistance furnace to temperature required to 350 DEG C;
5) plumbago crucible is put into pit furnace to run; Experiment outfit is put into box-type furnace run, dry to make instrument;
6) after plumbago crucible is dried, put into previously prepd aluminium ingot, after pit furnace runs for some time, after aluminium block feels like jelly fusing, add insulating covering agent, to prevent aluminium ingot to be oxidized, described insulating covering agent is 50%NaCl+50%KCl;
7) after aluminium ingot melts completely, with graphite bell jar by step 2) K that mixes 2tiF 6, KBF 4in powder press-in aluminium liquid, reaction 20min, period stirs once every 10min, all will add insulating covering agent, be oxidized to prevent molten aluminium after each stirring;
8) after 20min, by step 1) 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 master alloy adds in melt, reaction 30min.Period stirs once every 10min, all will add insulating covering agent after each stirring;
9) when the last 10min of whole reaction, add refining agent, refining agent will be added to bottom melt, stirs, adds insulating covering agent, and leave standstill, described refining agent is C 2cl 6;
10) after having reacted, skim, liquation is poured in ready mould (Φ 18mm), cast molding, thus Al-5Ti-1B-1 (La+Ce) the master alloy grain-refining agent of obtained 100%Ce, 100%La, 20%La+80%Ce, 40%La+60%Ce, 60%La+8%Ce or 80%La+20%Ce.
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CN104946920A (en) * 2015-06-17 2015-09-30 广东省工业技术研究院(广州有色金属研究院) Preparation method of grain refiner
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CN105463223A (en) * 2015-12-01 2016-04-06 永城金联星铝合金有限公司 Manufacturing method of Al-B-RE intermediate alloy
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
CN106048273A (en) * 2016-07-04 2016-10-26 东南大学 Aluminum silicon lanthanum boron quaternary intermediate alloy and preparing 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
CN107299240A (en) * 2017-05-17 2017-10-27 东北大学秦皇岛分校 It is a kind of to improve the method for al-ti-b refiner structure property
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
CN111560544A (en) * 2020-05-25 2020-08-21 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
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

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