CN101203622A - Metal composites and methods for forming the same - Google Patents

Metal composites and methods for forming the same Download PDF

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CN101203622A
CN101203622A CN200680017144.1A CN200680017144A CN101203622A CN 101203622 A CN101203622 A CN 101203622A CN 200680017144 A CN200680017144 A CN 200680017144A CN 101203622 A CN101203622 A CN 101203622A
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alloy
metal
metal composite
formation
spinodal
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瞿显荣
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • 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
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working

Abstract

A metal composite comprising a spinodal structure having at least one ductile phase and method of making same is disclosed. The metal composite is formed by forming an alloy comprising a positive heat of mixing in the liquid state; purifying the alloy; and forming a network structure of the alloy comprising at least one ductile sub-network.

Description

Metal composite and forming method thereof
Invention field
The present invention relates generally to a kind of metal composite and forming method thereof, more specifically, relate to a kind of metal composite with reticulated structure (network structure), this reticulated structure has the inferior netted crystal boundary of at least one ductile (ductile) (sub-network).
Background
Nano structural material is defined as the grain-size diameter at 1nm to 1, between the 000nm, and comprises lnm and 1, the material of 000nm.When comparing with the same material of the no nanostructure that forms, the existence of nanostructure has improved mechanical property in the material.
Nano structural material synthesizes by the powder sintered or thermal annealing and the flux processing (fluxing) of glassy metal usually.In powder sintered, the powder of nano-scale is pressed in together, and can be annealed, to make nano structural material.Normally discous by the powder sintered nano structural material that produces, the about 1cm of diameter, thickness are that 1mm is to 2mm.Powdered agglomerated material normally brittle (brittle), and show space and uneven grain growing.
As selection, the thermal annealing of amorphous metal produces nanocrystal in amorphous matrix.Metal melt is quenched to glass or amorphous metal, and it is annealed in the temperature near its second-order transition temperature subsequently, causes producing in amorphous matrix the nanocrystal that homogeneous distributes.When described amorphous matrix also crystallization, can produce crystalline nanostructured.
The flux treatment technology is used in the preparation nano structural material recently.In this method, liquid spinodal (spinodal) has taken place to have been decomposed, cause producing brittle solid spinodal.Typical Pd-Si nanostructure as shown in Figure 1.As can be seen from Figure 1, discrete Pd precipitation (showing with white) is positioned at the solid spinodal.But the discrete sedimentary volume fraction of Pd can be ignored, so that described solid spinodal remains brittle.
Therefore, the principal constituent of conventional nanostructure is brittle mutually, and has wide grain size distribution.Conventional nanostructure also has low strength and low impact fracture energy.And conventional amorphous metal has little overall size usually, and for example thickness is the band shape or the paper tinsel shape form of 30-50 micron, makes them be not suitable for commercial applications.
Summary of the invention
In one embodiment, the present invention relates to a kind of method, this method comprises with described composition and forms alloy, the described alloy of purifying, and forms the reticulated structure of described alloy, and this reticulated structure contains at least one ductile time reticulated structure.
Another embodiment relates to a kind of metal composite that contains ductility spinodal structure.Another embodiment relates to the metal that contains this metal composite.In another embodiment, described metal is a nanostructure composite material.
Another embodiment relates to the method that forms metal composite, this method comprises formation alloy, the described alloy of purifying, forms one or more spinodals, with the described one or more spinodals of heating, make in described one or more spinodal at least one be transformed into one or more ductility phases (ductile phase).
The detailed description of non-limiting embodiment of the present invention when considered in conjunction with the accompanying drawings, will make other advantages of the present invention, new characteristics and purpose apparent.When this specification sheets and by reference and bonded document when comprising conflicting disclosure then is as the criterion with this specification sheets.
The accompanying drawing summary
In the drawings:
Fig. 1 is that conventional Pd-Si nanostructure is the TEM Photomicrograph in 75,000 * time at ratio of enlargement.
Fig. 2 is to be the SEM Photomicrograph in 9,500 * time at ratio of enlargement, and it has shown the microstructure of conventional steel ball.
Fig. 3 A is to be the SEM Photomicrograph in 35,000 * time at ratio of enlargement, and it has shown Fe 80C 15Si 5The part of two-phase spinodal microstructure.
Fig. 3 B is to be the SEM Photomicrograph in 6,000 * time at ratio of enlargement, and it has shown another part of the two-phase spinodal microstructure among Fig. 3 A.
Fig. 3 C is to be the SEM Photomicrograph in 34,000 * time at ratio of enlargement, and it has shown another part of the two-phase spinodal microstructure among Fig. 3 A.
Fig. 3 D is to be the SEM Photomicrograph in 8,500 * time at ratio of enlargement, and it has shown another section of the two-phase spinodal microstructure among Fig. 3 A.
Fig. 3 E is to be the SEM Photomicrograph in 9,400 * time at ratio of enlargement, and it has shown the section of the two-phase spinodal microstructure among Fig. 3 A.
