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CN1195090C - Mixed salt process to preparing in-situ reinforced Mg-based composite material - Google Patents

Mixed salt process to preparing in-situ reinforced Mg-based composite material Download PDF

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Publication number
CN1195090C
CN1195090C CNB031161693A CN03116169A CN1195090C CN 1195090 C CN1195090 C CN 1195090C CN B031161693 A CNB031161693 A CN B031161693A CN 03116169 A CN03116169 A CN 03116169A CN 1195090 C CN1195090 C CN 1195090C
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magnesium
mixed salt
composite materials
based composite
preparing
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CN1441076A (en
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王浩伟
张修庆
滕新营
马乃恒
易宏展
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Shanghai Jiao Tong University
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Shanghai Jiao Tong University
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Abstract

The present invention relates to a technology for preparing in-situ reinforced magnesium-based composite materials by a mixed salt method, which belongs to the field of materials. In the present invention, the ingredients of alloy elements in composite materials are first determined according to the ingredients of alloy elements in standard magnesium alloy trademarks; wild phases are selected according to the wettability between a basal body and the wild phases, and the content of wild phase granules is controlled between 2 and 15%; a mixed salt system is prepared and pretreated, and the magnesium-based materials are then smelted; melt temperature is selected, and treated mixed salt is added to magnesium melts so as to carry out stirring operation; the melts are finally placed still and poured, and casting formation is realized. In the present invention, the mixed salt method has the assistance of the stirring operation, and the granule volume fractions, the melt temperature and the stirring time are selected so that the magnesium-based composite materials with the advantages of small wild phase granules, uniform distribution, favorable interface combination, and good mechanical and physical performance are prepared. Consequently, 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.

Description

Mixed salt method prepares original position and strengthens magnesium base composite material technology
Technical field
What the present invention relates to is a kind of technology for preparing matrix material, and particularly a kind of mixed salt method prepares original position and strengthens magnesium base composite material technology, belongs to the material field.
Background technology
In recent years, owing to concern to environment, energy problem, 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 specific tenacity, specific rigidity height, good castibility and dimensional stability, anti-electromagnetic interference and shielding are good, good damping performance is arranged, damping property is good, and in addition, the waste recovery utilization ratio of magnesium base composite material is up to more than 85%.So the development magnesium base composite material is significant to energy-saving and environmental protection.The preparation magnesium base composite material mainly is that application adds particle or fiber strengthens at present; its main preparation method has stirring casting, pressure impregnation method, powder metallurgic method etc.; these production technique are more complicated mostly; the cost height; and it is big to add the enhanced granule granularity; the interface is in conjunction with bad, and material mechanical performance is poor.The in-situ preparing matrix material is the preparation method that development in recent years is got up, and it is tiny that it has the enhanced granule granularity of preparation, and interface junction gets togather, the characteristics that the material over-all properties is high.The salts reaction method is a kind of in the in-situ preparing matrix material, finds by literature search, and people such as Chen Ziyong have delivered in June, 1997 " Special Processes of Metal Castings and non-ferrous alloy " (P1～4) that " salts reaction prepares TiB 2/ Al-4.5Cu composite study " literary composition, this article proposes the matrix material with the preparation of salts reaction method, and the wild phase particle of material is tiny, is evenly distributed.But in the salts reaction process, increased the air content of aluminum matrix composite, need advance the degasification refining to aluminum matrix composite, but because the melting degree of hydrogen in magnesium is lower, the complicated technology that does not have the refining degasification has reasonable prospect so be equipped with magnesium base composite material with the salts reaction legal system.But because the temperature that salts reaction needs is than higher, and the at high temperature easier burning of magnesium, so salts reaction is difficult to carry out in magnesium.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, provide a kind of mixed salt method to prepare original position and strengthen magnesium base composite material technology, by choosing suitable reacting salt system, utilize the reaction of mixing salt in the magnesium melt, and prepare by stirring technique that the wild phase particle is tiny, the uniform original position enhanced of distribution disperse magnesium base composite material, and composite material interface is in conjunction with good, and mechanical property is superior.
The present invention is achieved by the following technical solutions, and processing step of the present invention is as follows:
(1) determines the composition of the alloying element in the matrix material according to the alloy element component of stipulating in the standard magnesium alloy trade mark, and select TiB according to the wettability between matrix and the wild phase 2Or ZrB 2As wild phase, the wild phase granule content is controlled at 2～15%.According to the different mixing salt system of above requirement preparation, the mixing salt system of choosing is carried out pre-treatment.
The mixing salt system contains fluotitanate, fluoroborate, fluozirconate and fluoaluminate etc.; The pre-treatment of mixing salt system is: at first mix, dried 1～3 hour in 150 ℃～250 ℃ scope then.
(2) carry out the melting of magnesium matrix material.In fusion process, add ignition-proof element beryllium, calcium etc. and prevent the magnesium burning, adopt gas or flux protection in the fusion process.
(3) choose suitable melt temperature, will handle mixing salt well and add in the magnesium melt, stir.
The temperature of magnesium melt is to the very big influence that has of reaction, and the too low then reaction of temperature can not take place, and the too high burning that then can cause magnesium easily of temperature is so the melt temperature that the present invention chooses is 740 ℃～800 ℃.Utilize stirring one is fully carrying out of can promoting to react, and makes generated in-situ enhanced granule more tiny; The 2nd, can prevent the particulate reunion, promote the dispersion of particle in melt, make the dispersion disperse of enhancing body in body material even.Also there are very big influence churning time intensity and time to material, and stirring intensity helps the carrying out that react greatly, but also increases the chance that particle collides in melt, increase and reunite, so choose suitable stirring velocity synthetic very important to material; Churning time is short, and reaction can not exclusively reduce 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.
(4) melt is left standstill back cast, casting.The melt dwell temperature is 700 ℃～740 ℃, and time of repose is 5～20min, and cast can be adopted metal mold or sand mold.
The present invention has substantive distinguishing features and marked improvement, and the present invention adopts the novel process of mixing salt reaction and stirring to prepare original position enhanced magnesium base composite material.It is thick to add particle enhanced magnesium base composite material particle, disperse inhomogeneous, and the interface is bad, and the present invention utilizes mixed salt method and be aided with stirring, chooses suitable grain volume fraction, melt temperature, it is tiny that churning time has been prepared 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 of magnesium base composite material is laid a good foundation.
Embodiment
The present invention adopts mixed salt method to prepare original position enhanced magnesium base composite material, and the wild phase particle in the matrix material is tiny, and is evenly distributed in matrix, and matrix material also has the good mechanical performance.Content in conjunction with this technology provides following examples:
Embodiment 1 adopts pure magnesium pure as body material, KBF 4And K 2TiF 6As the reaction mixing salt, do not implement to stir, to pour into a mould after leaving standstill 5min for 700 ℃, preparation quality percentage ratio is 5% TiB 2Original position enhanced magnesium base composite material.The tensile strength of material is 275MPa, and unit elongation is 1.2%.
Embodiment 2 pure magnesium are as body material, KBF 4And K 2TiF 6As the reaction mixing salt, the steel oar stirs with 200r/min, and churning time is 10min, pours into a mould after leaving standstill 5min for 700 ℃, and preparation quality percentage ratio is 5% TiB 2The original position reinforced composite materials.The tensile strength of material is 280MPa, and unit elongation is 2.8%.
Embodiment 3ZM5 is as body material, KBF 4And K 2TiF 6As the reaction mixing salt, the steel oar stirs with 600r/min, and churning time is 20min, pours into a mould after leaving standstill 15min for 720 ℃, and preparation quality percentage ratio is 5% TiB 2The original position reinforced composite materials.The tensile strength of material is 282MPa, and unit elongation is 2.7%.
Embodiment 4ZM5 is as body material, KBF 4And K 2ZrF 6As the reaction mixing salt, the steel oar stirs with 1000r/min, and churning time is 30min, pours into a mould after leaving standstill 20min for 740 ℃, and preparation quality percentage ratio is 5% ZrB 2The original position reinforced composite materials.The tensile strength of material is 275MPa, and unit elongation is 2.5%.

