CN108441732A - A kind of Nano diamond particle reinforced magnesium base compound material and preparation method thereof - Google Patents

A kind of Nano diamond particle reinforced magnesium base compound material and preparation method thereof Download PDF

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Publication number
CN108441732A
CN108441732A CN201810260324.7A CN201810260324A CN108441732A CN 108441732 A CN108441732 A CN 108441732A CN 201810260324 A CN201810260324 A CN 201810260324A CN 108441732 A CN108441732 A CN 108441732A
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nano diamond
diamond particle
base compound
preparation
compound material
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CN108441732B (en
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马国俊
金培鹏
赵磊
李尚鹏
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Qinghai University
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Qinghai University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/04Alloys based on magnesium with zinc or cadmium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • C22C1/1047Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes

Abstract

The invention discloses a kind of Nano diamond particle reinforced magnesium base compound materials and preparation method thereof, and the preparation method comprises the following steps:(1) Nano diamond particle is added in ethyl alcohol, then ultrasonic vibration dispersion is stirred, magnesium alloy powder is added while stirring, obtains mixed solution;(2) vacuum drying after mixed solution Centrifugal dispersion is obtained into mixed-powder;(3) mixed-powder is subjected to hot extrusion, obtains presoma bar;(4) another that magnesium alloy powder is taken to carry out melting, it is passed through N in fusion process2And SF6Gaseous mixture is protected, and Matrix Solution is obtained;(5) presoma bar is added in Matrix Solution and is melted, stirred 30min, be then cast into base, hot extrusion obtains As-extruded Nano diamond particle reinforced magnesium base compound material bar.Nano diamond particle is evenly distributed in magnesium alloy substrate in composite material prepared by the present invention, and there is effective interface cohesion, mechanical property to significantly improve.