Fig. 4 A is to be the SEM Photomicrograph in 34,000 * time at ratio of enlargement, and it has shown Fe 40.5Co 40.5C 14Si 5The part of spinodal structure.
Fig. 4 B is to be the SEM Photomicrograph in 5,400 * time at ratio of enlargement, and it has shown another part of the spinodal structure among Fig. 4 A.
Fig. 4 C is to be the SEM Photomicrograph in 13,500 * time at ratio of enlargement, and it has shown the section of the spinodal structure among Fig. 4 A.
Fig. 4 D is to be the SEM Photomicrograph in 4,100 * time at ratio of enlargement, and it has shown another section of the spinodal structure among Fig. 4 A.
Fig. 5 A is to be the SEM Photomicrograph in 34,000 * time at ratio of enlargement, and it has shown Co 75Si 15B 10The part of spinodal structure.
Fig. 5 B is to be the SEM Photomicrograph in 2,000 * time at ratio of enlargement, and it has shown another part of the spinodal structure among Fig. 5 A.
Fig. 5 C is to be the SEM Photomicrograph in 5,400 * time at ratio of enlargement, and it has shown another part of the spinodal structure among Fig. 5 A.
Fig. 5 D is to be the SEM Photomicrograph in 1,400 * time at ratio of enlargement, and it has shown the section of the spinodal structure among Fig. 5 A.
Fig. 6 A is to be the SEM Photomicrograph in 4,100 * time at ratio of enlargement, and it has shown Fe 82C 18The part of spinodal structure.
Fig. 6 B is to be the SEM Photomicrograph in 9,500 * time at ratio of enlargement, and it has shown the section of the spinodal structure among Fig. 6 A.
Describe in detail
When the present invention uses, the details that illustrated structure and composition are arranged in that it is not limited to illustrate in the following description or the accompanying drawing. The present invention can have other embodiments, and can be put into practice or finish by different way. Equally, the wording of using in this literary composition and term are for the purpose of describing, and should not be considered to restrictive. " the comprising " of using in this literary composition, " comprising ", " having ", " containing ", " relating to " and their synonym mean to comprise project and their equivalent and the extra project of listing thereafter.
The invention provides metallic composite and forming method thereof, described metallic composite comprises the network of at least two spinodals or inferior netted crystal boundary. Term " spinodal " and " inferior netted crystal boundary " are in this commutative use, be defined in after liquid spinodal decomposition and the solidification subsequently, the solid forms in bunch (the isolated clusters) of isolation and/or interconnection district (interconnected regions) is learned. For example, the spinodal of bianry alloy decomposes and solidification subsequently causes producing netted crystal boundary two times. Similarly, the spinodal of ternary alloy three-partalloy decomposes and causes producing the netted crystal boundary of two or three times. Inferior netted crystal boundary can comprise discrete precipitation, but this precipitation is not to exist with significant amount.
In one embodiment, at least one spinodal of described metallic composite or inferior netted crystal boundary are the ductility phases. Word used herein " ductility phase " refers to malleable phase. Described ductility spinodal can be isolation bunch, part interconnection, fully interconnection, or their combination. In other words, the interconnection degree of described metallic composite ductility spinodal everywhere can be different. In one embodiment, described metallic composite comprises ductility spinodal and fragility spinodal. In another embodiment, described metallic composite comprises the first ductility spinodal and the second ductility spinodal. In an embodiment of the invention, described ductility phase can be changed with fragility relative volume mark mutually, changing any required character, such as but not limited to, hardness, fatigue strength, compression yield strength, wearability and maximum allowable operating temperature (M.A.O.T.).
Described metallic composite can be formed by any alloy, and condition is that main component and at least a other compositions of this alloy have the positive liquid heat of mixing. Word used herein " heat of mixing " is when being defined in temperature T, the enthalpy change when the mixture of 1mol is formed by its pure component. Term used herein " mainly " is defined as the main component of the expection of described alloy. Described liquid state can be stable or metastable. Example with alloy of positive heat of mixing composition comprises: monotectic alloy, eutectic alloy, Peritectic Alloy. Other examples with alloy of positive heat of mixing composition are documented in that Richard A.Swalin writes, John Wiley﹠Sons, Inc. in the textbook " thermodynamics of solids (thermodynamics of solids) " that publish (1962), be all purposes, by reference it merged in this literary composition. In one embodiment, described alloy can comprise metal and nonmetal.
In one embodiment, total mixture heat of all the components in the described alloy can be on the occasion of.In another embodiment, liquid total mixture heat of all the components can be negative value in the alloy.For example, can have negative total liquid mixture heat by first composition, second composition and the three one-tenth alloys that are grouped into, even described first composition (principal constituent) has positive liquid mixture heat with described second composition, and also has positive liquid mixture heat with described the 3rd composition.In this example, total negative mixture heat can be produced by the second and the ternary very big negative liquid mixture heat, and this liquid mixture heat of bearing has surpassed first principal component and second and ternary positive liquid mixture heat.
