CN105734329A - Method for preparing high-strength and high-toughness magnesium-based nano composite - Google Patents
Method for preparing high-strength and high-toughness magnesium-based nano composite Download PDFInfo
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- CN105734329A CN105734329A CN201610255865.1A CN201610255865A CN105734329A CN 105734329 A CN105734329 A CN 105734329A CN 201610255865 A CN201610255865 A CN 201610255865A CN 105734329 A CN105734329 A CN 105734329A
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
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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 discloses a method for preparing a high-strength and high-toughness magnesium-based nano composite. A microstructure with multi-stage structural features can be constructed while second-phase nano ceramic particles are added through a ball milling process, and therefore the strength of the magnesium material is improved, the good plasticity of the material is kept, and finally the magnesium-based nano composite with high-strength and high-toughness features is obtained. The method for preparing the nano composite has the advantages of being low in requirement for raw materials and easy to achieve, the preparation process of powder is effectively simplified, the performance of the material is improved, and the multistage-structure magnesium-based nano composite with the maximum compression strength reaching 250 MPa or above and the compressive strain reaching 40% or above is obtained.
Description
Technical field
The preparation method that the present invention relates to a kind of high-strength and high ductility Mg-based nanocomposite, is that a kind of PM technique prepares the new method with multistage microstructure Mg-based nanocomposite.
Background technology
Magnesium is one of element that on the earth, reserves are the abundantest, and the magnesium resource of China is also very abundant, and it is 2.3% at the resource content of veneer of crust metallic ore, be in common metal material the 3rd.And, magnesium elements is also widely distributed in salt lake and ocean.The density 1.74 of magnesium, is about the 1/4 of steel, the 2/5 of titanium, the 2/3 of aluminum, is desirable lightweight structural material.But, the intensity of pure magnesium and modulus are all relatively low, and magnesium has close-packed hexagonal structure, deformation processing difficulty, and this all makes it be difficult to use directly as structural material.
In order to put forward the mechanical property of high purity magnesium, form magnesium alloy often through interpolation alloying element and reach to improve the purpose of intensity, but magnesium alloy is owing to lacking effective precipitated phase, thus strengthening limited efficiency, the improvement of plasticity is also inconspicuous.By adding second phase particles, CNT or Graphene in pure magnesium or magnesium alloy, preparing magnesium base composite material is another approach improving magnesium material mechanical property.Conventional composite materials makes second phase particles, CNT or graphene uniform be distributed in magnesium matrix often by techniques such as casting, powder metallurgy, electrochemical deposition or agitating friction welderings, although this mode can be greatly improved the intensity of magnesium material, but plasticity infringement is serious, it is difficult to composite is carried out deformation processing.
Summary of the invention
Above deficiency in view of prior art.It is an object of the invention to the preparation method obtaining a kind of high-strength and high ductility Mg-based nanocomposite, enable by while adding second-phase nano-ceramic particle, construct the microstructure with multilevel hierarchy feature, thus while reaching to improve magnesium material intensity, and making it keep good plasticity, final acquisition has the Mg-based nanocomposite of high-strength and high ductility feature.
The object of the present invention is achieved like this: the preparation method of a kind of high-strength and high ductility Mg-based nanocomposite, adopts the micron-scale magnesium powder with laminated structure feature or magnesium alloy powder as matrix material；Adopt the ceramic powder with nano-scale as reinforcement raw material；Nano-ceramic particle being embedded in flaky powder surface region in the way of planetary type ball-milling and obtains composite material powder, after compression molding, sintering processes obtains the non-homogeneous dispersion of nano-ceramic particle and has the high-strength and high ductility Mg-based nanocomposite of microscopic features of multilevel hierarchy；Comprise following process step:
1), the preparation of composite material powder
The lamellar magnesium powder of 100 orders and 50nm nano carborundum powder 90-95:5-10 by volume are poured in stainless steel jar mill；Using zirconia ball as ball-milling medium, ratio of grinding media to material is 15:1, and adds stearic acid that mass fraction is 2% as process control medium；Ball grinder is passed into noble gas and carries out protection closure ball grinding jar；Ball grinder is placed on planetary ball mill, with certain operating condition ball milling 30 hours；Glove box is opened ball grinder, adds sealed cans after the stearic acid of 1%；Composite material powder is obtained after 10 hours with similarity condition ball milling again；
2), the sintering of composite material powder:
A), by 1) compression molding in glove box of gained composite material powder, the sample embossed is transferred to the heating rate of 100 DEG C of min to 400 DEG C insulation is got rid of in powder body for 1 minute at this temperature gas in hot-pressed sintering furnace, and pressure is increased to 50MPa after terminating by insulation；B), it is further continued for the heating rate with 100 DEG C/min to 535-550 DEG C, and is incubated 5min at this temperature, with the rate of temperature fall of 50 DEG C/min to 100 DEG C, naturally cool to room temperature subsequently；Obtain greatest compressive strength reach more than 250MPa and compression strain reach more than 40% the Mg-based nanocomposite with multilevel hierarchy；Described multilevel hierarchy refers to that the subregion of sintered body is proof gold symbolic animal of the birth year, and subregion is the composite phase that nano-ceramic particle strengthens, and two kinds of out of phase distribution characteristicss are non-uniform Distribution.