Description

A kind of Nano diamond particle reinforced magnesium base compound material and preparation method thereof
Technical field
The present invention relates to field of material technology, more particularly to a kind of Nano diamond particle reinforced magnesium base compound material and its Preparation method.
Background technology
Magnesium alloy has high specific strength, high-damping, a series of excellent characteristics such as excellent electromagnetic wave shielding, in army Thing, aerospace and industrial circle are gradually widely used.But for magnesium-based composite material, by selecting each The hard reinforcement that aspect is had excellent performance is added in metallic matrix, then when suitable technique being selected to be prepared, and can be obtained Compared to the more excellent composite material of matrix alloy comprehensive performance.
In the research of early period, researcher has selected different types of material as reinforcement, has carried out composite material Preparation, including SiC micron particles, antifungin/al whisker etc., during selective enhancement body, primary consideration factor is The compatibility of reinforcement and matrix, i.e. crucial interfacial effect;No matter which kind of preparation method is used, will ensure reinforcement and base The effective interface of body combines, rather than generates other negative effects, as the chemical reaction of reinforcement and matrix generates brittleness production Object or reinforcement just do not realize effective interface cohesion with matrix.Because for metal-base composites, interface exists Play vital role in the performance of material.The reinforcing effect of material is depended on effectively to be passed by interface progress load It passs.Toughness is influenced by interface crack deflection, and plasticity is similarly subjected to the release of interface vicinity peak stress.Chu et al. When studying carbon nanotube reinforced copper-base composite material, nanotube and matrix copper are effectively improved by incorporating metal chromium The performance of interface bonding state, material significantly improves.
Next, is exactly the uniformly dispersed of reinforcement, and the dispersibility of heterogeneous reinforcement is very crucial to the performance of material.It is logical Include stirring casting frequently with different preparation processes, method of impregnation, the effectively dispersion reinforcement such as powder metallurgic method is in the base Distribution.But for nano particle, due to existing Van der Waals force between sub-micron-powder, electrostatic attraction, what image force generated The factors such as electrostatic attraction and liquid bridge power easily generate reunion.
Therefore, during preparing nano particle enhanced magnesium-based composite material, it should ensure these ultra-fine reinforcements Grain can effectively be disperseed in the base, ensured to realize effective interface cohesion between reinforcement and matrix again, just must Corresponding technique is targetedly taken, to which qualified material be prepared, to meet its application under actual state.
Invention content
In order to solve problems in the prior art, it is multiple that an embodiment of the present invention provides a kind of Nano diamond particle reinforced Mg-bases The preparation method of condensation material.The technical solution is as follows:
On the one hand, a kind of preparation method of Nano diamond particle reinforced magnesium base compound material, includes the following steps:
(1) Nano diamond particle is added in ethyl alcohol, then ultrasonic vibration dispersion is stirred, is added while stirring Magnesium alloy powder obtains mixed solution;
(2) vacuum drying after mixed solution Centrifugal dispersion that step (1) obtains is obtained into mixed-powder;
(3) mixed-powder for obtaining step (2) carries out hot extrusion, obtains presoma bar;
(4) another that magnesium alloy powder is taken to carry out melting, it is passed through N in fusion process2And SF6Gaseous mixture is protected, and matrix is obtained Solution;
(5) presoma bar prepared by step (3) is added in Matrix Solution and is melted, stirred 30min, be then cast into Base, hot extrusion obtain As-extruded Nano diamond particle reinforced magnesium base compound material bar.
Further, by quality ratio, the magnesium alloy powder total amount used in step (1) and step (4):Nano diamond Grain=100:1.
Further, the magnesium alloy powder used in step (1) and step (4) is Mg-Zn-Zr alloy powders, wherein including 5.1wt% zinc and 0.18wt% zirconiums, remaining is magnesium.
Further, the extrusion ratio of hot extrusion is 15 in step (5):1, squeeze temperature 523K.
Further, the extrusion ratio of hot extrusion is 15 in step (3):1, temperature 523K is squeezed, after hot extrusion Obtain the presoma bar of diameter 24mm.
Further, the rotating speed of Centrifugal dispersion is 5000r/min, centrifugation time 15min in step (2).
Further, speed of agitator is 300r/min in step (1).
Further, drying temperature 333K, drying time 3h in step (2).
Further, ultrasonic time 30min in step (1).
On the other hand, a kind of Nano diamond particle reinforced magnesium base compound material contains nanogold by percentage to the quality Hard rock 0.1%, zinc 5.1%, zirconium 0.18%, remaining is magnesium.
The advantageous effect that technical solution provided in an embodiment of the present invention is brought is:The Nano diamond particle enhancing of the present invention Magnesium-based composite material and preparation method thereof realizes that nano particle is uniform in magnesium alloy substrate using powder metallurgy preparation technique Dispersion;For the nanometer reinforcement particle for being easy to reunite, using the processing method disperseed in the liquid phase;Melting processing The interface cohesion problem of nano particle and reinforcement particle.In the Nano diamond particle reinforced magnesium base compound material being prepared Nano diamond particle is evenly distributed in magnesium alloy substrate, and there is effective interface cohesion, mechanical property to significantly improve.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for For those of ordinary skill in the art, without creative efforts, other are can also be obtained according to these attached drawings Attached drawing.
Fig. 1 is magnesium alloy powder granule-morphology figure in the embodiment of the present invention;
Fig. 2 is Nano diamond particle surface shape appearance figure in the embodiment of the present invention;
Fig. 3 is scatter diagram of the Nano diamond particle in matrix magnesium alloy in the embodiment of the present invention;
Fig. 4 is Nano diamond particle in the embodiment of the present invention, matrix magnesium alloy and precipitated phase MgZn2Alternate interface knot Close figure.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention Formula is described in further detail.
Embodiment
The Nano diamond particle reinforced magnesium base compound material of the present invention is prepared with the following method:
It weighs 0.1g Nano diamond particles to be added in ethyl alcohol, ultrasonic vibration disperses 30min, then fills using mechanical agitation It sets and is stirred, speed of agitator 300r/min is added 25g magnesium alloy powders, obtains mixed solution while stirring.
By mixed solution with 5000r/min, Centrifugal dispersion 15min, then dried with temperature 333K in vacuum drying oven 3h obtains mixed-powder.
Mixed-powder is added in extrusion die and carries out hot extrusion, extrusion ratio 15:1, squeeze temperature 523K, hot extrusion The presoma bar of diameter 24mm is obtained after processing.
Melting is carried out to remaining 75g magnesium alloy powders in smelting furnace, N is passed through in fusion process2And SF6Gaseous mixture into Row protection is handled, and is gradually started to stir after magnesium alloy powder is at liquid state, is obtained Matrix Solution.
Presoma bar is added in Matrix Solution and is melted, continues to stir 30min, is then cast into base, further hot extrusion Pressure processing, extrusion ratio 15:1, temperature 523K is squeezed, As-extruded Nano diamond particle reinforced magnesium base compound material bar is obtained.
Use magnesium alloy powder (Mg-Zn-Zr) as matrix in present invention experiment, 50 μm of powder size, primary chemical at It is divided into 5.1wt%Zn, 0.18wt%Zr, macroscopic view and microscopic appearance are as shown in Figure 1.Nano diamond particle is reinforcement, granularity Size is 6.7nm, and microstructure is as shown in Figure 2.
Structure observation is carried out to the As-extruded Nano diamond particle reinforced magnesium base compound material bar that experiment is prepared And Mechanics Performance Testing.The dispersibility (Fig. 3) of reinforcement particle in the base is analyzed by scanning electron microscope (SEM), passes through transmission The interface cohesion behavior (Fig. 4) of Electronic Speculum (TEM) observation analysis matrix and nano particle.The Nano diamond particle that will be prepared Enhancing magnesium-based composite material is processed into standard tensile, compression sample, has carried out stretching on electronic universal material experiment-machine, compress Test experiments, and obtain corresponding material mechanical performance.
As seen from Figure 3, nano particle has obtained highly uniform distribution in the base, thus also indicates that the ultrasound point at initial stage Dissipating the techniques such as processing effectively realizes reinforcement being uniformly distributed in the base.
It is non-coherent structural, nevertheless, by scheming by Fig. 4 a as it can be seen that occurring wrong row between Nano diamond particle and matrix 4b can see, the MgZn being precipitated in Nano diamond particle and matrix2Mutually complete coherence realizes effective interface cohesion. The non-coherent structural of Nano diamond particle and matrix alloy, it is meant that matrix and Nano diamond particle combination effect are poor, no The effects such as effective load transmission can be realized, nevertheless, the second phase MgZn being precipitated in matrix2Mutually with Nano diamond with altogether Lattice structure matching, this also from connect it is effective realize the Nano diamond particle that is added in experiment can with matrix in addition to Except effective dispersion, while it can realize and be effectively combined, so as to effectively material be hindered to be moved in deformation process Dislocation, and significantly realize the reinforcing of composite property.
It can be seen that preparation process through the invention, efficiently solves Nano diamond particle reinforced Mg-base composite wood The technology of preparing problem of material.Although it is only 0.1wt%, the comprehensive mechanical property of material to be added to Nano diamond granule content But it is significantly improved.The mechanical property of Nano diamond particle reinforced magnesium base compound material is as shown in table 1.
1 Nano diamond particle reinforced magnesium base compound material mechanical property table of table
Material σ0.2/MPa σb/MPa δ (%) CYS(MPa) UCS(MPa) δ (%)
ZK60 339.1 368. 10.2 300 527 16.8
0.1%ND/ZK60 390.3 418.4 6.2 433 484 10.1
By table 1 as it can be seen that comparing matrix alloy, the mechanical property of Nano diamond particle reinforced magnesium base compound material obtains Significant to improve, tensile yield strength increases to 390.3MPa from 339.1MPa, while the stretch percentage elongation of material is not notable It reduces, stills remain in 6.2%;Compression yield strength (compression yield stress, CYS) is carried compared to matrix alloy It is high by nearly 30%;Simultaneously, asymmetry is surrendered in the significant tension and compression that the magnesium alloy prepared compared to traditional handicraft is shown (asymmetry is surrendered in tension and compression to feature:That is compression yield strength and tensile yield strength ratio).The nanometer obtained through the invention Diamond particles enhancing magnesium-based composite material tension and compression surrender asymmetry obtains the improvement of highly significant, i.e., compression yield strength with Tensile yield strength ratio reaches 1.11, and the improvement of this respect performance will be to this material in Practical Project condition, especially It is the magnesium alloy materials of tension and compression load to be recycled by high intensity, such as the application of crossbeam component will play very crucial effect.
The Nano diamond particle reinforced magnesium base compound material and preparation method thereof of the present invention, in order to realize that nano particle exists It is evenly dispersed in magnesium alloy substrate, use powder metallurgy preparation technique;The reinforcement particle of conventional micron grade size is usual It is to realize that the evenly dispersed of reinforcement mixes by way of carrying out ball-milling treatment with matrix alloy powder, and roll into a ball for easy Poly- nanometer reinforcement particle uses the mode for carrying out decentralized processing in the liquid phase, i.e., soaks superfine powder in the liquid phase, Then carry out ultrasonic disperse and centrifugal mixer processing so that the powder reunited together is opened under these active forces, is formed Independent primary partical or smaller aggregate, and enter magnesium alloy powder by amount addition in the later stage, realize uniformly mixing, then It dries again, extrusion process obtains blank;For the interface cohesion problem of nano particle and reinforcement particle, then take molten Melt processing mode, i.e., matrix magnesium alloy is heated to fusing point or more, using N2And SF6Gas shield is handled, and stirring simultaneously will early period system Standby blank incorporates in matrix, casts after stirring evenly, desired material is prepared.The Nano diamond particle being prepared Nano diamond particle is evenly distributed in magnesium alloy substrate in enhancing magnesium-based composite material, has effective interface cohesion, power Performance is learned to significantly improve.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.