Any metal all can be used to obtain required matrix material character, if selected Metal and Alloy at least a other compositions in conjunction with the time, have positive liquid mixture heat.For example, described metal can be the group VIII metal, for example Fe, Co, Ni, Ru, Rh, Pd, Os, Ir, Pt and their combination.In one embodiment, described metal can be selected from Fe, Co, Ni, Cu, Pd, Pt, Mn, Al, T, Zr, Cr, W and their combination.In one embodiment, described metal is Co.In another embodiment, described metal is Fe.In another embodiment, described metal is Ni.
As long as any nonmetal required matrix material character that all can be used to obtain is the selected nonmetal positive liquid mixture heat that has when combining with other main components.For example, described nonmetal can be any in B, C, Si, As, Sb, Te, Po and their combination.In one embodiment, described nonmetal can be any in B, C, Si and their combination.In another embodiment, described nonmetal be C.
In another embodiment, described alloy comprises Fe; And at least a among Si and the C.In this embodiment, Fe can change in the scope of about 70 atom % and about 92 atom %, and comprise 70 atom % and 92 atom %, Si can change in the scope of about 0 atom % and about 20 atom %, and comprise 0 atom % and 20 atom %, and C can change in the scope of about 0 atom % and about 30 atom %, and comprises 0 atom % and 30 atom %.Used scope is represented the minimum value and the maximum value of each composition, is appreciated that the combination of described each composition makes that the atomic percent of alloy is 100%.Think that when the method that discloses according to this literary composition is handled, these scopes of Fe, Si and C will cause producing ductility spinodal reticulated structure.Though the mixture (composition) beyond these scopes also can produce required ductility nanostructure, thinks that these scopes can be more effective under process conditions.
In one embodiment, described Fe-C-Si mixture can be at Fe 76C 24Si 0Fe 81C 19Si 0Fe 85.5C 0Si 14.5Fe 88.5C 0Si 11.5Change between all mixtures therebetween, and comprise these mixtures.Find this scope and all points wherein, after air cooling and sufficient mistake are cold, can cause producing the nanostructure that comprises the ductility spinodal.
In another embodiment, described Fe-C-Si mixture can be at Fe 81C 19Si 0Fe 84C 16Si 0Fe 90C 0Si 10Fe 88.5C 0Si 11.5Change between all therebetween points, and comprise these mixtures.In another embodiment, the Fe-C-Si mixture of another embodiment can be at Fe 73C 27Si 0Fe 76C 24Si 0Fe 84C 0Si 16Fe 85.5C 0Si 14.5Change between all therebetween points, and comprise these mixtures.Found in these scopes and all points therebetween, the part of the matrix material that is formed by these mixtures will form the nanostructure that comprises the ductility spinodal after air cooling.But, can use the speed of cooling of increase, so that make the entire sample of these mixtures all can form required nanostructure.
In another embodiment, described Fe-C-Si mixture can be at Fe 84C 16Si 0Fe 87C 13Si 0Fe 90C 0Si 10Fe 92C 0Si 8Change between all therebetween points, and comprise these mixtures.In another embodiment, the Fe-C-Si mixture of another embodiment can be at Fe 70C 30Si 0Fe 73C 27Si 0Fe 82C 0Si 18Fe 84C 0Si 16Change between all therebetween points, and comprise these mixtures.Think these scopes of utilizing, required nanostructure can be in the formation in the tower (drop tower) of dripping of aerification medium.
In another embodiment, B can be added in the Fe-C-Si alloy.For example, the add-on of B can be between about 0 atom % and about 5 atom %, and comprise 0 atom % and 5 atom %, and formation that can the described spinodal structure of remarkably influenced.
In another embodiment, described alloy can comprise the nonmetal of any Ge of being selected from, P, S and their combination.In one embodiment, Ge can replace Si or also use Ge except that Si, and can the described nanostructure of remarkably influenced.But in some cases, the existence of Ge causes the formation in space.In another embodiment, P can be added in the described alloy to increase the formation of spinodal structure.For example, about 0.5 atom % is to about 4 atom % and comprise that the P of 0.5 atom % and 4 atom % can be added in the described Fe-C-Si alloy, so that whole matrix material can contain the spinodal structure.Find in the Fe-C-Si alloy, to add P and reduced or eliminated the existence of eutectic structure, thereby increased the amount of spinodal structure.
In another embodiment, Ni can be added in the described Fe-C-Si alloy to increase the volume fraction of described ductility phase.For example about 1 atom % can be added in the Fe-C-Si alloy to increase the volume fraction of described ductility phase to the Ni greater than about 3 atom %.
The glass forming ability of described alloy (glass forming ability) (GFA) can be more than or equal to about 0.35, so that enough big of formed nanostructure, to give described matrix material required physical properties, described glass forming ability is meant second-order transition temperature (T g) and liquidus temperature (T 1) ratio.In one embodiment, GFA is more than or equal to about 0.49.For example, Fe 82.5B 17.5GFA be about 0.35; Fe 80B 20GFA be about 0.49; Fe 80C 7P 13GFA be about 0.58; Fe 79Si 10B 11GFA be about 0.58, and Co 75Si 15B 10GFA be about 0.56.