During actual enforcement, stearic acid or dehydrated alcohol can be adopted as process control medium.
The method adopting the present invention, can pass through while adding second-phase nano-ceramic particle, construct the microstructure with multilevel hierarchy feature, thus while reaching to improve magnesium material intensity, and making it keep good plasticity, final acquisition has the Mg-based nanocomposite of high-strength and high ductility feature.
Accompanying drawing explanation
Fig. 1: the picture of micron flakes magnesium powder of the present invention.
Fig. 2: the reinforcement volume fraction prepared by the present invention is the photo of the composite material powder of 10%.
Fig. 3: the reinforcement volume fraction prepared by the present invention is the metallograph of the high-strength and high ductility Mg-based nanocomposite of 10%.
Fig. 4: the load-deformation curve of the high-strength and high ductility Mg-based nanocomposite prepared by the present invention.
Detailed description of the invention
Embodiment 1: adopt planetary type ball-milling, the technique of discharge plasma sintering prepares high-strength and high ductility Mg-based nanocomposite
Concrete preparation process is as follows:
1. the preparation of composite material powder:
The lamellar magnesium powder of 100 orders and 50nm nano carborundum powder 95:5 by volume are poured in stainless steel jar mill；Using zirconia ball as ball-milling medium, ratio of grinding media to material is 15:1, and adds stearic acid that mass fraction is 2% as process control medium；Ball grinder is passed into noble gas and carries out protection closure ball grinding jar；Ball grinder is placed on planetary ball mill, with the rotational velocity ball milling 30 hours of the revolution speeds of 200 revs/min and 10 revs/min；Glove box is opened ball grinder, adds sealed cans after the stearic acid of 1%；Composite material powder is obtained after 10 hours with similarity condition ball milling again.
2. the sintering of composite material powder:
By composite material powder compression molding in glove box, the sample embossed is transferred in discharge plasma sintering stove with the heating rate of 100 DEG C/min to 400 DEG C insulation is got rid of in powder body for 1 minute at this temperature gas, pressure is increased to 50MPa after terminating by insulation, it is further continued for the heating rate with 100 DEG C/min to 535 DEG C, and it is incubated 5min at this temperature, with the rate of temperature fall of 100 DEG C/min to 200 DEG C, naturally cool to room temperature subsequently.
Embodiment 2: adopt planetary type ball-milling, the technique of hot pressed sintering prepares high-strength and high ductility Mg-based nanocomposite
1. the precompressed of ceramic powder:
The lamellar magnesium powder of 100 orders and 50nm nano carborundum powder 90:10 by volume are poured in stainless steel jar mill；Using zirconia ball as ball-milling medium, ratio of grinding media to material is 15:1, and adds stearic acid that mass fraction is 2% as process control medium；Ball grinder is passed into noble gas and carries out protection closure ball grinding jar；Ball grinder is placed on planetary ball mill, with the rotational velocity ball milling 30 hours of the revolution speeds of 200 revs/min and 10 revs/min；Glove box is opened ball grinder, adds sealed cans after the stearic acid of 1%；Composite material powder is obtained after 10 hours with similarity condition ball milling again.
2. the sintering of composite material powder:
By composite material powder compression molding in glove box, the sample embossed is transferred in hot-pressed sintering furnace with the heating rate of 100 DEG C/min to 400 DEG C insulation is got rid of in powder body for 1 minute at this temperature gas, pressure is increased to 50MPa after terminating by insulation, it is further continued for the heating rate with 100 DEG C/min to 550 DEG C, and it is incubated 5min at this temperature, with the rate of temperature fall of 50 DEG C/min to 100 DEG C, naturally cool to room temperature subsequently.
