CN101941065B - Method forming endogenic crystal plasticized block amorphous base composite material - Google Patents
Method forming endogenic crystal plasticized block amorphous base composite material Download PDFInfo
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- CN101941065B CN101941065B CN2010102813516A CN201010281351A CN101941065B CN 101941065 B CN101941065 B CN 101941065B CN 2010102813516 A CN2010102813516 A CN 2010102813516A CN 201010281351 A CN201010281351 A CN 201010281351A CN 101941065 B CN101941065 B CN 101941065B
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Abstract
The invention relates to a method forming an endogenic crystal plasticized block amorphous base composite material, which is characterized by comprising the following steps: (1) completely melting mother alloy, adjusting the temperature to be 200-250 DEG C above liquidus temperature, keeping the temperature for 10-300 s, adjusting the temperature to be 80-100 DEG C above the liquidus temperature, keeping the temperature for 10-300 s, introducing argon gas with the pressure of P0 from the upper end of a pot, and injecting the liquid mother alloy to a pulping chamber under action of the differential pressure; (2) enabling the liquid mother alloy to flow downwards along the inner wall of the infundibuliform pulping chamber which vibrates at low frequency and high amplitude, and since the temperature of the inner wall is 20-90 DEG C, enabling the liquid mother alloy to be converted into the liquid-solid coexistent alloy molten mass the endogenic crystal phase volume percentage of which is 5-15% when the liquid mother alloy flows out of the pulping chamber; and (3) after the mother alloy flows into a high pressure die-cast injection chamber, cooling the mother alloy at the rate of 0.05-0.5 DEG C/s, and when the volume percentage of the endogenic crystal phase in the liquid-solid coexistent alloy molten mass reaches 15-30%, filling under high pressure, and carrying out forced cooling. The endogenic crystal phase of the invention is fine particles, has favorable thixotropy and can realize near formation of thin-walled complex parts.
Description
Technical field
The invention belongs to non-crystaline amorphous metal forming technique field, a kind of manufacturing process of crystal plasticising bulk amorphous alloy based composites precision component is provided especially.Can be used for the shaping of bulk amorphous alloy based composites such as zirconium system, copper system, titanium system, group of the lanthanides, magnesium system, aluminium system.
Technical background
Block amorphous alloy is because its higher elastic limit, bigger stretching and compressive strength and stronger many characteristics such as resistance to corrosion cause numerous material science workers' concern.Yet most block amorphous alloys show brittle fracture when at room temperature carrying.Make alloy melt when cooling off, separate out plastic crystals earlier mutually through minute adjusting alloying component and control cooling rate; Remainder melt forms noncrystal substrate in follow-up cooling procedure; Give birth to crystal plasticising bulk amorphous alloy based composites (C.C.Hays in obtaining; C.P.Kim; W.L.Jonhson.Microstructure controlled shear band pattern formation and enhanced plasticity of bulk metallic glasses containing in situ formed ductile phase dendrite dispersions.Physical Review Letters, 2000 (84): 2901-2904.).This type of material crystal when bearing load has stoped single shear band to run through whole sample mutually, and has facilitated the formation of multiple shear bands, has finally improved the plasticity of material.Because the interface energy of crystal phase and noncrystal substrate is low, both can very stably combine, and said material is to have temperature-room type plasticity to combine the high-intensity amorphous composite material that has the practical applications potentiality most of amorphous.
At present, the metallic glass composite of interior living crystal plasticising all is to make (U.S. Pat 00/11790 through methods such as shrend, spray to cast-suction casting, electric arc melting suction castings; Hui Xidong, Chen Guoliang. block amorphous alloy. Chemical Industry Press, 2006.).These methods belong to extreme cooling, can not control along the cooldown rate of bar-shaped specimen finish direction, make that the top layer cooldown rate of sample is high, and the core cooldown rate is low, top layer content of amorphous height and the core crystalline content is high.In recent years; Utilize the Bridgman directional solidification technique obtaining very ten-strike (tall skirt prestige aspect preparation lanthanum base and the zirconium Ji Neisheng crystal/noncrystal substrate composite; Zhang Yong, Chen Guoliang. give birth to the zirconium-base amorphous composite of crystal plasticising in the directional solidification preparation. Acta Metallurgica Sinica, 2009; 45 (4): 410-414.), give birth to the distribution of crystal in this method can be improved to a certain extent at sample section.But said method all is unfavorable for the industrialization of material preparation, the more important thing is that they can only prepare billet, can not be used to produce complex-shaped part.Another kind of method is a thermoplastic forming, and the superplasticity of promptly utilizing metallic glass composite to show in supercooling liquid phase region realizes the precision form of complex parts.But the realization of this superplastic deformation of non-crystaline amorphous metal has strong temperature and sensitivity of strain rate.The supercooling liquid phase region width of most large block amorphous composites of finding at present has only tens degree, and the temperature range that can supply process is very narrow.Rate of deformation (10 slowly
-2～10
-4s
-1), not only cause working (machining) efficiency very low, but also be very easy to cause non-crystaline amorphous metal that crystallization takes place in deformation process.
