CN104630662A - Carbon nano tube reinforced Mg-Ni based amorphous composite material and preparation method thereof - Google Patents
Carbon nano tube reinforced Mg-Ni based amorphous composite material and preparation method thereof Download PDFInfo
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- CN104630662A CN104630662A CN201510043687.1A CN201510043687A CN104630662A CN 104630662 A CN104630662 A CN 104630662A CN 201510043687 A CN201510043687 A CN 201510043687A CN 104630662 A CN104630662 A CN 104630662A
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Abstract
The invention relates to a carbon nano tube reinforced Mg-Ni based amorphous composite material and a preparation method thereof and belongs to the technical field of metal alloy composite materials. The amorphous composite material provided by the invention takes Mg-Ni as major elements and comprises the ingredients as follows: (carbon nano tube)X-(Mg69Ni15Gd10Ag6)100-X. The preparation method comprises the following steps: smelting Ni, Gd and Ag into a Ni15Gd10Ag6 ternary intermediate alloy ingot; mixing the intermediate alloy ingot and a corresponding amount of metal Mg, and performing smelting to obtain a Mg69Ni15Gd10Ag6 master alloy; and grinding the master alloy into alloy powder, mixing the alloy powder and carbon nano tube particles, and performing smelting and die casting to obtain the carbon nano tube reinforced Mg-Ni based amorphous composite material with the ingredients of (carbon nano tube)X-(Mg69Ni15Gd10Ag6)100-X. The carbon nano tube reinforced Mg-Ni based amorphous composite material prepared according to the method has the advantages of high amorphous forming capability, higher strength and better toughness than a simplex Mg based amorphous alloy, and the like, so that Mg based bulk amorphous composite materials have wide application prospects in the fields of novel light-weight structural materials and the like.
Description
Technical field
The present invention relates to a kind of carbon nanotube and strengthen Ni-based amorphous composite of magnesium and preparation method thereof, belong to metal alloy technical field of composite materials.
Background technology
Developing rapidly of the industry such as automobile and space flight and aviation proposes requirements at the higher level to lightweight alloy, and lightweight requirements light metal alloy has high strength and high tenacity.Owing to having the weird atom arrangement architecture being different from crystal, non-crystalline material shows superelevation that traditional material cannot realize than specific performances such as strong, superelevation solidity to corrosion, low thermal coefficient of expansion.In addition amorphous material has excellent supercooled liquid precise forming, can realize the short route precision sizing of Irregular Shaped Parts, be subject to investigator's extensive concern.As high performance light material, bulk amorphous alloy has great application potential in leading-edge fields such as aerospacecrafts.Now, mainly concentrate on the essence of amorphous structure and Composition Design, amorphous material highly malleablized, amorphous material superplasticity around the fundamental research of non-crystalline material to process and the aspect such as precise form.Compared with other alloy system non-crystaline amorphous metal, magnesium base block amorphous alloy quality is light, low price, is the excellent candidate of high specific strength alloy, has a extensive future.At present, the research of magnesium base block amorphous alloy mainly concentrates on based on the cupric system of Mg-Cu-RE (RE is rare earth etc.).On the one hand, although have developed the series bulk amorphous alloying constituent of a large amount of Mg-Cu, in this individual system non-crystaline amorphous metal, Mg content is lower, generally lower than 65at.%, weakens the low-density advantage of magnesium alloy.Research shows, amorphous magnesium nickel system alloy has excellent hydrogen storage property and chemical property.Many researchers has done large quantity research in the preparation and property of magnesium nickel base alloys material, and achieves good achievement.But magnesium is base block amorphous is almost fragility soprano in all amorphous alloys, report display, the fracture toughness property K of Mg base non-crystalline material
i cbe low to moderate 2.0MPam
1/2, close to desirable fragility silicate glass, become the bottleneck problem of application further.Therefore, the obdurability that Mg base non-crystalline material toughening mechanisms is not only conducive to improving Mg base non-crystalline material itself is studied.Simultaneously also for the underlying issues such as research hard brittle material ruptures and toughness reinforcing provide ideal model.
