CN1980760A - Magnesium-base composite powder, magnesium-base alloy material and method for production thereof - Google Patents

Magnesium-base composite powder, magnesium-base alloy material and method for production thereof Download PDF

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CN1980760A
CN1980760A CNA2005800225841A CN200580022584A CN1980760A CN 1980760 A CN1980760 A CN 1980760A CN A2005800225841 A CNA2005800225841 A CN A2005800225841A CN 200580022584 A CN200580022584 A CN 200580022584A CN 1980760 A CN1980760 A CN 1980760A
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particle
powder
base
magnesium
press
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近藤胜义
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University of Tokyo NUC
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University of Tokyo NUC
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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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • C22C1/0408—Light metal alloys
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1084—Alloys containing non-metals by mechanical alloying (blending, milling)
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

Magnesium based composite powder that is a starting raw material to manufacture a Mg 2 Si dispersion type of magnesium based composite material comprises Mg based powder (7) that is a main component constituting the matrix of a magnesium alloy, and Mg 2 Si powder attached to the surface of the Mg based powder (7) through a binder (9).

Description

Magnesium base composite powder, the former material of magnesium base alloy and manufacture method thereof
Technical field
The present invention relates to comprise Mg with high rigidity 2The magnesium base composite powder of Si and former material of magnesium base alloy and manufacture method thereof.
Background technology
Magnesium alloy is feature because of its low-gravity with the lightweight effect, mainly obtains extensive goodsization, practicability in the housing of mobile phone and walkman.In the design of goods and parts, except the characteristic of the intensity of former material and this machinery of hardness, rigidity also is important material factor.
For example, when magnesium alloy is applied to automatic transmission (AT) with shell (case), even itself and present employed aluminium alloy (for example ADC12) have under the situation of equal tensile strength and creep strength, the rigidity of original magnesium alloy (Young's modulus) also has only the about about 60% of aluminium alloy, therefore can produce bending, distortion during imposed load under comparable size, wall thickness.Therefore, the problem that still exists in the practicability of magnesium alloy is so far, need carry out the wall thickening design according to goods, the part used, thereby can not get the lightweight effect.
In order to improve the rigidity with the metal material headed by the magnesium alloy, general effective method is to make to have the compound particles dispersion higher than this metal material rigidity, the i.e. utilization of composite.For example, magnesium silicide (Mg 2Si) its Young's modulus is 120GPa since with the Young's modulus of general magnesium alloy (43～44GPa) compare significant big, so in alloy, disperse can expect that rigidity improves in the composite of this particle.
Yet, when making Mg-Si and be alloy by fusion, casting, because there is eutectic point in weight standard in Si content near about 1%, so if when adding Si considerably beyond 1 weight %, the Mg that generates by the reaction of itself and Mg 2Si becomes to look thick.Containing so thick Mg 2In the magnesium alloy of Si, can take place because of concentrating the intensity that causes, the reduction of toughness, and follow the heating that the reaction of Mg and Si brings and have the danger of blast in the fusion processes etc. at the stress of its particle.In addition because of thick Mg 2The Si particle exists, and the casting performance in metal pattern (castability) reduces.Occur in the former material of casting alloy inside and have the such problem of a large amount of defectives and hole.Therefore, AS21 alloy (Mg-2%Al-1%Si) and AS41 alloy (Mg-4%Al-1%Si) etc. be can be with fusion, casting manufacturing contain Mg 2The magnesium alloy of Si.Yet, when the Si that adds about 1 weight %, because the Mg that generates 2It is all about 1% that the volume fraction of Si particle is still not enough, so be difficult to make the rigidity of magnesium alloy to significantly improve.
On the other hand, S.K.THAKUR (source: Metallurgical and MaterialsTransactions A, Vol.35A, March 2004, p.1167-1176) method of Ti Chuing is, be pre-formed the preform (preform) of 3 kinds of mixed-powders curing that will contain the Si powder, contain Mg by molten soaking (infiltration) manufactured that molten magnesium alloy pressurization is made it to soak into simultaneously at this 2The magnesium alloy of Si particle.Yet, in the method, by the Mg alloy of fusion and the synthetic Mg of reaction of Si 2Si with crystal grain-growth, consequently becomes the thick Mg about 70～100 μ m in this course of reaction 2Si is present in the magnesium alloy.This result is the problem that produces on the aforesaid various performances.
The present inventor is willing in 2003-2602 number (application on January 8th, 2003) the spy, discloses a kind of utilization powder metallurgic method and made and be dispersed with Mg 2The technology of the magnesium base composite material of Si particle.Proposed by mechanical bonding or used the bonding method of adhesive at this, made fine Si powder or SiO 2Powder is attached to the magnesium composite powder and the manufacture method thereof on the surface of magnesium base alloy powder.Propose in addition, implement plastic working between temperature, in this process, utilize Mg and Si or SiO for such composite powder 2Solid phase reaction and generate Mg 2The Si particle finally obtains making inside to disperse this Mg equably 2The magnesium base composite material of Si particle.
Be willing to that by the spy magnesium base composite material that disclosed technology obtains in 2003-2602 number demonstrates high-tensile, but need Mg and Si or SiO 2React required high temperature heating (for example about 400～550 ℃).At this moment can be attended by thickization of magnesium crystal grain.If in other words, promptly the low temperatureization of heating-up temperature is effectively in order to realize more high strength, but because the relation of above-mentioned solid phase reaction, for example the low-temperature heatization about 300 ℃ is very difficult.