The mixture of composition that can be by heating selected required ratio forms described alloy.Heating can utilize conventional equipment to carry out under the condition of the alloying of standard, and described equipment is radio-frequency induction smelting furnace or high-temperature smelting pot for example.
Randomly, formed alloy can be divided into the smaller portions of described alloy, for further processing.Described alloy can be placed on the first part of container, and this container also has the second section littler than described first part.Described container can be vacuumized.Described container can be heated, and makes described alloy melting to form first molten alloy.Utilize gas under pressure can force described first molten alloy to enter the second section of described container.Described container and described first molten alloy can be cooled to form solidified alloy.Described solidified alloy can be removed from the second section of described container, and can be allocated to required size or quality.
In one embodiment, the section area of the first part of described container is littler than the section area of described second section.Therefore, but described second section sufficiently long, in narrower section area, to hold whole described molten alloy.Cool off described first molten alloy and container, described solidified alloy can be cut into the various thickness that are suitable for required application.
The alloy of further not cut apart or further be divided into the solidified alloy of smaller portions can be handled, according to conventional methods further to remove impurity.For example, described solidified alloy can be heated to when having flux more than or equal to its liquidus temperature (T 1) temperature, to form second molten alloy.In one embodiment, described solidified alloy and flux material can be heated to above about 1,000 ℃ temperature.
Any flux all can be used, described second molten alloy reaction as long as it is got along well.For example, described flux can be boron oxide, glass, calcium oxide, barium oxide, aluminum oxide, magnesium oxide, Lithium Oxide 98min or their mixture.In one embodiment, described flux is glass.In another embodiment, described flux is boron oxide.Demarcate and be anhydrous boron oxide (B 2O 3), can be from Atomergic Chemetals Corporation (Farmingdale, NY) acquisition.
Described second molten alloy can be cooled to the temperature that is enough to form second solidified alloy subsequently.In one embodiment, can be by described second molten alloy be cooled under its liquidus temperature, and make the described second molten alloy undercooling.Described second molten alloy can be cooled to critical temperature T c, or under the critical temperature, be usually less than described liquidus temperature, decompose to produce liquid spinodal, thereby form the liquid spinodal.Be not bound by any particular theory, described second molten alloy of having thought described flux treating processes purifying makes described second molten alloy keep its liquid state under far below its liquidus temperature.By allowing described second molten alloy remain on liquid state under its liquidus temperature, described second molten alloy is metastable liquid, in case enter metastable miscibility gap (critical temperature T c) the spinodal decomposition just takes place, described metastable miscibility gap is starkly lower than the liquidus line of described alloy usually.During spinodal decomposed, described molten alloy split into many metastable liquid spinodals with liquid phase wavelength X.The wavelength of Shi Yonging (λ) is defined as the lateral dimension (lateraldimension) or the diameter of described spinodal herein.In one embodiment, the liquid phase λ of described metastable liquid can be less than about 300nm, preferably less than about 100nm.
After the cooling, described second molten alloy solidifies, and has spinodal or the cold sample of inferior cancellated mistake with formation.Described solid spinodal can be crystalline, amorphous, accurate crystalline, or their mixture.In one embodiment, to be cooled to Δ T be about 100 ° of K to about 500 ° of K to described alloy.Term Δ T used herein is defined as the difference (T between liquidus temperature and actual temperature 1-T).
Decomposing formed solid phase wavelength (λ) by the liquid spinodal of described second molten alloy changes to the nanometer at micron usually.The matrix material that is produced can have fine microstructure, and fine microstructure is defined as the grain-size diameter, or wavelength, at 1nm to 100, between the 000nm, and comprises 1nm and 100, the material of 000nm.Described matrix material can contain nanostructure, and a physical size of wherein a kind of one-tenth phase-splitting (constituent phase) is about 1,000nm or littler.Each spinodal in the structure of whole networking, or inferior netted crystal boundary can have solid phase wavelength close each other or that differ from one another.
In one embodiment, formed spinodal or inferior cancellated solid phase λ are less than about 50 microns.In another embodiment, formed spinodal or inferior cancellated solid phase λ are about 10 microns or littler.In another embodiment, the about 300nm of the solid phase λ of formed spinodal structure or littler is preferably less than about 100nm.
Described solid phase wavelength everywhere can be different at sample.For example, described solid phase wavelength can change during crystallization.During crystallization, crystallization forward position (crystallization front) passes through described melts, and described solid phase λ is increased, and produces more coarse spinodal structure effectively.So described solid phase wavelength can begin the site minimum in crystallization, and along with crystallization is increased by proceeding of site of beginning.The wavelength that begins the solid spinodal in site in crystallization may be similar to the wavelength of liquid spinodal.In one embodiment, the form that begins the spinodal in site away from described crystallization can be replaced (partially or even wholly) by other structures (comprising dendrite and eutectic crystal).
