CN1381604A - Method for adding particles to slurry in preparing particle reinforced Al-base composition by liquid state method - Google Patents

Method for adding particles to slurry in preparing particle reinforced Al-base composition by liquid state method Download PDF

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CN1381604A
CN1381604A CN 01113847 CN01113847A CN1381604A CN 1381604 A CN1381604 A CN 1381604A CN 01113847 CN01113847 CN 01113847 CN 01113847 A CN01113847 A CN 01113847A CN 1381604 A CN1381604 A CN 1381604A
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particle
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slurry
semi
metal
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CN1151295C (en
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秦孝华
韩维新
范存淦
戎利建
李依依
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Institute of Metal Research of CAS
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Abstract

A process for adding particles to the slurry used to prepare the particle reinforced Al-base composite material by liquid state method includes such steps as pickling, heating and warming the particles, smelting Al or Al-alloy, refining, removing slags, cooling to semi-solid state, then directly adding the said particles, and stirring to form slurry.

Description

Particulate addition method in slurry when liquid phase process prepares particle enhanced aluminum-based composite material
The present invention relates to matrix material, be specially liquid phase process particulate addition method in the slurry when preparing particle enhanced aluminum-based composite material.
Liquid phase process prepares particle reinforced aluminium-based (aluminum or aluminum alloy base), and matrix material is lower than the cost of solid state process, pays close attention to greatly so caused people.The initial stage for preparing particulate reinforced composite in liquid phase process, particulate adding method, be particle surface coat nickel and with air-flow be pressed in the matrix alloy and go [not. peace. Shane Battier and skin. gram. Luo Hateji: American foundryman's society's journal, 1969,77 volumes, 402-406 page or leaf (F.A.Badia and P.K.Rohatgi:AFS Trans., 1969, vol.77, pp.402-406.)], surface coated adding method coats near the enrichment of material particle easily, artificial component segregation occurs, and cost is higher; Occurred subsequently " vortex method " [not. the peace. Shane Battier, moral. not. MacDonald and Qiao. sieve. Pearson: American foundryman's society's journal, 1971,79 volumes, 265-268 page or leaf (F.A.Badia, D.f.MacDonald, and J.R.Person:AFS Trans., 1971, vol.79, pp.265-268.)], though the cost of vortex method is lower, technology is simple, but only is suitable for the bigger particle of diameter (diameter 50~100 μ m), and because the existence of vortex increases the inspiratory capacity of matrix material; In addition, the Duralcon method [in the Maas Europe 5. Qiao, breathe out mole. Fu Ge, like ground this. about the international conference communique of particles reiforced metal-base composition preparation, Montreal: 1990.24,68,82,84 (Masounave J, Hamel FG, eds.Proc.Of an International Conference on Fabrication ofParticulate Reinforced Metal Composites.Montreal:1990.24,68,82,84)], its equipment configuration is comparatively complicated.
Composite casting is comparatively advanced at present a kind of particle addition method, but matrix metal is had certain restriction, for example is difficult to add particle in metallic aluminium; In addition, adopt liquid phase process to prepare particle (for example SiC, Al 2O 3) when strengthening aluminium base (aluminum or aluminum alloy base) matrix material, in the set-up procedure of slurry, because the wettability between particle and the matrix metal is very poor, be difficult to particle is joined in the matrix metal, that is to say, improve particle and wettability between the matrix metal and be one of guardian technique of liquid phase process prepares particle reinforced aluminium-based (it is Al-alloy based that aluminium becomes) matrix material.
The objective of the invention is: providing a kind of can be that particle in 3.5~100 mu m ranges directly joins in the matrix metal aluminum or aluminum alloy with diameter, and particulate addition method in the slurry when making the liquid phase process that has good wettability between particle and the matrix metal prepare particle enhanced aluminum-based composite material.
Technical solution of the present invention is:
