CN1327021C - Process for preparing magnesium alloy and its composite material - Google Patents
Process for preparing magnesium alloy and its composite material Download PDFInfo
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- CN1327021C CN1327021C CNB2004100530697A CN200410053069A CN1327021C CN 1327021 C CN1327021 C CN 1327021C CN B2004100530697 A CNB2004100530697 A CN B2004100530697A CN 200410053069 A CN200410053069 A CN 200410053069A CN 1327021 C CN1327021 C CN 1327021C
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- magnesium alloy
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Abstract
The present invention relates to a preparation process of a new magnesium alloy and a preparation process of a magnesium alloy composite material, which makes a breakthrough to the existing magnesium alloy and composite material thereof powder metallurgical technique. The preparation process comprises the steps of smelting magnesium alloy ingots, grinding balls and preparing powder, hot pressing and sintering, hot rolling and processing, etc. Compacting powder and sintering powder are combined in the present invention so that the strength of the magnesium alloy and the composite material thereof is increased, and the toughness is improved; the present invention has the advantages of lowered sintering temperature, shortened sintering time and decreased energy consumption; an extra gas shield is not needed during the preparation process, but the material is not oxidized; the equipment used for preparing the present invention is simple, reliable, economical and practical.
Description
Technical field
The invention belongs to the metal-base composites processing technique field, the preparation technology of particularly a kind of magnesium alloy and matrix material thereof.
Background technology
Powder metallurgical technique is the solid-state preparation method of traditional preparation magnesium alloy and matrix material thereof.Its technology is with powder compression and be sintered to the master.Powder compression and sintering are two separate processes, and need a large amount of gas as protective atmosphere in preparation process, are used for preventing that magnesium or magnesium alloy are oxidized.The hot pressing of Chu Xianing afterwards or claim hot consolidation to comprise that single shaft is to pressurize simultaneously and heat to hot pressing and pressure sintering, hot isostatic pressing, hot extrusion and forge hot, first press molding post-heating sintering unlike conventional powder metallurgical technique, pressure is along an axis or from each face, unidirectional or two-way, statics or dynamic (dynamical) powder heatedly that acts on.
Hot pressing is to rely on the interatomic mutual diffusion in contact site to carry out under the high temperature of long period and little viscous deformation effect, the diffusion bonding process can be divided into three phases: the initial contact between (1) bonding surface, and the surface deforms, moves because heating and pressurization make, surface film destruction; (2) along with the time interfacial diffusion and bulk diffusion takes place, make contact surface adherence bonding; (3) because the thermodiffusion bonding interface finally disappears, the bonding process is finished.The significant parameter that influences the diffusion bonding process is the time of keeping under temperature, pressure and certain temperature and the pressure, and wherein temperature is the most important, and traditional hot pressing temperature is controlled between the solidus curve and liquidus line of matrix alloy.Pressure can change in a big way, but too high easy damage fiber, its selection is relevant with temperature, and the temperature high pressure can suitably reduce, and needs to prevent with controlled atmosphere magnesium and the magnesium alloy powder or the preform oxidation by air of heat simultaneously.Hot-press equipment is very complicated in addition, and investment is big, and benefit is low.
Summary of the invention
The object of the present invention is to provide does not a kind ofly need special gas or vacuum protection and prepares not oxidized, the magnesium alloy of excellent property and the preparation technology of matrix material thereof at lesser temps with in the short period, to enlarge the range of application and the value-added content of product of magnesium alloy and matrix material thereof.
Technical scheme of the present invention is: on traditional powder metallurgical technique basis, the magnesium of anticipating or magnesium alloy powder and strongthener are put into mould, mixture is pressurizeed, simultaneously by mould itself with resistive heating device it is heated, powder compression is combined with powder sintered.Concrete steps comprise melting magnesium alloy ingot, ball milling powder process, hot pressed sintering, heat bundle etc.
