CN1298879C - Process of preparing composite material with in situ particle inhancing magnesium base - Google Patents
Process of preparing composite material with in situ particle inhancing magnesium base Download PDFInfo
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- CN1298879C CN1298879C CNB2004100164262A CN200410016426A CN1298879C CN 1298879 C CN1298879 C CN 1298879C CN B2004100164262 A CNB2004100164262 A CN B2004100164262A CN 200410016426 A CN200410016426 A CN 200410016426A CN 1298879 C CN1298879 C CN 1298879C
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Abstract
The present invention relates to a technology for preparing reinforced magnesium-aluminum based composite materials of in-situ granules, which belongs to the field of materials. In the technology, wild phases are first selected according to the wettability between a basal body and the wild phases; parents of aluminum-magnesium based composite materials, which have 10 to 30% of granules according to the weight percentage, are prepared by a mixed salt method, and magnesium base body materials are then smelted; a melt temperature is selected, and the parents of the aluminum-magnesium based composite materials are added to magnesium melts to carry out stirring; the melts are finally poured, cast and molded after standing. In the technology, the parents of the aluminum-magnesium based composite materials are prepared through the mixed salt method, stirring is used as assistance, and the parents of the aluminum-magnesium based composite materials are re-melted and diluted; consequently, the magnesium based composite materials with the advantages of small wild phase granules, uniform distribution, good interface combination, and favorable mechanical and physical performance are prepared. A new path is opened up for preparing the magnesium-based composite materials, and a good foundation is laid for the wide application of the magnesium based composite materials in the industrial field.
Description
Technical field
What the present invention relates to is a kind of technology for preparing particle reinforced magnesium base compound material, and particularly a kind of prefabricated parent of aluminum matrix composite that utilizes prepares the technology that original position strengthens magnesium base composite material, belongs to the material field.
Background technology
In recent years, owing to concern to problems such as environment, the energy, the focus in magnesium base composite material research becoming material field.Magnesium base composite material is one of the lightest structured material, and magnesium base composite material has high specific tenacity, specific rigidity, good castibility and dimensional stability, anti-electromagnetic interference and shielding are good, and good damping performance is arranged, and damping property is good, little to environmental influence, pollution-free, its waste recovery utilization ratio has wide practical use in fields such as space flight and aviation, automobile, computer, network, communications up to 85%.So the development magnesium base composite material is significant to energy-saving and environmental protection.At present the preparation magnesium base composite material mainly is to use to add particle or fiber strengthens, and it is big to add the enhanced granule granularity, and the interface is in conjunction with bad, and material mechanical performance is poor; Fibre-reinforced composite material preparation process complexity, cost is restricted in production application than higher.The in-situ preparing matrix material is the preparation method that development in recent years is got up, and it has, and the enhanced granule granularity of preparation is tiny, and interface junction gets togather, and the characteristics that the material over-all properties is high are obtaining many successes aspect the preparation aluminum matrix composite.Find by literature search, Chinese patent publication number: 1441076, patent name is: mixed salt method prepares original position and strengthens magnesium base composite material technology, this patent has proposed to prepare with mixed salt method the technology of magnesium base composite material, this technology is chosen suitable wild phase reaction system, grain volume fraction, melt temperature, it is tiny that churning time is prepared the wild phase particle, be evenly distributed, the interface is in conjunction with good, and has a good mechanical, the magnesium base composite material of physicals, but because the specific activity of magnesium is bigger, easy and a lot of materials react, so mixed salt method prepares magnesium base composite material to the wild phase system, the fusant reaction temperature all has strict requirement, is not easy control in actual production, has certain restriction so mixed salt method prepares magnesium base composite material.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of technology that particle in-situ strengthens magnesium base composite material for preparing is provided.The present invention utilizes the prefabricated parent of mixed salt method in-situ preparing particle enhanced aluminium-magnesium base composite material, and then be diluted in the magnesium melt aluminium-magnesium base composite material preform carrier body weight is molten, it is tiny to have prepared the wild phase particle, the magnesium base composite material that is evenly distributed, the Interface for Mg Matrix Composites of preparation is in conjunction with good, and mechanical property, physicals are superior.
