CN103725947A - Ceramic particle enhanced magnesium-based composite material and preparation method thereof - Google Patents

Ceramic particle enhanced magnesium-based composite material and preparation method thereof Download PDF

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CN103725947A
CN103725947A CN201410010992.6A CN201410010992A CN103725947A CN 103725947 A CN103725947 A CN 103725947A CN 201410010992 A CN201410010992 A CN 201410010992A CN 103725947 A CN103725947 A CN 103725947A
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magnesium
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陈礼清
姚彦桃
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Northeastern University China
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Abstract

A method for preparing a magnesium-based composite material through a metal melt pressureless infiltration ceramic precast block is a preparation method which is low in cost, rapid and high-efficiency and realizes final forming. Because the wettability between ceramics and a metal system is low, the infiltration process is difficultly performed even cannot be performed. The invention provides a ceramic particle enhanced magnesium-based composite material and a preparation method thereof aiming at the problems. A small amount of the third-phase component metal Ti which has high melting point and is immiscible with a magnesium melt is added into the ceramic precast block to serve as a magnesium melt infiltration inducer, the wettability of a B4C/Mg composite material system is effectively improved, and a B4C/Mg series ultra-light wear-resistant ceramic particle enhanced magnesium-based composite material is prepared. The method comprises the following steps: mechanically and uniformly mixing B4C powder, Ti powder and an adhesive, performing cold pressing to prepare a ceramic precast block, putting the ceramic precast block and a pure magnesium ingot into an electric furnace for heating, melting the pure magnesium ingot, infiltrating the magnesium ingot into pores of the ceramic precast block, and preparing the ceramic particle enhanced magnesium-based composite material.

Description

A kind of ceramic particle reinforced magnesium-based composite material and preparation method thereof
Technical field
The invention belongs to material technology field, particularly a kind of ultralight high-wearing feature magnesium base composite material and preparation method thereof.
Background technology
Material is basis and the guide of science, social progress, is the milestone of human progress.But over nearly 40 years, scientific technological advance is rapid, the particularly development of the hard-core technology such as aerospace, automobile, the performance of material has been proposed to more and more stricter requirement, and traditional single-material cannot meet these requirements.At this moment, the appearance of matrix material just becomes the inexorable trend of the single-material application developments such as metal, pottery, is also the comprehensive distillation of various single-material performances.
Metal-base composites is to take metal or alloy as matrix, the matrix material that the fiber, whisker, particle etc. of pottery of take is reinforcement.It combines the good characteristics such as high strength, high elastic coefficient, wear resistance, high thermal resistance and solidity to corrosion of toughness, conduction, thermal conductivity and the pottery of metal, compare with traditional metallic substance, there is high specific tenacity, specific rigidity, specific modulus, high temperature resistant, wear-resistant, antifatigue, the excellent properties such as damping and amortization is good, thermal expansivity is little, chemical stability and good stability of the dimension, in aerospace and automotive field, demonstrate very wide application prospect.Magnesium base composite material is to take the pottery that pure magnesium or magnesium alloy be matrix to strengthen magnesium base composite material, because magnesium has the features such as low density, high specific tenacity and specific rigidity, therefore, magnesium base composite material has larger application potential in emerging technology field than traditional metal materials and aluminum matrix composite, and be described as the novel material of 21 century environmental protection and Sustainable development, in the fields such as aerospace, automobile making, Electronic Packaging and sports equipment, show huge application prospect.
Metal melt pressure-free impregnation ceramics preparative piece prepare magnesium base composite material be a kind of low cost, rapidly and efficiently, the composite material and preparation method thereof of near-net forming.But the prerequisite that realizes this process is that pottery must have good wettability with intermetallic.Generally, the wettability between pottery and metal system is not fine, and this is by the significantly reduction of the speed that causes infiltrating, and even infiltration process can not occur.Improving infiltration temperature is a method that solves ceramic-metal melt wettability; In general, temperature raises and plays certain effect to improving wettability, still, for the low melting point metal as magnesium, the small size rising of melt infiltration temperature is all by the quick volatilization of aggravation magnesium metal melt, and this has not only increased process costs, and causes preparation process to carry out.