The first step: melting magnesium alloy ingot
By weight proportion melting magnesium alloy under the Ar gas shiled of following component, smelting temperature is 700～800 ℃:
Mg：70～80
Al：10～16
Cu：3～5
Zn：2～5
Mn：1～2
RE：1～3
Si：0.5～1；
Second step: ball milling powder process
The magnesium alloy ingot that turning is melted obtains the powder of 0.6～0.3mm, again powder is carried out ball milling.Ball milling adopts dehydrated alcohol to carry out the liquid protection, and abrading-ball adopts steel ball during ball milling, and the ball milling time is 5～8 hours, and ratio of grinding media to material is 15: 1～20: 1, and rotating speed is 300～400r/min;
The 3rd step: hot pressed sintering
Employing obturation effect mould preferably carries out hot pressed sintering, and the mould sketch is seen accompanying drawing 1.Dress during mould on the die wall of contact pressed compact the coated with nano aluminum oxide powder be welded on the die wall to prevent pressed compact.300～450 ℃ of hot pressing temperatures, 15～20 ℃/min of temperature rise rate, soaking time 1～2 hour, pressure progressively applies, and reaches as high as 375Mpa.Whole process is not taked vacuum or other sfgd..Sintered compact after the demoulding is required magnesium alloy and matrix material thereof.
At last, generally also will carry out hot rolling to the material of hot pressed sintering handles.
Can further improve the density of sintered compact by hot rolling, improve the intensity of material, improve the unit elongation of material.Hot rolling is carried out at 200～300 ℃, and draft is between 30～50%, and speed of feed is between 0.1～0.3m/min.
Characteristics of the present invention are that magnesium or the magnesium alloy powder after adopting novel hot-press arrangement to ball milling carries out hot pressed sintering.Ball milling has reduced the granularity of magnesium or magnesium alloy powder, and makes its activation, can reduce sintering temperature and sintering time.During hot pressing, mould is given pressed compact with required shape, the pressure height that produces in the pressure ratio sintering oven, and therefore designing mould suitably, the device of heating will adapt to the characteristics of press and mould.Mould of the present invention is unidirectional pressing die, and pressurization and heating can be carried out simultaneously, and the temperature field is even.At metal former inner wall surface coated with nano aluminum oxide, can reduce the wearing and tearing of die wall, stop diffusion-bonded and welding between pressed compact and the die wall, keep former and the structural integrity of drift between the high-temperature zone of pressing cycle.The stopping property of mould itself is better, therefore can not use the protection of special gas or vacuum in hot pressing.Hot pressing pressure of the present invention is higher, and hot pressing temperature is starkly lower than the solidus curve of matrix alloy, and sintering time obviously reduces.
Description of drawings
Fig. 1 is hot pressed sintering apparatus structure diagram.
Fig. 2 is an A-A place sectional view among Fig. 1.
Number in the figure: 1 is upper punch, and 2 is lower punch, and 3 is former, and 4 is electroheat pair, and 5 is the resistance heating wire, and 6 is closed cell.
Embodiment
Embodiment 1: the preparation of powder Mg70-Al16-Cu3-Zn5-RE3-Mn2-Si1 alloy.
Magnesium alloy powder ball milling 5 hours under ethanol protection, ratio of grinding media to material is 20: 1, rotating speed is 300r/min.Theoretical density 2.0g/cm according to original magnesium alloy
3, the magnesium alloy powder 6.4g behind the selection ball milling, the volume after the compacting promptly is decided to be 3.2cm
3Magnesium alloy powder is put into hot pressing die.Earlier temperature is raised to 200 ℃ during hot pressing, is incubated half an hour, be warming up to 300 ℃ then, be incubated 1 hour, constantly regulate pressure in sintering process, the density that makes magnesium alloy is near its theoretical density.Whole sintering process is 2.5 hours.Heat is pricked and is carried out at 200 ℃, and temperature rise rate is 20 ℃/min, and draft is 50%, and speed of feed is 0.3m/min, material yield intensity σ
0.2Be 220Mpa, tensile strength sigma
bBe 258Mpa, room temperature unit elongation δ is 2%.
Embodiment 2: metal NiTi macrofiber strengthens the preparation of magnesium alloy.
