CN1195089C - Prepn process of particle-reinforced Mg-base composite mateiral - Google Patents
Prepn process of particle-reinforced Mg-base composite mateiral Download PDFInfo
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- CN1195089C CN1195089C CNB031161685A CN03116168A CN1195089C CN 1195089 C CN1195089 C CN 1195089C CN B031161685 A CNB031161685 A CN B031161685A CN 03116168 A CN03116168 A CN 03116168A CN 1195089 C CN1195089 C CN 1195089C
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Abstract
The present invention relates to a technology for preparing magnesium-based composite materials with granule reinforcement, which belongs to the field of materials. The present invention comprises the following steps that the ingredients and the wild phases of alloy elements in composite materials are determined, the content of wild phase granules is controlled between 2 and 15%, powders prepared according to a proportion are mixed, and the powders on which ball milling mixture is already carried out are taken out in a protective atmosphere; the mixed powders are pressed into blocks, block-shaped precast bodies are sintered under the protection of inert gas, and the wild phases of magnesium-based composite materials are synthesized in the process of sintering the mixed powders; the magnesium-based materials are smelted, and the precast bodies are melted; the precast bodies are first baked, melt temperature is selected, the precast bodies are added to magnesium melts, and stirring operation is carried out while the temperature is preserved; the melts are placed still and poured, and shaping is realized through casting. Magnesium-based composite materials with small wild phase granules, uniform distribution, good interface combination, and favorable mechanical and physical performance are prepared by the present invention; 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
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 remelting dilution method 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.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 remelting dilution method is one of method for preparing in-situ composite.People such as Cheng Xiulan were " Arms Material scientific and engineering " 1999 22 (3): write articles " research of in-situ Al-base composition remelting dilution " on 18～22, introduced the research of remelting dilution preparation in-situ Al-base composition in this article, in their research, the Al of strip appears coming in the matrix material
3Ti has influenced the mechanical property of matrix material.Moreover the remelting dilution method has many research in the preparation aluminum matrix composite, but is not applied to prepare at present the report and the document of magnesium base composite material.Further the technology of research remelting dilution method is controlled sintering process, and its preparation that is applied to magnesium base composite material, reasonable development prospect is arranged.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of technology for preparing particle reinforced magnesium base compound material is provided, make it utilize the reaction sintering preparation to strengthen precast body, and make particles dispersed even by stirring technique, it is tiny to prepare the wild phase particle, the magnesium base composite material that is evenly distributed, composite material interface be in conjunction with good, and mechanical property, physicals are 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, select TiC, ZrC, 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%, and according to the different precast body of above requirement preparation, the precast body that proportioning is good mixes under protective atmosphere with planetary ball mill, and the mixed powder of ball milling takes out under protective atmosphere.
Precast body is compound or the simple substance powder that contains the wild phase component, contains the alloying element powder of magnesium alloy.Can use aluminium powder, zinc powder, titanium valve, carbon dust, zirconium powder, boron carbide powder etc. as the precast body raw material powder, according to the composition proportion of material performance requirement design precast body.Ball milling can selected parameter: rotational speed of ball-mill is 150～500r/min, and the ball milling time is 30～600min, and ratio of grinding media to material is 5: 1～50: 1.
(2) select for use suitable pressure that the powder compression that mixes is become block, block precast body is carried out sintering under protection of inert gas.It is 5～30MPa that powder compression becomes bulk to select pressure for use, and the dwell time is 30～600s.Sintering process is incubated 10～60min then at first being warmed up to 500 ℃～650 ℃, is warmed up to 800 ℃～1500 ℃ again, is incubated 10～60min.
(3) melting of magnesium matrix material.In fusion process, add ignition-proof element beryllium, calcium etc. and prevent the melt burning, adopt gas or flux protection in the fusion process.
(4) carry out the fusion processes of precast body, precast body was at first dried 1～3 hour in 150 ℃～250 ℃ scope, chose suitable melt temperature again, and precast body is added in the magnesium melt, and insulation 10～60min stirs.
In order to quicken the fusion of precast body, precast body is handled in flux, flux mainly consist of villaumite and villiaumite mixture.The temperature of magnesium melt has very big influence to the fusion of precast body, and the too low then fusion of temperature slowly prolongs the process time, reduce production efficiency, the too high burning that then can cause magnesium easily of temperature, the scaling loss of increase oxide inclusion and magnesium is so the melt temperature that the present invention chooses is 740 ℃～800 ℃.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.Also there are bigger influence churning time intensity and time to material, and stirring intensity helps particulate to disperse greatly, but also increases 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, and churning time is 10～30min.