The present invention is achieved by the following technical solutions, the present invention at first selects wild phase according to the wettability between matrix and the wild phase, preparing weight percentage with mixed salt method is aluminium-magnesium base composite material parent of 10~30%, carry out the melting of magnesium matrix material then, choose melt temperature again, aluminium-magnesium base composite material parent is added in the magnesium melt, stir, at last melt is left standstill the back cast, casting.
Below to the inventive method further instruction, processing step is as follows:
(1) prepares aluminium-magnesium base composite material parent with mixed salt method.Mixing salt reaction system select titanium salt, boron salt or zirconates, preparation TiB
2Or ZrB
2Particle enhanced aluminium-magnesium base composite material, the content of enhanced granule are 10~30% weight percent.At first fine aluminium is melted, fusing back molten aluminium temperature remains on 750~850 ℃, add pretreated mixing salt, mixing salt pre-treatment dried 1~3 hour in 150 ℃~250 ℃ scope for mixing the back, stir after adding mixing salt, stir speed (S.S.) is at 200~1000r/min, and churning time is 10~60min, after stirring end, the reaction residue of bath surface is scooped out.In order to increase the flowability of aluminum matrix composite melt, add the MAG block of oven dry, add-on is weight percentage 5~10%.In order to guarantee the content at the magnesium base composite material wild phase, the granule content in aluminium-magnesium base composite material parent must reach certain numerical value, and in this technology, the granule content weight percent of aluminium-magnesium base composite material parent is 10~30%.
(2) melting of magnesium.Magnesium very easily burns, so the melting of magnesium also is an important step.Can adopt flux protection or gas shield in the fusion process of magnesium, and to add weight percent as required be that 0.001%~0.1% beryllium, 0.05%~0.2% calcium are as ignition-proof element.
(3) after the magnesium ingot fusing, choose the magnesium melt temperature, in the adding magnesium melt with the prefabricated parent of aluminium-magnesium base composite material, stir.
The density of pure magnesium is smaller, has only 1.74g/cm
3, and wild phase generally all is a ceramic particle, and the density of magnesium and wild phase differs bigger, and wild phase easier generation sedimentation phenomenon in magnesium is so the sedimentation of control wild phase in magnesium is the comparison critical step.Utilize to stir and to promote that particulate fully disperses, particle disperse in magnesium matrix is distributed, and can prevent that particulate from reuniting again, prevent settled generation.And stir and can promote the fusion of the prefabricated parent of aluminium-magnesium base composite material in the magnesium melt to disperse, be an important step so stir.Churning time intensity and time to the fusion of aluminium-magnesium base composite material parent, disperse and prevent that the particulate sedimentation from having bigger influence, stirring intensity helps particulate to disperse greatly, but also increase the chance that particle collides in melt, increase and reunite, so it is very important to synthesizing of material to choose suitable stirring velocity; Churning time is short, and particles dispersed is inhomogeneous, and sedimentation phenomenon is obvious, reduces the particulate recovery rate, but the oversize oxidation that then can increase melt.The mixing speed that the present invention chooses is 200~1000r/min.Churning time is 10~30min.In the prefabricated parent fusion processes of aluminium-magnesium base composite material, the temperature of magnesium melt also is the comparison key, and melt temperature is low, and aluminium-magnesium base composite material parent fusion slowly easily sinks to magnesium melt lower curtate, and the process time is prolonged, and reduces productivity.The too high oxidation that then can increase magnesium of magnesium melt temperature increases oxide inclusion, increases the scaling loss of magnesium.The temperature of this technology magnesium melt remains on 720 ℃~780 ℃.
(4) after stirring finishes melt is left standstill the back cast, casting obtains magnesium base composite material.The melt dwell temperature is 700 ℃~740 ℃, and time of repose is 5~20min, and cast can be selected metal mold or sand mold for use.
Aluminium is most important alloying element in the magnesium alloy, and aluminium content in magnesium alloy can reach in 12% about weight percent, and the fusing point of aluminium has only 660 ℃, fusing easily in magnesium, and diffusion so the operation of fusion aluminium is fairly simple in magnesium, realizes easily.The magnesium alloy of magnalium system such as AZ61A, AZ80A, widely used alloys such as AZ91A, AM100A, performances such as its specific tenacity, specific rigidity are higher than corresponding aluminium alloy.And with respect to magnesium, aluminium active less, the original position that can realize much strengthening body in molten aluminium easily is synthetic, and melt temperature also can change on a large scale, and wild phase composition, quantity also can well control.