Summary of the invention
The objective of the invention is to,, also can access and contain Mg in a large number even do not implement the high temperature heating 2The high rigidity of Si particle and high-intensity magnesium alloy.
The present application person to find, to make Mg in order making 2The magnesium base composite material that the Si particle disperses, effectively way is to use in the surface and/or the matrix inside of Mg based powders and has Mg 2The magnesium base composite powder of Si particle.And find not use as the spy and be willing to disclosed Si particle in 2003-2602 number, not to utilize the solid phase reaction of itself and Mg powder to synthesize Mg 2The method of Si particle, but adopt Mg 2The Si particle, and obtain following advantage thus.
(1) do not need to be used to promote that above-mentioned Si-Mg reacts near the high temperature heating required 400～550 ℃, consequently pass through thick, the growth of the Mg crystal grain of inhibition matrix, thereby the intensity that can suppress the basic alloy of Mg reduces.
(2), thereby can suppress Mg by avoiding the heating phenomenon in the Si-Mg course of reaction 2Thickization of Si particle and Mg.
In a word, even do not implement the needed high temperature heating of the solid phase reaction of aforesaid Mg and Si, also can make magnesium base alloy by extrusion process between about 200～400 ℃ temperature.Consequently, can access and contain fine Mg in a large number 2The high rigidity of Si particle and high-intensity magnesium base alloy.
According to magnesium base composite powder of the present invention, have the magnesium based powders and be scattered in either party the magnesium silicide (Mg at least of the surface and the matrix inside of magnesium based powders 2Si).
In above-mentioned magnesium base composite powder, Mg 2The maximum particle of Si directly is below the 50 μ m, is preferably below the 20 μ m, more preferably below the 5 μ m.In addition, with respect to the Mg of this magnesium base composite powder 2The content of Si is preferably 5～60% in volume reference.
According to the former material of magnesium base alloy of the present invention, be that above-mentioned magnesium base composite powder is done the press-powder shaping and carried out sintering, make and be dispersed with Mg in the matrix 2The Si particle.
In one embodiment, the manufacture method according to magnesium base composite powder of the present invention has following operation.
A) prepare magnesium (Mg) based powders and magnesium silicide (Mg 2Si) operation of particle.
B) in the operation of the surperficial coating adhesive of Mg based powders.
C) the Mg based powders and the Mg of adhesive will be coated with 2Si mix particles, stirring make the surface and the Mg of Mg based powders 2The operation of Si particle combination.
In other embodiment, the manufacture method of foundation magnesium base composite powder of the present invention has following operation.
A) prepare magnesium (Mg) based powders and magnesium silicide (Mg 2Si) operation of particle.
B) at allotment Mg based powders and Mg 2Carry out mechanicalness behind the Si particle and mix, make the surface and the Mg of Mg based powders 2The operation of Si particle combination mechanically.
In said method, make the surface and the Mg of Mg based powders 2The Si particle mechanically method of combination is for example to use ball mill, mix mechanically mixing preparation powder such as grater, roller type compacting machine (roller compactor) or roll mill.
In addition in other embodiments, the manufacture method according to magnesium base composite powder of the present invention has following operation.
A) prepare magnesium (Mg) based powders and magnesium silicide (Mg 2Si) operation of particle.
B) mix Mg based powders and Mg 2The operation of Si particle.
C) in metal die, the mixed-powder press-powder is shaped, makes being dispersed with Mg 2The operation of the Mg base press-powder formed body of Si particle.
D) sintering Mg base press-powder formed body makes being dispersed with Mg 2The operation of the Mg base sintered alloy of Si particle.
E) the Mg base sintered alloy is mechanically pulverized or machining and the operation of powder powdered.
In addition in other embodiments, the manufacture method according to magnesium base composite powder of the present invention has following operation.
A) operation of preparation magnesium (Mg) based powders and silicon (Si) particle.
B) operation of mixing Mg based powders and Si particle.
C) in metal die, the mixed-powder press-powder is shaped, makes the operation of the Mg base press-powder formed body that is dispersed with the Si particle.
D) heating Mg base press-powder formed body is by the synthetic Mg of the reaction of Mg and Si 2Si makes simultaneously and is dispersed with Mg 2The operation of the Mg base sintered alloy of Si particle.
E) the Mg base sintered alloy is mechanically pulverized or machining and the operation of powder powdered.
In addition in other embodiments, the manufacture method according to magnesium base composite powder of the present invention has following operation.
A) in magnesium base liquation, drop into magnesium silicide (Mg 2Si) operation of particle and stirring.
B) liquation is cast in mould to make the operation of the former material of casting.
C) to casting that former material is mechanically pulverized or machining and the operation of powder powdered.
In addition in other embodiments, the manufacture method according to magnesium base composite powder of the present invention has following operation.
A) prepare magnesium (Mg) based powders and magnesium silicide (Mg 2Si) operation of particle.
B) mix Mg based powders and Mg 2The operation of Si particle.
C) in metal die, the mixed-powder press-powder is shaped, makes being dispersed with Mg 2The operation of the Mg base press-powder formed body of Si particle.
D) Mg base press-powder formed body is fused, casts, make Mg 2The Si particle disperses the operation of the former material of Mg base casting.
E) the former material of Mg base casting is mechanically pulverized or machining and the operation of powder powdered.
In addition in other embodiments, the manufacture method according to magnesium base composite powder of the present invention has following operation.
A) operation of preparation magnesium (Mg) based powders and silicon (Si) particle.
