CN107177750B - A kind of Pressure Infiltration preparation method of metal-base composites - Google Patents
A kind of Pressure Infiltration preparation method of metal-base composites Download PDFInfo
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- CN107177750B CN107177750B CN201710401622.9A CN201710401622A CN107177750B CN 107177750 B CN107177750 B CN 107177750B CN 201710401622 A CN201710401622 A CN 201710401622A CN 107177750 B CN107177750 B CN 107177750B
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
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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
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1073—Infiltration or casting under mechanical pressure, e.g. squeeze casting
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Abstract
The present invention relates to field of composite material preparation, disclose a kind of Pressure Infiltration preparation method of metal-base composites, including：Material is sequentially loaded into jacket, jacket is put into mold, mold is put into hot-press arrangement, adjusting position of the mold in hot-press arrangement by the preparation of material, it is prepared according to certain temperature, pressure parameter, finally obtains metal-base composites of good performance.The present invention being capable of the preparation process simple, quickly, economic that carry out the composite material containing high-volume fractional infusibility constituent element in ingredient, there is higher bulk density and material consistency by the composite material that the process can be realized, and the interface binding power between each constituent element of obtained composite material is higher.
Description
(1) technical field
The present invention relates to field of composite material preparation, are prepared more particularly to a kind of Pressure Infiltration of metal-base composites
Method.
(2) background technology
When preparing metal or ceramic-metal composite, often need by the way that temperature is heated to the molten of high-melting-point constituent element
Change temperature or more, then the method by smelting or casting to prepare required material, this method needs to expend a large amount of heat
While energy and high cost of equipment are put into, also it is difficult to prevent the abnormal growth of the crystal grain in the preparation process of material.
When carry out the preparation of material by the method for stirring casting, since the wetability between ceramics and metal is poor so that institute
The uniformity consistency for preparing material is poor.In the method by powder metallurgy come when preparing material, advantage is that ingredient is easy to adjust,
Precise control, but be not easy to shrink due to high-melting-point constituent element, cause sintering a large amount of hole usually occur.When using hot pressing, only
It can carry out at relatively low temperature, the interface bond strength of material is low, not fine and close enough, if temperature is higher, reaches even
More than the melt temperature of low melting point constituent element, liquid is then usually extruded mold, and material preparation is caused to fail.Meanwhile using powder
Metallurgy method and pressure sintering carry out the preparation of material, it is difficult to be prepared to high-volume fractional infusibility phase material (ceramics), infusibility
The volume fraction of phase material is at maximum up to 55~60%.In for casting or the technique study smelted, with liquid injection mistake
High-speed flow in journey smashes coarse crystal grain so that the crystal grain of deposition becomes smaller, or directly sprays low melting point constituent element liquid, adds
Enter high-melting-point constituent element ceramics, the spray deposition that Direct precipitation is molded to obtain material requested is suggested, to solve in material preparation
In the process the problem of abnormal grain growth, but the technological parameter of this method is more difficult to control, can be in material during Direct precipitation
Inside generates a large amount of hole, and the composite material that this method prepares must be by secondary extrusion or hot isostatic pressing into traveling
The densification of one step can just obtain satisfactory material, complex technical process.And in high-volume fractional metallic composite
Preparation process in, since infusibility constituent element ceramics are difficult to carry out in the material high-densit accumulation, and dystectic ceramic constituent element
Usually there is higher intensity, it is difficult to be compressed, even if also being difficult to material using secondary extrusion or heat and other static pressuring processes
Carry out further densification.Liguid infiltration is the method that people largely used later, and this method is by making in advance
After going out the prefabricated component of high-melting-point constituent element ceramics, the liguid infiltration of low melting point constituent element metal is carried out to it.Liguid infiltration substantially can
The material or composite material met the requirements is enough prepared, but its production cycle is long and production cost is high, these factors make
It is expensive to obtain the material price being prepared in this way, is unfavorable for promoting the use of on a large scale.
Currently, liguid infiltration is mainly the following method：1) pressure-free impregnation, by prefabricated ceramic phase prefabricated section, by it
Into in metal liquid, pressure-free impregnation is carried out.The operation needs time overlength, stomata relatively more.2) gas pressure infiltration, this method
Need high air pressure, it usually needs special equipment.3) infiltration by squeeze casting, it usually needs the mold of super-pressure and good seal, cost
It is high.Under normal circumstances, pressure is more than 50MPa, and common 100MPa is produced, and be typically due to mold is difficult to sealing metal liquid
Body needs high pressure 100MPa that could obtain high-densit composite material.
