CN105695781A - Preparation method of high-performance in-situ nanoparticle reinforced magnesium matrix composite - Google Patents
Preparation method of high-performance in-situ nanoparticle reinforced magnesium matrix composite Download PDFInfo
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- CN105695781A CN105695781A CN201610064997.6A CN201610064997A CN105695781A CN 105695781 A CN105695781 A CN 105695781A CN 201610064997 A CN201610064997 A CN 201610064997A CN 105695781 A CN105695781 A CN 105695781A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention provides a preparation method of a high-performance in-situ nanoparticle reinforced magnesium matrix composite. The method comprises the following steps: simply and mechanically mixing pure magnesium powder or magnesium alloy powder with nanoscale heterogeneous powder; then carrying out ball milling reaction to implement in-situ generation of a nanoscale intermetallic compound particle phase in mixed powder; and finally hot pressing and sintering to prepare the high-performance magnesium matrix composite. The particles of the reinforced phase in the magnesium matrix composite prepared by the method are fine, are uniformly distributed, and are tightly bonded with the matrix interface; the composite has good mechanical property and lays a good foundation for wide application of the magnesium matrix composite.
Description
Technical field
The invention belongs to metallurgical technology field, the preparation method relating to a kind of magnesium base composite material, particularly to the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material。
Background technology
Magnesium base composite material is low due to its density, specific strength is high, excellent performance, it is subject to people more and more to pay close attention to, except having the mechanical property of excellence, magnesium base composite material also has very good electromagnetic wave shielding and radiation resistance, is also used as hydrogen storage material simultaneously and uses, and this makes it have very vast potential for future development and application potential at various high-technology fields。In general, no matter magnesium base composite material is as a kind of structural material or functional material, all has very huge value。
Particle reinforced magnesium base compound material has outstanding advantage in all kinds of magnesium base composite materials, has become as one of main contents of magnesium base composite material research。Chinese patent, the preparation method of Carbon Nanotubes/Magnesiuum Matrix Composite, CN103014399B, authorized announcement date on July 30th, 2014, disclose a kind of with Zn powder and CNT for raw material, first carry out mixing and ball milling, then be pressed into prefabricated section after composite powder and magnesium powder mix homogeneously, again prefabricated section is joined in Serum Magnesium, prepare magnesium base composite material with this。Owing to mixed-powder and magnesium do not react, improving performance in matrix magnesium in the way of mechanical enhancer, while tensile strength improves, other performance potentials must incur loss。And in patent disclosed in 11 days March in 2015 " preparation method that a kind of in-situ nano grade particles strengthens magnesium base composite material " (CN104404327A), have employed the Sn powder of nano-scale magnesium base composite material material is strengthened, it is sufficiently stirred for after melted, is cast into containing a nanometer Mg2The particle reinforced magnesium base compound material of Sn phase, although obtained magnesium base composite material material has good mechanical performance, but needs extraordinary atmosphere protection could reduce the scaling loss of Sn nanometer powder in preparation process。The patent " a kind of high-strength magnesium based composite material and preparation method thereof " (CN100432267C) that on November 12nd, 2008 authorizes, then disclose a kind of with Al12Mg17Nanometer powder and the zinc powder less than 1 micron, magnesium powder are raw material, by the method that semi-solid rheological press-forging technique prepares high-strength magnesium based composite material。The method is prepared raw material and is the powder body less than 1 micron, adds raw-material cost；Further, since Al12Mg17Still fall within outside addition, the interface cohesion degree between itself and magnesium matrix can be affected。
To sum up, there is some problem in the performance of the magnesium base composite material that some technique is obtained, and some technique is then complex, it is difficult to controls。Therefore, how by simple and effective technique, prepare everyway and there is the particle reinforced magnesium base compound material of premium properties become an important research direction。