B) operation of mixing Mg based powders and Si particle.
C) in metal die, the mixed-powder press-powder is shaped, makes the operation of the Mg base press-powder formed body that is dispersed with the Si particle.
D) heating Mg base press-powder formed body is by the synthetic Mg of the reaction of Mg and Si 2Si makes simultaneously and is dispersed with Mg 2The operation of the Mg base sintered alloy of Si particle.
E) the Mg base sintered alloy is fused, casts, make Mg 2The operation of the former material of Mg base casting that the Si particle disperses.
F) to casting that former material is mechanically pulverized or machining and the operation of powder powdered.
Manufacture method according to the former material of magnesium base alloy of the present invention has following operation: with the operation of above-mentioned magnesium base composite powder press-powder shaping; The operation of this press-powder formed body of heating in 200～400 ℃ inert gas atmospheres or non-oxidizing gas atmosphere; After heating, immediately the press-powder formed body is carried out extrusion process and makes its densified operation.
Put down in writing in following project about feature of the present invention and action effect.
Description of drawings
Fig. 1 is that expression is used for adhesive the surface of Mg based powders and makes Mg 2The diagram figure of one example of the method that the Si particle adheres to.
Fig. 2 is that expression is used for adhesive the surface of Mg based powders and makes Mg 2The diagram figure that another of the method that the Si particle adheres to is routine.
Fig. 3 be illustrated in the Mg based powders surface attachment Mg 2The diagram figure of one example of the magnesium base composite powder of Si particle.
Fig. 4 be illustrated in the Mg based powders surface attachment Mg 2Another routine diagram figure of the magnesium base composite powder of Si particle.
Fig. 5 is the figure of an example of the expression method of making magnesium base composite powder.
Fig. 6 is that expression makes in the matrix of Mg magnesium based powders and disperses Mg 2The diagram figure of one example of the magnesium base composite powder of Si particle.
Fig. 7 is the figure of another example of the expression method of making magnesium base composite powder.
Fig. 8 is the figure of another other examples of the expression method of making magnesium base composite powder.
Fig. 9 is the figure of another other examples of the expression method of making magnesium base composite powder.
Figure 10 is the figure of another other examples of the expression method of making magnesium base composite powder.
Figure 11 represents to make in the Mg magnesium-base alloy material to disperse Mg 2The microphotograph of one example of the section tissue of the magnesium base composite powder of Si particle.
Figure 12 is the X-ray diffraction result's of expression magnesium base composite powder the figure of an example.
Figure 13 is the X-ray diffraction result's of expression magnesium base composite powder the figure of another example.
The specific embodiment
(1) magnesium base composite powder
(A) Mg 2The content of Si
Magnesium base alloy powder integral body is 100% o'clock, contains 5～60% Mg in dimension criteria 2Si.In addition, the viewpoint of the machining property (machinability) of the magnesium base alloy that obtains from composite powder is cured, more preferably Mg 2The content of Si counts 20～40% with dimension criteria.Mg 2The content of Si is lower than under 5% the situation, the magnesium alloy that can not get having abundant rigidity.On the other hand, work as Mg 2The content of Si particle surpasses at 60% o'clock, is containing Mg 2Produce Mg in the magnesium base composite powder of Si particle 2Such powder is solidified in the segregation of Si particle, aggegation and the reduction of intensity and toughness can take place for the magnesium base alloy that obtains.In order to have the rigidity with the aluminium alloy peer-level, and in order to ensure the intensity of excellence and machinability and more preferably Mg 2The content of Si particle counts 20～40% with dimension criteria.
(B) Mg 2The maximum particle diameter of Si
The Mg that magnesium base composite powder is contained 2The maximum particle diameter of Si is below the 50 μ m, is preferably below the 20 μ m, more preferably below the 5 μ m.If Mg 2The maximum particle diameter of Si surpasses 50 μ m, and the mechanical property and the machinability that then can produce the magnesium base alloy that obtains reduce such problem.This value is that 20 μ m are when following, even containing the Mg that surpasses 40 volume % 2Also can keep good machinability under the situation of Si particle.Mg is arranged again 2The maximum particle diameter of Si particle is 5 μ m when following, and the machinability of magnesium base alloy improves, simultaneously because fine Mg 2The Si dispersion of nano-particles, this tensile strength of alloys improves.
(C) rigidity (Young's modulus)
The Young's modulus of magnesium base alloy is 48～90GPa.If Young's modulus is lower than 48GPa, then the increment rate with respect to the Young's modulus of original magnesium alloy is below 10%, is difficult to be applicable to that automobile is with the housing member of lid, the related member of shell and PC and mobile device etc. etc.On the other hand, as described, when Young's modulus surpasses 90GPa, Mg 2The content of Si surpasses 60% in dimension criteria, so the toughness of the former material of alloy and machinability reduction.
(2) manufacture method of magnesium base composite powder
(A) used the magnesium base composite powder that utilizes adhesive bond
Fig. 1 and Fig. 2 have represented to use the manufacture method of the Mg base composite powder of binder solution, have represented to Fig. 3 medelling to utilize the cross-section structure of the basic composite powder of Mg that the method obtains.
In the method, adopt wet type comminutor and spray dryer to make composite powder.According to method shown in Figure 1, be in container 1, to drop into Mg based powders and Mg 2The mixture 2 of Si particle is from the underfeed temperature wind 3 of container 1 and this mixture 2 is floated.Under this state, binder solution 4 is sprayed to mixture 2 as spraying from top, thereby adhesive is coated the surface of each particle, make its high temperature drying simultaneously.Its result has Mg by adhesive 9 on the surface of Mg based powders 7 as shown in Figure 3 2 Si particle 8 adheres to, combination.
