CN101302589B - Coordinating control method of alpha2 phase and silicide in near-alpha high temperature titanium alloy - Google Patents
Coordinating control method of alpha2 phase and silicide in near-alpha high temperature titanium alloy Download PDFInfo
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Abstract
The invention provides a method for coordinating and controlling alpha2 phase and silicide in a near-alpha titanium alloy. The method comprises the following steps of: 1. determination of an alloy system; 2. determination of variation ranges of contents of Al elements and Si elements; 3. determination of a smelting process; 4. determination of a rolling deformation process; 5. determination of solid solution microstructure; 6. selection of an aging heat treatment process. The method determines the compositional variation range of the Al elements and the Si elements in the near-alpha titanium alloy, determines a corresponding system of the heat treatment process, ensures that the alpha 2 and the silicide can be coordinated and controlled, and can simultaneously guarantee higher heat resistant performance and higher thermal stability.
Description
Technical field
The present invention relates to α in a kind of nearly α high-temperature titanium alloy
2The control method for coordinating of phase and silicide particularly contains α in the nearly α high-temperature titanium alloy of Si
2The control method for coordinating of phase and silicide is such as α in the Ti-Al-Sn-Zr-Mo-Si alloy system
2The control method for coordinating of phase and silicide.
Background technology
Near is first-selected high-temperature titanium alloy when temperature is used more than 600 ℃, and under the situation that microstructure, interpolation element are fully guaranteed, the fundamental way that improves its high temperature use properties is the precipitation strength of disperse phase.Although α
2Phase and silicide causes the reduction of alloy thermostability easily as the disperse precipitated phase, but also can play strengthening effect really.Such as, at IMI550, IMI679, IMI685, IMI829, IMI834 and Ti-55, Ti-600, in the Ti-60 alloy, α
2Phase and silicide has improved the creep property of alloy effectively, yet, cause the thermostability of alloy obviously to descend.
α in the near
2With Ti
3Al be main body, have a DO
19Ordered phase structure, that generally separate out in ag(e)ing process or hot process-exposed.When the electron density of alloy surpasses feature electron density (N
C=∑ N
if
i=2.12) time, α under suitable aging condition
2Phase (Ti
3X) just will separate out α
2Be the product of timeliness and hot process-exposed mutually.Its separate out grow up with the Ti-Al two component system in α
2Phase (Ti
3Al) separate out to grow up has identical feature.With the reduction of timeliness temperature, α
2The separating out of phase only show as successively separate out near the dislocation, dislocation and crystal boundary is preferentially separated out and evenly separate out three kinds of features in alloy.
To α
2The understanding of the embrittling effect of phase is of long duration, and almost may separate out α
2In the nearly α type of all of the phase high-temperature titanium alloy, all find α
2The embrittlement that causes alloy of separating out of phase is inclined to, and reduces temperature-room type plasticity.α is pointed out in relevant research
2The embrittling effect degree and the α of phase
2The content of phase, size, shape, it is relevant to distribute.And α
2The hot strength of phase is far above the α phase, and this just makes and utilizes α
2Strengthen mutually and become possibility.
Because α
2It is relevant with many-sided factors such as alloying constituent, solid solution structure, aging temp and times that the separating out of phase grown up, and its influence is also relevant with separating out of the content of element silicon and silicide simultaneously, thus α
2Separate out and the growth control of phase is still still unsolved difficulty.
Si has been proved to be effective strengthening element as a kind of interpolation element of important high-temperature titanium alloy.IMI550, IMI679, IMI685, IMI829, IMI834 and Ti-55, Ti-600, Ti-60 are the high-temperature titanium alloys that contains Si.In nearly α high-temperature titanium alloy, the content of Si is generally between 0.1～0.5 (wt%).Si exists with two states, i.e. Si solid solution is separated out with the form of silicide in the matrix neutralization.These two kinds exist form is exactly the precipitation strength of Si solution strengthening and silicide to the alloy Effect on Performance.
Si can strengthen sosoloid effectively, and its solubleness in the β titanium is much larger than the solubleness in the α titanium, the raising of the solubility with temperature of Si in the α titanium and strengthening.Therefore, adopt in β district or the processing on β+alpha phase zone top makes the Si solid solution, in lesser temps (such as 650 ℃) timeliness down, can obtain silicide tiny, the disperse distribution then.