If after described metastable liquid alloy carries out metastable liquid spinodal decomposition, do not carry out crystallization, described liquid spinodal is in case further cooling can be solidified into the amorphous spinodal.Described curing can be carried out equably,, can not begin sclerosis (hardening) in any one position that is.When further cooling off, continue sclerosis, become amorphous solid up to all liquid spinodals.Be expected in the curing of this pattern, described solid phase λ is homogeneous basically, so that the liquid phase λ of described liquid spinodal can be close with the solid phase λ of described amorphous spinodal.The solid spinodal also can the amorphous spinodal and the form of crystalline spinodal mixture form so that λ everywhere can be different at described solid.
Phase in described spinodal, if crystalline, can be but nonessential, formation contains the microstructure of driving fit crystal boundary (coherent grain boundary).Term used herein " driving fit crystal boundary " is defined as driving fit interface (coherent interface) and/or half driving fit interface (semi-coherent interface).The driving fit interface has about 10 to about 100mJ/m 2Interfacial energy, and appear at two crystal in interface plane place Perfect Matchings, so that two lattices are successive at described interface.When half driving fit interface appears at described interface and has the dislocation of a series of edges or spiral, and has about 200mJ/m 2To about 500mJ/m 2Interfacial energy.
In another embodiment of the present invention, any fragility spinodal that is present in the sample can be further processed, and to change mutually, becomes one or more ductility spinodals.For example, during annealing, Fe 3Si resolves into Fe and graphite, thereby further increases the intensity and the impact fracture (impact fracture) of sample.In one embodiment, one or more fragility spinodals can be annealed, to form the ductility phase.The ductility that is produced can be mutually isolate bunch, partially or substantially interconnection fully, and their combination.Described ductility can interconnect mutually with other ductility mutually, and/or interconnects mutually with fragility.
Described metal composite can be the bulk material (bulk material) with any suitable specific purpose shape.The material that word used herein " bulk material " is defined as having definite shape, and the sectional dimension of its any direction is all more than or equal to about 1mm.For example, described matrix material can be sphere, taper shape, pyramid, square, rectangle or irregularly shaped.In one embodiment, described matrix material is spherical.In another embodiment, described at least one sectional dimension of determining the shape material is about 2.54cm, preferably about 1cm.In another embodiment, described metal composite can be the sphere with diameter of any suitable specific purpose.For example, described metal composite can be diameter be respectively less than about 1 inch, be less than or equal to about 2cm, be less than or equal to about 1.0cm and be less than or equal to the sphere of about 5mm.In another embodiment, the diameter of described spherical metal matrix material can be about 0.1mm.When comparing with the method for the manufacturing steel ball of routine, the described method that metal composite is configured as sphere (for example ball) is favourable.For example, expensive usually process can replace with simple and cheap flux treating processes, and conventional heat-treatment process can be removed.
Embodiment
Can further understand the present invention with reference to the following example, these embodiment are illustrative, and not as the restriction of the present invention to defining in the claim.
Below the alloy of listed every kind of mixture prepare as follows:
Required starting material mixture is made alloy in the radio-frequency induction smelting furnace, under about 1,000 ℃ of minimum temperature, described starting material are selected from Fe, Co, Ni, C, Si, B, Ge and P.Described alloy, and is placed in the major part of fused silica tube solidifying subsequently by air cooling.Described fused silica tube has internal diameter arrives about 8mm for about 2mm to the major part of 30mm and internal diameter for about 10mm the smaller portions than length.The length of described smaller portions arrives about 600mm for about 10mm.The silica tube that contains described alloy is found time with mechanical pump and is placed the sufficiently long time in the enough high temperature smelting furnace, to melt described alloy.When described alloy melts fully, gas under pressure is introduced the major part of described silica tube, to promote the smaller portions that described molten alloy advances the described silica tube of people.Described silica tube and alloy are cooled, and form bar-shaped alloy.With described bar-shaped alloy from described silica tube, shift out and cut into each thickness at about 1mm to about 10mm, and comprise the less plate-like sheet of about 1mm and about 10mm.
Each plate-like sheet all with anhydrous B 2O 3Be placed on together in the independent fused silica tube, between about 15mm, length arrives about 100mm for about 10mm to the internal diameter of described fused silica tube at about 3mm.Many alloy disc (alloy disk) and anhydrous B of containing 2O 3Fused silica tube be placed on diameter for about 20mm to about 100mm than in the big fused silica tube.Described big silica tube is vacuumized, containing each alloy disc and anhydrous B 2O 3Independent pipe in produce vacuum.Described big silica tube heats specific time subsequently under sufficiently high temperature, specific time can be about 15 minutes to about 8 hours, to melt described alloy fully.Described molten alloy cools off under following Δ T temperature and crystallization.
Example I.
Fe:80 atom %
C:15 atom %
Si:5 atom %
This alloy is by when being higher than its liquidus temperature, purifying fusion Fe in flux 80C 15Si 5, be lower than undercooling under the temperature of its liquidus line subsequently, thus preparation.
Described Fe-C-Si system is shaped as accurate ball, and its some character is listed in table 1.The comparing result of conventional chromium steel ball (from FAG Bearing, Danbury, CT acquisition) is also listed in table.