According to method shown in Figure 2, be in container 1, to make Mg based powders and Mg with lower air quantity 2The mixture 2 of Si particle is floated, under this state with respect to wind direction vertically from bottom spray adhesive solution 4.
In addition, though not shown, in binder solution, mix, stir Mg 2The Si particle, the Mg based powders that this binder solution is floated for utilizing warm wind as spraying is coated with, and can make Mg by adhesive equally thus 2The Si particle adheres to, is incorporated into Mg based powders surface.
In addition as additive method, the Mg amount powder of ormal weight is dropped into container, add the oleic acid that becomes adhesive therein, oleic acid counts 0.2～0.5% with respect to the Mg based powders with weight rate, make integral container vibration or rotation afterwards, thereby to the surface of the Mg based powders in container coating oleic acid.In container add Mg thereafter, 2The Si particle, vibration or rotary container make the Mg based powders surface attachment Mg that is coated with oleic acid once again 2The Si particle.So obtain Mg base composite powder as shown in Figure 3.
(B) utilize the magnesium base composite powder of mechanicalness combination
On the other hand, as the method for mechanicalness combination, be with Mg based powders and Mg 2The Si particle drops into ball mill, mixes grater, roller type compacting machine or roll mill etc. with the state of its mixing, mixed powder is applied compression, shears processing etc., thereby obtain on Mg based powders surface combination mechanically, adhered to Mg 2The Mg base particle of Si particle.The Mg base composite powder that utilize to pulverize as required,, sieving machine can be obtained having cross-section structure as shown in Figure 4 and be had the given size shape by this particle.In Mg base composite powder 15 shown in Figure 4, be attached with Mg in the combination mechanically of the surface of Mg based powders 7 2 Si particle 8.
(C) adopted Mg 2The Si particle disperses the magnesium base composite powder of Mg base sintered alloy
(a) method shown in Figure 5
Prepare Mg based powders and Mg 2The Si particle is as initial feed, with the allotment ratio of regulation both is filled in the metal die after mixing, stirring, and carries out cure under pressure, is dispersed with Mg with making 2The Mg base press-powder formed body of Si particle.
In inert gas or non-oxidizing gas or vacuum, heat above-mentioned press-powder formed body, thereby obtain Mg by the solid-state diffusion between the Mg based powders with the fusing point that is lower than the Mg based powders 2Si particle dispersion-type Mg base sintered alloy.
The processing of the pulverizer by ball mill and crushing machine etc. or cutting etc. is with above-mentioned Mg 2Si particle dispersion-type Mg base sintered alloy powderization obtains the Mg base composite powder 16 of the size shape that is cross-section structure shown in Figure 6 and has regulation thus.Mg base composite powder 16 shown in Figure 6 mainly is to be dispersed with Mg in the matrix inside of Mg based powders 7 2The Si particle.
Also have, at above-mentioned Mg 2In the Si particle dispersion-type Mg base sintered alloy, in dimension criteria at Mg 2The content of Si particle surpasses at 60% o'clock, Mg 2The segregation of Si particle, aggegation produce, and produce the such problem of reduction life tools in the machining in addition.From this viewpoint, Mg 2The content of Si particle is preferably below 60%.
(b) method shown in Figure 7
Prepare Mg based powders and Si particle as initial feed, with the allotment ratio of regulation both are filled in the metal die after mixing, stirring, and carry out cure under pressure, be dispersed with the Mg base press-powder formed body of Si particle with making.
In inert gas or non-oxidizing gas or vacuum,, utilize the synthetic Mg of solid phase reaction between Si-Mg thus to be lower than the above-mentioned press-powder formed body of fusing point heating of Mg based powders 2Si obtains Mg by the solid-state diffusion between the Mg based powders simultaneously 2Si particle dispersion-type Mg base sintered alloy.
The processing of the pulverizer by ball mill and crushing machine etc. or cutting etc. is with above-mentioned Mg 2Si particle dispersion-type Mg base sintered alloy powderization obtains the Mg that contains of the size shape that is cross-section structure shown in Figure 6 and has regulation thus 2The Mg base composite powder of Si particle.
(D) adopted Mg 2The Si particle disperses the magnesium base composite powder of Mg base casting alloy
(a) method shown in Figure 8
The Mg that will prepare as initial feed 2After the Si particle drops into Mg base alloy liquation and stirs, be cast in the mould.The Mg base casting alloy that takes out from mould, be dispersed with the Mg of interpolation equably 2The Si particle.
The processing of the pulverizer by ball mill and crushing machine etc. or cutting etc. is above-mentioned casting alloy powderization, obtains the Mg that contains of the size shape that is cross-section structure shown in Figure 6 and has regulation thus 2The Mg base composite powder of Si particle.Also have, drop into Mg 2The melting temperature of the Mg base alloy liquation behind the Si particle is lower than Mg and Mg in the Si-Mg equilibrium state diagram 2The solidus temperature of Si.Otherwise if be heated to more than the solidus temperature, Mg then 2Si solid solution in Mg base alloy liquation is created in Mg in the process of setting after the cast 2Thick, the such problem of growing up of Si.
