(2) As for in-situ formed intermetallic compounds reinforced Mg-Al-Zn alloys, friction stir process was used to fabricate bulk multi-element Mg base alloys with different fractions of AZ31 sheets, Al and Zn foils. Multi-passes and high fractions of Al and Zn elements results in apparent grain refinement, proved by the broadening of diffraction peaks and from SEM results. After multi-passes, some intermetallic compound phases were generated. Some intermetallic compounds are quasi-crystals with icosahedral point group symmetry. The average hardness of the multi-element Mg base alloy made by FSP reached nearly 350 in Hv scale, especially in the Mg50Al5Zn45 or Mg37.5Al25Zn37.5 system, due to the generation of intermetallic compounds and grain refinement. With increasing FSP operation to 10 passes, the microstructure and hardness in the stirred zone become much more refined and uniform.
(3) As for Mg based composites reinforced by extrinsic reinforcements, friction stir processing successfully fabricated bulk Mg-AZ31 based composites with 10~20 vol% of nano-ZrO2 particles and 5~10 vol% of nano-SiO2 particles. The distribution of nano-particles after four FSP passes resulted in satisfactorily uniform distribution. The average grain size of the AZ31 matrix of the 4P FSP composites could be effectively refined to 2~4 μm, as compared with the ~6 μm in the FSP AZ31 alloy (without particles) processed under the same FSP condition. The crystalline ZrO2 phase is very stable, no reaction between the ZrO2 and Mg phases occurred during the FSP mixing.
(4) The hardness properties at room temperature of the AZ31 composites with nano-fillers were improved (up to Hv~105), as compared with the AZ31 cast billet (Hv~50). The hardened bulk section or surface layer would greatly improve the wear resistance that is vital for practical applications. The effective hardness of the present particle reinforced composites can be approximately predicted by the iso-stress model when the hardness of
the hard particle is much higher than that of the soft matrix and the volume fraction of the particles is much lower than that of the matrix.
(5) The ultrafine grain size in solid solution hardened AZ31 Mg alloy is successfully achieved by one-pass FSP coupled with rapid heat sink. With proper control of the working temperature history, an ultrafine and uniform grained structure processed by FSP can be achieved. The grain boundaries are well defined and the mean grain size can be refined to 100~300 nm from the initial 75 μm by one single FSP pass. The ultrafine grained structure can drastically increases the microhardness from the initial 50 up to 120 Hv, or an increment factor of 2.4 times. The low working temperature is critical in achieving UFG AZ31 alloy. The estimated high strain rate and low working temperature during FSP with rapid heat sink also agree self-consistently with the achieved ultrafine grains.
(6) The finest grain size ever found in solid solution hardened AZ31 Mg alloy can be achieved by two passes FSP coupled with rapid heat sink. However, the subsequent second pass has lower heat input than first pass. The resulting microstructure exhibits equiaxed grains ranging from 40 nm to 200 nm with an average grain size of less than 100 nm, clearly illustrating that a nanocrystalline structure can be achieved by described two-pass FSP. The nanocrystalline grains can be shown in the TEM observations and the diffraction rings also can be seen in SAD patterns. The highest hardness point can reach
~150 Hv which is equal to triple of the AZ31 matrix, and the mean hardness increase up to around 134 Hv from initial 50 Hv. The process and mechanism of nanocrystallization of AZ31 alloy during the FSP with subsequent second pass is proposed as a two-type recrystallization mechanism.
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Table 1-1 Comparison among Mg alloy, Al alloy, Ti alloy, steel and plastics.
Material Cast Mg
Wrought
Mg Steel Cast Al
Wrought
Al Ti Plastics (PC/ABS) Alloy/
Grade AZ91 AZ31 -H24
Galva-nized A356-T6 6061-T6 Ti-3Al
Dow Pulse 2000 Process/
Product Die cast Sheet Sheet Die cast Extrusion Injection molding Density
(g/cm3) 1.81 1.77 7.80 2.76 2.70 4.2 1.13
Elastic Modulus
(GPa)
45 45 210 72 70 140 2.3 Yield
Strength (MPa)
160 220 200 186 275 925 53 Ultimate
Tensile Strength
(MPa)
240 290 320 262 310 1000 55
Elongation
(%) 3 15 40 5 12 16
5 at yield and 125 at
break Melting
Temp.
