CN105734329B - A kind of preparation method of high-strength and high ductility Mg-based nanocomposite - Google Patents
A kind of preparation method of high-strength and high ductility Mg-based nanocomposite Download PDFInfo
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- CN105734329B CN105734329B CN201610255865.1A CN201610255865A CN105734329B CN 105734329 B CN105734329 B CN 105734329B CN 201610255865 A CN201610255865 A CN 201610255865A CN 105734329 B CN105734329 B CN 105734329B
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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
Abstract
The invention discloses a kind of preparation method of high-strength and high ductility Mg-based nanocomposite, can be by ball-milling technology while the second phase nano-ceramic particle is added, construct the microstructure with multilevel hierarchy feature, so as to reach while raising magnesium material intensity, and it is kept good plasticity, it is final to obtain the Mg-based nanocomposite with high-strength and high ductility feature.This nano composite material preparation method has the advantages that ingredient requirement is low, be easily achieved, effectively simplify the preparation process of powder, improve material property, obtain greatest compressive strength reach more than 250MPa and compression strain reach more than 40% the Mg-based nanocomposite with multilevel hierarchy.
Description
Technical field
It is one kind PM technique the present invention relates to a kind of preparation method of high-strength and high ductility Mg-based nanocomposite
Prepare the new method with multistage microstructure Mg-based nanocomposite.
Background technology
Magnesium is one of reserves most abundant element on the earth, and the magnesium resource of China also enriches very much, and it is in veneer of crust gold
The resource content for belonging to ore deposit is 2.3%, be in common metal material the 3rd.Moreover, magnesium elements be also widely distributed in salt lake and
In ocean.The 1/4 of the density 1.74, about steel of magnesium, the 2/5 of titanium, the 2/3 of aluminium, it is preferable lightweight structural material.But, it is pure
The intensity and modulus of magnesium is all relatively low, and magnesium has close-packed hexagonal structure, and deformation processing is difficult, and this all causes it to be difficult to directly
Connect and used as structural material.
In order to put forward the mechanical property of high purity magnesium, intensity is improved to reach often through addition alloying element formation magnesium alloy
Purpose, but magnesium alloy is due to lacking effective precipitated phase, thus reinforcing effect is limited, the improvement to plasticity is not also obvious.It is logical
Second phase particles, CNT or graphene are added in passing pure magnesium or magnesium alloy, it is to improve magnesium to prepare magnesium-based composite material
Another approach of material mechanical performance.Conventional composite materials are rubbed often by casting, powder metallurgy, electrochemical deposition or stirring
Wiping the techniques such as weldering causes second phase particles, CNT or graphene uniform to be distributed in magnesium matrix, although this mode can
The intensity of magnesium material is greatly improved, but serious is damaged to plasticity, it is difficult to carry out deformation processing to composite.
The content of the invention
In view of prior art is not enough above.The purpose of the present invention is to obtain a kind of high-strength and high ductility Mg-based nanocomposite
Preparation method, enable by add the second phase nano-ceramic particle while, construct with multilevel hierarchy feature
Microstructure so that while reaching raising magnesium material intensity, and its is kept good plasticity, final obtain has high-strength height
The Mg-based nanocomposite of tough feature.