1) with the quality percentage composition is 0.1~0.8% HF or HNO 3Particle is carried out pickling, remove the zone of oxidation or the adsorbent of particle surface, with heating installation particle is heated to 673~873K then, and is incubated 20~40 minutes, remove granule surface activity water, particle is disperseed automatically;
2) in non-vacuum induction furnace the matrix metal aluminum or aluminum alloy is heated to liquid state, feeds argon gas liquid towards metal then and carry out refining, the liquid towards metal is lowered the temperature after skimming;
3) liquid metal is cooled to semi-solid state, the semi-solid temperature of described aluminium is 983K~1013K, the semi-solid temperature of described aluminium alloy is 933K~1003K, directly particle is joined the semi-solid-state metal surface then, with the stepless speed regulation agitator it is stirred, stirring total time is 30~50 minutes, and segmentation is stirred: the fs stirring velocity is 30~100 rev/mins, and churning time is 20~30 minutes; The subordinate phase stirring velocity is 100~500 rev/mins, and churning time is 5~10 minutes; The phase III stirring velocity is 500~800 rev/mins, and churning time is 5~10 minutes; Thereby the formation slurry with the non-vacuum induction furnace insulation, is protected with argon gas in operating process; Described particle is graphite, SiC or Al 2O 3Particle, its diameter are 3.5~100 μ m.
The present invention by means of the stirring action of mechanical external force, directly joins particle in the semi-solid matrix metal aluminum or aluminum alloy after the pre-treatment by particle is carried out, thereby has solved the problem of wettability difference between particle and the matrix metal.
The present invention has following advantage:
1. the present invention can particularly can directly add the particle that density is greater than or less than matrix metal at aluminium alloy in metallic aluminium, makes to have good wettability between aluminum or aluminum alloy and the particle; And the particle minimum particle size can reach 3.5 μ m, for the preparation of particle reinforced aluminium-based (aluminum or aluminum alloy base) matrix material provides good slurry.
2. the present invention is liquid phase process, and simple to operate, cost is low.
Fig. 1 is that the embodiment of the invention 1 is the Al of 100 μ m with diameter 2O 3Particle joins prepared slurry in the matrix ZL109 aluminium alloy, after rotary casting is solidified, and the photo that obtains with the scanning electron microscope imaging.
Fig. 2 is the embodiment of the invention 2 with diameter is that the SiC particle of 10 μ m joins prepared slurry in the matrix ZL109 aluminium alloy, after rotary casting is solidified, and the photo that obtains with the scanning electron microscope imaging.
Fig. 3 is the embodiment of the invention 3 with diameter is that the SiC particle of 3.5 μ m joins prepared slurry in the matrix ZL109 aluminium alloy, after rotary casting is solidified, and the photo that obtains with the scanning electron microscope imaging.
Fig. 4 is wooden inventive embodiments 4 with diameter is that the graphite granule of 100 μ m joins slurry prepared in the matrix metal aluminium, after air cooling, and the photo that obtains with microscope imaging.
The invention will be further described below in conjunction with embodiment and accompanying drawing.
Embodiment 1
1. with the quality percentage composition 0.5% HNO 3To diameter is the Al of 100 μ m 2O 3Particle carries out pickling, removes the zone of oxidation or the adsorbent of particle surface, with resistance furnace particle is heated to 873K then, and is incubated 30 minutes, removes granule surface activity water, and particle is disperseed automatically, after the cooling, take by weighing 0.2 kilogram standby;
2. in antivacuum medium-frequency induction furnace 2 kilograms of ZL109 aluminium alloys are heated to liquid state, feed argon gas liquid towards metal and carry out refining, the liquid towards metal is lowered the temperature after skimming;
3. liquid metal is cooled to semi-solid state (983K), then directly with ready Al 2O 3Particle joins the semi-solid-state metal surface, with the stepless speed regulation agitator it is stirred, and stirring total time is 30 minutes, and segmentation is stirred: the fs stirring velocity is 50 rev/mins, and churning time is 20 minutes; The subordinate phase stirring velocity is 300 rev/mins, and churning time is 5 minutes; The phase III stirring velocity is 600 rev/mins, and churning time is 5 minutes; Thereby the formation slurry with antivacuum medium-frequency induction furnace insulation, is protected with argon gas in operating process.