(5) melt is left standstill back cast, casting.The melt dwell temperature is 700 ℃～800 ℃, and time of repose is 5～20min, and cast can be selected metal mold or sand mold for use.
The present invention has substantive distinguishing features and marked improvement, and the present invention adopts the novel process of reaction sintering, remelting dilution and stirring to prepare original position enhanced magnesium base composite material.The present invention chooses suitable grain volume fraction, sintering system, suitable sintering process, melt temperature, churning time is carried out the remelting dilution method and is aided with stirring, it is tiny to have 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 the remelting dilution 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.Matrix material also has good mechanical, physicals.Provide embodiment below in conjunction with content of the present invention, specific as follows:
Embodiment 1 adopts pure magnesium as body material, be divided into the precast body raw material with aluminium powder, titanium valve, boron monoxide, with rotational speed of ball-mill 150r/min, 5: 1 batch mixings of ratio of grinding media to material 30 minutes are got powder then, pressure with 5MPa is suppressed, pressurize 30s is placed on sintering in the vacuum oven with the precast body that suppresses, and is warmed up to 500 ℃ of insulations 10 minutes, be warmed up to 800 ℃ of sintering 10min then, the precast body that the cold taking-up of stove sinters.Precast body is put into precast body 740 ℃ magnesium melt then at 150 ℃ of pre-treatment 60min, stirs behind the insulation 10min, the steel oar stirs with 200r/min, churning time is 10min, leaves standstill the 5min cast behind the stirring 10min, and preparation quality percentage ratio is 5% (TiB
2+ TiC) mixing enhanced ZM5 is the magnesium base composite material of matrix.The tensile strength of material is 213MPa, and unit elongation is 1.5%.
Embodiment 2 adopts pure magnesium as body material, be divided into the precast body raw material with aluminium powder, titanium valve, carbon dust, with rotational speed of ball-mill 300r/min, 20: 1 batch mixings of ratio of grinding media to material 5 hours are got powder then, pressure with 15Mpa is suppressed, pressurize 300s is placed on sintering in the vacuum oven with the precast body that suppresses, and is warmed up to 600 ℃ of insulations 35 minutes, be warmed up to 1100 ℃ of sintering 40min then, the precast body that the cold taking-up of stove sinters.Precast body is at 200 ℃ of pre-treatment 120min, then precast body is put into 760 ℃ magnesium melt, stir behind the insulation 40min, the steel oar stirs with 600r/min, churning time is 20min, leave standstill the 10min cast after stirring 20min, preparation quality percentage ratio is that 5% TiC mixing enhanced ZM5 is the magnesium base composite material of matrix.The tensile strength of material is 315MPa, and unit elongation is 2.4%.
Embodiment 3 adopts pure magnesium as body material, be divided into the precast body raw material with aluminium powder, titanium valve, boron monoxide, with rotational speed of ball-mill 500r/min, 50: 1 batch mixings of ratio of grinding media to material 10 hours are got powder then, pressure with 30Mpa is suppressed, pressurize 600s is placed on sintering in the vacuum oven with the precast body that suppresses, and is warmed up to 650 ℃ of insulations 60 minutes, be warmed up to 1500 ℃ of sintering 60min then, the precast body that the cold taking-up of stove sinters.Precast body is put into precast body 800 ℃ magnesium melt then at 250 ℃ of pre-treatment 180min, stirs behind the insulation 60min, the steel oar stirs with 1000r/min, churning time is 30min, leaves standstill the 20min cast behind the stirring 30min, and preparation quality percentage ratio is 5% (TiB
2+ TiC) mixing enhanced ZM5 is the magnesium base composite material of matrix.The tensile strength of material is 324MPa, and unit elongation is 2.6%.
Claims (8)
1, a kind of technology for preparing particle reinforced magnesium base compound material is characterized in that processing step 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, select TiC, ZrC, 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%, and according to above requirement preparation precast body, the precast body that proportioning is good mixes under protective atmosphere with planetary ball mill, and the mixed powder of ball milling takes out under protective atmosphere;
(2) select for use pressure that the powder compression that mixes is become block, block precast body is carried out sintering under protection of inert gas, the wild phase of mixed powder synthetic magnesium base composite material in sintering process;
(3) melting of magnesium matrix material;
(4) carry out the fusion processes of precast body, precast body was at first dried 1～3 hour in 150 ℃～250 ℃ scope, chose melt temperature again, and precast body is added in the magnesium melt, and insulation 10～60min stirs;
(5) melt is left standstill back cast, casting.
2, the technology of preparation particle reinforced magnesium base compound material according to claim 1, it is characterized in that, in the step (1), precast body is compound or the simple substance powder that contains the wild phase component, the alloying element powder that contains magnesium alloy selects for use wherein three kinds of aluminium powder, zinc powder, titanium valve, carbon dust, zirconium powder, boron carbide powder as the precast body raw material powder.