The interior crystal plasticising bulk amorphous alloy based composites of giving birth to is to constitute mutually with low-melting noncrystal substrate mutually by giving birth to crystal in dystectic.Between composite liquidus temperature and solidus temperature, interior living crystal phase and liquid phase coexistence form liquid-solid coexistence alloy melt.If interior living crystal is fine particle and evenly distributes that then this liquid-solid coexistence alloy melt has thixotropic behavior mutually, under the shearing force effect, viscosity reduces, and can be used for the shaping form complicated parts, is equipped with quick cooling simultaneously, and liquid phase will change noncrystal substrate into.The applicant has developed a kind of manufacturing process of bulk amorphous alloy based composites for this reason, (Guo Hongmin, Yang Xiangjie etc., the manufacturing process of bulk amorphous composite materials, application number: 201010178242.1), the precision component of the bulk amorphous alloy based composites that successfully is shaped.This invention at first adopts existing non-crystalline material technology of preparing to obtain high-purity bulk amorphous composite materials; Be cut to the ingot blank of specific dimensions according to formation of parts; Again billet is reheated the liquidus temperature and the solidus temperature interval of this composite; And then obtain liquid-solid coexistence alloy melt, and operation is more loaded down with trivial details, and cost is higher.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, propose a kind of interior manufacturing process of giving birth to crystal plasticising bulk amorphous alloy based composites.
The present invention is conceived to earlier interior living crystal plasticising bulk amorphous alloy based composites melted fully through the control heating, afterwards it is cooled to liquidus temperature and solidus temperature interval; Give birth to form, size and the distribution of crystal phase in the control; Obtain liquid-solid coexistence alloy melt, should fill mold cavity by liquid-solid coexistence alloy melt under external force, and under high pressure impel it to force cooled and solidified; Matrix is amorphous to obtain high-accuracy parts simultaneously keeping; Promptly directly obtain liquid-solid coexistence alloy melt, thereby shorten the manufacturing cycle and the cost of part significantly, a kind of former corresponding with it is provided simultaneously from liquid state.
The present invention realizes through following processing step:
(1) foundry alloy with interior living crystal plasticising bulk amorphous composite materials melts in crucible; The temperature of foundry alloy of fusing is fully adjusted to its more than liquidus temperature 200～250 ℃; Insulation 10～300s; And then should liquid state foundry alloy temperature adjusting to more than the liquidus temperature 80～100 ℃, insulation 10～300s; Importing pressure from the crucible upper end is P
0Argon gas, P is formed on the bottom
1Pressure, at pressure differential P
0-P
1Effect under, with liquid foundry alloy from the crucible spray to the infundibulate pulping chamber;
(2) liquid foundry alloy flows downward along the inwall with infundibulate pulping chamber of low frequency high amplitude vibration effect; Simultaneously; The inner wall temperature of infundibulate pulping chamber is controlled at 20～90 ℃, make liquid foundry alloy when flowing out the infundibulate pulping chamber, be transformed in life crystal phase volume percentage be 5～15% liquid-solid coexistence alloy melt;
(3) this liquid-solid coexistence alloy melt is flowed into the injection chamber of Hpdc, and in injection chamber, cool off with 0.05～0.5 ℃/s cooling velocity; When the percent by volume of the interior living crystal phase in the liquid-solid coexistence alloy melt reaches 15～30%, through high pressure this liquid-solid coexistence alloy melt is filled type, and make it under high pressure force cooling, and then obtain high-performance, high-accuracy part.
In the inventive method, the liquid phase in the liquid-solid coexistence alloy melt should possess very high glass forming ability, can select non-crystaline amorphous metal compositions such as zirconium system, copper system, titanium system, group of the lanthanides, magnesium system, aluminium system.