With diameter is the Al of 100 μ m 2O 3Particle joins slurry prepared in the matrix ZL109 aluminium alloy after rotary casting is solidified, and obtains photo with the scanning electron microscope imaging, as shown in Figure 1.
Embodiment 2
1. with the quality percentage composition 0.8% HNO 3To diameter is that the SiC particle of 10 μ m carries out pickling, removes the zone of oxidation or the adsorbent of particle surface, with resistance furnace particle is heated to 773K then, and be incubated 40 minutes, and remove granule surface activity water, particle is disperseed automatically, after the cooling, take by weighing 0.12 kilogram standby;
2. in antivacuum medium-frequency induction furnace 1.5 kilograms ZL109 aluminium alloy is heated to liquid state, feeds argon gas liquid towards metal and carry out refining, the liquid towards metal is lowered the temperature after skimming;
3. liquid metal is cooled to semi-solid state (1003K), directly ready SiC particle is joined the semi-solid-state metal surface then, with the stepless speed regulation agitator it is stirred, stirring total time is 35 minutes, and segmentation is stirred: the fs stirring velocity is 30 rev/mins, and churning time is 25 minutes; The subordinate phase stirring velocity is 250 rev/mins, and churning time is 5 minutes; The phase III stirring velocity is 600 rev/mins, and churning time is 5 minutes; Thereby the formation slurry with antivacuum medium-frequency induction furnace insulation, is protected with argon gas in operating process.
With diameter is that the SiC particle of 10 μ m joins slurry prepared in the matrix ZL109 aluminium alloy after rotary casting is solidified, and retouches the Electronic Speculum imaging with button and obtains photo, as shown in Figure 2.
Embodiment 3
1. be 0.2% HF to diameter with the quality percentage composition be that the SiC particle of 3.5 μ m carries out pickling, remove the zone of oxidation or the adsorbent of particle surface, with resistance furnace particle is heated to 673K then, and be incubated 20 minutes, remove granule surface activity water, particle is disperseed automatically, after the cooling, take by weighing 0.4 kilogram standby;
2. in antivacuum medium-frequency induction furnace 2.5 kilograms ZL109 aluminium alloy is heated to liquid state, feeds argon gas liquid towards metal and carry out refining, the liquid towards metal is lowered the temperature after skimming;
3. liquid metal is cooled to semi-solid state (933K), directly ready SiC particle is joined the semi-solid-state metal surface then, with the stepless speed regulation agitator it is stirred, stirring total time is 40 minutes, and segmentation is stirred: the fs stirring velocity is 40 rev/mins, and churning time is 30 minutes; The subordinate phase stirring velocity is 350 rev/mins, and churning time is 5 minutes; The phase III stirring velocity is 550 rev/mins, and churning time is 5 minutes; Thereby the formation slurry with antivacuum medium-frequency induction furnace insulation, is protected with argon gas in operating process.
With diameter is that the SiC particle of 3.5 μ m joins slurry prepared in the matrix ZL109 aluminium alloy after rotary casting is solidified, and obtains photo with the scanning electron microscope imaging, as shown in Figure 3.
Embodiment 4
1. be 0.1% HF to diameter with the quality percentage composition be that the graphite granule of 100 μ m carries out pickling, remove the zone of oxidation or the adsorbent of particle surface, with resistance furnace particle is heated to 673K then, and be incubated 20 minutes, remove granule surface activity water, particle is disperseed automatically, after the cooling, rice get 0.15 kilogram standby;
2. in antivacuum medium-frequency induction furnace 1.5 kilograms metallic aluminium is heated to liquid state, feeds argon gas liquid towards metal and carry out refining, the liquid towards metal is lowered the temperature after skimming;
3. liquid metal is cooled to semi-solid state (983K), directly ready graphite granule is joined the semi-solid-state metal surface then, with the stepless speed regulation agitator it is stirred, stirring total time is 30 minutes, and segmentation is stirred: the fs stirring velocity is 30 rev/mins, and churning time is 20 minutes; The subordinate phase stirring velocity is 300 rev/mins, and churning time is 5 minutes; The phase III stirring velocity is 600 rev/mins, and churning time is 5 minutes; Thereby the formation slurry with antivacuum medium-frequency induction furnace insulation, is protected with argon gas in operating process.
After resulting slurry cooled off, obtain photo with microscope imaging, as shown in Figure 4 in air.