Table 1
Character The Fe-C-Si system The chromium steel ball (from FAG Bearing, Danbury, CT obtains)
Hardness (HV) fatigue strength (maximum compression pressure (MPA)) *Compression yield strength (MPA) maximum operating temperature 750-850＞3,600 **About 7,000550 ℃ ＜2,600 ***About 3,600150 ℃
*Fatigue strength come to determine by periodic force of compression (cyclic compressive force), and minimal compression pressure (compressive pressure) is about 3 for about 0MPA and maximum cycle compression pressure, and 600MPA carries out 10 7The individual cycle.
*After test was finished, sample was still excellent.
* *Sample does not hold out against test.
Found that the Fe-C-Si system has and about identical wear resistance and the hardness of conventional steel ball.But the ball that is produced by the Fe-C-Si system shows almost twice, and (7,000MPA is compared to 3,600MPA) in the compression yield strength of described conventional steel ball.Ball by the manufacturing of Fe-C-Si system also shows 3, and 600MPA does not have the bigger fatigue strength that damages down, and conventional ball just damages during 600MPA 2.Similarly, show than bigger Young's modulus of conventional steel ball and bigger thermostability by the ball of Fe-C-Si system manufacturing.In addition, described Fe-C-Si system ball shows the impact fracture energy that approaches the ceramic meticulous ball made by SiN.
Fig. 3 A is Fe 80C 15Si 5The SEM of the two-phase spinodal microstructure of ball.The described Fe of variant position analysis in this ball 80C 15Si 5Photomicrograph among Fig. 3 A shows the two-phase spinodal structure with interconnection microstructure.Two-phase all is a crystalline, and mean wavelength is about 300nm.The randomness of described microstructure shows that this is the site that crystallization begins.Fig. 3 B is the Photomicrograph at sample center among Fig. 3 A.Fig. 3 B has shown the different directions near the arrangement (alignment) of the spinodal structure at described sample center and arrangement.Fig. 3 C is the Photomicrograph of described sample and described beginning site opposing ends.Fig. 3 C has shown the formation with the eutectic structure of described beginning site opposing ends.Fig. 3 D has shown the fracture behaviour of this system, and wherein section is flaky or cloud form.White curve among Fig. 3 D is crestal line (ridges), illustrates to have produced ductile fracture.Fig. 3 E is another Photomicrograph of the sample among Fig. 3 A, and it has shown the microstructure on the described sample section.Two solid spinodals in the described metal composite are Fe 3Si and body-centered cubic (BCC) Fe, or the sosoloid of Fe.Spinodal before is brittle, and afterwards be ductile.In case fracture, described ductility spinodal is formed on the crestal line on the section.Be not bound by any particular theory, think that high strength and HI high impact failure energy are to be caused by BCC Fe (or sosoloid of Fe).
Under very large Δ T, 100-500 ° of K for example, described melts splits into two liquid spinodals.These two liquid spinodals are metastable, so tend to crystallization.Crystallization begins (being called beginning crystallization site) in lip-deep certain site of described fusing sample.Extend subsequently in the crystallization forward position, becomes crystal up to whole fusing sample.During crystallization, release of heat (heat of crystallization), this is to cause along with gradually away from described beginning crystallization site, the partly cause that microstructure changes.Begin the site in crystallization, because crystal growth is very fast and heat release is less relatively, so the morphology of liquid spinodal may be similar to the morphology of solid spinodal.Leave described beginning crystallization site, the morphology of spinodal develops gradually.
In contrast, Fig. 2 is the SEM of conventional steel ball microstructure, and described steel ball is the mixture of austenite and martensite normally, by ordinary method production.Usually make the steel of wire spiral (being still the softish austenite) form.Be cut into the short cylindrical section by this wire, and in upsetting press (heading machine) cold forging.Grind with ball grinder (flashingmachine) on the surface of heading ball (headed ball).This ball hardens in smelting furnace subsequently, will be hard martensite more than the austenitic transformation of half.After the sclerosis, this ball carries out two grinding steps (grinding and polishing) again, to produce required surface finish.Thereby this ball is cleaned and polishes.The shortcoming of the ordinary method of preparation steel ball comprises that needs use high-quality wire spiral, and need guarantee that thermal treatment can be not martensite with all austenitic transformations.In addition,, use, for example be higher than 150 ℃ application so conventional steel ball may be not suitable for high temperature because not every austenite is all changed.
Be not subjected to the constraint of any one particular theory, think and compare with similar object with the ordinary method manufacturing, the microstructure that contains the ductility phase of the present invention provides unique physical properties for the object of microstructure or nanostructure, for example: bigger compression yield strength, bigger Young's modulus, bigger fatigue resistance and bigger thermostability, keep similar wear resistance and hardness simultaneously, also show the impact fracture energy similar simultaneously to Ceramic Balls.
Example II.
