CN100445415C - Heat processing technique for thinning TiAl-base alloy sheet interlayer spacing - Google Patents
Heat processing technique for thinning TiAl-base alloy sheet interlayer spacing Download PDFInfo
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- CN100445415C CN100445415C CNB2007101197661A CN200710119766A CN100445415C CN 100445415 C CN100445415 C CN 100445415C CN B2007101197661 A CNB2007101197661 A CN B2007101197661A CN 200710119766 A CN200710119766 A CN 200710119766A CN 100445415 C CN100445415 C CN 100445415C
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Abstract
A heat treatment of TiAl based alloy is used to fine lamellar distance, which is available for TiAl with 45-51at% Al content or TiAl with 42-46at% Al and 5-10at% Nb. Cast ingots are treated by homogenizing, heat isopressing, and aging at alpha and gamma zones cyclically. Parameters, e.g. heating and cooling rates, temperatures are all controlled to refine layer distance while keeping lamellar status.
Description
Technical field
The present invention relates to a kind of heat treatment of alloy technology, specifically, be meant the thermal treatment process about the refinement of TiAl base alloy sheet interlayer spacing, the alloy sheet interlayer tissue after the refinement has good homogeneous and stability.
Background technology
TiAl base alloy is a kind of novel high-temperature structural material, have high-melting-point, low density, high elastic coefficient and advantages such as hot strength, fire retardancy, oxidation-resistance preferably, be a kind of novel light high-temperature structural material of having very much an application prospect, the aircraft engine of future generation that is considered to have competition potential is with one of structured material.Its superiority is mainly reflected in following three aspects: the first, and TiAl base alloy has high specific tenacity.As structured material, TiAl base alloy has higher modulus of elasticity, and is high more about 50% than the structured material of present application, and its density has only 3.7～3.9g/cm
3, to compare with nickel base superalloy, the density of TiAl base alloy is lower than nickel base superalloy density (7.9～9.5g/cm
3) half, this is for the aircraft engine parts, its superiority is self-evident; Second, the creep temperature limit of TiAl base alloy is 750 ℃～950 ℃, the oxidation resistance temperature limit is 800 ℃～950 ℃, near 870 ℃～1090 ℃ of 800 ℃～1090 ℃ of the creep temperature limit of nickel base superalloy and the oxidation resistance temperature limit, so the TiAl base alloy big nickel base superalloy of potential alternative density and as the material of some parts; The 3rd, TiAl base alloy has the good flame performance, and is suitable with nickel base superalloy, can substitute expensive flame retardant resistance titanium base alloy parts.Yet lower temperature-room type plasticity, hot strength and the fracture toughness property of TiAl base alloy seriously hindered it and entered the process of practicability.
At the problem of TiAl base alloy temperature-room type plasticity difference, from present present situation, the reason of temperature-room type plasticity difference mainly contains: the order and the interatomic covalent bonds characteristic of atomic arrangement in (one) TiAl base alloy; (2) the less and deformation mechanism complexity of microdeformation mode; (3) coarse microstructure and interface bond strength are low etc.For this reason, improve its temperature-room type plasticity by alloying, change material preparation and methods such as moulding process, the hot-work of change material and thermal treatment process.Result of study shows that its room-temperature mechanical property in the microstructure remarkably influenced of TiAl base alloy, and tiny, uniform microstructure can make alloy in the higher mechanical behavior under high temperature of maintenance, obtains higher room-temperature mechanical property.Can change the structural state of TiAl base alloy cast ingot effectively by thermal treatment or hot mechanical treatment, make its microstructure obtain effective refinement.The heat treating method of having reported mainly contains quenching/tempering heat treatment, cycle heat treatment, two warm processing etc., the main starting point of these technologies is to obtain even, the tiny microstructure of crystal particle scale, lay particular emphasis on the refinement of crystal particle scale, and at the sheet interlayer spacing problem of its inside, generally be to obtain thin brilliant intermediate phase transformation tissue (being generally bifurcation tissue or nearly γ tissue) by thermal treatment afterwards, to be heated to α single phase region solid solubility temperature T once more
αMore than handle, come the size of control strip interlamellar spacing by controlled chilling speed.Yet, full lamella TiAl base alloy at tool using value, no matter the size of its crystal particle scale, whether carry out Overheating Treatment, to control its sheet interlayer spacing by solid solution/refrigerative mode, can there be following 2 problems: the first, the phenomenon of growing up of crystal grain unavoidably can appear in the solution treatment process, and wayward, in the α single phase region, crystal particle scale and soaking time satisfy D=kt
n(k represents the constant relevant with thermal treatment temp and alloying constituent, and n represents the grain growth factor) relation; The second, speed of cooling has the featheriness tissue too soon, Wei Shi body tissue occurs, and influences structure stability.