Summary of the invention
For the deficiencies in the prior art, the preparation method that the present invention provides a kind of high-performance in-situ nano particle reinforced magnesium base compound material, it is therefore an objective to solving magnesium alloy substrate intensity not high, Nano-size Reinforced Particle not easily efficiently introduces magnesium matrix and the problem of high cost。
The technical solution adopted in the present invention comprises the following steps:
Step one, according to required enhancing phase kind, by the volume of magnesium matrix powder remaining after micron order magnesium matrix powder and nanoscale xenogenesis powder ball-milling reaction more than 50% dispensing of cumulative volume after ball-milling reaction, by nanoscale xenogenesis powder and the simple and mechanical mixing of micron order magnesium matrix powder。Wherein, magnesium matrix powder includes pure magnesium dust or the magnesium alloy powder of 1～350 μm；The xenogenesis powder added mutually for original position formation enhancing granule includes one or more in the glass putty of 10～100nm, copper powder, germanium powder, antimony powder, bismuth meal, silica flour, calcium powder。
Step 2, loads abrading-ball and the mixed powder of Single Mechanical in ball grinder jointly by the ratio of grinding media to material of 5:1～50:1。Ball sealer grinding jar, it is ensured that ball grinder internal medium reaches air-tight state, uses air pump to be re-filled with noble gas as protective atmosphere after ball grinder is evacuated to vacuum state or vacuum subsequently。High-energy ball milling, ball milling revolution 100～1000rpm, Ball-milling Time 2～300h is carried out, it is possible to before ball milling, add stearic acid when vacuum or inert gas shielding。After ball milling terminates, placement a period of time opens ball grinder in vacuum glove box, takes out obtained mixed powder airtight preservation after being completely cooled down to room temperature state to ball grinder, prepares the Powdered magnesium base composite material strengthening phase containing in-situ nano。Containing Nano-size Reinforced Particle in Powdered magnesium base composite material；Described noble gas includes argon or nitrogen。
Step 3, loads the Powdered magnesium base composite material obtained in step 2 in hot pressing die, then puts it in hot-pressed sintering furnace。Hot-pressed sintering furnace is evacuated to less than applying argon gas after 50Pa or nitrogen；Composition according to composite, heats up with the heating rate of 1～15 DEG C/min, and temperature is 5～50MPa at dwell pressure after rising to sintering temperature 350～620 DEG C, carries out hot pressed sintering when the dwell time is 10～60min。After terminating, after cooling completely, take out mould, the block suppressed is taken out, it is thus achieved that high-performance in-situ nano particle reinforced magnesium base compound material。
Nanometer in situ synthetic technology, Mechanic Alloying Technology and hot pressing and sintering technique are organically combined by the present invention, for the preparation of particle reinforced magnesium base compound material。The enhancing particle size that the method obtains is little, is evenly distributed, and is well combined with matrix, and the performance for magnesium base composite material is obviously enhanced, and preparation technology is simple simultaneously, and production cost is low, is suitable to large-scale production。
The present invention has feature highlighted below compared with current existing technology:
1) technique is relatively easy, it is easy to popularization and application, carries out scale commodity production。It is a feature of the present invention that successfully preparing nano-scale particle strengthens magnesium base composite material, strengthens granule in-situ endogenic in the base, nano-scale particle reinforced effects is notable, substantially increases the mechanical performance of magnesium alloy, sees following table:
The compression performance of various materials
2) magnesium base composite material that the present invention prepares can remelting or carry out secondary deformation processing, therefore pouring into a mould the strand (part) obtained can as the original blank of the semi-solid blank of diecast magnesium alloy or high-performance wrought magnesium alloy。
Detailed description of the invention
Below by way of four concrete examples, technical scheme and effect are further elaborated。
Embodiment 1: a kind of containing Mg2The magnesium base composite material of Sn hardening constituent, comprises the following steps:
Step one, magnesium matrix powder selects pure magnesium dust, and it is of a size of 10 μm；Forming, for original position, the xenogenesis powder selection glass putty that intermetallic compound particle adds, it is of a size of 40～60nm。Wherein, the mass fraction of nanometer glass putty is 25wt%。The powder chosen is carried out simple and mechanical mixing；
Step 2, after simple and mechanical mixing, loads abrading-ball and mixed-powder in ball grinder jointly by the ratio of grinding media to material of 10:1。Ball sealer grinding jar, it is ensured that ball grinder internal medium reaches air-tight state, uses air pump that ball grinder is evacuated to vacuum state subsequently。Carry out high-energy ball milling, ball milling revolution 250rpm, Ball-milling Time 20h under vacuum, after ball milling terminates, then place after a period of time is completely cooled down to room temperature state to ball grinder, in vacuum glove box, open ball grinder, take out obtained mixed powder airtight preservation。Now, prepare containing original position Mg2The Powdered magnesium base composite material of Sn nanometer reinforcing phase；
Step 3, will containing a nanometer Mg2The magnesium base composite material mixed-powder of Sn reinforcement granule loads in hot pressing die, puts it into subsequently in hot-pressed sintering furnace。Hot-pressed sintering furnace is evacuated to less than inflated with nitrogen after 50Pa；Heating up with the heating rate of 8.5 DEG C/min, temperature is 40MPa at dwell pressure after rising to sintering temperature 550 DEG C, carries out hot pressed sintering when the dwell time is 20min again。After terminating, after cooling completely, take out mould, the block suppressed is taken out, it is thus achieved that high-performance original position Mg2Sn nano-particle reinforcement block magnesium base composite material。
Embodiment 2: a kind of containing Mg2The magnesium base composite material of Cu hardening constituent, comprises the following steps:
Step one, magnesium matrix powder selects AZ61 magnesium alloy powder, and it is of a size of 40 μm；Forming, for original position, the xenogenesis powder selection copper powder that intermetallic compound particle adds mutually, it is of a size of 50～70nm。Wherein, the mass fraction of copper nanoparticle is 20wt%。The powder chosen is carried out simple and mechanical mixing；
Step 2, after simple and mechanical mixing, loads abrading-ball and mixed-powder in ball grinder jointly by the ratio of grinding media to material of 20:1。Ball sealer grinding jar, it is ensured that ball grinder internal medium reaches air-tight state, after using air pump that ball grinder is evacuated to vacuum state subsequently, is filled with high-purity argon gas as protective atmosphere。Carry out high-energy ball milling when argon shield, ball milling revolution is 250rpm, Ball-milling Time 30h; after ball milling terminates, then place after a period of time is completely cooled down to room temperature state to ball grinder, in vacuum glove box, open ball grinder; take out obtained mixed powder airtight preservation。Now, prepare containing original position Mg2The Powdered magnesium base composite material of Cu nanometer reinforcing phase；
Step 3, will containing Mg2The magnesium base composite material mixed-powder of Cu nanometer of reinforcement granule loads in hot pressing die, puts it into subsequently in hot-pressed sintering furnace。Hot-pressed sintering furnace is evacuated to less than applying argon gas after 50Pa；Heating up with the heating rate of 10 DEG C/min, temperature is 30MPa at dwell pressure after rising to sintering temperature 600 DEG C, carries out hot pressed sintering when the dwell time is 25min again。After terminating, after cooling completely, take out mould, the block suppressed is taken out, it is thus achieved that high-performance original position Mg2Cu nano-particle reinforcement block magnesium base composite material。
Embodiment 3: a kind of containing Mg2The magnesium base composite material of Si hardening constituent, comprises the following steps:
Step one, magnesium matrix powder selects ZK60 magnesium alloy powder, and it is of a size of 200 μm；Being formed for original position and strengthen the xenogenesis powder selection silica flour that granule adds mutually, it is of a size of 60～80nm。Wherein, the mass fraction of nano silica fume is 15wt%。The powder chosen is carried out simple and mechanical mixing；
Step 2, after simple and mechanical mixing, loads abrading-ball and mixed-powder in ball grinder jointly by the ratio of grinding media to material of 50:1。Ball sealer grinding jar, guarantee that ball grinder internal medium reaches air-tight state, using air pump that ball grinder is evacuated to vacuum state subsequently, carry out high-energy ball milling under vacuum, ball milling revolution is 500rpm, Ball-milling Time 50h, after ball milling terminates, then place after a period of time is completely cooled down to room temperature state to ball grinder, in vacuum glove box, open ball grinder, take out obtained mixed powder airtight preservation。Now, prepare containing original position Mg2The Powdered magnesium base composite material of Si nanometer reinforcing phase；