Fe:40.5 atom %
CO:40.5 atom %
C:14 atom %
Si:5 atom %
Described Tc is about 800 ℃.Fig. 4 A-4D has shown formed Fe 40.5CO 40.5C 14Si 5The microstructure of ingot (ingot) (sample).Fig. 4 A has shown the at first microstructure of crystalline part sample, is positioned at the sample free surface.In Fig. 4 A, two solid spinodals are arranged, be different phases, they form random network together.Fig. 4 B has shown the microstructure of last crystalline part sample, at the end relatively of sample.Find out that from Fig. 4 B described microstructure is the mixing of spinodal form and eutectic structure.Fig. 4 C has shown the section of sample, and wherein Ming Liang crestal line shows in two spinodals one ductile fracture has taken place.The distribution of crestal line is consistent with the prediction of spinodal mechanism.In the dominant zone of eutectic, the eutectic form is presented on the section shown in Fig. 4 D.
EXAMPLE III.
CO:75 atom %
Si:15 atom %
B:10 atom %
Crystallization occurs in about 800 ℃.Formed CO 75Si 15B 10The microstructure of ingot (sample) is presented among Fig. 5 A-5D.Fig. 5 A shown crystalline part sample at first microstructure, be positioned at the free surface of described ingot.In Fig. 5 A, two out of phase solid spinodals are arranged, form network.The form of described network begins the site and changes along with sample position leaves crystallization.Shown in Fig. 5 B, towards the center of sample, a tangible solid spinodal fragments into elongated grains (elongated grains).Described elongated grains may be above about 20 microns.One deck is multiple phase separates described elongated grains.Fig. 5 C has shown the microstructure from farther position, described beginning crystallization site.Shown in Fig. 5 C, the layer around elongated grain of last crystalline sample part seems it is homogeneous basically.Fig. 5 D has shown the section of described sample, shows that around the layer of described elongated grains be ductile.
Be not bound by any particular theory, think that described ductility layer provides impact fracture energy and intensity for described sample.
EXAMPLE IV.
Fe:82 is former in %
C:18 atom %
Tc is about 650 ℃.Fig. 6 A has shown the Fe of such preparation 82C 18The microstructure of sample ingot.In Fig. 6 A, many zones (domains) are arranged, wherein the network spline structure (network-like structure) that all is arranged on together of each zone is occupied.Border relatively flat between the zone, and be significantly (sharp) near the arrangement of the network on border.Obviously, the rearrangement form of network branches during crystallization, occurs, formed described border.Fig. 6 B has shown the microstructure of sample section among Fig. 6 A.As shown in Figure 6A, find two vertical lines, represent above-mentioned border at center near Photomicrograph.These borders have arrangement feature (alignedfeatures), and are similar to dendrite.From farther place, described border, the structure of flaky or cloud form occupies the major portion of described microstructure again.The ridge of ductile fracture has been experienced in bright part representative among Fig. 6 B.
Described several aspects of at least one embodiment of the present invention, should be understood that various changes, modification and improvement will carry out for a person skilled in the art easily.Expect that such change, modification and improvement all are a part of this disclosure, and expection is included within essence of the present invention and the scope.Therefore, the description of front and accompanying drawing all are exemplary.

Claims (69)

1. method, this method comprises:
Form alloy;
The described alloy of purifying;
Formation comprises the reticulated structure of at least one ductility time cancellated described alloy.
2. the process of claim 1 wherein the T of alloy of described formation gWith T 1Ratio more than or equal to about 0.35.
3. the method for claim 2, the T of the alloy of wherein said formation gWith T 1Ratio more than or equal to about 0.49.
4. the method for claim 2, the alloy of wherein said formation comprises metal and nonmetal.
5. the method for claim 4, wherein the described alloy of purifying comprises:
Heat described alloy to form molten alloy; With
Described molten alloy is contacted with flux material.
6. the method for claim 2 wherein forms reticulated structure and comprises the described molten alloy of cooling.
7. the method for claim 6 is wherein cooled off described molten alloy and was comprised cold described molten alloy.
8. it is that about 100 ° of K are to about 500 ° of K that the method for claim 7, wherein said molten alloy are cooled to Δ T.
9. the method for claim 4, the alloy of wherein said formation comprise and are selected from following metal: Fe, Co, Cu, Ni, Pd, Pt, Mn, Al, Ti, Zr, Cr, W and their combination.
10. the method for claim 9, the alloy of wherein said formation comprise and are selected from following metal: Fe, Co, Ni and their combination.
11. the method for claim 10, the alloy of wherein said formation comprises Ni.
12. the method for claim 10, the alloy of wherein said formation comprises Co.
13. the method for claim 10, the alloy of wherein said formation comprises Fe.
14. the method for claim 4, the alloy of wherein said formation comprise be selected from following nonmetal: B, Si, C and their combination.
15. the method for claim 4, the alloy of wherein said formation further comprise be selected from following nonmetal: Ge, P, S and their combination.
16. the method for claim 14, wherein said nonmetal be C.
17. comprising, the method for claim 10, the alloy of wherein said formation be selected from following element: C, Si and their combination.