Adopt the Mg80-Al10-Cu5-Zn2-RE1-Mn1.5-Si0.5 alloy as body material, ball milling is 8 hours under the ethanol protection, and ratio of grinding media to material is 15: 1, and rotating speed is 400r/min.Magnesium alloy powder and NiTi fiber are put into hot pressing die by sandwich structure.Earlier temperature is raised to 200 ℃ during hot pressing, is incubated half an hour, be warming up to 320 ℃ then, be incubated 2 hours, in sintering process, exert pressure gradually, be up to 375Mpa.Whole sintering process is 3.5 hours.The microstructure of composite that makes is even, and fiber is in conjunction with better.Heat is pricked and is carried out at 300 ℃, and temperature rise rate is 15 ℃/min, and draft is 30%, and speed of feed is 0.1m/min.Matrix material yield strength σ
0.2Reach 260Mpa, tensile strength sigma
bBe 300Mpa, room temperature unit elongation δ is 3%.
Embodiment 3: metallic aluminium titanium staple fibre strengthens the preparation of magnesium alloy.
Adopt the Mg70-Al16-Cu5-Zn5-RE2-Mn1-Si1 alloy as body material, ball milling is 8 hours under the ethanol protection, and ratio of grinding media to material is 15: 1, and rotating speed is 400r/min.Magnesium alloy powder and aluminium titanium fiber are mixed by ball milling, and the ball milling time is 15 minutes once more, rotating speed 300r/min, vacuum protection.Mixture is put into hot pressing die hot pressing, earlier temperature is raised to 200 ℃, be incubated half an hour, be warming up to 450 ℃ then, be incubated 1 hour, in sintering process, exert pressure gradually.Whole sintering process is 3 hours.The microstructure of composite that makes is even, and fiber is in conjunction with better.Heat is pricked and is carried out at 250 ℃, and temperature rise rate is 15 ℃/min, and draft is 40%, and speed of feed is 0.1m/min.Matrix material yield strength σ
0.2Reach 286Mpa, tensile strength sigma
bBe 325Mpa, room temperature unit elongation δ is 2%.
In the foregoing description, hot pressed sintering all carries out in hot-press arrangement, and the structure of this device as depicted in figs. 1 and 2.It is constituted by upper punch 1, lower punch 2, former 3, and former 3 is provided with electroheat pair 4, is provided with resistance heating wire 5 in the lower punch 2, and there is closed cell 6 in the outside between lower punch 2 and the former 3.
Device outside dimension: 94.8 * 94.8 * 84mm, 700 ℃ of the Heating temperature upper limits, maximum allowble pressure 1 * 10
6N.On the former wall, smear earlier aluminum oxide powder and the agent of alcoholic acid mix during use, treat that ethanol volatilization rear oxidation aluminium powder overlays on the die wall uniformly, lower punch from insert former, is put into magnesium or magnesium alloy powder and strongthener then, again upper punch is inserted from the former the other end.A whole set of mould is placed on the press, inserts thermopair and resistance heating wire, just can begin hot pressing.
Claims (2)
1, a kind of preparation technology of magnesium alloy materials is characterized in that concrete steps are as follows:
The first step: melting magnesium alloy ingot
By weight proportion melting magnesium alloy under the Ar gas shiled of following component, smelting temperature is 700～800 ℃:
Mg：70～80
Al：10～16
Cu：3～5
Zn：2～5
Mn：1～2
RE：1～3
Si：0.5～1；
Second step: ball milling powder process
The magnesium alloy ingot that turning is melted obtains the powder of 0.6～0.3mm, again powder is carried out ball milling; Ball milling adopts dehydrated alcohol to carry out the liquid protection, and the ball milling time is 5～8 hours, and ratio of grinding media to material is 15: 1～20: 1, and rotating speed is 300～400r/min;
The 3rd step: hot pressed sintering
Adopt closed mold to carry out hot pressed sintering, dress during mould on the die wall of contact pressed compact the coated with nano aluminum oxide powder be welded on the die wall to prevent pressed compact, 300～450 ℃ of hot pressing temperatures, 15～20 ℃/min of temperature rise rate, soaking time 1～2 hour, pressure progressively applies, and is up to 375Mpa, and the sintered compact after the demoulding is required magnesium alloy materials.