In actually operating, no matter be, all unavoidably face the thick problem of sheet interlayer spacing in the preparation of TiAl base alloy or in hot-work, heat treatment process, be unfavorable for TiAl base alloy structure and optimization in Properties.For TiAl base alloy, its sheet interlayer spacing and alloy strength satisfy the Hall-Petch relation, and hour at crystal particle scale, the refinement of sheet interlayer spacing is obvious further to the alloy Effect on Performance, be that the refinement slices interlamellar spacing can effectively improve TiAl base alloy at room temperature plasticity, room temperature and hot strength, can improve fracture toughness property, the reduction crack growth rate of alloy simultaneously.So at full lamella TiAl base alloy, when not destroying photomacrograph layer tissue form, keeping it to organize superiority, the heat treating regime of exploring the refinement slices interlamellar spacing has very big realistic meaning and using value.
Summary of the invention
For problem such as solve TiAl base alloy temperature-room type plasticity and fracture toughness property is poor, intensity is low, the present invention proposes a kind of thermal treatment process of thinning TiAl-base alloy sheet interlayer spacing.Mainly be the circulation ageing treatment of carrying out in the α+γ two-phase region of TiAl base alloy by a kind of, effectively refinement its sheet interlayer spacing, thereby improved TiAl base alloy at room temperature plasticity and fracture toughness property, and improved its room temperature and hot strength.The present invention is a kind of thermal treatment process of thinning TiAl-base alloy sheet interlayer spacing, and this thermal treatment process comprises pre-treatment and circulation ageing treatment two portions, and described circulation ageing treatment is carried out in α+γ two-phase region, and concrete processing step is:
The first step: will be heated to 1200 ± 20 ℃ of first humidity provinces of α+γ two-phase region, insulation 2～5min through pretreated TiAl base alloy;
Second step: with rate of heating v
hTiAl base alloy after first step is handled is heated to 1300 ± 20 ℃ of second humidity provinces, insulation 15～30min;
Described rate of heating v
h=1.0 * 10
-3～2.0 * 10
-1℃/s;
The 3rd step: with speed of cooling v
cTo be cooled to 1200 ± 20 ℃ of first humidity provinces through the base of the TiAl after second step process alloy, and be incubated 2～5min;
Described speed of cooling v
c=1.0 * 10
-3～9.0 * 10
-1℃/s;
The 4th step: repeat second step and third step 2～6 times, cool to room temperature, taking-up then with the furnace, obtain the TiAl base alloy of sheet interlayer spacing refinement.
In the present invention, described pre-treatment includes homogenizing and hip treatment, and the temperature that homogenizing is handled is 800 ℃～1100 ℃, and soaking time is 12～48h; The temperature of hip treatment is 1200～1300 ℃, and pressure is 170～220MPa, and soaking time is 3～5h.
In the present invention, the TiAl base alloy sheet interlayer spacing is after thinning processing, and its temperature-room type plasticity is improved significantly, and can reach 2.5%～3.0%, improves about 20%～30% than the TiAl base alloy without the lamella refinement; Simultaneously, the hot strength of TiAl after lamella refinement base alloy and fracture toughness property be improved significantly, improve about 10%～25% than TiAl base alloy without the lamella refinement.On the other hand, this technology is not only applicable to the TiAl base alloy of Al content 45at%～51at%, but also is applicable to the high-Nb TiAl-base alloy of Al content 42at%～46at%, content of niobium 5at%～10at%; Be not only applicable to the as-cast state TiAl based alloy of the type that is smelted into, and be applicable to general T iAl base alloy and high-Nb TiAl-base alloy after Overheating Treatment with thick sheet interlayer spacing.Because this technology is simple, easy to operate, the spacing thinning effect is obvious and be easy to realization, so the present invention has bigger using value.