Claims (2)

1. particulate addition method in slurry when liquid phase process prepares particle enhanced aluminum-based composite material, utilize non-vacuum induction furnace, it is characterized in that: particle is carried out after the pre-treatment, stirring action by means of mechanical external force, directly particle is joined in the semi-solid matrix metal aluminum or aluminum alloy, concrete steps are as follows:
1) with the quality percentage composition is 0.1~0.8% HF or HNO 3Particle is carried out pickling, remove the zone of oxidation or the adsorbent of particle surface, with heating installation particle is heated to 673~873K then, and is incubated 20~40 minutes, remove granule surface activity water, particle is disperseed automatically;
2) in non-vacuum induction furnace the matrix metal aluminum or aluminum alloy is heated to liquid state, feeds argon gas liquid towards metal then and carry out refining, the liquid towards metal is lowered the temperature after skimming;
3) liquid metal is cooled to semi-solid state, the semi-solid temperature of described aluminium is 983K~1013K, the semi-solid temperature of described aluminium alloy is 933K~1003K, directly particle is joined the semi-solid-state metal surface then, with the stepless speed regulation agitator it is stirred, stirring total time is 30~50 minutes, and segmentation is stirred: the fs stirring velocity is 30~100 rev/mins, and churning time is 20~30 minutes; The subordinate phase stirring velocity is 100~500 rev/mins, and churning time is 5~10 minutes; The phase III stirring velocity is 500~800 rev/mins, and churning time is 5~10 minutes; Thereby the formation slurry with the non-vacuum induction furnace insulation, is protected with argon gas in operating process.
2. particulate addition method in the slurry when preparing particle enhanced aluminum-based composite material according to the described liquid phase process of claim 1, it is characterized in that: described particle is graphite, SiC or Al 2O 3Particle, its diameter are 3.5~100 μ m.
CNB011138475A 2001-04-13 2001-04-13 Method for adding particles to slurry in preparing particle reinforced Al-base composition by liquid state method Expired - Fee Related CN1151295C (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100464898C (en) * 2007-06-18 2009-03-04 北京科技大学 Process for making SiC particle reinforced composite material electronic package shell using semi-soild-state technology
CN100577831C (en) * 2007-11-23 2010-01-06 中国铝业股份有限公司 Apparatus for industrialized preparation of granule-reinforced aluminium-based composite material
CN102400006A (en) * 2010-09-16 2012-04-04 北京有色金属研究总院 Foamy carbon/copper matrix or aluminum matrix composite material and preparation method thereof
CN102632221A (en) * 2012-04-28 2012-08-15 昆明理工大学 Method for compounding SiC grains on surface of semisolid A356 aluminum alloy
CN102703771A (en) * 2012-06-17 2012-10-03 山东正诺机械科技有限公司 Preparation method for silicon carbide/aluminium alloy composite material for brake disc
CN103100700A (en) * 2013-01-21 2013-05-15 东北大学 Cladding casting device for aluminum alloy composite ingot casting and cladding casting method
CN105525153A (en) * 2015-11-30 2016-04-27 中国铁道科学研究院 Brake disc prepared from silicon carbide particle reinforced aluminum matrix composite material
CN105568034A (en) * 2015-12-17 2016-05-11 华南理工大学 Granular mixed reinforced aluminum-based composite material and method for preparing same
CN105908020A (en) * 2016-05-17 2016-08-31 广东省材料与加工研究所 Preparation method of aluminum-tungsten composite material
CN107604191A (en) * 2016-07-11 2018-01-19 广东科达洁能股份有限公司 The preparation method of high quality fraction SiCp/Al composites and carborundum stirring adding set in a kind of Monosized powder
CN109811173A (en) * 2019-01-29 2019-05-28 清华大学深圳研究生院 A kind of TiB2The preparation method and TiB of-Al composite material2- Al composite material
CN111101028A (en) * 2019-12-27 2020-05-05 宁波吉胜铸业有限公司 Engine body aluminum casting support
CN112605349A (en) * 2020-12-08 2021-04-06 安徽中鑫精密铸造科技有限公司 Semi-solid forming process for water-cooling plate for bearing automobile chip
CN116043059A (en) * 2023-01-18 2023-05-02 江苏大学 Method for preparing micro-nano particle hybrid reinforced aluminum matrix composite