(oC)
598 630 1515 615 652 1600 143 (softening
temp.)
Table 1-2 The standard four-part ASTM designation system of alloy and temper for the magnesium alloy [13].
First part Second part Third part Fourth part
Statement
Indicates the two principal alloying element
Indicates the amount of the two principal elements
Distinguishes between different alloys with the same percentage of the two principal alloying elements
Indicates condition (temper)
Method
Consists of two code letters representing the two main alloying elements arranged in order of decreasing percentage (or alphabetically if percentage are equal)
Consists of two numbers corresponding to rounded-off
percentage of the two main alloying
elements and arranged in same designation in first part
Consists of a letter of the alphabet assigned in order as
compositions become standard
Consists of a letter followed by a number ( separated from the third part of the designation by a hyphen
Example
A- Al E- rare earth H- Th K- Zr M- Mn Q- Ag S- Si T-Sn W- Y Z- Zn
Whole numbers Letters of alphabet except I and O
F- as fabricated O- annealed H10 and H11-strain hardened
H23, H24 and H26- strain hardened and partially annealed T4- solution heat treated
T5- artificially aged only
T6- solution heat treated and artificially aged
Table 1-3 The effect of separate solute addition on the mechanical properties [14].
Alloying element
Melting and casting behavior Mechanical and technological properties
Corrosion behavior I/M produced
Ag Improves elevated temperature tensile
and creep properties in the presence of rare earths
Detrimental influence on corrosion behavior
Al Improves castability, tendency to microporosity
Solid solution hardener, precipitation hardening at low temperature (<
120oC)
Minor influence
Be Significantly reduces oxidation of melt surface at very low concentration (< 30 ppm), leads to coarse grains
Ca Effective grain refining effect, slight suppression of oxidation of the molten metal
Improve creep properties Detrimental influence on corrosion behavior
Cu System with easily forming metallic glasses, improves castability
Detrimental influence on corrosion behavior, limitation necessary
Fe Magnesium hardly reacts with mild steel crucibles
Detrimental influence on corrosion behavior, limitation necessary
Li Increases evaporation and burning behavior, melting only in protected and sealed furnaces
Solid solution and precipitation hardening at ambient temperatures, reduce density, enhances ductility
Decreases corrosion properties strongly, coating to protect from humidity is necessary
Mn Control of Fe content by precipitating Fe-Mn compound, refinement of precipitates
Increases creep resistivity Improves corrosion properties due to iron control effect
Ni System with easily forming metallic glasses
Detrimental influence on corrosion behavior, limitation necessary
Rare earth
Improve castability, reduce microporosity
Solid solution and precipitation hardening at ambient and elevated temperatures; improve elevated temperature tensile and creep properties
Improve corrosion behavior
Si Decreases castability, forms stable silicide compounds with many other alloying elements, compatible with Al, Zn and Ag, weak grain refiner
Improve creep properties Detrimental influence
Th Suppresses microporosity Improves elevated temperature tensile and creep properties, improves ductilities, most efficient alloying element
Y Grain refining effect Improves elevated temperature tensile and creep properties
Improves corrosion behavior
Zn Increases Fluidity of the melt, weak grain refiner, tendency to
microporostiy
Precipitation hardening, improves strength at ambient temperatures, tendency to brittleness and hot shortness unless Zn refined
Minor influence, sufficient Zn content compensates for the detrimental effect of Cu
Zr Most effective grain refiner, incompatible with Si, Al and Mn, removes Fe, Al, and Si from the melt
Improves ambient temperature tensile properties slightly
Table 1-4 Mechanical properties of magnesium matrix composites by various processing means.
