CN100537802C - A kind of method for preparing high dense TiAl-base alloy - Google Patents
A kind of method for preparing high dense TiAl-base alloy Download PDFInfo
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- CN100537802C CN100537802C CNB2007100343834A CN200710034383A CN100537802C CN 100537802 C CN100537802 C CN 100537802C CN B2007100343834 A CNB2007100343834 A CN B2007100343834A CN 200710034383 A CN200710034383 A CN 200710034383A CN 100537802 C CN100537802 C CN 100537802C
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Abstract
A kind of method for preparing high dense TiAl-base alloy is a raw material with Ti powder, Al powder and other micro-powder, and raw material powder carries out homogenizing and mixes back employing mold pressing or isostatic cool pressing cold-press moulding, retrains presintering in the sintering mould, high temperature sintering, hot isostatic pressing.The raw material that the present invention adopts is element ti powder, Al powder and other alloying element powder, and raw materials cost is low; Compare with hot pressing, extrusion process, technology of the present invention is simple, and equipment is conventional equipment, can effectively reduce cost; The density height of the TiAl alloy material of preparation can reach more than 98% through average density after the hip treatment; To compared with the metallurgical method for preparing high dense TiAl-base alloy of other element powders, as hot pressing, extruding etc., the big (d＞100mm), be suitable for suitability for industrialized production of size of the TiAl base alloy billet that the present invention is prepared.
Description
Technical field
The present invention relates to a kind of preparation method of high dense TiAl-base alloy, belong to field of powder metallurgy.
Background technology
The castability of TiAl base alloy is relatively poor, easily produce the as cast condition defective, and powder metallurgy process has clear superiority at aspects such as eliminating macroscopical component segregation, loose, shrinkage cavity, the while powder metallurgy process prepares TiAl base alloy and also has homogeneous microstructure, tiny, can realize the newly net forming of product, thereby the difficulty that can avoid TiAl base alloy to be difficult to plastic making and mechanical workout reduces production costs and waits process characteristic, makes powder metallurgy process become a kind of important method for preparing the basic alloy of TiAl.Divide by starting material, utilize powder metallurgy process to prepare TiAl base alloy and can be divided into prealloy powder method and element powders method.Owing to fusing point height, the activity of Ti are big, the preparation of TiAl base alloy pre-alloyed powder needs strict CONTROL PROCESS, and with impurity such as minimizing oxygen, nitrogen, so price is very expensive.The element powders method adopts element ti, Al powder, do not need expensive prealloy powder and complicated processing unit, can effectively reduce production cost, simultaneously can also add various high molten alloy elements very easily, mix and pyroreaction by homogenizing, can effectively avoid component segregation, these all make the element powders method become a kind of very promising TiAl base alloy preparation technology.
Ti, Al element powders usually with the expansion significantly of volume, adopt the porosity of conventional vacuum sintering gained can arrive 30%～40% when TiAl base alloy is produced in reaction, even adopt the postorder hip treatment all to eliminate.Because the compactness extent of sintered metal product has decisive influence to its use properties, volumetric expansion is very unfavorable to follow-up processing and use.At present, the volumetric expansion significantly that produces during for restricted T i, the reaction of Al element powder, the technology that the metallurgical TiAl base of the high dense powder of multiple preparation alloy occurred is as heat pressing process, extruding and vacuum sintering, hot isostatic pressing process combined and Ceracon quasi-iso static pressing technology etc.Adopt heat pressing process can effectively suppress powder Ti, the Al expansion behavior in reaction process, and under the assistance of pressure, promote the densification behavior of Ti, Al element powders, thereby can effectively eliminate hole, obtain the material of high-compactness, the Liu Yong of Central South University etc. has been systematic research [Processing TiAl-Based alloy by Elemental Powder Metallurgy, Journal of MaterialsScience to the hot pressed sintering behavior of element ti, Al; Technology, 2000,16 (6), 605～610].Volumetric expansion effect when extruding and vacuum sintering, hot isostatic pressing process combined also can effectively reduce sintering obtains near fully dense TiAl base alloy [Wang G X, Dahms M.Synthesizing Gamma-TiAl Alloys by Reactive PowderProcessing.JOM, 1993 (5): 52～56], the purpose of extruding mainly is to destroy the oxide film of Ti, Al particle surface, by big extrusion ratio element ti, Al homogenizing on microcosmos area is more mixed simultaneously, thereby help the diffusion reaction of element ti, Al; Blank after the extruding is fibrous in the tissue topography that is parallel to the direction of extrusion, because the Al particle is extruded into fiber fines, the hole that stays after reaction is finished is very little, can effectively eliminate by vacuum sintering and follow-up hot isostatic pressing.But when this cold-pressing deformation method refinement Ti, Al constituent element size, must adopt the superelevation extrusion ratio, (extrusion ratio is 350), thereby this method is difficult to practical application industrial.In addition, someone also adopts Ceracon quasi-iso static pressing technology to obtain the TiAl base alloy [TaguchiK of high-compactness, Ayada M, et al.Near-net shape processing of TiAl intermetallic compounds ovapscudo HIP-SHS route.Intermetallics, 1995,3:91～98], in this technology when unidirectional stress is on ceramic particle, ceramic particle can evenly pass to pressure on the pressed compact as transmission medium, pressed compact is finished the densification behavior under the effect of three-dimensional stress (quasi-iso static pressing power).