The object of the present invention is achieved like this：A kind of preparation method of high-strength and high ductility Mg-based nanocomposite, is used
Micron-scale magnesium powder or magnesium alloy powder with laminated structure feature are used as matrix material；Using the ceramic powder with nano-scale
Body is used as reinforcement raw material；Nano-ceramic particle is embedded in into flaky powder surface region in the way of planetary type ball-milling to be answered
Condensation material powder, sintering processes obtain the non-homogeneous dispersion of nano-ceramic particle and aobvious with multilevel hierarchy after compression molding
The high-strength and high ductility Mg-based nanocomposite of micro- feature；Include following process step：
1), the preparation of composite material powder
By the sheet magnesium powder and 50nm nano carborundum powders of 100 mesh 90-95 by volume:5-10 pours into stainless steel jar mill
In；Using zirconia ball as ball-milling medium, ratio of grinding media to material is 15:1, and add mass fraction be 2% stearic acid as excessively program control
Medium processed；Ball grinder is passed through into inert gas to be protected and close ball grinder；Ball grinder is placed on planetary ball mill, with
Certain operating condition ball milling 30 hours；Ball grinder is opened in glove box, sealed cans after 1% stearic acid are added；With same
Ball milling obtains composite material powder to condition after 10 hours again；
2), the sintering of composite material powder：
A), by 1) gained composite material powder compression molding in glove box, the sample being molded is transferred to hot pressed sintering
It is incubated the gas excluded in powder for 1 minute, insulation knot in stove to 400 DEG C and at this temperature with 100 DEG C of min heating rate
Pressure is increased into 50MPa after beam；B) heating rate with 100 DEG C/min, is further continued for 535-550 DEG C, and at this temperature
5min is incubated, with 50 DEG C/min rate of temperature fall to 100 DEG C, room temperature is then naturally cooled to；Greatest compressive strength is obtained to reach
More than 250MPa and compression strain reach more than 40% Mg-based nanocomposite with multilevel hierarchy；The multilevel hierarchy
The subregion for referring to sintered body is proof gold symbolic animal of the birth year, and subregion is the enhanced composite phase of nano-ceramic particle, and two kinds are not
Distribution characteristics with phase is non-uniform Distribution.
During actual implementation, process control medium can be used as using stearic acid or absolute ethyl alcohol.
Using method of the invention, it is possible to by while the second phase nano-ceramic particle is added, constructing with many
The microstructure of level structure feature, thus while reaching raising magnesium material intensity, and it is kept good plasticity, it is final to obtain
Mg-based nanocomposite with high-strength and high ductility feature.
Brief description of the drawings
Fig. 1：The picture of micron flakes magnesium powder of the present invention.
Fig. 2：The photo for the composite material powder that reinforcement volume fraction prepared by the present invention is 10%.
Fig. 3：The gold for the high-strength and high ductility Mg-based nanocomposite that reinforcement volume fraction prepared by the present invention is 10%
Phase photo.
Fig. 4：The load-deformation curve of high-strength and high ductility Mg-based nanocomposite prepared by the present invention.
Embodiment
Embodiment 1：High-strength and high ductility magnesium-base nano composite wood is prepared using the technique of planetary type ball-milling, discharge plasma sintering
Material
Specific preparation process is as follows：
1. the preparation of composite material powder：
By the sheet magnesium powder and 50nm nano carborundum powders of 100 mesh by volume 95:5 pour into stainless steel jar mill；With
Zirconia ball is as ball-milling medium, and ratio of grinding media to material is 15:1, and add mass fraction be 2% stearic acid be situated between as process control
Matter；Ball grinder is passed through into inert gas to be protected and close ball grinder；Ball grinder is placed on planetary ball mill, with 200
Rev/min revolution speed and 10 revs/min of rotational velocity ball milling 30 hours；Ball grinder is opened in glove box, 1% is added
Sealed cans after stearic acid；With similarity condition, ball milling obtains composite material powder after 10 hours again.
2. the sintering of composite material powder：
The compression molding in glove box by composite material powder, the sample being molded is transferred in discharge plasma sintering stove
The gas excluded in powder for 1 minute is incubated to 400 DEG C and at this temperature with 100 DEG C/min heating rate, after insulation terminates
Pressure is increased into 50MPa, is further continued for 100 DEG C/min heating rate to 535 DEG C, and is incubated 5min at this temperature, with
100 DEG C/min rate of temperature fall then naturally cools to room temperature to 200 DEG C.
Embodiment 2：High-strength and high ductility Mg-based nanocomposite is prepared using the technique of planetary type ball-milling, hot pressed sintering
1. the precompressed of ceramic powder：
By the sheet magnesium powder and 50nm nano carborundum powders of 100 mesh by volume 90:10 pour into stainless steel jar mill；With
Zirconia ball is as ball-milling medium, and ratio of grinding media to material is 15:1, and add mass fraction be 2% stearic acid be situated between as process control
Matter；Ball grinder is passed through into inert gas to be protected and close ball grinder；Ball grinder is placed on planetary ball mill, with 200
Rev/min revolution speed and 10 revs/min of rotational velocity ball milling 30 hours；Ball grinder is opened in glove box, 1% is added
Sealed cans after stearic acid；With similarity condition, ball milling obtains composite material powder after 10 hours again.