Summary of the invention
For the problems referred to above of existing on existing performance of magnesium-based composite material and in technique, the invention provides a kind of ceramic particle reinforced magnesium-based composite material and preparation method thereof, by in ceramics preparative piece, add a small amount of high-melting-point and with the immiscible third phase constituent element of magnesium melt metal Ti as magnesium melt infiltration inducer, effectively improve B 4the wettability of C/Mg composite system, prepares B 4c/Mg is ultralight high-wearing feature ceramic particle reinforced magnesium-based composite material.
The technical solution used in the present invention is, a kind of ceramic particle reinforced magnesium-based composite material, is comprised of pure magnesium matrix and ceramic enhanced granule, and wherein pure magnesium matrix volume accounts for 40~50% of total composite volume, and ceramic enhanced granule is by B 4c and Ti form, and Ti volume accounts for 6~8% of ceramic enhanced granule cumulative volume; Ti and B 4c forms particle packing structure, and Mg infiltrates in the hole of particle packing structure.
The density of above-mentioned ceramic particle reinforced magnesium-based composite material is at 2.09~2.22g/cm 3.
Another one technical scheme of the present invention is, a kind of preparation method of ceramic particle reinforced magnesium-based composite material, and step is as follows:
(1) be averaged the B that granularity is 5~28 μ m 4ti powder and the tackiness agent of C powder, mean particle size≤25 μ m, mechanically mixing is even, obtains powder mix; Wherein, Ti powder amount is B 46~8% of C powder and Ti powder cumulative volume, amount of binder is Ti powder and B 45%~10% of C powder cumulative volume;
(2) by powder mix, by the unidirectional density that is cold-pressed into of press, be 50~60% ceramics preparative piece;
(3) get the pure magnesium ingot that size is identical with ceramics preparative piece, the two is put into graphite jig, magnesium ingot is positioned at ceramics preparative piece top, and the consistent size of the two contact surface;
(4) graphite jig that ceramics preparative piece and pure magnesium ingot are housed is put into the flat-temperature zone of vacuum resistance furnace, under mobile argon gas atmosphere condition, with 10K/min, be warming up to 275~285 ℃, insulation 10~15min, overflows tackiness agent volatilization; And then being warming up to 680~720 ℃ with 10K/min, insulation 90~150min, makes under capillary force action, to be infiltrated up in the hole in ceramics preparative piece after pure magnesium ingot fusing, makes ceramic particle reinforced magnesium-based composite material.
Above-mentioned tackiness agent is natural rubber.
The above-mentioned unidirectional density that is cold-pressed into is that 50~60% ceramics preparative piece refers to ceramic powder mix is placed in to compacting tool set, and adopting press is 50~60% corresponding height values by its Uniaxial Compression to density; Relation between density and prefabricated section height:
Figure BDA0000455113500000021
wherein,
Figure BDA0000455113500000022
for ceramics preparative piece density, m surveyfor the quality of ceramics preparative piece actual measurement, ρ reasonfor ceramics preparative piece theoretical density, φ is the diameter of the prefabricated section of compacting, the height that h is prefabricated section.
Purity >=99.95% of above-mentioned pure magnesium ingot.
Above-mentioned B 4purity>=99.5% of C powder, purity>=99.5% of Ti powder.
Purity >=99.999% of above-mentioned argon gas.