Investigator finds, additional second-phase can be utilized to hinder the expansion of shear zone, promotes the formation of multiple shear bands, thus strengthens the obdurability of non-crystalline material.Compared with other wild phase, carbon nanotube has very excellent over-all properties, is desirable second-phase.Carbon nanotube is hollow seamless tubulose structure, has lower density (1.35g/cm
3left and right) and good structural stability; Thermostability is strong, and in below 973K temperature, carbon nanotube does not change in atmosphere substantially; Theoretical Calculation shows, the Young's modulus average out to 1.8TPa of carbon nanotube, and tensile strength is 100 times (being more than 20 times of high-strength carbon fiber) of steel, and flexural strength is 14.2GPa.Carbon nanotube, by as wild phase, has carried out large quantity research in the crystalline state matrix materials such as Fe base, Al base, Cu base and Ni base.
Therefore, the carbon nanotube developing high-strong toughness strengthens Mg base amorphous composite and has important Research Significance.
Summary of the invention
The object of the invention is to propose a kind of carbon nanotube and strengthen Ni-based amorphous composite of magnesium and preparation method thereof, by adding carbon nanotube, prepare the base block amorphous matrix material of magnesium, to overcome the too low problem of current magnesium base amorphous alloy toughness, enrich amorphous alloy component system, obtain the amorphous composite with high amorphous formation ability, high strength and higher toughness.
The carbon nanotube that the present invention proposes strengthens the Ni-based amorphous composite of magnesium, and take Mg-Ni as principal element, its composition is (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-X, wherein X is the volume percent of carbon nanotube, X=1 ~ 10.
The carbon nanotube that the present invention proposes strengthens the preparation method of the Ni-based amorphous composite of magnesium, comprises the following steps:
(1) after W metal, Gd and Ag being weighed according to mass percent 28.4%:50.7%:20.9%; mutual mixing; it is melting 30 seconds at 2700 DEG C in the high-purity argon gas protective atmosphere of 99.99% in purity; protective atmosphere pressure is 0.8 normal atmosphere; melting limit, limit induction stirring; to ensure alloy uniformity, it is Ni that cooling obtains composition
15gd
10ag
6ternary intermediate alloy ingot;
(2) mix with the metal M g phase of respective quality after ternary intermediate alloy ingot fragmentation above-mentioned steps (1) obtained, in induction furnace, melting obtains composition is Mg
69ni
15gd
10ag
6master alloy ingot;
(3) master alloy ingot prepared by above-mentioned steps (2) is worn into the powdered alloy that particle diameter is less than or equal to 1 millimeter, powdered alloy is mixed mutually with carbon nanotube particulate, volume ratio shared by carbon nanotube particulate is 1 ~ 10%, by stirring and ultrasonic vibration, powdered alloy and carbon nanotube particulate are mixed, obtains mixture;
(4) mixture of step (3) is pressed into block under 10 normal atmosphere, by block 800 DEG C of meltings 20 seconds, obtain blend melt, by blend melt die casting in metal mold cavity, pressure is 0.5MPa, obtains composition for (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-Xthe base block amorphous matrix material of carbon nanotube magnesium.
The carbon nanotube that the present invention proposes strengthens the preparation method of the Ni-based amorphous composite of magnesium, its advantage is, the Ni-based amorphous composite of the magnesium prepared by the inventive method, there is high amorphous formation ability, than simple Mg base noncrystal alloy, there is the advantages such as higher intensity and better toughness, the base block amorphous matrix material of magnesium is had broad application prospects in fields such as novel light structured materials.
Accompanying drawing explanation
Fig. 1 is comparative example Mg
69ni
15gd
10ag
6(carbon nanotube) that non-crystaline amorphous metal and the present invention propose
x-(Mg
69ni
15gd
10ag
6)
100-Xthe X-ray diffraction analysis collection of illustrative plates of amorphous composite, wherein X=1-4.
Fig. 2 is comparative example Mg
69ni
15gd
10ag
6(carbon nanotube) that non-crystaline amorphous metal and the present invention propose
x-(Mg
69ni
15gd
10ag
6)
100-Xthe differential scanning calorimetry curve of amorphous composite, wherein X=1-4.