In summary the advantage and disadvantage of various methods need a kind of economically feasible and can prepare high volume with large-scale use
The process of the metal-base composites of score ceramics.
(3) invention content
It can contain height in carry out ingredient simple, quickly, economic the technical problem to be solved in the present invention is to provide a kind of
The Pressure Infiltration preparation method of the metal-base composites of volume fraction infusibility constituent element can be realized to obtain by the process
Composite material there is higher bulk density and material consistency, and the interface between each constituent element of obtained composite material
Binding force is higher.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of Pressure Infiltration preparation method of metal-base composites, includes the following steps：
(1) low-melting-point metal constituent element and high-melting-point ceramics constituent element powder with certain bulk density are sequentially loaded into one end
In closed jacket, wherein high-melting-point ceramics constituent element powder be prepare total composite volume than 45%~90%；It is packed into
After jacket, high-melting-point ceramics constituent element powder is close to the open end of jacket；
(2) with the open end of the closed jacket in one end in end socket closing step (1)；For closing jacket open end
End socket be equipped with a through-hole, through-hole can be connected to inside and outside jacket；Jacket is packed into mold；The blind end of the jacket with
The upper die head of mold fits, and the end socket of jacket open end and the lower die head of mold fit；
(3) mold that jacket is housed in step (2) is put into hot-press equipment, by the lower die head of mold and hot-press equipment
Cooling pressure head fits；After being forced into 0~5MPa, it is molten that low-melting-point metal constituent element is warming up to the heating rate of 2~100 DEG C/min
Or more 5~150 DEG C；Simultaneously so that the temperature at the lower die head of mold be maintained at low-melting-point metal constituent element fusing point or less 5~
150℃；Keep the temperature 0~10min；
(4) during step (3) is kept the temperature, it is forced into 5~30MPa, until insulating process terminates；
(5) after step (3) are kept the temperature, room temperature is reduced to the rate of temperature fall of 2~100 DEG C/min；
(6) after step (5) terminates, blow-on is removed from the molds jacket, then takes out sample from jacket, obtains institute
The metal-base composites needed.
In a preferred embodiment of the invention, the high-melting-point ceramics constituent element powder include boron carbide ceramics powder,
Silicon carbide ceramics powder, zirconium carbide ceramic powder, titanium carbide ceramic powder, titanium nitride ceramic powder, zirconium nitride ceramic powders, silicon
A kind of in powder or tungsten powder or wherein component be combined with each other two-by-two.
In a preferred embodiment of the invention, the low-melting-point metal constituent element includes aluminium, copper, magnesium, aluminium alloy, magnesium conjunction
Gold or copper alloy in any one.
Compared with prior art, beneficial effects of the present invention are as follows：
The present invention provides a kind of Pressure Infiltration preparation method of metal-base composites, can it is simple, quickly, warp
The preparation process for carrying out the composite material containing high-volume fractional infusibility constituent element in ingredient of Ji, can be real by the process
The composite material now obtained has higher bulk density and material consistency, and between each constituent element of obtained composite material
Interface binding power it is higher.
Liguid infiltration method is improved during this process prepares composite material, is carried out using similar wrapping structure
Outer cladding, carries out Pressure Infiltration in hot pressing furnace, and wrapping structure limits the direction that metal liquid overflows mold；In the envelope of jacket
Through-hole is equipped at head, the metal liquid of liquid can be quickly flow under the effect of the pressure where high-melting-point ceramics constituent element powder
Position, and then jacket is gone out by through-hole section bit stream, due to being fitted on the outside of jacket with having the lower die head of cooling effect, metal
Liquid is rapidly frozen, and secondary seal is carried out to through hole, to ensure that it is further excessive that metal liquid does not occur.In this way,
Under the action of lower pressure, low-melting-point metal constituent element and high-melting-point ceramics constituent element powder in jacket can be carried out adequately
Mixing, infiltration, to obtain, the interface binding power between consistency is high, density is high, bulk density is high and each constituent element is high to answer
Condensation material.
It, can be to being wrapped in 10~40MPa after being sealed jacket during carrying out the preparation of composite material
Pressure under carry out the pre- press operation of 5~10min, fine and close composite material can preferably be prepared.
In preparation process, it can be padded in jacket and set one layer of graphite paper, ensure that the same of the uniformity of heat conduction
When, but also being more easy when taking out the composite material prepared from jacket.