The principle of method foundation of the present invention is:
1, pure magnesium melt infiltration B 4c ceramics preparative piece is a process extremely slowly, and the spontaneous infiltration that does not add third phase constituent element metal is impossible occur, or carry out extremely slow, and when lower than 750 ℃, spontaneous infiltration process can not realize.But while having a small amount of metal Ti to participate in, while adopting the refractory metal that do not dissolve each other to bring out infiltration, during temperature more than a little higher than MAGNESIUM METAL fusing point, the speed that this process is carried out improves greatly, but also has avoided volatilization; This is mainly because add third phase constituent element refractory metal titanium (Ti) in ceramics preparative piece, can reduce surface tension and liquid/liquid/solid interface tension force of molten metal, thereby improve B 4wettability between C pottery and metal M g melt; Even a small amount of titanium particle, also can bring out magnesium melt and realize carrying out fast of infiltration process, thus make ultralight and have height resistance to abrasion particle reinforced magnesium base compound material.
2, B 4the density of C pottery is low, is only 2.52g/cm 3, and be the high and very competent material of anti-neutron radiation of a kind of wear resistance, the density of magnesium is also very low, is 1.74g/cm 3, therefore, by B 4the particle reinforced magnesium base compound material density that C and a small amount of Ti form is still lower, remains a kind of desirable lightweight, matrix material that wear resisting property is good.
Feature of the present invention is:
1, the invention provides a kind of pottery and strengthen magnesium base composite material, this matrix material combines magnesium and B 4the advantage of C pottery, has low density, simultaneously B 4c plays the effect of strengthening to magnesium matrix, wear resistance is also improved, and its density is 2.09~2.22g/cm 3, the purer magnesium of wear resistance has improved 22.2%~27.7%, can be used as the material of wearing piece.
2, consider metal melt impregnated porcelain prefabricated section before make demands, optimization design to add in ceramics preparative piece third phase high-melting-point, with the immiscible metal constituent element of metal melt Ti, improve pottery and intermetallic wettability, realized the quick infiltration of metal melt to ceramics preparative piece.
3, utilize preparation method of the present invention, ceramics preparative piece and pure magnesium ingot can complete metal melt to the quick infiltration of ceramics preparative piece at lesser temps (680~720 ℃), add tackiness agent to be conducive to strengthen the intensity of prefabricated section, be convenient to carrying out smoothly of infiltration process.
4, utilize preparation method of the present invention, can obtain ultralight, wear-resisting ceramic particle reinforced magnesium-based composite material, for the synthetic and application of low-cost mixing reinforced magnesium based composites is laid a good foundation, also for the intermetallic matrix material that utilizes refractory metal to bring out other system of infiltration preparation provides reference.
Accompanying drawing explanation
Fig. 1 is the ceramic particle reinforced magnesium-based composite material microstructure picture figure of preparation in the embodiment of the present invention 1; In figure, white bright particle is B 4c particle, the part of black is Mg matrix, Ti particle volume seldom, does not almost observe.
Fig. 2 is the ceramic particle reinforced magnesium-based composite material microstructure picture figure of preparation in the embodiment of the present invention 1; In figure, cross mark place is Ti particle.
Fig. 3 is the ceramic particle reinforced magnesium-based composite material wear test graphic representation of preparing in the embodiment of the present invention; In figure, each curve is followed successively by the abrasion loss curve of MAGNESIUM METAL from top to bottom, the ceramic particle reinforced magnesium-based composite material wear curve of the ceramic particle reinforced magnesium-based composite material wear curve of embodiment 3, embodiment 2 and the ceramic particle reinforced magnesium-based composite material wear curve of embodiment 1.
Embodiment
In the embodiment of the present invention, density measurement adopts: plum Teller-Tuo benefit surmounts series of X S analytical balance (METTLER TOLEDO XS105Dual Range), and maximum capacity scope is 41g/120g, and readability is 0.01mg/0.1mg.
In the embodiment of the present invention, to the microstructure observation of ceramic particle reinforced magnesium-based composite material, adopt FEI Quanta600 type scanning electronic microscope to characterize; Its thing adopts X ' Pert Pro type X-ray diffractometer to determine mutually.