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100464898C (en) * 2007-06-18 2009-03-04 北京科技大学 Process for making SiC particle reinforced composite material electronic package shell using semi-soild-state technology
CN100577831C (en) * 2007-11-23 2010-01-06 中国铝业股份有限公司 Apparatus for industrialized preparation of granule-reinforced aluminium-based composite material
CN102400006B (en) * 2010-09-16 2013-05-22 北京有色金属研究总院 Foamy carbon/copper matrix or aluminum matrix composite material and preparation method thereof
CN102400006A (en) * 2010-09-16 2012-04-04 北京有色金属研究总院 Foamy carbon/copper matrix or aluminum matrix composite material and preparation method thereof
CN102632221A (en) * 2012-04-28 2012-08-15 昆明理工大学 Method for compounding SiC grains on surface of semisolid A356 aluminum alloy
CN102632221B (en) * 2012-04-28 2015-03-11 昆明理工大学 Method for compounding SiC grains on surface of semisolid A356 aluminum alloy
CN102703771A (en) * 2012-06-17 2012-10-03 山东正诺机械科技有限公司 Preparation method for silicon carbide/aluminium alloy composite material for brake disc
CN102703771B (en) * 2012-06-17 2013-08-14 山东正诺机械科技有限公司 Preparation method for silicon carbide/aluminium alloy composite material for brake disc
CN103100700A (en) * 2013-01-21 2013-05-15 东北大学 Cladding casting device for aluminum alloy composite ingot casting and cladding casting method
CN105525153A (en) * 2015-11-30 2016-04-27 中国铁道科学研究院 Brake disc prepared from silicon carbide particle reinforced aluminum matrix composite material
CN105568034A (en) * 2015-12-17 2016-05-11 华南理工大学 Granular mixed reinforced aluminum-based composite material and method for preparing same
CN105568034B (en) * 2015-12-17 2018-01-05 华南理工大学 A kind of particle hybrid composite and preparation method thereof
CN105908020A (en) * 2016-05-17 2016-08-31 广东省材料与加工研究所 Preparation method of aluminum-tungsten composite material
CN107604191A (en) * 2016-07-11 2018-01-19 广东科达洁能股份有限公司 The preparation method of high quality fraction SiCp/Al composites and carborundum stirring adding set in a kind of Monosized powder
CN109811173A (en) * 2019-01-29 2019-05-28 清华大学深圳研究生院 A kind of TiB2The preparation method and TiB of-Al composite material2- Al composite material
CN111101028A (en) * 2019-12-27 2020-05-05 宁波吉胜铸业有限公司 Engine body aluminum casting support
CN112605349A (en) * 2020-12-08 2021-04-06 安徽中鑫精密铸造科技有限公司 Semi-solid forming process for water-cooling plate for bearing automobile chip
CN116043059A (en) * 2023-01-18 2023-05-02 江苏大学 Method for preparing micro-nano particle hybrid reinforced aluminum matrix composite

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