Fig. 3 is carbon nanotube existence schematic diagram in the composite in the embodiment of the present invention.
Fig. 4 is comparative example Mg
69ni
15gd
10ag
6(carbon nanotube) prepared by non-crystaline amorphous metal and the inventive method
x-(Mg
69ni
15gd
10ag
6)
100-X(X=1-4) the stress-strain curve comparison diagram of amorphous composite.
Embodiment
The carbon nanotube that the present invention proposes strengthens the Ni-based amorphous composite of magnesium, and take Mg-Ni as principal element, its composition is (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-X, wherein X is the volume percent of carbon nanotube, X=1 ~ 10.Wherein the purity of each metallic element is not less than 99.9%, and carbon nanotube is chemical Vapor deposition process preparation, and many wall-shaped, purity is more than 95%.
The carbon nanotube that the present invention proposes strengthens the preparation method of the Ni-based amorphous composite of magnesium, comprises the following steps:
(1) after W metal, Gd and Ag being weighed according to mass percent 28.4%:50.7%:20.9%; mutual mixing; it is melting 30 seconds at 2700 DEG C in the high-purity argon gas protective atmosphere of 99.99% in purity; protective atmosphere pressure is 0.8 normal atmosphere; melting limit, limit induction stirring; to ensure alloy uniformity, it is Ni that cooling obtains composition
15gd
10ag
6ternary intermediate alloy ingot;
(2) mix with the metal M g phase of equal in quality after ternary intermediate alloy ingot fragmentation above-mentioned steps (1) obtained, in induction furnace, melting obtains composition is Mg
69ni
15gd
10ag
6master alloy ingot;
(3) master alloy ingot prepared by above-mentioned steps (2) is worn into the powdered alloy that particle diameter is less than or equal to 1 millimeter, powdered alloy is mixed mutually with carbon nanotube particulate, volume ratio shared by carbon nanotube particulate is 1 ~ 10%, by stirring and ultrasonic vibration, powdered alloy and carbon nanotube particulate are mixed, obtains mixture;
(4) mixture of step (3) is pressed into block under 10 normal atmosphere, by block 800 DEG C of meltings 20 seconds, obtain blend melt, by blend melt die casting in metal mold cavity, pressure is 0.5MPa, obtains composition for (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-Xthe base block amorphous matrix material of carbon nanotube magnesium.
In preparation method of the present invention, the melting of W metal, Gd and Ag can in electric arc furnace, and protective atmosphere can be high-purity argon gas, and protective atmosphere pressure is 0.8 normal atmosphere, and temperature is 2700-3000 DEG C, and the used time is about 30s.Cooling obtains ternary intermediate alloy ingot-Ni
15gd
10ag
6.Alloy melt back 3-4 time in fusion process, and in melting, adopt induction stirring, to ensure alloy uniformity; The high-purity argon gas protection of purity 99.99% is filled with after vacuumizing before melting.Ternary intermediate alloy ingot Ni
15gd
10ag
6with the melting of Mg after broken, can use ceramic crucible, smelting temperature is 700-1000 DEG C, and the time is 10-15min, melting obtain last needed for the master alloy ingot-Mg of uniform composition
69ni
15gd
10ag
6.Final mixture is pressed into block, metal mold differential pressure die-casting system can be used, pressure system adopts hydraulic drive, and temperature is at 800-1000 DEG C, and smelting time is 20s, powdered block is fused into liquid, negative pressure is filled with and is opened, and melting cavity is taken out negative pressure, and hydraulic efficiency system is opened, from top by quick for liquid die casting to metal mold cavity, obtain the base block amorphous matrix material of carbon nanotube magnesium (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-X.The metal die used is water-cooled copper mold.
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated: the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
In embodiment 1-5, embodiment 1 is comparative example of the present invention, prepares the Mg that diameter is 3.0mm
69ni
15gd
10ag
6non-crystaline amorphous metal, embodiment 2-5 is preparations (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-Xblock (X=1,2,3,4) amorphous composite.