More than a common ground of all multi-methods be exactly that technology is all comparatively complicated, cost is higher, is difficult to realize suitability for industrialized production.
Summary of the invention:
The object of the present invention is to provide the technology of preparing of the metallurgical TiAl base of the cheap relatively high fine and close element powders of a kind of cost alloy, this technology adopts Ti powder, Al powder and other element powders directly to produce high fine and close TiAl base alloy material through low temperature control presintering+high temperature sintering.
A kind of method for preparing high dense TiAl-base alloy comprises:
1, be raw material with Ti powder, Al powder and other micro-powder, the constituent atoms proportioning is 50～60%Ti powder, 40～50%Al powder, 0～10% micro-powder; The particle diameter of Ti powder is 20～100 μ m, and the particle diameter of Al powder is 10～100 μ m, and trace element comprises Nb, Mn, C, Si, B, W, Y, Ce, TiB or TiB
2In one or several, the particle diameter of micro-powder is 20～100 μ m;
2. raw material powder carries out adopting mold pressing or isostatic cool pressing cold-press moulding to make the base of colding pressing after homogenizing is mixed, and pressure is 50～600Mpa during die forming, and pressure is 50～200Mpa during cold isostatic compaction;
3, the base of will colding pressing is put into constraint sintering mould, carries out vacuum and do not have the presintering of pressure and get the presintering base in vacuum sintering furnace, and vacuum tightness is 1 x 10
-1～10
-3Pa; The presintering system is: 200 ℃～250 ℃, and time 0.5～2h, 400 ℃～450 ℃, time 0.5～2h, 600 ℃～650 ℃, time 3～5h, 700 ℃～750 ℃, time 1～3h, each section temperature rise rate is 5 ℃/min, and top temperature is 800 ℃, and total treatment time is 5～12h;
4, remove constraint sintering mould after presintering is finished, the presintering base is carried out high temperature sintering again, high temperature sintering vacuum tightness is 1 x 10
-1～10
-3Pa is at 1200～1400 ℃ of insulation 1～3h, cold with stove;
5, the alloy billet behind high temperature sintering is carried out hot isostatic pressing to eliminate remaining hole, hot isostatic pressing carries out under Ar gas atmosphere, and pressure is 150～200Mpa, and temperature is 1200～1300 ℃, and the time is 3～5h.
The presintering process is carried out in constraint sintering mould, and constraint sintering mould is combined by gland, internal mold and external mold; Internal mold is the type of the carving structure of the symmetric band tapering of two lobes, and conicity angles alpha (angle of inclined-plane and vertical direction) is 15 °～45 °; When pressed compact was put into internal mold, sandwiching a layer thickness between base substrate and mould inner wall was the molybdenum sheet interlayer of 1mm; Internal mold integral body is put into external mold, low pressure compacting on pressing machine then after gland is bumped into the internal mold opening end.
Raw material of the present invention is element ti powder, Al powder and other alloying element powder, and raw materials cost is low; Compare with hot pressing, extrusion process, technology of the present invention is simple, and equipment is conventional equipment, can effectively reduce cost; Though low temperature, high-temperature sintering process are to adopt pressureless sintering among the present invention, but the density height of the TiAl alloy material of its preparation, can reach more than 98% through average density after the hip treatment, this density than the TiAl base alloy of the pressureless sintering method preparation of routine is much higher, close with the density of the TiAl of prepared such as hot pressing, extruding base alloy, and the each several part porosity difference of blank is little; To prepare the method for high dense TiAl-base alloy compared with other element powders metallurgy, as hot pressing, extruding etc., the size of the prepared TiAl of the present invention base alloy billet big (d〉100mm), and the profile of blank can do suitable adjustment as required, is suitable for suitability for industrialized production.