(b) method shown in Figure 9
Prepare Mg based powders and Mg 2The Si particle is as initial feed, with the allotment ratio of regulation both is filled in the metal die after mixing, stirring, and carries out cure under pressure, makes being dispersed with Mg 2The Mg base press-powder formed body of Si particle.After stirring liquation fully, be cast in the mould.
The Mg base casting alloy that takes out from mould, the Mg that is scattered here and there equably and adds 2Si particle, the processing of the pulverizer by ball mill and crushing machine etc. or cutting etc. be this alloy powderization, obtains the Mg that contains of the size shape that is cross-section structure shown in Figure 6 and has regulation thus 2The Mg base composite powder of Si particle.
(c) method shown in Figure 10
Prepare Mg based powders and Si particle as initial feed, with the allotment ratio of regulation both are filled in the metal die after mixing, stirring, and carry out cure under pressure, make the Mg base press-powder formed body that is dispersed with the Si particle thus.
In inert gas or non-oxidizing gas or vacuum,, utilize the synthetic Mg of solid phase reaction between Si-Mg thus to be lower than the above-mentioned press-powder formed body of fusing point heating of Mg based powders 2Si obtains Mg by the solid-state diffusion between the Mg based powders simultaneously 2Si particle dispersion-type Mg base sintered alloy.
With heating in the above-mentioned sintered alloy input crucible, make being dispersed with Mg 2The Mg base alloy liquation of Si particle.After stirring liquation fully, be cast in the mould.The Mg base casting alloy that takes out from mould, the Mg that is scattered here and there equably and adds 2Si particle, the processing of the pulverizer by ball mill and crushing machine etc. or cutting etc. be this alloy powderization, obtains the Mg that contains of the size shape that is cross-section structure shown in Figure 6 and has regulation thus 2The Mg base composite powder of Si particle.
Also have, because the cutting oil of using when machining is re-used as the raw material use attached on the Mg base composite powder afterwards so will go cutting oil to be divided into by cleaning treatment.
(3) the former material of magnesium base alloy
With the above-mentioned Mg that contains 2The Mg base composite powder of Si particle obtains the Mg that is scattered here and there as initial feed by it is shaped to solidify 2The Mg base alloy of Si particle.
After the shaping of Mg base composite powder press-powder, to its heating and enforcement extrusion process or forging processing or rolling processing, but the heating-up temperature of formed body at this moment is preferably about 200～400 ℃.If be lower than 200 ℃, the situation of extrusion process difficulty then takes place.On the other hand, if surpass 400 ℃, then along with the high speed of extrusion process speed, the temperature of the former material after the extrusion process rises, and the situation that causes the intensity reduction because of thickization of crystal grain is also arranged.
In the matrix of the Mg base alloy that as above-mentioned, obtains, the Mg2Si particle that is scattered here and there fine equably.Owing to be scattered in the Mg in the alloy 2Particle diameter in the particle diameter of Si particle and the Mg base composite powder is identical, so the Mg in the Mg base alloy 2The big particle diameter of the amount of Si particle is below the 50 μ m, is preferably below the 20 μ m, more preferably below the 5 μ m.Mg in Mg base alloy in addition 2The content of Si counts 5～60% with dimension criteria.The possibility that creates that consequently has high rigidity and high-intensity Mg base alloy.
Embodiment 1
Prepare pure Mg powder (purity 99.9%, average grain diameter 350 μ m) and Si powder (purity 99.9%, average grain diameter 22 μ m), with Mg: Si=2: behind two kinds of powder of 1 (mol ratio) allotment, carry out 30 minutes mixed processing with ball mill.This mixed-powder is positioned over the discharge plasma sintering device with the state that is filled into carbon molding jig (internal diameter 35mm_), in a vacuum pressure is adjusted into 100MPa, specimen temperature and is adjusted into 600 ℃ and implement 15 minutes sintering.Consequently obtain by Mg 2The external diameter 35mm_ that Si constitutes, the disc shaped test piece of thick 12mm.
Pulverize above-mentioned disc shaped test piece with jet mill, carrying out maximum particle diameter is that the following fine pulverizing of 15 μ m, sieve powder are handled, and is made into the Mg as initial feed 2The Si particle.On the other hand, as the Mg based powders, AZ31 (nominal the is formed Mg-3Al-1Zn/mass%) alloy powder about preparation diameter 2mm is as initial feed.
Based on method shown in Figure 5, at first with the regulation ratio mixing AZ31 powder and Mg 2The Si particle also is filled into the metal die of diameter 60mm_, applies the pressure of 400MPa, is made into the press-powder formed body.In nitrogen atmosphere,, obtain having disperseed Mg thus for 550 ℃ * 1 hour sintering of this press-powder formed body enforcement 2The AZ31 sintered alloy of Si particle.Make Mg base composite powder about diameter 0.5～3mm by machining by this sintered alloy then.
With respect to Mg base composite powder integral body, Mg 2The content of Si particle is counted 16% o'clock composite powder with dimension criteria section structure observation result is represented by Figure 11.Particle diameter is the following Mg of 15 μ m 2The Si particle can segregation and aggegation, but is dispersed in equably in the AZ31 matrix, thereby obtains based on Mg base composite powder of the present invention.
Embodiment 2
Based on method shown in Figure 7, at first prepare pure Mg powder (purity 99.9%, average grain diameter 350 μ m) and Si powder (purity 99.9%, average grain diameter 22 μ m), behind the two kinds of powder of ratio allotment with regulation, carry out 30 minutes mixed processing with ball mill.This mixed-powder with in the metal die that is filled into diameter 60mm_ and apply the pressure of 400MPa, is made the press-powder formed body.