2, preparation technology according to claim 1 is characterized in that the material of hot pressed sintering is further carried out the hot rolling processing, and hot-rolled temperature is 200-300 ℃, and draft is 30-50%, and speed of feed is 0.1-0.3m/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100530697A CN1327021C (en) | 2004-07-22 | 2004-07-22 | Process for preparing magnesium alloy and its composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004100530697A CN1327021C (en) | 2004-07-22 | 2004-07-22 | Process for preparing magnesium alloy and its composite material |
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| CN1587429A CN1587429A (en) | 2005-03-02 |
| CN1327021C true CN1327021C (en) | 2007-07-18 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005033835A1 (en) * | 2005-07-20 | 2007-01-25 | Gkss-Forschungszentrum Geesthacht Gmbh | Magnesium secondary alloy |
| CN100432267C (en) * | 2006-09-22 | 2008-11-12 | 中国科学院长春应用化学研究所 | High-strength magnesium based composite material and preparation method thereof |
| CN101376276B (en) * | 2007-08-31 | 2012-09-19 | 清华大学 | Magnesium-base compound material and preparation method thereof |
| CN101967586B (en) * | 2010-11-12 | 2012-04-25 | 哈尔滨工业大学 | Method for preparing self-lubricating radiation-proof Al-Bi alloy |
| CN103451463B (en) * | 2013-08-27 | 2015-11-25 | 朱育盼 | A kind of Mg 2si strengthens the preparation method of Mg alloy composite materials |
| CN103464764B (en) * | 2013-08-28 | 2015-05-27 | 盐城工学院 | Metal matrix wear-resistant corrosion-resistant surface coating composite and preparation method thereof |
| CN110076333A (en) * | 2019-04-08 | 2019-08-02 | 江苏豪然新材料有限公司 | Al-Si-Cu-Mg alloy powder hot-pressing sintering method is shaped using injection |
| CN112718860B (en) * | 2020-09-25 | 2022-03-22 | 中南大学 | Production method of magnesium alloy sheet |
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|---|---|---|---|---|
| US5074936A (en) * | 1989-04-05 | 1991-12-24 | The Dow Chemical Company | Amorphous magnesium/aluminum-based alloys |
| CN1085259A (en) * | 1993-07-07 | 1994-04-13 | 广西冶金研究所 | Rare-earth-Al-Mg alloy powder and preparation method thereof |
| CN1375567A (en) * | 2001-09-13 | 2002-10-23 | 吉林大学 | Prepn. of particle reinforced magnesium-base composite material |
| CN1441074A (en) * | 2003-04-03 | 2003-09-10 | 上海交通大学 | Prepn process of Mg-based composite material |
| CN1515697A (en) * | 2003-01-07 | 2004-07-28 | 死海镁有限公司 | Creep eresistant magnesium alloy with improved casting property |
| US6846451B2 (en) * | 2001-08-23 | 2005-01-25 | The Japan Steel Works, Ltd. | Magnesium alloy and magnesium alloy member superior in corrosion resistance |
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2004
- 2004-07-22 CN CNB2004100530697A patent/CN1327021C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5074936A (en) * | 1989-04-05 | 1991-12-24 | The Dow Chemical Company | Amorphous magnesium/aluminum-based alloys |
| CN1085259A (en) * | 1993-07-07 | 1994-04-13 | 广西冶金研究所 | Rare-earth-Al-Mg alloy powder and preparation method thereof |
| US6846451B2 (en) * | 2001-08-23 | 2005-01-25 | The Japan Steel Works, Ltd. | Magnesium alloy and magnesium alloy member superior in corrosion resistance |
| CN1375567A (en) * | 2001-09-13 | 2002-10-23 | 吉林大学 | Prepn. of particle reinforced magnesium-base composite material |
| CN1515697A (en) * | 2003-01-07 | 2004-07-28 | 死海镁有限公司 | Creep eresistant magnesium alloy with improved casting property |
| 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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| COMPRESSIVE MECHANICAL PROPERTIES OF Mg-Ti-CNANOCOMPOSTITE SYNTHESISED BY MECHANICALMILLING S.Hwang et al,Scripta Materialia,Vol.Vol.44 No.No.10 2001 * |
| COMPRESSIVE MECHANICAL PROPERTIES OF Mg-Ti-CNANOCOMPOSTITE SYNTHESISED BY MECHANICALMILLING S.Hwang et al,Scripta Materialia,Vol.Vol.44 No.No.10 2001;粉末冶金制备MB15镁基复合材料组织及性能的研究 郗雨林 等，热加工工艺，第1期 2002 * |
| 粉末冶金制备MB15镁基复合材料组织及性能的研究 郗雨林 等，热加工工艺，第1期 2002 * |
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