Compared with prior art, the present invention is added to aluminum matrix composite in the magnesium melt, the matrix material of preparation magnalium base, at first utilize mixed salt method to prepare aluminium-magnesium base composite material parent, be aided with stirring, carry out the remelting dilution of aluminium-magnesium base composite material parent, it is tiny to prepare the wild phase particle, be evenly distributed, the interface is in conjunction with good, and the magnesium base composite material with good mechanical, physicals, for the preparation magnesium base composite material opens up a new way, for the widespread use at industrial circle of magnesium base composite material is laid a good foundation.
Embodiment
Content in conjunction with technology of the present invention provides following examples:
Embodiment 1
With fine aluminium as prefabricated parent body material, KBF
4And K
2TiF
6As mixing salt, 150 ℃ of oven dry 1 hour.The molten aluminium temperature is selected 750 ℃, stirs 10min with the steel oar with the speed of 200r/min, stir to finish the back and be pressed into 5% magnesium with bell jar, has at first prepared mass percent and be 10% TiB
2Original position enhanced aluminium-magnesium base composite material parent.Add the prefabricated parent of aluminium-magnesium base composite material when the magnesium melt temperature keeps 720 ℃, the steel slurry stirs with 200r/min, and churning time is 10min, stirs to finish the back melt and pour into a mould after leaving standstill 5min at 700 ℃, has prepared TiB
2Original position enhanced magnalium based composites.The tensile strength of material is 343~352MPa, and unit elongation is 3.8~4.0%.
Embodiment 2
With fine aluminium as prefabricated parent body material, KBF
4And K
2TiF
6As mixing salt, 200 ℃ of oven dry 2 hours.The molten aluminium temperature is selected 800 ℃, stirs 30min with the steel oar with the speed of 600r/min, stir to finish the back and be pressed into 8% magnesium with bell jar, has at first prepared mass percent and be 15% TiB
2Original position enhanced aluminium-magnesium base composite material parent.Add the prefabricated parent of aluminium-magnesium base composite material when the magnesium melt temperature keeps 740 ℃, the steel slurry stirs with 600r/min, and churning time is 20min, stirs to finish the back melt and pour into a mould after leaving standstill 10min at 720 ℃, has prepared TiB
2Original position enhanced magnalium based composites.The tensile strength of material is 363~378MPa, and unit elongation is 4.1~4.8%.
Embodiment 3
With fine aluminium as prefabricated parent body material, KBF
4And K
2ZrF
6As mixing salt, 200 ℃ of oven dry 2 hours.The molten aluminium temperature is selected 800 ℃, stirs 40min with the steel oar with the speed of 600r/min, stir to finish the back and be pressed into 8% magnesium with bell jar, has at first prepared mass percent and be 15% ZrB
2Original position enhanced aluminium-magnesium base composite material parent.Add the prefabricated parent of aluminium-magnesium base composite material when the magnesium melt temperature keeps 740 ℃, the steel slurry stirs with 600r/min, and churning time is 20min, stirs to finish the back melt and pour into a mould after leaving standstill 10min at 720 ℃, has prepared ZrB
2Original position enhanced magnalium based composites.The tensile strength of material is 333~342MPa, and unit elongation is 3.9~4.3%.
Embodiment 4
With fine aluminium as prefabricated parent body material, KBF
4And K
2TiF
6As mixing salt, 250 ℃ of oven dry 3 hours.The molten aluminium temperature is selected 850 ℃, stirs 60min with the steel oar with the speed of 1000r/min, stir to finish the back and be pressed into 10% magnesium with bell jar, has at first prepared mass percent and be 30% TiB
2Original position enhanced aluminium-magnesium base composite material parent.Add the prefabricated parent of aluminium-magnesium base composite material when the magnesium melt temperature keeps 780 ℃, the steel slurry stirs with 1000r/min, and churning time is 30min, stirs to finish the back melt and pour into a mould after leaving standstill 20min at 740 ℃, has prepared TiB
2Original position enhanced magnalium based composites.The tensile strength of material is 308~321MPa, and unit elongation is 3.7~4.2%.