Claims (10)

1. the preparation method of Nano diamond particle reinforced magnesium base compound material, which is characterized in that include the following steps:
(1) Nano diamond particle is added in ethyl alcohol, then ultrasonic vibration dispersion is stirred, magnesium is added while stirring and closes Bronze end, obtains mixed solution;
(2) vacuum drying after the mixed solution Centrifugal dispersion that step (1) obtains is obtained into mixed-powder;
(3) mixed-powder for obtaining step (2) carries out hot extrusion, obtains presoma bar;
(4) another that magnesium alloy powder is taken to carry out melting, it is passed through N in fusion process2And SF6Gaseous mixture is protected, and it is molten to obtain matrix Liquid;
(5) the presoma bar prepared by step (3) is added in described matrix solution and is melted, stirred 30min, then cast At base, hot extrusion obtains As-extruded Nano diamond particle reinforced magnesium base compound material bar.
2. the preparation method of Nano diamond particle reinforced magnesium base compound material as described in claim 1, which is characterized in that with Mass ratio meter, the magnesium alloy powder total amount used in the step (1) and step (4):Nano diamond particle=100:1.
3. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 2, which is characterized in that institute It is Mg-Zn-Zr alloy powders to state magnesium alloy powder used in step (1) and step (4), wherein comprising 5.1wt% zinc and 0.18wt% zirconiums, remaining is magnesium.
4. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 3, which is characterized in that institute The extrusion ratio for stating hot extrusion in step (5) is 15:1, squeeze temperature 523K.
5. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 4, which is characterized in that institute The extrusion ratio for stating hot extrusion in step (3) is 15:1, temperature 523K is squeezed, before obtaining diameter 24mm after hot extrusion Drive body bar.
6. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 5, which is characterized in that institute The rotating speed for stating Centrifugal dispersion in step (2) is 5000r/min, centrifugation time 15min.
7. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 6, which is characterized in that institute It is 300r/min to state speed of agitator in step (1).
8. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 7, which is characterized in that institute State drying temperature 333K, drying time 3h in step (2).
9. the preparation method of Nano diamond particle reinforced magnesium base compound material as claimed in claim 8, which is characterized in that institute State ultrasonic time 30min in step (1).
10. a kind of Nano diamond particle reinforced magnesium base compound material, which is characterized in that by percentage to the quality, contain nanometer Diamond 0.1%, zinc 5.1%, zirconium 0.18%, remaining is magnesium.
CN201810260324.7A 2018-03-27 2018-03-27 Nano-diamond particle reinforced magnesium-based composite material and preparation method thereof Active CN108441732B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110551909A (en) * 2019-09-30 2019-12-10 青海大学 Method for improving heat conductivity of magnesium-based composite material by using nano diamond and magnesium-based composite material
CN113732311A (en) * 2021-09-03 2021-12-03 长沙学院 Nano-diamond enhanced biological magnesium alloy and preparation method thereof
CN114632937A (en) * 2022-03-07 2022-06-17 青海大学 High-strength ZK60 magnesium alloy, magnesium-based composite material and preparation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1441075A (en) * 2003-04-03 2003-09-10 上海交通大学 Prepn process of particle-reinforced Mg-base composite mateiral
CN105624457A (en) * 2016-03-22 2016-06-01 北京工业大学 Graphene enhanced magnesium-based composite and preparing method thereof
CN107653409A (en) * 2017-09-19 2018-02-02 安徽恒利增材制造科技有限公司 A kind of high intensity zinc-aluminium magnesium alloy ingot and preparation method thereof
CN107675056A (en) * 2017-09-19 2018-02-09 安徽恒利增材制造科技有限公司 A kind of high-strength aluminium-magnesium alloy cast ingot and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1441075A (en) * 2003-04-03 2003-09-10 上海交通大学 Prepn process of particle-reinforced Mg-base composite mateiral
CN105624457A (en) * 2016-03-22 2016-06-01 北京工业大学 Graphene enhanced magnesium-based composite and preparing method thereof
CN107653409A (en) * 2017-09-19 2018-02-02 安徽恒利增材制造科技有限公司 A kind of high intensity zinc-aluminium magnesium alloy ingot and preparation method thereof
CN107675056A (en) * 2017-09-19 2018-02-09 安徽恒利增材制造科技有限公司 A kind of high-strength aluminium-magnesium alloy cast ingot and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110551909A (en) * 2019-09-30 2019-12-10 青海大学 Method for improving heat conductivity of magnesium-based composite material by using nano diamond and magnesium-based composite material
CN113732311A (en) * 2021-09-03 2021-12-03 长沙学院 Nano-diamond enhanced biological magnesium alloy and preparation method thereof
CN114632937A (en) * 2022-03-07 2022-06-17 青海大学 High-strength ZK60 magnesium alloy, magnesium-based composite material and preparation method

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