In a vacuum above-mentioned press-powder formed body is implemented 590 ℃ * 1 hour heat treated, utilized the synthetic Mg of solid phase reaction of Si and Mg thus 2The Si particle promotes the sintering between the Mg powder simultaneously, obtains Mg 2The Si particle disperses Mg sintering material.Utilize ball mill to pulverize this sintering material then, make the Mg base composite powder about diameter 0.3～1mm.
With respect to Mg base composite powder integral body, Mg 2The content of Si particle is counted 7% o'clock composite powder with dimension criteria X-ray diffraction result is represented by Figure 12.Have only Mg and Mg 2The peak value of Si is detected, owing to be not used in the peak value of the Si of initial feed, so itself and Mg complete reaction and at Mg 2Be consumed in Si synthetic.In addition owing to there not being the peak value of MgO, so do not produce the oxidation in the sintering process yet yet.
In addition, the result based on the structure observation of light microscope is to be dispersed in the Mg in the powder matrix 2The average grain diameter of Si is about 24 μ m, because equal with the particle diameter as the Si powder of initial feed, grows up so in the course of reaction of above-mentioned and Mg significant thick grain takes place.Consequently, obtained the Mg of the present invention's regulation 2The Si particle is scattered in the Mg base composite powder in the matrix equably.
Embodiment 3
Prepare pure Mg powder (purity 99.9%, average grain diameter 350 μ m) and Si powder (purity 99.9%, average grain diameter 22 μ m), with Mg: Si=2: behind two kinds of powder of 1 (mol ratio) allotment, carry out 30 minutes mixed processing with ball mill.This mixed-powder is positioned on the discharge plasma sintering device with the state that is filled into carbon molding jig (internal diameter 35mm_), in a vacuum pressure is adjusted into 100MPa, specimen temperature and is adjusted into 600 ℃ and implement 30 minutes sintering.Consequently obtain by Mg 2The external diameter 35mm_ that Si constitutes, the disc shaped test piece of thick 12mm.
Pulverize the above-mentioned disc shaped test piece of processing machine pulverizing with spraying, carrying out maximum particle diameter is that the following fine pulverizing of 10 μ m, sieve powder are handled, and is made into the Mg as initial feed 2The Si particle.
Based on method shown in Figure 8, at first in carbon system crucible, prepare AZ61 (nominal is formed Mg-6Al-1Zn/mass%) alloy liquation.The liquation management under 720～740 ℃ state, is added above-mentioned Mg with the ratio of stipulating 2After Si particle and abundant the stirring, be poured in the metal die, make being dispersed with Mg 2The former material of AZ61 casting alloy of Si particle.
By machining, make the Mg base composite powder that constitutes by the AZ61 alloy about diameter 0.5～3mm by above-mentioned casting alloy.Expression is with respect to the Mg of the former material integral body of casting alloy in the table 1 2The content of Si particle (dimension criteria).The operating conditions of cutting the superhard system instrument in the family processing when result of the section structure observation of the composite powder that obtains in addition, and making powder shows in table.
In sample No.1～5, because of containing the Mg of appropriate amount as example of the present invention 2Si, thus in Mg base composite powder, do not produce Mg 2The segregation of Si particle and aggegation, Mg 2The Si particle is dispersed in the matrix equably.In addition, with regard to the tool wear (damage status) when utilizing machining to make Mg base composite powder,, be in the state that does not constitute problem although confirm a bit to slight scratch.
On the other hand, in sample No.6 as a comparative example, because Mg 2Si content reaches 65%, so in the powder matrix Mg is arranged 2The aggegation of Si particle takes place, when making powder by machining in addition, because casting alloy contains the Mg of hard in a large number 2Si so the damage of the degree of depth has taken place on the instrument, has the such problem of Mg aggegation to produce in its damaged portion simultaneously.
[table 1]
Test portion No. Mg 2Si content (volume fraction) Mg 2Si dispersion of nano-particles situation The damage status of instrument
1 7 In matrix, evenly disperse Tool surfaces is good
2 12 The same The same
3 28 The same The same
4 38 The same Slight scratch seldom
5 57 The same Slight scratch
6 65 Mg 2The cohesion of Si particle takes place Very dark damage is being coagulated at its part Mg
Embodiment 4
Prepare pure Mg powder (purity 99.9%, average grain diameter 350 μ m) and Si powder (purity 99.9%, average grain diameter 22 μ m), with two kinds of powder with Mg: Si=2: after 1 (mol ratio) allotment, carry out 30 minutes mixed processing with ball mill.
Above-mentioned mixed-powder is positioned on the discharge plasma sintering device with the state that is filled into carbon molding jig (internal diameter 35mm_), in a vacuum pressure is adjusted into 100MPa, specimen temperature and is adjusted into 600 ℃ and implement 15 minutes sintering.Consequently obtain by Mg 2The external diameter 35mm_ that Si constitutes, the disc shaped test piece of thick 12mm.
Pulverize the above-mentioned discoid test portion of processing machine pulverizing with spraying.At this moment processing conditions is pulverized in change, to make the different Mg of maximum particle diameter 2The Si particle.
Based on method shown in Figure 9, as the Mg based powders, AM60 (nominal the is formed Mg-6Al-0.5Mn/mass%) alloy powder of preparing diameter 3mm is as initial feed, with the ratio of regulation with itself and Mg 2The Si particle is mixed, and is filled in the metal die of diameter 60mm_ and applies the pressure of 400MPa, makes the press-powder formed body.