In the embodiment of the present invention, wear resistance is measured and is adopted MG-2000 type high-speed and high-temperature friction wear testing machine, and maximum positive voltage power is 2000N, maximum speed 3200r/min; Test parameter is set as: sliding velocity is 250r/min, and sliding time is 5min, and pressure is set as 20N successively, 40N, and 60N, 80N, take plane perpendicular to axial direction as abrasion surface; Concrete grammar is: before and after wearing and tearing, sample, friction pair all will clean 20min with ultrasonic wave alcohol, on the electronic balance that is then 0.1mg in precision, weigh, and try to achieve sample mass loss during abrasion, using abrasion loss as the standard of weighing wear resistance.
B in the embodiment of the present invention 4c powder and Ti powder are commercial product; B 4weight purity>=99.5% of C powder, weight purity>=99.5% of Ti powder.
Natural rubber in the embodiment of the present invention is commercial Industrial products.
Magnesium ingot in the embodiment of the present invention is commercial product, weight purity >=99.95%.
Argon gas in the embodiment of the present invention is commercial product, bulk purity >=99.999%.
The material of the graphite jig in the embodiment of the present invention is the high purity graphite of weight purity 99.9%.
It is that 50~60% ceramics preparative piece refers to ceramic powder mix is placed in to compacting tool set that unidirectional in the embodiment of the present invention is cold-pressed into density, adopts ρ reasonpress is 50~60% corresponding height values by its Uniaxial Compression to density; Relation between density and prefabricated section height:
Figure BDA0000455113500000051
wherein, for ceramics preparative piece density, m surveyfor the quality of ceramics preparative piece actual measurement, ρ reasonfor ceramics preparative piece theoretical density, φ is the diameter of the prefabricated section of compacting, the height that h is prefabricated section.This formula is net result, and derivation formula does not outline one by one.
Embodiment 1
A preparation method for ceramic particle reinforced magnesium-based composite material, step is as follows:
1, be averaged the B that granularity is 28 μ m 4the liquid natural rubber of the Ti powder of C powder, mean particle size≤25 μ m and binding agent, mechanically mixing is even, obtains powder mix; Wherein, Ti powder amount is Ti powder and B 48% of C powder cumulative volume, amount of binder is Ti powder and B 45% of C powder cumulative volume;
2, by powder mix, by the unidirectional density that is cold-pressed into of press, be 60% ceramics preparative piece;
3, get the pure magnesium ingot that size is identical with ceramics preparative piece, the two is put into graphite jig, magnesium ingot is positioned at ceramics preparative piece top, and the consistent size of the two contact surface;
4, the graphite jig that ceramics preparative piece and magnesium ingot are housed is put into the flat-temperature zone of vacuum resistance furnace, under mobile argon gas atmosphere condition, with 10K/min, be warming up to 275 ℃, insulation 10min, so that binding agent vaporization at high temperature, and then with 10K/min speed, be warming up to 720 ℃, insulation 150min, make under capillary force action, to be infiltrated up in the hole in ceramics preparative piece after pure magnesium ingot fusing, make ceramic particle reinforced magnesium-based composite material.
This ceramic particle reinforced magnesium-based composite material is comprised of Mg matrix and ceramic enhanced granule, and the two volume ratio is 40%:60%, and ceramic enhanced granule is by B 4c and Ti form, and Ti volume accounts for 8% of ceramic enhanced granule cumulative volume, Ti and B 4c forms particle packing structure, and Mg infiltrates in the hole of particle packing structure; The density of this matrix material is 2.22g/cm 3;
Adopt MG-2000 type high-speed and high-temperature friction wear testing machine to carry out wear test, with magnesium ingot, be contrast experiment, experimental result as shown in Figure 3; Microstructure picture as depicted in figs. 1 and 2.