Silicide separate out the influence that is subjected to aging temp and time, improve aging temp and time and cause the increase of silicide; The separating out distribution, pattern, particle size and can in a big way, change of silicide.Silicide is mainly separated out at the interface at single-phase α ' lamellar structure or alpha-beta, and also normal discovery is separated out at organization internal; Its shape can be equiaxial, ellipsoid, is rendered as blocky sometimes; Its size can change to the hundreds of nanometer in tens nanometers.
The main effect that the Si element adds is solution strengthening, and this point is generally accepted.
Precipitation strength to silicide then has two kinds of visibly different understanding.Some studies show that, silicide tiny, that disperse distributes helps strengthening crystal boundary and phase boundary, and when Si and Zr, Mo comprehensive action, strengthening effect is best; Other researchs then show, silicide is separated out the reduction that can cause creep resistance and the increase of fatigue crack growth speed.In fact can think that the separating out of the strengthening effect of silicide and silicide, growth process and distribution are closely related.With α
2The embrittling effect of phase is similar, separates out with the increase and the silicide of Si content, and the stretching plastic of high-temperature titanium alloy obviously reduces.
Because it is relevant with many-sided factors such as alloying constituent, solid solution structure, aging temp and times that the separating out of silicide grown up, its influence of while also with α
2Separating out of phase is relevant, thereby separating out with growth control of silicide is still still unsolved difficulty.
Owing to pursue the heat resistance of high-temperature titanium alloy, guarantee its thermostability again simultaneously, therefore, just must effectively control α
2Process of growth is separated out in uniting of phase and silicide, coordinates the action effect of the two.As previously mentioned, because α
2The complicacy of the precipitation process of phase and silicide, at present, α
2The coordination control of phase and silicide is still a still unsolved difficulty.
In sum, there is following defective in existing technological method, that is, the heat resistance that improves nearly α high-temperature titanium alloy can will be a cost to reduce thermostability (often representing with the stretching plastic index) often; And to guarantee higher thermostability, be difficult to the heat resistance energy that reaches higher simultaneously again.
Summary of the invention
The present invention provides α in a kind of nearly α high-temperature titanium alloy
2The control method for coordinating of phase and silicide.This method has been determined the composition variation range of Al, Si element in the nearly α high-temperature titanium alloy, has determined corresponding system of heat treatment process, makes α
2Phase and silicide obtains coordinating control, can guarantee higher heat resistance energy and higher thermostability simultaneously.
Technical scheme of the present invention is: α in the nearly α high-temperature titanium alloy provided by the invention
2The control method for coordinating of phase and silicide comprises successively:
1, determining of alloy system: the nearly α high-temperature titanium alloy of determining is that Ti-Al-Sn-Zr-Mo-Si is an alloy, and wherein the content of Sn, Zr, Mo is respectively: the Sn weight percent is 4.8, the Zr weight percent is 2.0, and the Mo weight percent is 1.0; The Ti weight percent is 85.95-86.25, and all the other are the content of Al, Si.
2, determining of the variation range of Al, Si constituent content: determine that Ti-Al-Sn-Zr-Mo-Si is the variation range of Al in the alloy, Si constituent content, wherein the variation range of the weight percent of Al is that the variation range of the weight percent of 5.6-6.0, Si is 0.25-0.35; And when the Al constituent content takes off in limited time the content capping of Si element; During Al constituent content capping, the content of Si element takes off limit.
3, determining of smelting technology: determined to use 0 grade of titanium sponge (Ti), zirconium sponge (Zr) and fine aluminium (Al) and master alloy Ti-Sn alloy, Al-Si alloy, Al-Mo alloy raw material, be pressed into electrode through hydropress, adopt vaccum consumable electrode electric arc furnace, through three meltings, be prepared into ingot casting, the excision rising head is so that further roll forming.
4, determining of rolling deformation technology: with titan alloy casting ingot at the β phase region through water pressure engine cogging forging, finish forge, rolling bar, cutting processing process, be rolled into required bar at the alpha+beta two-phase region at last.