Use material purity>=99.9% Mg, Ni, Gd, Ag in mass ratio 35.1%:18.4%:32.9%:13.6% prepare mother alloy-Mg
69ni
15gd
10ag
6.Add purity >=95%, many wall-shaped carbon nanotube, prepare the base block amorphous matrix material of final magnesium.
First Ni, Gd, Ag are prepared burden according to mass percent 28.4%:50.7%:20.9%, in electric arc furnace, melting obtains the intermediate alloy ingot of uniform composition.Before melting, electric arc furnace cavity is evacuated to 1.2 × 10
-30.8 atmospheric high-purity argon gas is filled with as shielding gas after Pa.First fusion process wants the little ingot casting of the pure titanium of melting; titanium has stronger bonding force with oxygen, can be further purified shielding gas like this, will overturn before each melting to master alloy; by electric arc and electromagnetism, metal liquid is stirred in fusion process, to guarantee intermediate alloy ingot-Ni
15gd
10ag
6uniform composition.The intermediate alloy ingot-Ni that arc melting obtains
15gd
10ag
6surface finish clean and broken after mix according to mass percent 64.9%:35.1% with pure MAGNESIUM METAL, together put into crucible.In induction melting furnace, carry out induction melting, vacuumize before melting and reach 1.2 × 10
-3be filled with high-purity argon gas protection after Pa, obtain master alloy ingot-Mg by the mode of induction melting
69ni
15gd
10ag
6.
Secondly under the protection of high-purity argon gas, master alloy ingot is ground into small-particle, clays into power in ball mill, then add different volumes mark (1-4vol.%) through pretreated carbon nanotube.Wherein in embodiment 1, be the non-crystaline amorphous metal-Mg not adding carbon nanotube
69ni
15gd
10ag
6, as a comparison case.Master alloy powder mixes with the mode of ultrasonic vibration by stirring with carbon nanotube, is pressed into column, melts in the pressure chamber of differential pressure die casting equipment.Vacuumize in differential pressure die casting equipment cavity in advance before melting, vacuum tightness is filled with high-purity argon gas after reaching requirement; Adopt induction heating fusing mother alloy, then by solidification forming in quick for aluminium alloy die casting to mould (logical recirculated cooling water) die cavity; While die casting, open the negative-pressure cup be connected with mold cavity, make to produce negative pressure in die cavity.So just, can obtain (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-Xprepared by bulk amorphous composite materials.
Detect and differential scanning calorimetric analysis test through X-ray diffraction, the 3mm barred body of preparation is amorphous structure, and sample X ray diffracting spectrum is shown in Fig. 1, and differential scanning calorimetric analysis curve is shown in Fig. 2.Fig. 3 to be volume percent be 3% the distribution situation of carbon nanotube in amorphous composite.The stress-strain curve of this matrix material is shown in Fig. 4.The bulk amorphous composite materials thermomechanical property that the present embodiment obtains is as shown in table 1, comprises amorphous transition temperature T
g, crystallization temperature T
x, fusing point T
m, liquidus temperature T
l, reduced glass transition temperature T
rg(=T
g/ T
m), supercooling liquid phase region width Delta T
x(=T
x– T
g), γ=T
x/ (T
l+ T
g).
The block amorphous alloy thermomechanical property of table 1. embodiment 1-5
| Embodiment is numbered | Carbon nanotube (vol.%) | T g(K) | T x(K) | T m(K) | T l(K) | γ | T rg | ΔT x(K) |
| 1 | 0 | 417.4 | 471.6 | 673.8 | 702.4 | 0.421 | 0.594 | 54.2 |
| 2 | 1 | 418.3 | 472.9 | 682.3 | 702.4 | 0.422 | 0.596 | 54.6 |
| 3 | 2 | 421.6 | 473.0 | 678.2 | 704.2 | 0.420 | 0.599 | 51.4 |
| 4 | 3.0 | 416.2 | 468.2 | 681.5 | 706.4 | 0.417 | 0.589 | 52.0 |
| 5 | 4 | 415.5 | 459.4 | 682.4 | 706.1 | 0.410 | 0.588 | 43.9 |
From table 1, data are known, (carbon nanotube) provided by the present invention
x-(Mg
69ni
15gd
10ag
6)
100-Xbulk amorphous composite materials has higher supercooled liquid phase sector width, and the interpolation of a small amount of carbon nanotube can make amorphous formation ability effectively improve, and suitable carbon nanotube adds can not affect magnesium base amorphous Forming ability.