Embodiment 2
A preparation method for ceramic particle reinforced magnesium-based composite material, step is as follows:
1, be averaged the B that granularity is 10 μ m 4the liquid natural rubber of the Ti powder of C powder, mean particle size≤25 μ m and binding agent, mechanically mixing is even, obtains powder mix; Wherein, Ti powder amount is Ti powder and B 47% of C powder cumulative volume, amount of binder is Ti powder and B 48% of C powder cumulative volume;
2, by powder mix, by the unidirectional density that is cold-pressed into of press, be 55% ceramics preparative piece;
3, get the pure magnesium ingot that size is identical with ceramics preparative piece, the two is put into graphite jig, magnesium ingot is positioned at ceramics preparative piece top, and the consistent size of the two contact surface;
4, the graphite jig that ceramics preparative piece and magnesium ingot are housed is put into the flat-temperature zone of vacuum resistance furnace, under mobile argon gas atmosphere condition, with 10K/min, be warming up to 280 ℃, insulation 12min, so that binding agent vaporization at high temperature, and then with 10K/min speed, be warming up to 700 ℃, insulation 120min, make under capillary force action, to be infiltrated up in the hole in ceramics preparative piece after pure magnesium ingot fusing, make ceramic particle reinforced magnesium-based composite material.
This ceramic particle reinforced magnesium-based composite material is comprised of Mg matrix and ceramic enhanced granule, and the two volume ratio is 45%:55%, and ceramic enhanced granule is by B 4c and Ti form, and Ti volume accounts for 7% of ceramic enhanced granule cumulative volume, Ti and B 4c forms particle packing structure, and Mg infiltrates in the hole of particle packing structure; The density of this matrix material is 2.15g/cm 3.
Adopt MG-2000 type high-speed and high-temperature friction wear testing machine to carry out wear test, with magnesium ingot, be contrast experiment, experimental result as shown in Figure 3.
Embodiment 3
A preparation method for ceramic particle reinforced magnesium-based composite material, step is as follows:
1, be averaged the B that granularity is 5 μ m 4the liquid natural rubber of the Ti powder of C powder, mean particle size≤25 μ m and binding agent, mechanically mixing is even, obtains powder mix; Wherein, Ti powder amount is Ti powder and B 46% of C powder cumulative volume, amount of binder is Ti powder and B 410% of C powder cumulative volume;
2, by powder mix, by the unidirectional density that is cold-pressed into of press, be 50% ceramics preparative piece;
3, get the pure magnesium ingot that size is identical with ceramics preparative piece, the two is put into graphite jig, magnesium ingot is positioned at ceramics preparative piece top, and the consistent size of the two contact surface;
4, the graphite jig that ceramics preparative piece and magnesium ingot are housed is put into the flat-temperature zone of vacuum resistance furnace, under mobile argon gas atmosphere condition, with 10K/min, be warming up to 285 ℃, insulation 15min, so that binding agent vaporization at high temperature, and then with 10K/min speed, be warming up to 680 ℃, insulation 90min, make under capillary force action, to be infiltrated up in the hole in ceramics preparative piece after pure magnesium ingot fusing, make ceramic particle reinforced magnesium-based composite material.
This ceramic particle reinforced magnesium-based composite material is comprised of Mg matrix and ceramic enhanced granule, and the two volume ratio is 50%:50%, and ceramic enhanced granule is by B 4c and Ti form, and Ti volume accounts for 6% of ceramic enhanced granule cumulative volume, Ti and B 4c forms particle packing structure, and Mg infiltrates in the hole of particle packing structure; The density of this matrix material is 2.09g/cm 3.
Adopt MG-2000 type high-speed and high-temperature friction wear testing machine to carry out wear test, with magnesium ingot, be contrast experiment, experimental result as shown in Figure 3.

Claims (6)

1. a ceramic particle reinforced magnesium-based composite material, is comprised of pure magnesium matrix and ceramic enhanced granule, it is characterized in that, described pure magnesium matrix volume accounts for 40~50% of total composite volume, and ceramic enhanced granule is by B 4c and Ti form, and Ti volume accounts for 6~8% of ceramic enhanced granule cumulative volume.