Magnesium matrix
composites Processing D
(μm) d (μm)
E (GPa)
σ0.2 (MPa)
UTS (MPa)
Hardness (HV)
Elongation
(%) Reference
Pure Mg; 30 vol% SiC casting + extruded 20 40 59 229 258 57 2 [66]
Pure Mg; 4.3 vol% SiC casting -- 25 45 112 191 -- 0.057 [68]
ZK51A; 15 vol% SiCw (whiskers with diameter of 0.3~1 μm and
lengths of 15~50 μm)
squeeze casting -- -- 58 305 325 -- 1.2 [69]
AZ91; Al18B4O33(whiskers with diameter of 0.5~1 μm and lengths
of 10~30 μm)
squeeze casting + 250oC annealing
100 hours -- -- 71 270 368 -- 0.96 [70]
AZ91; 20 vol% SiC with Al(PO3)3
binder (whiskers with diameter of 0.1~1 μm and lengths of 30~100
μm,)
squeeze casting -- -- 85 220 355 175 1.38 [71]
AZ91; 20 vol% SiC without Al(PO3)3 binder (whiskers with diameter of 0.1~1 μm and lengths
of 30~100 μm,)
squeeze casting -- -- 77 202 314 174 1.29 [71]
Pure Mg; 30 vol% Y2O3 casting -- 0.33 -- 268 363 -- 15 [72]
Pure Mg; 30 vol% Y2O3 casting + extruded 0.88 0.33 65 344 455 -- 0 [72]
AZ91; 10 vol% TiC semi-solid slurry stirring -- 5 -- -- 214 83 4 [72]
AZ91; 5 wt% SiC ultrasonic -- 0.03 -- -- -- 135 -- [75]
**D: grain size, d: particle size
Table 1-4 Mechanical properties of magnesium matrix composites by various processing means.
Magnesium matrix
composites Processing D
(μm) d (μm)
E (GPa)
σ0.2 (MPa)
UTS
(MPa) Hardness Elongation
(%) Reference
AZ91; 10 vol% SiC PM + extrusion 17.2 8 58 271 360 -- 3 [76]
AZ91; 10 vol% SiC PM + extrusion 24 30 58 243 350 -- 3 [76]
AZ91; 10 vol% SiC PM + extrusion 28.2 50 58 236 350 -- 2 [76]
Pure Mg; 10 vol % TiB2 PM -- 10 -- -- -- 45 HB -- [77]
Pure Mg; 20 vol % TiB2 PM -- 10 -- -- -- 66 HB -- [77]
Pure Mg; 30 vol % TiB2 PM -- 10 -- -- -- 90 HB -- [77]
Pure Mg; 10 vol % B4C ball milling + PM -- 6 -- -- -- 44 HB -- [78]
Pure Mg; 20 vol % B4C ball milling + PM 6 -- -- -- 133 HB -- [78]
Pure Mg; 0.5 wtl% Al2O3 PM 61 0.05 42.5 169 232 44 HV 6.5 [79]
Pure Mg; 2.5 wt% Al2O3 PM 31 0.05 44.5 194 250 70 HV 6.9 [79]
**D: grain size, d: particle size
Table 1-5 Microstructure-mechanical property and fracture correlations for metal matrix composites [81].
Microstructure condition Mechanical property response
Addition of reinforcement Increase in strength, modulus, fatigue life, creep properties, abrasion resistance, impact strength, high temperature strength, decrease in ductility (elongation to failure), and fracture toughness
Reinforcement type In general, fibrous reinforcements give higher mechanical properties than particulate at equal volume fraction. Particulate reinforcement, however, gives higher elongation to failure and fracture toughness.
Reinforcement orientation Fibrous reinforcement aligned along test axis gives approximately 25%
higher strength than particulate or transverse fibrous reinforcement.
Fatigue and creep properties are improved in aligned fibrous composites.
Ductility and fracture toughness is generally lower in the aligned material.
Reinforcement distribution Banding and or clustering enhances crack initiation and growth, and hence lowers strength, ductility, and toughness.
Particle size Mp effect on modulus; strength properties decrease with particle size increase
Aspect ratio Influence modulus, strength, fracture toughness, ductility and fracture mechanism
Interface condition Strong bonding increases modulus and strength but decreases ductility.
Can be embrittled as a of excessive result of excessive precipitation and/or diffusion of alloying ingredients or impurities to interface
Matrix phases Normal precipitate phases increase yield and ultimate strength. Impurity particles and preferential precipitation decrease strength, fracture toughness, fatigue, creep, and ductility
Heat treatment Heat treatment increases mechanical properties; however, overaging minimizes the benefits. Precipitation kinetics can be altered by the addition of reinforcement; hence time and temperature for peak aging may differ
Secondary processing Secondary processing affects microstructure and hence mechanical properties. Extrusion aligns fibrous reinforcements but induces banding or reinforcements-free areas. Rolling homogenizes microstructure, giving higher properties, but can damage matrix-reinforcement bonds and lead to overaging. Material must be heat-treated to regain properties.
z These comments assume well-bonded reinforcements.