Description of drawings
Fig. 1 is the structural transformation synoptic diagram in two-phase region " heating-insulation-cooling " process.
Fig. 2 A is a pretreated Ti-47Al-2Cr-2Nb alloy sheet interlayer tissue topography.
Fig. 2 B, 2C, 2D are that heat-up rate is respectively 3.33 * 10
-2℃/s, 6.67 * 10
-2℃/s, 1.33 * 10
-1℃/the lamellar structure pattern of the Ti-47Al-2Cr-2Nb alloy of s correspondence.
Fig. 3 is a Ti-47Al-2Cr-2Nb alloy at room temperature tensile property correlation curve after the thinning processing.
Fig. 4 is the Ti-Al binary phase diagram.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention is a kind of thermal treatment process of thinning TiAl-base alloy sheet interlayer spacing, is to carrying out through casting or the TiAl of scull moulding base alloy cast ingot, and this thermal treatment process comprises pre-treatment and circulation ageing treatment two portions.
Wherein, pre-treatment includes homogenizing and hip treatment, and the temperature that homogenizing is handled is 800 ℃～1100 ℃, and soaking time is 12～48h; The treatment temp of hot isostatic pressing is 1200～1300 ℃, and pressure is 170～220MPa, and soaking time is 3～5h.
Wherein, the circulation ageing treatment is carried out in α+γ two-phase region, and concrete implementation step has:
The first step: will be heated to 1200 ± 20 ℃ of first humidity provinces of α+γ two-phase region, insulation 2～5min through pretreated TiAl base alloy;
Second step: with rate of heating v
hTiAl base alloy after first step is handled is warming up to 1300 ± 20 ℃ of second humidity provinces, insulation 15～30min;
Described rate of heating v
h=1.0 * 10
-3～2.0 * 10
-1℃/s;
The 3rd step: with speed of cooling v
cTo be cooled to 1200 ± 20 ℃ of first humidity provinces through the base of the TiAl after second step process alloy, and be incubated 2～5min;
Described speed of cooling v
c=1.0 * 10
-3～9.0 * 10
-1℃/s;
The 4th step: repeat second step and third step 2～6 times, cool to room temperature, taking-up then with the furnace, obtain the TiAl base alloy of sheet interlayer spacing refinement.
After above-mentioned processing, the sheet interlayer spacing of TiAl base alloy has obtained effective refinement, can keep better tissues homogeneity and stability simultaneously.Wherein, crucial α+γ two-phase region circulation ageing treatment adopts vacuum heat treatment furnace, and the time of circular treatment is shorter, and generally through 2～6 circular treatment, its sheet interlayer spacing is effectively refinement just, and the treatment time only is 3～6h.
The thermal treatment process of this thinning TiAl-base alloy sheet interlayer spacing provided by the invention mainly is by relevant parameters such as control rate of heating, speed of cooling, holding temperature, soaking times, comes the sheet interlayer spacing of effective thinning TiAl-base alloy.It is in order to eliminate the problems such as dendritic segregation, component segregation and internal stress in the castingprocesses, to improve the homogeneity and the stability of tissue that homogenizing is handled; Hot isostatic pressing is in order to eliminate casting flaws such as pore, shrinkage porosite.In short, homogenizing and hip treatment are the pre-treatment of as-cast state TiAl based alloy, are the prerequisites of subsequent disposal, only need carry out hip treatment for the TiAl after thermal treatment base alloy.α+γ two-phase region circulation ageing treatment is a core of the present invention; its key is the nucleation rate that changes with γ → α in the control heat-processed by the control rate of heating; generate the α nucleus of some amount in synusia inside configuration (being generally γ/γ at the interface); and in heating and insulating process the newborn α crystal grain phenomenon of can growing up, it is grown by the initial alpha lath that the step growth mechanism is parallel in the synusia structure with the lath form.The big more α crystal grain that then forms of the nucleation rate of α phase is many more in the heat-processed, and the secondary α phase lath that forms after the insulation is just many more; Simultaneously, in process of cooling, change, can decomposite secondary γ phase lath in the thick α phase lath by α → γ.Like this, can effectively control the also sheet interlayer spacing of thinning TiAl-base alloy by circular treatment.