2. a kind of ceramic particle reinforced magnesium-based composite material according to claim 1, is characterized in that, the density of described ceramic particle reinforced magnesium-based composite material is 2.09~2.22g/cm 3.
3. a preparation method for ceramic particle reinforced magnesium-based composite material, is characterized in that, step is as follows:
(1) be averaged the B that granularity is 5~28 μ m 4ti powder and the tackiness agent of C powder, mean particle size≤25 μ m, mechanically mixing is even, obtains powder mix; Wherein, Ti powder amount is Ti powder and B 46~8% of C powder cumulative volume, amount of binder is Ti powder and B 45%~10% of C powder cumulative volume;
(2) by powder mix, by the unidirectional density that is cold-pressed into of press, be 50~60% ceramics preparative piece;
(3) get the pure magnesium ingot that size is identical with ceramics preparative piece, the two is put into graphite jig, magnesium ingot is positioned at ceramics preparative piece top, and the consistent size of the two contact surface;
(4) graphite jig that ceramics preparative piece and pure magnesium ingot are housed is put into the flat-temperature zone of vacuum resistance furnace, under mobile argon gas atmosphere condition, with 10K/min, be warming up to 275~285 ℃, insulation 10~15min, overflows tackiness agent volatilization; And then being warming up to 680~720 ℃ with 10K/min, insulation 90~150min, makes under capillary force action, to be infiltrated up in the hole in ceramics preparative piece after pure magnesium ingot fusing, makes ceramic particle reinforced magnesium-based composite material.
4. the preparation method of a kind of ceramic particle reinforced magnesium-based composite material according to claim 3, is characterized in that, described tackiness agent is natural rubber.
5. the preparation method of a kind of ceramic particle reinforced magnesium-based composite material according to claim 3, is characterized in that, purity >=99.999% of described argon gas.
6. the preparation method of a kind of ceramic particle reinforced magnesium-based composite material according to claim 1 or a kind of ceramic particle reinforced magnesium-based composite material claimed in claim 3, is characterized in that, purity>=99.95% of described pure magnesium ingot, B 4purity>=99.5% of C powder, purity>=99.5% of Ti powder.
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CN105349817A (en) * 2015-10-29 2016-02-24 无锡桥阳机械制造有限公司 Technology for preparing composite material
CN105734329A (en) * 2016-04-22 2016-07-06 西南交通大学 Method for preparing high-strength and high-toughness magnesium-based nano composite
CN108546841A (en) * 2018-03-24 2018-09-18 深圳万佳互动科技有限公司 A kind of pressure-free impregnation prepares magnesium alloy and preparation method thereof
CN109396440A (en) * 2018-12-27 2019-03-01 吉林大学 A kind of forming method of ceramic particle reinforced aluminium base composite material
CN110438373A (en) * 2019-08-29 2019-11-12 东北大学 A kind of preparation method of magnesium-based composite material
WO2021035776A1 (en) * 2019-08-29 2021-03-04 东北大学 Method for preparing magnesium-based composite material
CN114669743A (en) * 2022-03-18 2022-06-28 辽宁石油化工大学 Boron carbide reinforced foamed aluminum composite material and preparation method thereof
CN114669743B (en) * 2022-03-18 2023-12-05 辽宁石油化工大学 Boron carbide reinforced foam aluminum composite material and preparation method thereof
CN114935279A (en) * 2022-04-08 2022-08-23 北京理工大学 Metal casting prestressed ceramic composite protective armor and preparation method thereof
CN114985707A (en) * 2022-05-30 2022-09-02 长飞光纤光缆股份有限公司 Preparation method of aluminum-clad metal-based diamond composite material
CN114985707B (en) * 2022-05-30 2024-01-23 长飞光纤光缆股份有限公司 Preparation method of aluminum-clad Jin Shuji diamond composite material

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