Claims (9)
1. a preparation method for high-strength and high ductility Mg-based nanocomposite, adopts the micron-scale magnesium powder with laminated structure feature or magnesium alloy powder as matrix material；Adopt the ceramic powder with nano-scale as reinforcement raw material；Nano-ceramic particle being embedded in flaky powder surface region in the way of planetary type ball-milling and obtains composite material powder, after compression molding, sintering processes obtains nano-ceramic particle non-homogeneous dispersion and has the high-strength and high ductility Mg-based nanocomposite of multilevel hierarchy microscopic features；Comprise following process step:
1), the preparation of composite material powder
Lamellar magnesium powder/magnesium alloy powder and nano-ceramic powder 70-95:5-30 by volume are poured in stainless steel jar mill；Using zirconia ball as ball-milling medium, ratio of grinding media to material is 15:1, and adds the process control medium that mass fraction is 1-5%；Ball grinder is passed into noble gas and carries out protection closure ball grinding jar；Ball grinder is placed on planetary ball mill, with certain operating condition ball milling 30 hours；Glove box is opened ball grinder, adds sealed cans after the stearic acid of 1%；Composite material powder is obtained after 10 hours with similarity condition ball milling again；
2), the sintering of composite material powder:
A), by 1) compression molding in glove box of gained composite material powder, the sample embossed is transferred to and is heated to 400 DEG C with the heating rate of 100 DEG C of min in hot-pressed sintering furnace and is incubated the gas got rid of in powder body for 1 minute at this temperature, and pressure is increased to 50MPa after terminating by insulation；B), it is further continued for the heating rate with 100 DEG C/min to 500-550 DEG C, and is incubated 5min at this temperature, be cooled to 100 DEG C with certain rate of temperature fall, naturally cool to room temperature subsequently；Obtain greatest compressive strength reach more than 250MPa and compression strain reach more than 40% the Mg-based nanocomposite with multilevel hierarchy feature；Described multilevel hierarchy refers to that the subregion of sintered body is proof gold symbolic animal of the birth year, and subregion is the composite phase that nano-ceramic particle strengthens, and two kinds of out of phase distribution characteristicss are non-uniform Distribution.
2. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that adopt lamellar magnesium powder or magnesium alloy powder as raw material.
3. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that adopt planetary ball mill to prepare composite material powder, and be sintered molding with discharge plasma sintering stove SPS or hot-pressed sintering furnace.
4. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that described step 1) in planetary ball mill with the rotational velocity operating of the revolution speed of 150-200 rev/min and 10-50 rev/min.
5. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that adopt stearic acid or dehydrated alcohol as process control medium.
6. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that described step 2) in b) refer to the rate of temperature fall with 50-100 DEG C/min to 100 DEG C with certain rate of temperature fall cooling described in step.
7. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that described step 2) in multilevel hierarchy refer to that there is proof gold symbolic animal of the birth year.
8. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that described step 2) in multilevel hierarchy refer to that there is the composite phase that nano-ceramic particle strengthens.
9. according to claim 1, the preparation method of high-strength and high ductility Mg-based nanocomposite, it is characterised in that described step 2) in multilevel hierarchy refer to that the distribution characteristics of nano-ceramic particle is non-uniform Distribution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106555089A (en) * | 2016-11-01 | 2017-04-05 | 成都天智轻量化科技有限公司 | A kind of CNT and nano-ceramic particle mixing reinforced magnesium based composites and preparation method thereof |
| CN109504869A (en) * | 2018-12-12 | 2019-03-22 | 西南交通大学 | A kind of metal-base nanometer composite material and preparation method thereof with bionical multilevel structure |
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| CN1837392A (en) * | 2006-04-03 | 2006-09-27 | 重庆大学 | Composite material of magnesium alloy and method for preparing the same |
| CN101748306A (en) * | 2008-12-02 | 2010-06-23 | 苏州有色金属研究院有限公司 | Multiphase ceramic hybrid composite reinforced metal matrix composite material and preparation process thereof |
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Patent Citations (6)
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| CN1837392A (en) * | 2006-04-03 | 2006-09-27 | 重庆大学 | Composite material of magnesium alloy and method for preparing the same |
| CN101748306A (en) * | 2008-12-02 | 2010-06-23 | 苏州有色金属研究院有限公司 | Multiphase ceramic hybrid composite reinforced metal matrix composite material and preparation process thereof |
| CN102728818A (en) * | 2012-06-07 | 2012-10-17 | 中国兵器工业第五九研究所 | Method for preparing SiCp enhanced AZ91D composite material blank |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106555089A (en) * | 2016-11-01 | 2017-04-05 | 成都天智轻量化科技有限公司 | A kind of CNT and nano-ceramic particle mixing reinforced magnesium based composites and preparation method thereof |
| CN106555089B (en) * | 2016-11-01 | 2019-03-29 | 成都天智轻量化科技有限公司 | A kind of carbon nanotube and nano-ceramic particle mixing reinforced magnesium-base composite material and preparation method |
| CN109504869A (en) * | 2018-12-12 | 2019-03-22 | 西南交通大学 | A kind of metal-base nanometer composite material and preparation method thereof with bionical multilevel structure |
| CN109504869B (en) * | 2018-12-12 | 2020-09-18 | 西南交通大学 | Metal-based nanocomposite material with bionic multilevel structure and preparation method thereof |
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