In the present invention, the signal of the structural transformation in α+γ two-phase region " heating-insulation-cooling " process as shown in Figure 1.According to Ti-Al binary phase diagram (referring to shown in Figure 4) as can be known, at the TiAl of various compositions base alloy, change at α+when the γ two-phase region carries out circular treatment,, α → γ can take place change, and in temperature-rise period, reverse γ take place → α with the reduction of temperature.Because heat-processed is a dynamic nonequilibrium process, obviously can have the superheated problem, in the present invention, the superheating temperature relational expression is Δ T=T-T in the dynamic heat process
e=T
i+ v
hT-T
e, in the formula, T represents the dynamic heat temperature, its maximum value is positioned at 1300 ± 20 ℃ of second humidity provinces of α+γ two-phase region; T
eExpression eutectoid transformation temperature; T
iBe illustrated in the initial temperature of α+γ two-phase region circulation ageing treatment, be positioned at 1200 ± 20 ℃ of first humidity provinces of α+γ two-phase region; v
hThe expression rate of heating; T represents heat-up time.
From the superheating temperature relational expression as can be seen, rate of heating v
hBig more, superheating temperature Δ T is just big more, and is just many more by crossing thermogenetic free energy, and the γ in the heat-processed → α transformation motivating force is mainly derived from overheated free energy, and like this with the increase of rate of heating, the nucleation rate of α phase is just big more in the transition process.Simultaneously, the α nucleus is grown up with the lath morphological dilation in heat-processed, but because γ → α changes atomic diffusion mechanism into, growing up of α phase lath needs the certain reaction time, so rate of heating v
hIncrease, the real reaction time just reduces, and the phenomenon of growing up of α phase lath is just not obvious more, but tiny α crystal grain reaches corresponding the increasing of quantity of the short discontinuous α phase of secondary lath, and this grows up for the expansion of α phase lath in insulating process provides vantage point.
In the second humidity province insulating process of α+γ two-phase region, tiny α crystal grain and the discontinuous α phase of secondary lath can continue by step growth mechanism expansion growth, the phase driving force of this moment is mainly derived from free energy of chemistry, and the selection of soaking time mainly is to guarantee to have the enough time to decompose in the alligatoring that impels growing up of secondary α phase lath to prevent laminated structure simultaneously.
For the block crystal grain of equiaxial γ, when it takes place to decompose, α meets, and { four of 111} γ are used to separate out on the face of analysing at it, and in this research, all secondary α phase laths all are parallel to initial alpha lath (or γ phase lath), when this illustrated that γ → α takes place to be changed in laminated structure inside, the forming core growth of α phase had certain preferred orientation.
α → γ can take place in α+γ two-phase region temperature-fall period to be changed because α has only a solid matter face (0001) face mutually, so in process of cooling, α crystal grain can by its unique solid matter face be transformed into a position to γ crystal grain.In laminated structure, newborn γ also is parallel to initial alpha phase lath with the form of lath mutually and separates out.
On the other hand, because the synusia structure of TiAl base alloy has the low energy semicoherent interface
Has the intensive structure stability; isothermal treatment for short time can not make the synusia generation alligatoring of colony inside in the two-phase region circulating treatment procedure; simultaneously; owing to ceaselessly carry out " heating-insulation-cooling " circular treatment in the two-phase region; a small amount of α that separates out at lamella group interface or γ crystal grain can change tiny laminated structure into by changing mutually once more in circular treatment subsequently, do not influence macroscopical lamella form of TiAl base alloy.
Embodiment 1TiAl base alloy (Ti-47Al-2Cr-2Nb) ingot casting with full lamella form through cast molding is carried out the lamella thinning processing, and concrete processing step is:
The first step: the Ti-47Al-2Cr-2Nb alloy is carried out 900 ℃/48h homogenizing handle, carry out hip treatment then, its processing specification is 1280 ℃/175MPa/4h.