In the methods of the invention, foundry alloy fusing, the preparation of liquid-solid coexistence alloy melt and the whole technical process of shaping are all carried out in an operating room.At first, the vacuum that vacuumizes in the operating room reaches 3 * 10
-3Pa charges into the pressure of argon gas in the operating room then and reaches P
1
In said step (1), the pressure differential P that crucible is inside and outside
0-P
1Should be controlled at 14～50kPa, the angle between injection direction and pulping chamber central axis should be controlled at 0～60 degree.
In said step (2), liquid foundry alloy is flowed through in the infundibulate pulping chamber process, and the infundibulate pulping chamber is done the vibration of low frequency high amplitude around its central axis, and frequency is 0.5～5 time/second, and amplitude is 0～5 degree (and ≠ 0); Infundibulate pulping chamber outer wall is provided with the cooling duct, and the type of cooling is recirculated water, wet goods, and the inner wall temperature of infundibulate pulping chamber is controlled at 20～90 ℃.
In the inventive method, in said step (3), the cooling velocity of liquid-solid coexistence alloy melt in mold cavity should reach 1～200 ℃/s, guarantees the extremely cold fast formation noncrystal substrate of liquid in the liquid-solid coexistence alloy melt.
The present invention compares with existing manufacturing process, has following remarkable advantage:
(1) liquid-solid coexistence alloy melt complete filling mold cavity in a few tens of milliseconds, this will cause higher cooling velocity.The effect of high pressure makes and more closely contacts between the liquid-solid coexistence alloy melt and mould type wall in the whole freezing period, thereby increases the heat exchange coefficient of liquid-solid coexistence alloy melt and mould type wall surface, thereby improved cooling velocity.Therefore the present invention has improved amorphous formation ability, and then enlarges the range of application of manufacturing process of the present invention, can be widely used in amorphous composite materials such as zirconium system, copper system, titanium system, group of the lanthanides, magnesium system.
(2) liquid-solid coexistence alloy melt has higher viscosity, guarantees steadily to fill type, avoids casting flaws such as pore and contraction effectively.And liquid-solid coexistence alloy melt has been realized partial coagulation before shaping, so forming temperature is low, has greatly reduced in being shaped the thermal shock of mould, greatly improves die life.
(3) the interior living crystal in the liquid-solid coexistence alloy melt that obtains of the present invention is the fine particle shape mutually, but not thick dendroid, thereby liquid-solid coexistence alloy melt has good thixotropy, can realize the nearly shaping of thin-wall complicated part.
Description of drawings
Fig. 1 is the used Hpdc device sketch map of interior living crystal plasticising bulk amorphous composite materials shaping.Among the figure: drift, 4d die casting, 4e die cavity, 5 vacuum systems, 6 gas protection system and 7 temperature acquisitions and the control system of the injection chamber of 1 operating room, 2a crucible, 2b high-frequency induction heating apparatus, 2c gases at high pressure control module, 3 infundibulate pulping chambers, 4a die casting machine, 4b Frequency Induction Heating unit, 4c die casting machine.
Fig. 2 is an infundibulate pulping chamber sketch map.Among the figure: 3a inner core, 3b cooling duct, 3c cooling medium, the outlet of 3d cooling medium, 3e cooling medium inlet.
Fig. 3 is Hpdc Zr
36.6Ti
31.4Cu
5.9Nb
7Be
19.1The XRD spectrum of alloy part.
The specific embodiment
The present invention will be described further through following examples.