The architectural characteristic of jacket makes in preparation process, is respectively at liquid and solid low-melting-point metal constituent element and height
Melting ceramic constituent element powder can be contacted preferably, the effect mutual in powder particle of high-melting-point ceramics constituent element powder
Under, cause pile up effect, the low-melting-point metal constituent element of liquid that can be infiltrated in liquid form to high-melting-point ceramics constituent element powder,
And enter in through-hole structure by high-melting-point ceramics constituent element powder and then solidified under the cooling effect of lower die head in turn, to packet
Set is sealed, and the low-melting-point metal constituent element for the liquid that can not be overflowed will invade each high-melting-point constituent element in liquid form
In gap between grain, and high-melting-point constituent element is further infiltrated under the conditions of certain temperature, pressure, is completed entire
The process that most important liquid solid-state infiltrates mutually in technique so that the composite material finally obtained has better material consistent
Property, composite material obtained final compactness extent and density feature are also affected to a certain extent.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
(4) it illustrates
The present invention will be further described below with reference to the drawings.
Fig. 1 is the structural schematic diagram of inventive die and jacket.
In figure, 1, mold, 2, lower die head, 3, upper die head, 4, jacket, 5, graphite paper, 6, low-melting-point metal constituent element, 7, Gao Rong
The ceramic constituent element powder of point, 8, end socket, 9, through-hole.
(5) specific implementation mode
In order to clarify the technical characteristics of the invention, below by specific implementation mode, and its attached drawing is combined, to this hair
It is bright to be described in detail.
Embodiment 1：
Referring to Fig. 1, in the present embodiment, the high-melting-point ceramics constituent element powder 7 and low-melting-point metal of metal-base composites
Silica flour and aluminium is respectively adopted in constituent element 6, and to prepare AlSi60, the material theoretical volume ratio of silica flour and aluminium is 6:4, preparation method is such as
Under：
1) silica flour prepared needed for material is taken, by grain mixture ratio, the bulk density for obtaining silica flour is 60%, spare, is taken
One piece of aluminium block, the wherein material of silica flour and aluminium are 1.07 according to weight ratio:1 feeding, in 4 inside liner graphite paper 5 of jacket, by aluminium
Block and silica flour are sequentially loaded into the closed jacket in one end 4；After being packed into jacket 4, silica flour is close to the open end of jacket 4；
2) with the open end of the closed jacket in one end in an end socket 8 closing step (1) 4；It is open for closing jacket 4
The end socket 8 at end is equipped with a through-hole 9, and through-hole 9 can be connected to inside and outside jacket 4；Jacket 4 is packed into mold 1；The jacket 4
The upper die head 3 of blind end and mold 1 fit, the end socket 8 of 4 open end of jacket is affixed with the lower die head 2 of mold 1
It closes；
(3) mold 1 that jacket 4 is housed in step (2) is put into hot-press equipment, lower die head 2 and the hot pressing of mold 1 is set
Standby cooling pressure head fits；After being forced into 1MPa, 700 DEG C are warming up to the heating rate of 20 DEG C/min；Meanwhile opening hot pressing
The cooling pressure head of equipment so that the temperature at the lower die head 2 of mold 1 is maintained at 620 DEG C；Keep the temperature 5min；
(4) during step (3) is kept the temperature, it is forced into 10MPa so that the aluminium of liquid is filled up completely silica flour
In particle voids, until insulating process terminates；
(5) after step (3) are kept the temperature, room temperature is reduced to the rate of temperature fall of 20 DEG C/min；
(6) after step (5) terminates, blow-on takes out jacket 4 from mold 1, then takes out sample from jacket 4, obtains
Required metal-base composites AlSi60, density reach 2.45g/cm3。
Embodiment 2：
Referring to Fig. 1, in the present embodiment, the high-melting-point ceramics constituent element powder 7 and low-melting-point metal of metal-base composites