Second step: will the Ti-47Al-2Cr-2Nb alloy after the first step is handled put into vacuum heat treatment furnace and carry out α+γ two-phase region circulation ageing treatment.Concrete steps are:
(A) with rate of heating 8.33 * 10
-2℃/s is warming up to 1180 ℃ of α+first humidity province, γ two-phase region with the Ti-47Al-2Cr-2Nb alloy, and insulation 5min;
(B) with rate of heating v
h=3.33 * 10
-2℃/s will be warming up to 1280 ℃ of α+second humidity province, γ two-phase region through the Ti-47Al-2Cr-2Nb alloy of (A) step process, insulation 15min;
(C) with speed of cooling v
c=1.67 * 10
-2℃/s is cooled to 1180 ℃ of first humidity province, and insulation 5min;
(D) repeat (B) step and (C) go on foot 3 times, after circular treatment, cool to room temperature, taking-up with the furnace, make the Ti-47Al-2Cr-2Nb alloy of sheet interlayer spacing refinement.
Adopt above-mentioned same steps as, identical speed of cooling v
c=1.67 * 10
-2℃/s, the different heating speed v
hThe Ti-47Al-2Cr-2Nb alloy is carried out sheet interlayer spacing refinement thermal treatment, rate of heating v
hBe respectively 6.67 * 10
-2℃/s and 1.33 * 10
-1℃/s.
Adopt scanning electronic microscope (SEM) that sheet interlayer spacing is carried out quantitative analysis, record pretreated lamellar structure, sheet interlayer spacing is 5.70 μ m (shown in Fig. 2 A); Rate of heating v
h=3.33 * 10
-2℃/ tissue after s handles, sheet interlayer spacing is 3.89 μ m (shown in Fig. 2 B); Rate of heating v
h=6.67 * 10
-2℃/ tissue after s handles, sheet interlayer spacing is 3.37 μ m (shown in Fig. 2 C); Rate of heating v
h=1.33 * 10
-1℃/ tissue after s handles, sheet interlayer spacing is 1.98 μ m (shown in Fig. 2 D).
The Ti-47Al-2Cr-2Nb alloy carries out the room temperature tensile performance test when adopting MTS880 material mechanical performance trier, as shown in Figure 3, among the figure as can be seen, after the sheet interlayer spacing thinning processing, Ti-47Al-2Cr-2Nb alloy at room temperature plasticity can be stablized and reaches 2.5%～3.0%, and its room temperature strength is improved significantly simultaneously.
By as can be seen, under the constant condition of other conditions, can effectively control the sheet interlayer spacing of alloy by changing the α+rate of heating of γ two-phase region circulation ageing treatment, promptly with rate of heating v to the thinning processing of Ti-47Al-2Cr-2Nb alloy sheet interlayer spacing
hIncrease, the obvious refinement of TiAl base alloy sheet interlayer spacing, after the thinning processing alloy at room temperature plasticity, fracture toughness property, intensity etc. be improved significantly.
Embodiment 2TiAl base alloy (Ti-45Al-8.5Nb-0.1C) ingot casting through the moulding of vacuum consumable scull is carried out the lamella thinning processing, and concrete processing step is:
The first step: the Ti-45Al-8.5Nb-0.1C alloy is carried out 1050 ℃/12h homogenizing handle, carry out hip treatment then, its processing specification is 1250 ℃/200MPa/3h.
Second step: will the Ti-45Al-8.5Nb-0.1C alloy after the first step is handled put into vacuum heat treatment furnace and carry out α+γ two-phase region circulation ageing treatment.Concrete steps are:
(A) with rate of heating 8.33 * 10
-2℃/s is warming up to 1200 ℃ of α+first humidity province, γ two-phase region with the Ti-45Al-8.5Nb-0.1C alloy, and insulation 3min;
(B) with rate of heating v
h=5.00 * 10
-2℃/s will be warming up to 1300 ℃ of second humidity province through the Ti-45Al-8.5Nb-0.1C alloy of (A) step process, insulation 20min;
(C) with speed of cooling v
c=2.00 * 10
-2℃/s is cooled to 1200 ℃ of first humidity province, and insulation 3min;
(D) repeat (B) step and (C) go on foot 3 times, after circular treatment, cool to room temperature, taking-up with the furnace, make the Ti-45Al-8.5Nb-0.1C alloy of sheet interlayer spacing refinement.