Claims (3)
1, a kind of technology for preparing in-situ particle reinforced magnesium-based composite material is characterized in that, at first selects TiB according to the wettability between matrix and the wild phase
2Perhaps ZrB
2As wild phase, adopt titanium salt and boron salt or zirconates and boron salt as mixing salt, preparation TiB
2Or ZrB
2Particle enhanced aluminium-magnesium base composite material parent, its step is at first melting fine aluminium, fusing back molten aluminium temperature remains on 750~850 ℃, add pretreated mixing salt, mixing salt pre-treatment dried 1~3 hour in 150 ℃~250 ℃ scope for mixing the back, stir after adding mixing salt, stirring velocity is 200~1000r/min, churning time is 10~60min, after stirring end, the reaction residue of bath surface is scooped out, and the magnesium ingot that adds weight percent 5~10% oven dry increases the flowability of aluminum matrix composite melt, and preparing the enhanced granule weight percent with mixed salt method is after aluminium-magnesium base composite material parent of 10~30%, carry out the melting of magnesium matrix material, choosing melt temperature is 720~780 ℃, and aluminium-magnesium base composite material parent is added in the magnesium melt, stirs, stirring velocity is 200~1000r/min, churning time is 10~30min, at last melt is left standstill the back cast, casting.
2, the technology of preparation in-situ particle reinforced magnesium-based composite material according to claim 1; it is characterized in that: in the melting of described magnesium matrix material: adopt flux protection or gas shield, and to add weight percent be that 0.001%~0.1% beryllium, 0.05%~0.2% calcium are as ignition-proof element.
3, the technology of preparation in-situ particle reinforced magnesium-based composite material according to claim 1 is characterized in that, described melt dwell temperature is 700 ℃~740 ℃, and time of repose is 5~20min, and metal mold or sand mold are adopted in cast.
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CN102352449B (en) * | 2011-10-12 | 2013-05-22 | 南昌大学 | Preparation method of in-situ ZrB2 particle reinforced magnesium-based composite |
CN102765953B (en) * | 2012-08-07 | 2013-12-11 | 营口鲅鱼圈耐火材料有限公司 | Magnesia carbon brick containing composite antioxidant and preparation thereof |
CN103031475A (en) * | 2012-12-28 | 2013-04-10 | 山东大学 | In-situ synthesized Al3BC reinforced magnesium matrix composite and fabrication method thereof |
CN105063404A (en) * | 2015-06-25 | 2015-11-18 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of titanium matrix graphene alloy |
CN105112694A (en) * | 2015-06-25 | 2015-12-02 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of magnesium base graphene alloy |
Citations (5)
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JPH098778A (en) * | 1995-06-07 | 1997-01-10 | At & T Corp | Wholly double data communication system using different transmission and reception data code lengths |
US6143371A (en) * | 1997-05-28 | 2000-11-07 | Suzuki Motor Corporation | Process for producing an MG-based composite material or an MG alloy-based composite material |
CN1396284A (en) * | 2002-01-27 | 2003-02-12 | 吉林大学 | Process for preparing particle reinforced Mg-base composite |
CN1441076A (en) * | 2003-04-03 | 2003-09-10 | 上海交通大学 | Mixed salt process to preparing in-situ reinforced Mg-based composite material |
CN1441074A (en) * | 2003-04-03 | 2003-09-10 | 上海交通大学 | Prepn process of Mg-based composite material |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH098778A (en) * | 1995-06-07 | 1997-01-10 | At & T Corp | Wholly double data communication system using different transmission and reception data code lengths |
US6143371A (en) * | 1997-05-28 | 2000-11-07 | Suzuki Motor Corporation | Process for producing an MG-based composite material or an MG alloy-based composite material |
CN1396284A (en) * | 2002-01-27 | 2003-02-12 | 吉林大学 | Process for preparing particle reinforced Mg-base composite |
CN1441076A (en) * | 2003-04-03 | 2003-09-10 | 上海交通大学 | Mixed salt process to preparing in-situ reinforced Mg-based composite material |
CN1441074A (en) * | 2003-04-03 | 2003-09-10 | 上海交通大学 | Prepn process of Mg-based composite material |
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