Silicon carbide powder and aluminium is respectively adopted in constituent element 6, and to prepare AlSiC70, the material theoretical volume ratio of silicon carbide powder and aluminium is 7:
3, preparation method is as follows：
1) silicon carbide powder prepared needed for material is taken, by grain mixture ratio, the bulk density for obtaining silicon carbide powder is
70%, it is spare, one piece of aluminium block is taken, wherein the material of silicon carbide powder and aluminium is according to weight ratio 2.3:1 feeding, inside jacket 4
Aluminium block and silicon carbide powder are sequentially loaded into the closed jacket in one end 4 by liner graphite paper 5；After being packed into jacket 4, carborundum powder
End is close to the open end of jacket 4；
2) with the open end of the closed jacket in one end in an end socket 8 closing step (1) 4；It is open for closing jacket 4
The end socket 8 at end is equipped with a through-hole 9, and through-hole 9 can be connected to inside and outside jacket 4；Jacket 4 is packed into mold 1；The jacket 4
The upper die head 3 of blind end and mold 1 fit, the end socket 8 of 4 open end of jacket is affixed with the lower die head 2 of mold 1
It closes；
(3) mold 1 that jacket 4 is housed in step (2) is put into hot-press equipment, lower die head 2 and the hot pressing of mold 1 is set
Standby cooling pressure head fits；After being forced into 5MPa, 700 DEG C are warming up to the heating rate of 20 DEG C/min；Meanwhile opening hot pressing
The cooling pressure head of equipment so that the temperature at the lower die head 2 of mold 1 is maintained at 630 DEG C；Keep the temperature 5min；
(4) during step (3) is kept the temperature, it is forced into 30MPa so that the aluminium of liquid is filled up completely silicon carbide
In the particle voids of powder, until insulating process terminates；
(5) after step (3) are kept the temperature, room temperature is reduced to the rate of temperature fall of 30 DEG C/min；
(6) after step (5) terminates, blow-on takes out jacket 4 from mold 1, then takes out sample from jacket 4, obtains
Required metal-base composites AlSiC70, density reach 3.04g/cm3。
Embodiment 3：
Referring to Fig. 1, in the present embodiment, the high-melting-point ceramics constituent element powder 7 and low-melting-point metal of metal-base composites
Silicon carbide powder and magnesium is respectively adopted in constituent element 6, and to prepare MgSiC65, the material theoretical volume ratio of silicon carbide powder and aluminium is
6.5:3.5, preparation method is as follows：
1) silicon carbide powder prepared needed for material is taken, by grain mixture ratio, the bulk density for obtaining silicon carbide powder is
65%, it is spare, one piece of MAG block is taken, wherein the weight of material of silicon carbide powder and MAG block is according to 2.84:1 feeding；Inside jacket 4
MAG block and silicon carbide powder are sequentially loaded into the closed jacket in one end 4 by liner graphite paper 5；After being packed into jacket 4, carborundum powder
End is close to the open end of jacket 4；
2) with the open end of the closed jacket in one end in an end socket 8 closing step (1) 4；It is open for closing jacket 4
The end socket 8 at end is equipped with a through-hole 9, and through-hole 9 can be connected to inside and outside jacket 4；Jacket 4 is packed into mold 1；The jacket 4
The upper die head 3 of blind end and mold 1 fit, the end socket 8 of 4 open end of jacket is affixed with the lower die head 2 of mold 1
It closes；
(3) mold 1 that jacket 4 is housed in step (2) is put into hot-press equipment, lower die head 2 and the hot pressing of mold 1 is set
Standby cooling pressure head fits；After being forced into 5MPa, 670 DEG C are warming up to the heating rate of 20 DEG C/min；Meanwhile opening hot pressing
The cooling pressure head of equipment so that the temperature at the lower die head 2 of mold 1 is maintained at 630 DEG C；Keep the temperature 5min；
(4) during step (3) is kept the temperature, it is forced into 30MPa so that the magnesium of liquid is filled up completely silicon carbide
Particle voids in, until insulating process terminates；
(5) after step (3) are kept the temperature, room temperature is reduced to the rate of temperature fall of 30 DEG C/min；
(6) after step (5) terminates, blow-on takes out jacket 4 from mold 1, then takes out sample from jacket 4, obtains
Required metal-base composites MgSiC65.