Adopt above-mentioned same steps as, identical rate of heating v
h=5.00 * 10
-2℃/s, different cooling v
cThe Ti-45Al-8.5Nb-0.1C alloy is carried out sheet interlayer spacing refinement thermal treatment, speed of cooling v
cBe respectively 6.00 * 10
-2℃/s and 1.20 * 10
-1℃/s.
Adopt scanning electronic microscope (SEM) that sheet interlayer spacing is carried out quantitative analysis, the sheet interlayer spacing that records pretreated lamellar structure is 1.95 μ m, speed of cooling v
c=2.00 * 10
-2℃/s, 6.00 * 10
-2℃/s and 1.20 * 10
-1℃/s handles the corresponding sheet interlayer spacing in back and is respectively 1.50 μ m, 0.93 μ m, 0.37 μ m.
By as can be seen, under the constant condition of other conditions, can effectively control the sheet interlayer spacing of alloy by changing the α+speed of cooling of γ two-phase region circulation ageing treatment, promptly with speed of cooling v to the thinning processing of Ti-45Al-8.5Nb-0.1C alloy sheet interlayer spacing
cIncrease, the obvious refinement of TiAl base alloy sheet interlayer spacing.
Rate of heating v in the present invention
h=1.0 * 10
-3～2.0 * 10
-1℃/s, speed of cooling v
c=1.0 * 10
- 3～9.0 * 10
-1℃/the s condition under, the sheet interlayer spacing of TiAl after thinning processing base alloy is 0.2～5.0 μ m.
Claims (5)
1, a kind of thermal treatment process of thinning TiAl-base alloy sheet interlayer spacing, this thermal treatment process comprise pre-treatment and circulation ageing treatment two portions, it is characterized in that described circulation ageing treatment carries out in α+γ two-phase region, and concrete processing step is:
The first step: will be heated to 1200 ± 20 ℃ of first humidity provinces of α+γ two-phase region, insulation 2～5min through pretreated TiAl base alloy;
Second step: with rate of heating v
hTiAl base alloy after first step is handled is heated to 1300 ± 20 ℃ of second humidity provinces, insulation 15～30min;
Described rate of heating v
h=1.0 * 10
-3～2.0 * 10
-1℃/s;
The 3rd step: with speed of cooling v
cTo be cooled to 1200 ± 20 ℃ of first humidity provinces through the base of the TiAl after second step process alloy, and be incubated 2～5min;
Described speed of cooling v
c=1.0 * 10
-3～9.0 * 10
-1℃/s;
The 4th step: repeat second step and third step 2～6 times, cool to room temperature, taking-up then with the furnace, obtain the TiAl base alloy of sheet interlayer spacing refinement.
2, the thermal treatment process of TiAl base alloy sheet interlayer spacing according to claim 1 refinement, it is characterized in that: described pre-treatment includes homogenizing and hip treatment, and the temperature that homogenizing is handled is 800 ℃～1100 ℃, and soaking time is 12～48h; The temperature of hip treatment is 1200～1300 ℃, and pressure is 170～220MPa, and soaking time is 3～5h.
3, the thermal treatment process of a kind of thinning TiAl-base alloy sheet interlayer spacing according to claim 1, it is characterized in that: this technology is applicable to that Al content is the TiAl base alloy of 45at%～51at%, and perhaps Al content is that 42at%～46at%, content of niobium are the high-Nb TiAl-base alloy of 5at%～10at%.
4, the thermal treatment process of a kind of thinning TiAl-base alloy sheet interlayer spacing according to claim 1 is characterized in that: the TiAl base alloy at room temperature plasticity of sheet interlayer spacing refinement is 2.5%～3.0%.
5, the thermal treatment process of a kind of thinning TiAl-base alloy sheet interlayer spacing according to claim 1 is characterized in that: at rate of heating v
h=1.0 * 10
-3～2.0 * 10
-1℃/s, speed of cooling v
c=1.0 * 10
-3～9.0 * 10
-1℃/sheet interlayer spacing of TiAl base alloy under the s condition is 0.2～5.0 μ m.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11807911B2 (en) | 2021-12-15 | 2023-11-07 | Metal Industries Research & Development Centre | Heat treatment method for titanium-aluminum intermetallic and heat treatment device therefor |
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| CN101100731A (en) | 2008-01-09 |
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