Step 3, will containing Mg2The magnesium base composite material mixed-powder of Si nanometer of reinforcement granule loads in hot pressing die, puts it into subsequently in hot-pressed sintering furnace。Hot-pressed sintering furnace is evacuated to less than inflated with nitrogen after 50Pa；Heat up with the heating rate of 5 DEG C/min again, after temperature rises to sintering temperature 500 DEG C, be 40MPa at dwell pressure, when dwell time 40min, carry out hot pressed sintering。After terminating, after cooling completely, take out mould, the block suppressed is taken out, it is thus achieved that high-performance original position Mg2Si nano-particle reinforcement block magnesium base composite material。
Embodiment 4: a kind of containing Mg2Sn+Mg2The magnesium base composite material of Cu hardening constituent, comprises the following steps:
Step one, magnesium matrix powder selects AZ61 magnesium alloy powder, and it is of a size of 120 μm；Xenogenesis powder selection glass putty and copper powder, its size respectively 40～60nm and 60～80nm that intermetallic compound particle adds mutually is formed for original position。Wherein, the mass fraction of nanometer glass putty and copper powder respectively 10wt% and 20wt%。The powder chosen is carried out simple and mechanical mixing；
Step 2, after simple and mechanical mixing, loads abrading-ball and mixed-powder in ball grinder jointly by the ratio of grinding media to material of 35:1。Ball sealer grinding jar, guarantee that ball grinder internal medium reaches air-tight state, use air pump that ball grinder is evacuated to vacuum state subsequently, carry out high-energy ball milling under vacuum, ball milling revolution is 500rpm, and Ball-milling Time 50h, after ball milling terminates, place after a period of time is completely cooled down to room temperature state to ball grinder again, in vacuum glove box, open ball grinder, take out obtained mixed powder airtight preservation。Now, prepare containing original position Mg2Sn and Mg2The Powdered magnesium base composite material of Cu nanometer reinforcing phase；
Step 3, will containing Mg2Sn and Mg2The magnesium base composite material mixed-powder of Cu nanometer of reinforcement granule loads in hot pressing die, puts it into subsequently in hot-pressed sintering furnace。Hot-pressed sintering furnace is evacuated to less than applying argon gas after 50Pa；Heat up with the heating rate of 5 DEG C/min again, after temperature rises to sintering temperature 500 DEG C, be 40MPa at dwell pressure, when dwell time 40min, carry out hot pressed sintering。After terminating, after cooling completely, take out mould, the block suppressed is taken out, it is thus achieved that the multiple nano-particle reinforcement block magnesium base composite material of high-performance。
Claims (10)
1. the preparation method of a high-performance in-situ nano particle reinforced magnesium base compound material, it is characterised in that comprise the following steps:
Step one, according to required enhancing phase kind, by the volume of magnesium matrix powder remaining after magnesium matrix powder and xenogenesis powder ball-milling reaction more than 50% dispensing of cumulative volume after ball-milling reaction, by xenogenesis powder and the simple and mechanical mixing of magnesium matrix powder；Described magnesium matrix powder size is 1～350 μm, and described xenogenesis powder size is 10～100nm；
Step 2, puts in ball grinder by abrading-ball and simple and mechanical mixed powder, to powder high-energy ball milling 2～300h under vacuum or inert gas shielding, after temperature is cooled to room temperature in ball grinder, obtains strengthening the Powdered magnesium base composite material of phase containing in-situ nano；
Step 3, Powdered magnesium base composite material is loaded in hot pressing die, put into hot-pressed sintering furnace, applying argon gas after evacuation in hot-pressed sintering furnace, after being warming up to sintering temperature 350～620 DEG C, under dwell pressure, Powdered magnesium base composite material is carried out hot pressed sintering 10～60min, after cooling completely, take out mould, obtain high-performance in-situ nano particle reinforced magnesium base compound material。
2. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 1, it is characterised in that described magnesium matrix powder includes pure magnesium dust or magnesium alloy powder；Described xenogenesis powder includes the one in glass putty, copper powder, germanium powder, antimony powder, bismuth meal, silica flour, calcium powder and combination thereof。
3. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 1 and 2, it is characterised in that in described step 2, the ratio of grinding media to material of powder after abrading-ball and mechanical mixture is 5:1～50:1；In described step 2, rotational speed of ball-mill is 100～1000rpm。
4. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 1 and 2, it is characterised in that in described step 2, inert atmosphere includes argon or nitrogen；Described step 2 is added stearic acid before ball milling。
5. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 3, it is characterised in that in described step 2, inert atmosphere includes argon or nitrogen；Described step 2 is added stearic acid before ball milling。
6. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 1 or 2 or 5, it is characterised in that in described step 3, heating rate is 1～15 DEG C/min；In described step 3, dwell pressure is 5～50MPa。
7. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 3, it is characterised in that in described step 3, heating rate is 1～15 DEG C/min；In described step 3, dwell pressure is 5～50MPa。
8. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 4, it is characterised in that in described step 3, heating rate is 1～15 DEG C/min；In described step 3, dwell pressure is 5～50MPa。
9. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 1 or 2 or 5 or 7 or 8, it is characterised in that in described step 3, hot-pressed sintering furnace is evacuated to less than 50Pa。
10. the preparation method of a kind of high-performance in-situ nano particle reinforced magnesium base compound material according to claim 3, it is characterised in that in described step 3, hot-pressed sintering furnace is evacuated to less than 50Pa。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502800A (en) * | 2017-09-08 | 2017-12-22 | 燕山大学 | A kind of preparation method of the magnesium-based composite material of nano-MgO particle enhancing |
| CN107671118A (en) * | 2017-11-03 | 2018-02-09 | 沈阳大学 | The method for repairing DDT and heavy metal chromium combined contamination soil simultaneously |
| CN108149096A (en) * | 2018-01-24 | 2018-06-12 | 山东建筑大学 | A kind of preparation method of nano-SiC particle enhancing magnesium-based composite material |
| CN108467958A (en) * | 2018-03-26 | 2018-08-31 | 湖北工业大学 | The preparation method of antimony magnesium whisker-magnesium silicide Particles dispersed enhancing magnesium-based composite material |
| CN109175349A (en) * | 2018-10-15 | 2019-01-11 | 微山钢研稀土材料有限公司 | Double rare earth solid solution base hydrogen storage materials of a kind of high-performance and preparation method thereof |
| CN113174519A (en) * | 2021-03-23 | 2021-07-27 | 山东科技大学 | Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof |
| CN113909480A (en) * | 2020-07-08 | 2022-01-11 | 核工业西南物理研究院 | Preparation method of in-situ nano zirconium oxide particle dispersion reinforced tungsten alloy |
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| JPH10102163A (en) * | 1996-09-24 | 1998-04-21 | Hiroshima Pref Gov | Intermetallic compound reinforced magnesium base composite material and its production |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502800A (en) * | 2017-09-08 | 2017-12-22 | 燕山大学 | A kind of preparation method of the magnesium-based composite material of nano-MgO particle enhancing |
| CN107502800B (en) * | 2017-09-08 | 2019-07-26 | 燕山大学 | A kind of preparation method of the magnesium-based composite material of nano-MgO particle enhancing |
| CN107671118A (en) * | 2017-11-03 | 2018-02-09 | 沈阳大学 | The method for repairing DDT and heavy metal chromium combined contamination soil simultaneously |
| CN108149096A (en) * | 2018-01-24 | 2018-06-12 | 山东建筑大学 | A kind of preparation method of nano-SiC particle enhancing magnesium-based composite material |
| CN108467958A (en) * | 2018-03-26 | 2018-08-31 | 湖北工业大学 | The preparation method of antimony magnesium whisker-magnesium silicide Particles dispersed enhancing magnesium-based composite material |
| CN108467958B (en) * | 2018-03-26 | 2019-07-23 | 湖北工业大学 | Antimony magnesium whisker-magnesium silicide Particles dispersed enhancing magnesium-based composite material preparation method |
| CN109175349A (en) * | 2018-10-15 | 2019-01-11 | 微山钢研稀土材料有限公司 | Double rare earth solid solution base hydrogen storage materials of a kind of high-performance and preparation method thereof |
| CN113909480A (en) * | 2020-07-08 | 2022-01-11 | 核工业西南物理研究院 | Preparation method of in-situ nano zirconium oxide particle dispersion reinforced tungsten alloy |
| CN113174519A (en) * | 2021-03-23 | 2021-07-27 | 山东科技大学 | Superfine vanadium particle reinforced fine-grain magnesium-based composite material and preparation method thereof |
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