Embodiment 4：
Referring to Fig. 1, in the present embodiment, the high-melting-point ceramics constituent element powder 7 and low-melting-point metal of metal-base composites
Tungsten powder and copper is respectively adopted in constituent element 6, and to prepare W70Cu, the material theoretical volume ratio of tungsten powder and copper is 7:3, preparation side
Method is as follows：
1) tungsten powder prepared needed for material is taken, by grain mixture ratio, the bulk density for obtaining tungsten powder is 52%, standby
With taking one piece of copper billet, wherein the material of tungsten powder and copper billet is according to weight ratio 7:3.6 feeding；In 4 inside liner graphite paper of jacket
5, copper billet and tungsten powder are sequentially loaded into the closed jacket in one end 4；After being packed into jacket 4, opening of the tungsten powder close to jacket 4
End；
2) with the open end of the closed jacket in one end in an end socket 8 closing step (1) 4；It is open for closing jacket 4
The end socket 8 at end is equipped with a through-hole 9, and through-hole 9 can be connected to inside and outside jacket 4；Jacket 4 is packed into mold 1；The jacket 4
The upper die head 3 of blind end and mold 1 fit, the end socket 8 of 4 open end of jacket is affixed with the lower die head 2 of mold 1
It closes；
(3) mold 1 that jacket 4 is housed in step (2) is put into hot-press equipment, lower die head 2 and the hot pressing of mold 1 is set
Standby cooling pressure head fits；After being forced into 5MPa, 1100 DEG C are warming up to the heating rate of 20 DEG C/min；Meanwhile opening heat
Press the cooling pressure head of equipment so that the temperature at the lower die head 2 of mold 1 is maintained at 1040 DEG C；Keep the temperature 5min；
(4) during step (3) is kept the temperature, it is forced into 30MPa so that the copper of liquid is filled up completely of tungsten
In grain gap, until insulating process terminates；
(5) after step (3) are kept the temperature, room temperature is reduced to the rate of temperature fall of 30 DEG C/min；
(6) after step (5) terminates, blow-on takes out jacket 4 from mold 1, then takes out sample from jacket 4, obtains
Required metal-base composites W70Cu, density reach 14.2g/cm3。
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.Place is not described in detail by the present invention,
For the known technology of those skilled in the art of the present technique.
Claims (2)
1. a kind of Pressure Infiltration preparation method of metal-base composites, which is characterized in that include the following steps：
(1) low-melting-point metal constituent element and high-melting-point constituent element powder with certain bulk density are sequentially loaded into the closed packet in one end
In set, wherein high-melting-point constituent element powder be prepare total composite volume than 45%~90%；After being packed into jacket, high-melting-point
Constituent element powder is close to the open end of jacket；
(2) with the open end of the closed jacket in one end in end socket closing step (1)；In the envelope for closing jacket open end
Head is equipped with a through-hole, and through-hole can be connected to inside and outside jacket；Jacket is packed into mold；The blind end and mold of the jacket
Upper die head fit, the end socket of jacket open end and the lower die head of mold fit；
(3) mold that jacket is housed in step (2) is put into hot-press equipment, by the cooling of the lower die head of mold and hot-press equipment
Pressure head fits；After being forced into 0~5MPa, with the heating rate of 2~100 DEG C/min be warming up to low-melting-point metal constituent element fusing point with
Upper 5~150 DEG C；Meanwhile the temperature at the lower die head of mold is maintained at 5~150 DEG C of low-melting-point metal constituent element fusing point or less；Heat preservation
0~10min；
(4) during step (3) is kept the temperature, it is forced into 5~30MPa, until insulating process terminates；
(5) after step (3) are kept the temperature, room temperature is reduced to the rate of temperature fall of 2~100 DEG C/min；
(6) after step (5) terminates, blow-on is removed from the molds jacket, then takes out sample from jacket, obtains required
Metal-base composites；
The high-melting-point constituent element powder includes high-melting-point ceramics constituent element powder, silica flour or tungsten powder；
The low-melting-point metal constituent element includes any one in aluminium, copper, magnesium, aluminium alloy, magnesium alloy or copper alloy.
2. the Pressure Infiltration preparation method of metal-base composites according to claim 1, which is characterized in that the height
Melting ceramic constituent element powder includes boron carbide ceramics powder, silicon carbide ceramics powder, zirconium carbide ceramic powder, titanium carbide ceramic
A kind of in end, titanium nitride ceramic powder, zirconium nitride ceramic powders or wherein component be combined with each other two-by-two.
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| CN109396399B (en) * | 2018-12-13 | 2020-07-28 | 吉林大学 | Preparation device and preparation method of metal-based composite material combining pressure infiltration and negative pressure adsorption |
| CN109822077B (en) * | 2019-01-14 | 2021-07-27 | 东莞理工学院 | SiC prepared by extrusion infiltration method3DMethod for preparing/Al composite material |
| CN110791674B (en) * | 2019-11-13 | 2021-03-30 | 哈尔滨工业大学 | Preparation method of refractory carbide particle reinforced tungsten copper infiltrated composite material |
| CN110883496B (en) * | 2019-11-27 | 2021-08-24 | 哈尔滨工业大学 | High-volume-fraction SiC nanowire reinforced aluminum matrix composite densification device and method based on three-dimensional constrained deformation |
| CN112974773B (en) * | 2021-02-05 | 2021-12-10 | 哈尔滨工业大学 | Method for preparing high-strength plastic beryllium-aluminum composite material by pressure infiltration |
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