Then, after input press-powder formed body and abundant the stirring, be poured in the metal die in the preparation AM60 alloy liquation (melt temperature: 720～740 ℃) in carbon system crucible, make being dispersed with Mg 2The former material of AM60 casting alloy of Si particle.By machining, being made with the AM60 alloy by this casting alloy is the Mg base composite powder (diameter: about 0.5～3mm) of former material then.Also has the Mg in the Mg base casting alloy that obtains 2The content of Si counts 22% with dimension criteria.
In order to calculate the Mg that is dispersed in the above-mentioned Mg base composite powder matrix 2The maximum particle diameter of Si particle, and utilize the cross-section structure of observation by light microscope composite powder, try to achieve Mg according to this result by graphical analysis 2The maximum particle diameter of Si particle.Its result is represented by table 2.The damage status of the superhard system instrument in the machining when making Mg base composite powder by casting alloy in addition shows in table.
In sample No.7～10, has suitable particle diameter Mg owing in casting alloy, contain as example of the present invention 2Si, the instrument abrasion when therefore making powder by machining, damage do not take place, and present the surface of good proterties.
On the other hand, in sample No.11～12 as a comparative example, because the contained Mg of casting alloy 2The maximum particle diameter of Si surpasses 50 μ m, so the damage of the degree of depth takes place on the instrument when machining, has the such problem of Mg aggegation to produce in this damaged portion simultaneously.
[table 2]
Test portion No. Mg 2Si maximum particle diameter (μ m) The damage status of instrument
7 3 Tool surfaces is good
8 12 The same
9 26 The same
10 42 Very dark damage is being coagulated at its part Mg
11 75 Very dark damage is being coagulated at its part Mg
12 92 Very dark damage is being coagulated at its part Mg
Embodiment 5
Mg base composite powder with the above embodiments 3 and embodiment 4 records is an initial feed, the press-powder body that is shaped and makes each powder by metal die.After in being controlled to be 350 ℃ nitrogen atmosphere, each press-powder body heating being kept 5 minutes, implement extrusion process (extrusion ratio 37) immediately, make the former material of extruding.Push former material by each and make the tension test sheet, estimate the tensile characteristics (tensile strength and fracture are extended) under the normal temperature, and measure Young's modulus.Its result of table 3 expression.
In sample No.1～5 and No.7～10, can access and have excellent intensity and the magnesium base alloy of toughness, particularly sample No.4 and 5 and have the high rigidity that can be equal to mutually with aluminium alloy as example of the present invention.In addition, shown in sample No.7 and 8, the Mg in being dispersed in alloy 2The maximum particle diameter of Si particle is to be lower than under the so fine situation of 5 μ m or 20 μ m, and except intensity, extending also significantly increases.
On the other hand, in sample No.6 as a comparative example, because Mg 2Si content is many, thus Mg base alloy become fragile, based on the making difficulty of the tensile test sheet of machining.In addition in sample No.11～12 as a comparative example, because Mg 2The maximum particle diameter of Si is big must to surpass 50 μ m, thus the toughness reduction of Mg base alloy, and tensile strength also reduces.
[table 3]
Test portion No. Tensile strength (MPa) (%) extended in fracture Young's modulus (GPa) Reference
1 278 18 49
2 293 16 53
3 314 13 63
4 322 9 70
5 326 5 82
6 - - 109 Because crisp tensile test fails to take
7 310 19 59
8 307 17 58
9 303 15 59
10 294 12 58
11 221 7 57
12 206 4 57
Embodiment 6
Prepare pure Mg powder (purity 99.9%, average grain diameter 350 μ m) and Si powder (purity 99.9%, average grain diameter 22 μ m), with two kinds of powder with Mg: Si=2: after 1 (mol ratio) allotment, carry out 30 minutes mixed processing with ball mill.This mixed-powder is positioned on the discharge plasma sintering device with the state that is filled into carbon molding jig (internal diameter 35mm_), in a vacuum pressure is adjusted into 100MPa, specimen temperature and is adjusted into 600 ℃ and implement 30 minutes sintering.Consequently obtain by Mg 2The external diameter 35mm_ that Si constitutes, the disc shaped test piece of thick 18mm.
Pulverize the above-mentioned disc shaped test piece of processing machine pulverizing with spraying, carrying out maximum particle diameter is that the following pulverizing of 10 μ m, sieve powder are handled, and is made into the Mg as initial feed 2The Si particle.
Then, in the plastic container of volume 350ml, drop into the pure Mg powder of particle diameter 0.5～2mm (purity 99.9%) 200g, use the oscillatory type ball mill, make container vibration 15 minutes with the state that among this container, has added the oleic acid of 0.6g, thus the uniform surface of the pure Mg powder in container ground coating oleic acid.Among this container, add above-mentioned Mg again 2Si particle (in dimension criteria, being 13% with respect to mixed-powder integral body) applies vibration in 15 minutes again, makes pure Mg powder surface adhere to Mg 2The Si particle is made the Mg base composite powder of the present invention's regulation thus.
The X-ray diffraction result of the Mg base composite powder that obtains as above-mentioned is shown by Figure 13.Only detect as the Mg and the Mg that drop into raw material 2The peak value of Si in the result who scans the type electron microscope observation, also confirms Mg in addition 2The Si particle attached to thick Mg powder surface, is confirmed by above equably, when using as adhesive with oleic acid, also can make Mg base composite powder.