Description of drawings:
Fig. 1, process flow sheet of the present invention;
The structural representation of constraint sintering mould among Fig. 2, the present invention;
The process curve figure of control presintering process among Fig. 3, the present invention;
The TiAl base alloy material photomacrograph that Fig. 4, the present invention produce.
Embodiment
Embodiment 1: the employing granularity is that Ti powder and the granularity of 20～50 μ m is the Al powder of 20～50 μ m, carries out batch mixing by the composition proportion of Ti-50at.%Al; Die forming under the pressure of 200Mpa subsequently, making diameter is 120mm, the base of colding pressing of high 45mm; As Fig. 2, the base 4 of will colding pressing is put into constraint sintering internal mold 3, and pressed compact and interior intermode separate with molybdenum interlayer 2, then internal mold integral body are put into sintering external mold 5, on use gland 1 low pressure compacting on pressing machine.The constraint sintering mould that assembles is put into vacuum sintering furnace adopts process curve shown in Figure 3 to carry out vacuum presintering; Remove constraint sintering mould subsequently, the presintering blank is carried out the high-temperature vacuum sintering, sintering schedule is 1300 ℃, and 2h is cold with stove; Carry out hip treatment at last under Ar atmosphere, processing condition are 1250 ℃, 130Mpa, 4h.The TiAl alloy material that makes is of a size of d110mm * 35mm, and density is 97%.
Embodiment 2: the employing granularity is that Ti powder, the granularity of 20～50 μ m is the Al powder of 20～50 μ m and Nb powder and the W powder that granularity is 20～50 μ m, carries out batch mixing by the composition proportion of Ti-45Al-7Nb-0.4W (at.%); Die forming under the pressure of 200Mpa subsequently, making diameter is 120mm, the base of colding pressing of high 45mm; Pressed compact is put into constraint sintering mould, adopt process curve shown in Figure 3 to carry out vacuum presintering; Carry out vacuum high-temperature sintering subsequently, sintering schedule is: 1300 ℃, 2h is cold with stove; Carry out hip treatment at last, processing condition are 1250 ℃, 130Mpa, 4h; The fine and close base of TiAl base alloy that makes is of a size of d108mm * 34mm, and density is 97.5%.
Claims (4)
1. method for preparing high dense TiAl-base alloy is characterized in that: comprising:
(1) be raw material with Ti powder, Al powder and other micro-powder, the constituent atoms proportioning is 50～60%Ti powder, 40～50%Al powder, 0～10% micro-powder; The particle diameter of Ti powder is 20～100 μ m, and the particle diameter of Al powder is 10～100 μ m, and the particle diameter of micro-powder is 20～100 μ m;
(2) raw material powder carries out adopting die forming to make the base of colding pressing after homogenizing is mixed, and pressure is 50～600Mpa during die forming;
(3) base of will colding pressing is put into constraint sintering mould, carries out vacuum and do not have the presintering of pressure and get the presintering base in vacuum sintering furnace, and vacuum tightness is 1 x 10
-1～10
-3Pa; The presintering system is: 200 ℃～250 ℃, and time 0.5～2h, 400 ℃～450 ℃, time 0.5～2h, 600 ℃～650 ℃, time 3～5h, 700 ℃～750 ℃, time 1～3h, each section temperature rise rate is 5 ℃/min, and top temperature is 800 ℃, and total treatment time is 5～12h;
(4) remove constraint sintering mould after presintering is finished, the presintering base is carried out high temperature sintering again, high temperature sintering vacuum tightness is 1 x 10
-1～10
-3Pa is at 1200～1400 ℃ of insulation 1～3h, cold with stove;
(5) alloy billet behind high temperature sintering is carried out hot isostatic pressing to eliminate remaining hole, hot isostatic pressing carries out under Ar gas atmosphere, and pressure is 150～200Mpa, and temperature is 1200～1300 ℃, and the time is 3～5h.
2. method according to claim 1 is characterized in that: described trace element comprises Nb, Mn, C, Si, B, W, Y, Ce, TiB or TiB
2In one or several.
3. method according to claim 1 is characterized in that: raw material powder carries out also can adopting the isostatic cool pressing cold-press moulding to make the base of colding pressing after homogenizing is mixed in the step (2), and pressure is 50～200Mpa during cold isostatic compaction.
4. a constraint sintering mould that is used for the described method of claim 1 is characterized in that: retrain the sintering mould and combined by gland, internal mold and external mold; Internal mold is the type of the carving structure of the symmetric band tapering of two lobes, and conicity angles alpha is 15 °～45 °; When pressed compact was put into internal mold, sandwiching a layer thickness between base substrate and mould inner wall was the molybdenum sheet interlayer of 1mm.
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