Fig. 1 is the interior living crystal plasticising bulk amorphous composite materials Hpdc building mortion applicable to embodiment of the present invention.Mainly comprise: operating room 1, place foundry alloy fusing spray portion 2, infundibulate pulping chamber 3 and Hpdc forming section 4 in the operating room, and vacuum system 5, gas protection system 6, temperature acquisition and control system 7.Fusing spray portion 2 comprises crucible 2a, places high-frequency induction heating apparatus 2b around this crucible 2, places the gases at high pressure control module 2c of these crucible 2 tops for the liquid foundry alloy M in this crucible 2 of spray for the foundry alloy M in this crucible 2 of heat fused; These crucible 2 bottoms have the aperture of certain diameter; Liquid foundry alloy M can not flow out from this crucible 2a when no ambient pressure, and the pressure that produces at gases at high pressure control module 2c is P
0The effect of high pressure argon gas under, can the liquid foundry alloy M among the crucible 2a be sprayed into infundibulate pulping chamber 3 from this aperture.Infundibulate pulping chamber 3 is made up of inner core 3a, cooling duct 3b, cooling medium 3c, cooling medium outlet 3d, cooling medium inlet 3e; Liquid foundry alloy M is through inner core 3a inflow suitable for reading, and the liquid-solid coexistence alloy melt that forms through cooling flows into Hpdc portion 4 through inner core 3a end opening.Hpdc portion 4 is made up of injection chamber 4a, Frequency Induction Heating unit 4b, the drift 4c of die casting machine, die casting 4d, the die cavity 4e of die casting machine.Vacuum system 5 is responsible for extracting the gas in the operating room 1 out and reaching vacuum 3 * 10
-3Pa, gas protection system 6 is responsible in operating room 1, charging into protective gas, acts on down at both, and the operating pressure in the operating room 1 is P
1Temperature acquisition and control system 7 are responsible for gathering and the temperature of the interior foundry alloy M of control crucible 2a and the temperature of injection chamber 4a.The structure of infundibulate pulping chamber 3 is seen Fig. 2, and the vertical height of inner core 3a is 400～600mm, back cut diameter 100～600mm, lower port diameter 10～400mm.For circulating cooling medium 3c, this cooling medium 3c flows into from cooling medium inlet 3e in the arranged outside cooling duct 3b, this cooling duct 3b, and 3d flows out from the cooling medium outlet.Intermediate frequency induction heating device 4b is set, the cooling of the liquid-solid coexistence alloy melt in temperature acquisition and 7 this injection chamber of the regulation and control 4a of control system around the injection chamber 4a of Hpdc portion 4.The die casting 4d of Hpdc portion 4 is high pressure resistant copper mold, and inside is provided with the cooling duct, makes the liquid extremely cold fast formation noncrystal substrate in die cavity 4e in the liquid-solid coexistence alloy melt.
The foundry alloy M that gives birth to crystal plasticising bulk amorphous composite materials in high-purity is placed crucible 2a.Vacuum system 5 vacuumizes operating room 1 up to 3 * 10
-3Pa charges into argon gas through gas protection system 6 in operating room 1, the pressure in operating room 1 reaches P
1High-frequency induction heating apparatus 2b adjusts to its more than liquidus temperature 200～250 ℃ with foundry alloy M fusing and with its temperature; And be incubated 10～300s; Then through temperature acquisition and control system 7 should the liquid state foundry alloy temperature adjusting to more than the liquidus temperature 80～100 ℃, insulation 10～300s.It is P that gases at high pressure control module 2c imports pressure
0Argon gas, at pressure differential P
0-P
1Effect under, the infundibulate pulping chamber is gone in liquid foundry alloy M spray.Liquid foundry alloy M flows downward along the inwall of inner core 3a; Cooling duct 3b can make the temperature of inner core 3a be controlled at 20～90 ℃; Infundibulate pulping chamber 3 is done the vibration of low frequency high amplitude around its central axis simultaneously; Frequency is 0.5～5 time/second, and amplitude is 0～5 degree (and ≠ 0), make liquid foundry alloy M when flowing out infundibulate pulping chamber 3, be transformed in life crystal phase volume percentage be 5～15% liquid-solid coexistence alloy melt.This liquid-solid coexistence alloy melt flows in the injection chamber 4a of Hpdc forming section 4, and slowly cooling, and cooling velocity is 0.05～0.5 ℃/s.When the percent by volume of the interior living crystal phase in the liquid-solid coexistence alloy melt reaches 15～30%; Drift 4c starts; Liquid-solid coexistence alloy melt is pushed fast among the die cavity 4e of die casting 4d; Pressurize also makes liquid-solid coexistence alloy melt under high pressure force cooling, and cooling velocity should reach 1～200 ℃/s.
The above is merely embodiment of the present invention, does not limit the present invention, all within spirit of the present invention and principle any modification, be equal to replacement and improve, all should be included in protection scope of the present invention.
Embodiment.