2. the sintering of composite material powder：
The compression molding in glove box by composite material powder, the sample being molded is transferred in hot-pressed sintering furnace with 100
DEG C/min heating rate is to 400 DEG C and is incubated the gas excluded in powder for 1 minute at this temperature, insulation terminate after by pressure
Increase to 50MPa, be further continued for 100 DEG C/min heating rate to 550 DEG C, and be incubated 5min at this temperature, with 50 DEG C/
Min rate of temperature fall then naturally cools to room temperature to 100 DEG C.
Claims (3)
1. a kind of preparation method of high-strength and high ductility Mg-based nanocomposite, using the micron-scale magnesium with laminated structure feature
Powder or magnesium alloy powder are used as matrix material；Reinforcement raw material is used as using the ceramic powder with nano-scale；With planetary ball
Nano-ceramic particle is embedded in flaky powder surface region and obtains composite material powder by the mode of mill, is sintered after compression molding
Processing obtains nano-ceramic particle non-homogeneous dispersion and the high-strength and high ductility magnesium-base nano composite wood with multilevel hierarchy microscopic features
Material；Include following process step：
1), the preparation of composite material powder
By sheet magnesium powder/magnesium alloy powder and nano-ceramic powder 70-95 by volume:5-30 is poured into stainless steel jar mill；Nanometer
Ceramic powder is carborundum powder；Using zirconia ball as ball-milling medium, ratio of grinding media to material is 15:1, and it is 1-5%'s to add mass fraction
Process control medium；Ball grinder is passed through into inert gas to be protected and close ball grinder；Ball grinder is placed in planetary type ball-milling
On machine, with certain operating condition ball milling 30 hours；Ball grinder is opened in glove box, sealed cans after 1% stearic acid are added；
With similarity condition, ball milling obtains composite material powder after 10 hours again；
2), the sintering of composite material powder：
A), by 1) gained composite material powder compression molding in glove box, the sample being molded is transferred in hot-pressed sintering furnace
The gas for being heated to 400 DEG C with 100 DEG C of min heating rate and being incubated at this temperature in 1 minute exclusion powder, insulation terminates
Pressure is increased into 50MPa afterwards；B) heating rate with 100 DEG C/min, is further continued for 500-550 DEG C, and is protected at this temperature
Warm 5min, 50-100 DEG C/min rate of temperature fall are cooled to 100 DEG C, then naturally cool to room temperature；Obtain greatest compressive strength
Reach more than 250MPa and compression strain reach more than 40% the Mg-based nanocomposite with multilevel hierarchy feature；It is described
Multilevel hierarchy refers to that the subregion of sintered body is proof gold symbolic animal of the birth year, and subregion is the enhanced composite of nano-ceramic particle
Phase, two kinds of out of phase distribution characteristics are non-uniform Distribution.
2. a kind of preparation method of high-strength and high ductility Mg-based nanocomposite according to claim 1, it is characterised in that institute
State step 1) in planetary ball mill operated with the rotational velocity of 150-200 revs/min of revolution speed and 10-50 revs/min.
3. the preparation method of a kind of high-strength and high ductility Mg-based nanocomposite according to claim 1, it is characterised in that adopt
Process control medium is used as with stearic acid or absolute ethyl alcohol.
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| CN201610255865.1A CN105734329B (en) | 2016-04-22 | 2016-04-22 | A kind of preparation method of high-strength and high ductility Mg-based nanocomposite |
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| CN105734329B true CN105734329B (en) | 2017-10-24 |
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| 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 |
| 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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| CN100376703C (en) * | 2006-04-03 | 2008-03-26 | 重庆大学 | Composite material of magnesium alloy and method for preparing the same |
| CN101748306B (en) * | 2008-12-02 | 2011-12-07 | 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 |
| CN103725947B (en) * | 2014-01-09 | 2016-04-13 | 东北大学 | A kind of ceramic particle reinforced magnesium-based composite material and preparation method thereof |
| CN103866168B (en) * | 2014-03-17 | 2015-10-21 | 天津理工大学 | A kind of preparation method of nano-particle reinforcement magnesium base Biocomposite material |
| CN104498753A (en) * | 2014-12-02 | 2015-04-08 | 常熟市东涛金属复合材料有限公司 | Preparation method of biological ceramic-metal compound material |
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