The bulk amorphous composite materials mechanical property that comparative example of the present invention and embodiment 5 obtain is as shown in table 2, comprises breaking tenacity σ
f, elastic deformation amount ε
e, amount of plastic deformation ε
p, density p and stronger per mass unit σ
f/ ρ.
The mechanical property of non-crystal alloy of table 2. embodiment 1-5
| Embodiment is numbered | Carbon nanotube (vol.%) | σ f(MPa) | ε e(％) | ε p(％) | ρ(g/cm3) | σ f/ρ(kN·m·kg-1) |
| 1 | 0 | 830 | 1.79 | 0.12 | 4.11 | 202 |
| 2 | 1 | 865 | 2.05 | 0.27 | 4.09 | 211 |
| 3 | 2 | 927 | 2.12 | 0.35 | 3.98 | 233 |
| 4 | 3 | 1015 | 2.25 | 0.42 | 3.9 | 260 |
| 5 | 4 | 809 | 2.04 | 0.38 | 3.83 | 211 |
From table 2, data are known, and bulk amorphous composite materials provided by the present invention has more excellent mechanical property than simple magnesium base amorphous alloy.But when content of carbon nanotubes is too high, there will be a large amount of crystal phases, thus reduce mechanical property, therefore, select suitable carbon nanotube addition most important.
In one embodiment of the present of invention, the carbon nanotube of use utilizes chemical Vapor deposition process to prepare by Tsing-Hua University's Materials Academy nano material machining experiment room, and many wall-shaped, purity is more than 95%.
Claims (2)
1. carbon nanotube strengthens the Ni-based amorphous composite of magnesium, and it is characterized in that the Ni-based amorphous composite of this magnesium take Mg-Ni as principal element, its composition is (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-X, wherein X is the volume percent of carbon nanotube, X=1 ~ 10.
2. carbon nanotube as claimed in claim 1 strengthens a preparation method for the Ni-based amorphous composite of magnesium, it is characterized in that preparation method comprises the following steps:
(1) after W metal, Gd and Ag being weighed according to mass percent 28.4%:50.7%:20.9%; mutual mixing; it is melting 30 seconds at 2700 DEG C in the high-purity argon gas protective atmosphere of 99.99% in purity; protective atmosphere pressure is 0.8 normal atmosphere; melting limit, limit magnetic stirs; to ensure alloy uniformity, it is Ni that cooling obtains composition
15gd
10ag
6ternary intermediate alloy ingot;
(2) mix with the metal M g phase of equal in quality after ternary intermediate alloy ingot fragmentation above-mentioned steps (1) obtained, in induction furnace, melting obtains composition is Mg
69ni
15gd
10ag
6master alloy ingot;
(3) master alloy ingot prepared by above-mentioned steps (2) is worn into the powdered alloy that particle diameter is less than or equal to 1 millimeter, powdered alloy is mixed mutually with carbon nanotube particulate, volume ratio shared by carbon nanotube particulate is 1 ~ 10%, by stirring and ultrasonic vibration, powdered alloy and carbon nanotube particulate are mixed, obtains mixture;
(4) mixture of step (3) is pressed into block under 10 normal atmosphere, by block 800 DEG C of meltings 20 seconds, obtain blend melt, by blend melt die casting in metal mold cavity, pressure is 0.5MPa, obtains composition for (carbon nanotube)
x-(Mg
69ni
15gd
10ag
6)
100-Xthe base block amorphous matrix material of carbon nanotube magnesium.
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Cited By (2)
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| CN113913709A (en) * | 2021-10-09 | 2022-01-11 | 华中科技大学 | In-situ authigenic hybrid phase reinforced magnesium-based amorphous composite material based on selective phase dissolution and preparation method thereof |
| CN115475947A (en) * | 2022-10-17 | 2022-12-16 | 吉林大学 | Preparation method and application of transition metal carbide particles with {100} crystal face cube surfaces |
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