3, the technology of preparation particle reinforced magnesium base compound material according to claim 1 is characterized in that, in the step (1), the ball milling selected parameter: rotational speed of ball-mill is 150～500r/min, and the ball milling time is 30～600min, and ratio of grinding media to material is 5: 1～50: 1.
4, the technology of preparation particle reinforced magnesium base compound material according to claim 1 is characterized in that, in the step (2), it is 5～30MPa that powder compression becomes bulk to select pressure for use, and the dwell time is 30～600s.
5, the technology of preparation particle reinforced magnesium base compound material according to claim 1 is characterized in that, in the step (2), sintering process is at first being warmed up to 500 ℃～650 ℃, be incubated 10～60min then, be warmed up to 800 ℃～1500 ℃ again, be incubated 10～60min.
6, the technology of preparation particle reinforced magnesium base compound material according to claim 1 is characterized in that, in the step (3), adds ignition-proof element beryllium, calcium etc. and prevent the melt burning in fusion process, adopts gas or flux protection in the fusion process.
7, the technology of preparation particle reinforced magnesium base compound material according to claim 1 is characterized in that, in the step (4), the melt temperature of choosing is 740 ℃～800 ℃, and the mixing speed of choosing is 200～1000r/min, and churning time is 10～30min.
8, the technology of preparation particle reinforced magnesium base compound material according to claim 1 is characterized in that, in the step (5), the melt dwell temperature is 700 ℃～800 ℃, and time of repose is 5～20min, and metal mold or sand mold are selected in cast for use.
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| CNB031161685A CN1195089C (en) | 2003-04-03 | 2003-04-03 | Prepn process of particle-reinforced Mg-base composite mateiral |
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| CNB031161685A CN1195089C (en) | 2003-04-03 | 2003-04-03 | Prepn process of particle-reinforced Mg-base composite mateiral |
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| CN1195089C true CN1195089C (en) | 2005-03-30 |
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Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306051C (en) * | 2003-09-18 | 2007-03-21 | 上海交通大学 | Preparation process for quasi-crystal particles reinforced magnesium base composite material |
| CN1316048C (en) * | 2005-04-07 | 2007-05-16 | 上海交通大学 | Coppered carborundum particle reinforced Mg-based compound material |
| JP4849402B2 (en) * | 2006-09-15 | 2012-01-11 | トヨタ自動車株式会社 | High strength magnesium alloy and method for producing the same |
| CN101899586B (en) * | 2010-07-23 | 2012-05-23 | 西安交通大学 | A kind of preparation technology of composite material prefabricated body |
| CN105063446B (en) * | 2015-08-12 | 2017-09-19 | 中国兵器工业第五九研究所 | A kind of particle reinforced magnesium base compound material preparation method |
| CN105132771A (en) * | 2015-09-14 | 2015-12-09 | 苏州法斯特信息科技有限公司 | Foamed magnesium/ceramic composite material and preparation method thereof |
| CN105200291A (en) * | 2015-11-02 | 2015-12-30 | 苏州金仓合金新材料有限公司 | Novel intermediate alloy for enhancing performance of magnesium alloy for structural components |
| CN106636704B (en) * | 2016-12-15 | 2018-03-27 | 太原理工大学 | A kind of preparation method for the wear-resisting magnesium alloy for adulterating titanium diboride |
| CN108342605A (en) * | 2018-01-15 | 2018-07-31 | 江苏理工学院 | A kind of TiC particles enhance the preparation method of 7085 aluminum matrix composites |
| CN108441732B (en) * | 2018-03-27 | 2020-01-14 | 青海大学 | Nano-diamond particle reinforced magnesium-based composite material and preparation method thereof |
| US11692242B2 (en) | 2019-11-04 | 2023-07-04 | King Fahd University Of Petroleum And Minerals | Method of producing biodegradable magnesium composite by spark plasma sintering |
| CN110918998B (en) * | 2019-11-24 | 2022-02-11 | 桂林理工大学 | High-damping 5083Al/Ti composite material and preparation method thereof |
| CN111349834B (en) * | 2020-03-09 | 2021-11-12 | 上海交通大学 | Micro-nano dual-phase hybrid particle reinforced magnesium-lithium-based composite material and preparation method thereof |
| CN111304506B (en) * | 2020-03-11 | 2021-08-03 | 上海交通大学 | A kind of preparation method of micro-nano-scale TiB2 particle reinforced magnesium-lithium-based composite material |
| CN117363918B (en) * | 2023-10-13 | 2024-03-19 | 榆林学院 | Preparation method of annular magnesium-aluminum-based composite material |
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