18. the method for claim 15, the alloy of wherein said formation further comprises Ge.
19. the method for claim 5, wherein said alloy contacts with flux material, and described flux material is selected from B 2O 3, glass, calcium oxide, barium oxide, aluminum oxide, magnesium oxide, Lithium Oxide 98min and their combination.
20. the method for claim 19, wherein said alloy contacts with flux material, and described flux material is selected from B 2O 3, glass and their combination.
21. the method for claim 20, wherein said alloy and B 2O 3Contact.
22. the method for claim 20, wherein said alloy and glass contact.
23. the method for claim 4, this method comprise that further described alloy of heating and described flux material are to being higher than about 1,000 ℃ temperature.
24. the method for claim 1, this method further comprises:
Described alloy is placed on the first part of container;
The first part of the described container of heating under vacuum makes described alloy melting and flow into the second section of described container; With
Cool off the second section of described container.
25. the process of claim 1 wherein that the cancellated solid phase λ of described formation is about 50 microns or littler.
26. the method for claim 25, the cancellated solid phase λ of wherein said formation is about 10 microns or littler.
27. the method for claim 26, the cancellated solid phase λ of wherein said formation is about 300 nanometers or littler.
28. the method for claim 27, the cancellated solid phase λ of wherein said formation is about 100 nanometers or littler.
29. the process of claim 1 wherein that the described alloy with positive liquid mixture heat is a kind of in monotectic alloy, eutectic alloy and the Peritectic Alloy.
30. the method for claim 25, wherein the spinodal structure of Xing Chenging has basic liquid phase λ and the solid phase λ that equates.
31. the method for claim 30, wherein said basic liquid phase λ that equates and solid phase λ are in position that crystallization begins.
32. the process of claim 1 wherein that described alloy is to be formed by at least two kinds of compositions with liquid positive mixture heat.
33. the method for claim 32, wherein said liquid state is metastable.
34. the method for claim 32, wherein said liquid state is stable.
35. a metal composite, this metal composite contain ductility spinodal structure.
36. the metal composite of claim 35, wherein said spinodal structure comprises the driving fit crystal boundary.
37. the metal composite of claim 35, wherein said matrix material are the shape materials of determining.
38. the metal composite of claim 37, the liquid phase λ of wherein said spinodal structure are about 50 microns or littler.
39. the metal composite of claim 37, the solid phase λ of wherein said spinodal structure are about 50 microns or littler.
40. the metal composite of claim 38, wherein said spinodal structure have basic liquid phase λ and the solid phase λ that equates.
41. the metal composite of claim 35, this material further contains metal and nonmetal.
42. the metal composite of claim 41, wherein said metal are selected from Fe, Co, Cu, Ni, Pd, Pt, Mn, Al, Ti, Zr, Cr, W and their combination.
43. the metal composite of claim 42, wherein said metal are selected from Fe, Co, Ni and their combination.
44. the metal composite of claim 43, wherein said metal is Ni.
45. the metal composite of claim 43, wherein said metal is Co.
46. the metal composite of claim 43, wherein said metal is Fe.
47. the metal composite of claim 41, wherein said nonmetal be selected from B, Si, C and their combination.
48. the metal composite of claim 41, this material further contain Ge, P, S and their combination.
49. the metal composite of claim 47, wherein said nonmetal be selected from C, Si and their combination.
50. the metal composite of claim 42, this material further contains Si.
51. the metal composite of claim 42, this material further contains C.
52. the metal composite of claim 42, this material further comprise the T more than or equal to about 0.35 gWith T 1The ratio.
53. the metal composite of claim 52, this material further comprise the T more than or equal to about 0.49 gWith T 1The ratio.
54. metal that contains the described metal composite of claim 34.
55. the metal of claim 54, wherein said article are spherical.
56. the metal of claim 55, wherein said spheric diameter are about 1 inch or littler.
57. the metal of claim 56, wherein said spheric diameter is about 2cm or littler.
58. the metal of claim 57, wherein said spheric diameter is about 1cm or littler.
59. the metal of claim 58, wherein said spheric diameter is about 5mm or littler.
60. the metal of claim 59, wherein said spheric diameter is about 0.1mm.
61. the metal of claim 54, wherein said article further contain the eutectic structure.
62. the metal of claim 54, wherein said metal is a nanostructure composite material.
63. a method that forms metal composite, this method comprises:
Form alloy;
The described alloy of purifying;
Form one or more spinodals; With
Heat described one or more spinodal, make in described one or more fragility spinodal at least one change one or more ductility phases into.
64. the method for claim 63 wherein forms one or more spinodals and comprises the one or more fragility spinodals of formation.
65. the method for claim 63, wherein said one or more ductility interconnect mutually.
66. the method for claim 65, wherein said one or more ductility are the part interconnection mutually.
67. the method for claim 65, wherein said one or more ductility interconnect mutually basically fully.
68. the method for claim 65, wherein said one or more ductility interconnect mutually with fragility mutually.
69. the method for claim 63, wherein said one or more ductility are isolated bunch mutually.
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