Claims (3)

1、一种混合盐法制备原位增强镁基复合材料工艺，其特征在于工艺步骤如下：1. A process for preparing in-situ reinforced magnesium-based composite materials by a mixed salt method, characterized in that the process steps are as follows: (1)根据标准镁合金牌号中规定的合金元素成分确定复合材料中的合金元素的成分，并根据基体和增强相之间的润湿性选择TiB2或ZrB2作为增强相，根据以上要求配制混合盐体系，混合盐体系含有氟钛酸盐、氟硼酸盐、氟锆酸盐和氟铝酸盐，并将选取的混合盐体系进行预处理；混合盐体系的预处理为：首先进行混合，然后在150℃～250℃的范围内烘干1～3小时；(1) Determine the alloy element composition in the composite material according to the alloy element composition specified in the standard magnesium alloy grade, and select TiB 2 or ZrB 2 as the reinforcement phase according to the wettability between the matrix and the reinforcement phase, and prepare according to the above requirements Mixed salt system, the mixed salt system contains fluorotitanate, fluoroborate, fluorozirconate and fluoroaluminate, and the selected mixed salt system is pretreated; the pretreatment of the mixed salt system is: firstly mix , and then dry in the range of 150°C to 250°C for 1 to 3 hours; (2)然后进行镁基体材料的熔炼；(2) Carry out the smelting of magnesium matrix material then; (3)再选取熔体温度，将处理好的混合盐加入镁熔体中，进行搅拌，熔体温度为740℃～800℃，搅拌转速为200～1000r/min，搅拌时间为10～30min；(3) Select the melt temperature again, add the processed mixed salt into the magnesium melt, and stir, the melt temperature is 740°C-800°C, the stirring speed is 200-1000r/min, and the stirring time is 10-30min; (4)最后将熔体静置后浇注，铸造成型。(4) Finally, pour the melt after standing still, and cast it into shape. 2、根据权利要求1所述的混合盐法制备原位增强镁基复合材料工艺，其特征是，步骤(2)中所述的进行镁基体材料的熔炼，在熔炼过程中添加阻燃元素铍、钙防止镁燃烧，熔炼过程中采用气体或熔剂保护。2. The process for preparing in-situ reinforced magnesium-based composite materials by the mixed salt method according to claim 1 is characterized in that, in step (2), the magnesium matrix material is smelted, and the flame-retardant element beryllium is added during the smelting process , Calcium prevents magnesium from burning, and gas or flux protection is used during the smelting process. 3、根据权利要求1所述的混合盐法制备原位增强镁基复合材料工艺，其特征是，步骤(4)中所述的熔体静置温度为700℃～740℃，静置时间为5～20min，浇注采用金属型或砂型。3. The process for preparing in-situ reinforced magnesium-based composite materials by the mixed salt method according to claim 1, characterized in that the resting temperature of the melt in step (4) is 700°C to 740°C, and the resting time is 5 to 20 minutes, metal mold or sand mold is used for casting.
CNB031161693A 2003-04-03 2003-04-03 Mixed salt process to preparing in-situ reinforced Mg-based composite material Expired - Fee Related CN1195090C (en)

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