Adopting Hpdc device shaping cross dimensions illustrated in figures 1 and 2 is the column of 3mm, and foundry alloy is Zr
36.6Ti
31.4Cu
5.9Nb
7Be
19.1Alloy, about 1100 ℃ of liquidus temperature, the interior crystal phase volume percentage of giving birth to is about 41% during as cast condition.Vacuum system is evacuated down to 3 * 10 with the operating room
-3Pa, gas protection system charges into argon gas in the operating room, and atmosphere of the pressure ratio in the operating room forces down 16kPa.With Zr
36.6Ti
31.4Cu
5.9Nb
7Be
19.1Foundry alloy melts in crucible, and the temperature of foundry alloy of fusing is fully adjusted to its more than liquidus temperature 200 ℃, and insulation 10s regulates and control this alloy liquid temp to more than the liquidus temperature 80 ℃ insulation 60s then.Import the argon gas than the big 20kPa pressure of atmospheric pressure from the crucible upper end, from spray in the crucible to the infundibulate pulping chamber, injection direction is parallel with infundibulate pulping chamber central axis with liquid foundry alloy.The temperature of infundibulate pulping chamber inner core is controlled at 50 ℃; The type of cooling is a recirculated water; Simultaneously the infundibulate pulping chamber is done vibration around its central axis with the parameter of frequency 2 times/second, amplitude 3 degree, make liquid foundry alloy when flowing out the infundibulate pulping chamber, be transformed in life crystal phase volume percentage be 8% liquid-solid coexistence alloy melt.This liquid-solid coexistence alloy melt flows into the injection chamber of Hpdc, and cools off with the speed of 0.1 ℃/s.When the percent by volume of the interior living crystal phase in the liquid-solid coexistence alloy melt reached 20%, drift pushed the mold cavity that high pressure resistant copper mold constitutes with the speed of 30mm/s with this liquid-solid coexistence alloy melt, and pressurize 10 seconds.
Fig. 3 is Zr
36.6Ti
31.4Cu
5.9Nb
7Be
19.1The XRD of column section spectrum behind the alloy Hpdc, obviously the bright and sharp diffraction maximum corresponding to crystal second phase is superimposed upon on the climing scattering peak with typical amorphous characteristic.In addition do not find anyly, show that part behind the Hpdc gives birth to crystal in having mutually and two microstructures mutually of noncrystal substrate obviously corresponding to the diffraction maximum of other crystal phase.The interior crystal of giving birth to is fine particle, about 26 microns of size mutually, on sample section, is evenly distributed.The die casting porosity is 0.5%, and main mechanical performance index is: tensile strength 1620MPa, yield strength 1512MPa, percentage elongation 11.3%.
Claims (5)
1. give birth to the manufacturing process of crystal plasticising bulk amorphous alloy based composites in one kind, it is characterized in that:
(1) adjust to its more than liquidus temperature 200～250 ℃ with foundry alloy fusing fully in crucible, and with its temperature, insulation 10～300s, and then should liquid state foundry alloy temperature adjusting to more than the liquidus temperature 80～100 ℃, be incubated 10～300s; Importing pressure from the crucible upper end is P
0Argon gas, P is formed on the bottom
1Pressure, at pressure differential P
0-P
1Effect under, with liquid foundry alloy from the crucible spray to the infundibulate pulping chamber;
(2) liquid foundry alloy flows downward along the inwall with infundibulate pulping chamber of low frequency high amplitude vibration effect; Simultaneously; The inner wall temperature of infundibulate pulping chamber is controlled at 20～90 ℃, make liquid foundry alloy when flowing out the infundibulate pulping chamber, be transformed in life crystal phase volume percentage be 5～15% liquid-solid coexistence alloy melt;
(3) this liquid-solid coexistence alloy melt is flowed into the injection chamber of Hpdc, and in injection chamber, cool off with 0.05～0.5 ℃/s cooling velocity; When the percent by volume of the interior living crystal phase in the liquid-solid coexistence alloy melt reaches 15～30%, through high pressure this liquid-solid coexistence alloy melt is filled type, and make it under high pressure force cooling.
2. weigh described method according to claim, it is characterized in that the liquid phase in the liquid-solid coexistence alloy melt is that zirconium system, copper system, titanium system, group of the lanthanides, magnesium system or aluminium are the non-crystaline amorphous metal composition.
3. method according to claim 1 is characterized in that in said step (1), the pressure differential P that crucible is inside and outside
0-P
1Should be controlled at 14～50kPa, the angle between injection direction and pulping chamber central axis should be controlled at 0～60 degree.
4. method according to claim 1 is characterized in that in said step (2), and liquid foundry alloy is flowed through in the infundibulate pulping chamber process, and the infundibulate pulping chamber is done the vibration of low frequency high amplitude around its central axis, and frequency is 0.5～5 time/second, 0＜amplitude≤5 degree; Infundibulate pulping chamber outer wall is provided with the cooling duct, and the type of cooling is recirculated water or oil.
5. method according to claim 1 is characterized in that in said step (3) cooling velocity of liquid-solid coexistence alloy melt in mold cavity is 1～200 ℃/s.
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