More than, with reference to drawing this working of an invention mode has been described, but this invention is not limited to illustrated embodiment.Invent in the same scope therewith or in the impartial scope, can be in addition various corrections and the change of illustrated embodiment.
The industrial possibility of utilizing
The magnesium base alloy that obtains according to the present invention, existing magnesium alloy is significantly improved as the low rigidity of the problem on the performance, can advantageously utilize the automobile at engine part and speed changer part etc. to have like this with member with part and structure on the purposes of high rigidity requirement.

Claims (14)

1. a magnesium base composite powder wherein, has: the magnesium based powders; Be scattered in the either party's at least of the surface of described magnesium based powders and matrix inside magnesium silicide Mg 2Si.
2. magnesium base composite powder according to claim 1, wherein, described Mg 2The maximum particle diameter of Si is below the 50 μ m.
3. magnesium base composite powder according to claim 1, wherein, described Mg 2The maximum particle diameter of Si is below the 20 μ m.
4. magnesium base composite powder according to claim 1, wherein, described Mg 2The maximum particle diameter of Si is below the 5 μ m.
5. magnesium base composite powder according to claim 1, wherein, with respect to the described Mg of this magnesium base composite powder 2The content of Si counts 5～60% with dimension criteria.
6. the former material of magnesium base alloy wherein, carries out press-powder to the described magnesium base of claim 1 composite powder and is shaped and sintering, makes Mg 2The Si particle is dispersed in the matrix.
7. the manufacture method of a magnesium base composite powder wherein, has:
Prepare Mg based powders and Mg 2The operation of Si particle;
Operation at the surperficial coating adhesive of described Mg based powders;
The Mg based powders and the described Mg of described adhesive will be coated with 2Si mix particles, stirring make Mg 2The operation that the Si particle combines with the surface of Mg based powders.
8. the manufacture method of a magnesium base composite powder wherein, has:
Prepare Mg based powders and Mg 2The operation of Si particle;
At described Mg based powders of allotment and described Mg 2Mechanically mix behind the Si particle, make Mg 2The operation that Si particle and the surface of Mg based powders mechanically combine.
9. the manufacture method of a magnesium base composite powder wherein, has following operation:
Prepare Mg based powders and Mg 2The operation of Si particle;
Mix described Mg based powders and described Mg 2The operation of Si particle;
In metal die, described mixed-powder press-powder is shaped, makes being dispersed with described Mg 2The operation of the Mg base press-powder formed body of Si particle;
The described Mg base of sintering press-powder formed body makes being dispersed with described Mg 2The operation of the Mg base sintered alloy of Si particle;
Described Mg base sintered alloy is mechanically pulverized or machining and carry out the operation of powder powdered.
10. the manufacture method of Mg base composite powder wherein, has:
Prepare the operation of Mg based powders and Si particle;
The operation of mixing described Mg based powders and described Si particle;
In metal die, described mixed-powder press-powder is shaped, makes the operation of the Mg base press-powder formed body that is dispersed with described Si particle;
Heat described Mg base press-powder formed body, by the synthetic Mg of the reaction of Mg and Si 2Si makes simultaneously and is dispersed with Mg 2The operation of the Mg base sintered alloy of Si particle;
Described Mg base sintered alloy is mechanically pulverized or machining and carry out the operation of powder powdered.
11. the manufacture method of a magnesium base composite powder wherein, has:
In magnesium base liquation, drop into Mg 2Si particle and the operation that stirs;
Described liquation is poured in the mould to make the operation of the former material of casting;
The former material of described casting is mechanically pulverized or machining and carry out the operation of powder powdered.
12. the manufacture method of a magnesium base composite powder wherein, has:
Prepare Mg based powders and Mg 2The operation of Si particle;
Mix described Mg based powders and Mg 2The operation of Si particle;
In metal die, described mixed-powder press-powder is shaped, makes being dispersed with described Mg 2The operation of the Mg base press-powder formed body of Si particle;
Described Mg base press-powder formed body is fused, casts, make Mg 2The operation of the former material of Mg base casting that the Si particle disperses;
The former material of described casting is mechanically pulverized or machining and carry out the operation of powder powdered.
13. the manufacture method of a magnesium base composite powder wherein, has:
Prepare the operation of Mg based powders and Si particle;
The operation of mixing described Mg based powders and described Si particle;
In metal die, described mixed-powder press-powder is shaped, makes the operation of the Mg base press-powder formed body that is dispersed with described Si particle;
Heat described Mg base press-powder formed body, by the synthetic Mg of the reaction of Mg and Si 2Si makes simultaneously and is dispersed with Mg 2The operation of the Mg base sintered alloy of Si particle;
Described Mg base sintered alloy is fused, casts, make Mg 2The operation of the former material of Mg base casting that the Si particle disperses;
The former material of described casting is mechanically pulverized or machining and carry out the operation of powder powdered.
14. the manufacture method of the former material of magnesium base alloy wherein, has:
The described magnesium base of claim 1 composite powder is carried out the operation that press-powder is shaped;
The operation of the described press-powder formed body of heating in 200～400 ℃ inert gas atmospheres or non-oxidizing gas atmosphere;
After described heating, immediately described press-powder formed body is carried out extrusion process and makes its densified operation.
CNA2005800225841A 2004-07-08 2005-06-27 Magnesium-base composite powder, magnesium-base alloy material and method for production thereof Pending CN1980760A (en)

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