5, determining of solid solution structure: titanium alloy rod bar is carried out solution heat treatment, temperature is selected in the following 10-12 of alpha+beta/beta transus temperature ℃, through 2 hours isothermal processes and in air naturally cooling, the solid solution structure of gained is the bifurcation tissue, that is 20% the nascent bifurcation mixed structure that waits the β transformation lamellar structure of axle α tissue and 80%.
6, the selection of aging thermal treating process: refer to the selection of aging temp and aging time, should guarantee α
2Fully separating out of phase and silicide grown up, and the plasticity of avoiding again causing thus reduces; For Ti-Al-Sn-Zr-Mo-Si is alloy, and when Al content took off limit, Si content capping, selecting temperature was that 700 ℃, time are to carry out timeliness in 10-15 hour; When Al content capping, Si content take off in limited time, selecting temperature is that 760 ℃, time are to carry out timeliness in 5-10 hour.
By mentioned component determine, α such as thermal treatment process is determined
2The control method for coordinating of phase and silicide, obtaining Ti-Al-Sn-Zr-Mo-Si is alloy sample.Adopt transmission electron microscope that sample is observed, find α
2Wait axle α evenly to separate out in organizing to grow up nascent, size is at 5-10nm, and separates out hardly or less separating out in β transformation lamellar structure; Control separating out of silicide simultaneously and grow up more evenly along remaining β phase (the nascent interfacial phase that waits axle α tissue and β to change lamellar structure) distribution, do not produce obvious agglomeration, size is in the 150-220nm scope.
Compare with prior art, the present invention reaches purpose of the present invention by three aspects: (1) has determined that nearly α high-temperature titanium alloy is that Ti-Al-Sn-Zr-Mo-Si is the content and the variation range of each element of alloy, Al constituent content and variation range have particularly been determined, determined that bifurcation is organized as solid solution structure, determine aging temp and aging time, thereby determined α
2The distribution of separating out Yu growing and the size of phase have also just realized α
2Separating out and growth control of phase; (2) determined that nearly α high-temperature titanium alloy is that Ti-Al-Sn-Zr-Mo-Si is the content and the variation range of each element of alloy, Si constituent content and variation range have particularly been determined, determined that bifurcation is organized as solid solution structure, aging temp and aging time have been determined, thereby determined the distribution of separating out Yu growing and the size of silicide, also just realized separating out and growth control of silicide; (3) determined that Ti-Al-Sn-Zr-Mo-Si is the variation range and the concrete obtaining value method of Al in the alloy, Si constituent content, and corresponding timeliness thermal treatment temp and time have been determined, so just realize Whole Process Control, thereby realize α from aspects such as alloying constituent, solid solution structure, aging temp and times
2The coordination control of phase and silicide, under the prerequisite that guarantees thermostability, the high heat-intensity of the titanium alloy that reaches a high temperature.
According to α in the nearly α high-temperature titanium alloy proposed by the invention
2The control method of phase and silicide, under the standard test condition and standard test sample condition that adopt country to formulate, can obtain above-mentioned Ti-Al-Sn-Zr-Mo-Si is the heat resistance energy of alloy sample and the matched well of thermal stability.The specific performance index is as follows:
Tensile property: the tensile property after sample exposes through solid solution, timeliness thermal treatment and 600 ℃/100h blank heat, use yield strength σ
0.2, tensile strength sigma
b, elongation after fracture δ and relative reduction in area Ψ be represented, dividing in addition is 980-1010MPa, 1060-1100MPa, 14.5-16.5%, 26.0-30.0%;
Enduring quality: the enduring quality after the solid solution of sample process, the timeliness thermal treatment, represent by the rupture time of sample under 600 ℃ of temperature, the load 310MPa experiment condition, can reach 150-200 hour;
Creep property: the creep property after the solid solution of sample process, the timeliness thermal treatment, represent by the creep elongation (plastic elongation) of sample under 600 ℃ of temperature, load 160MPa, the time 100h experiment condition, can reach 0.15%-0.30%.
Embodiment:
Embodiment 1: α among the nearly α high-temperature titanium alloy 86.25Ti-5.6Al-4.8Sn-2.0Zr-1.0Mo-0.35Si
2The control method for coordinating of phase and silicide the steps include: 1, the determining of alloy system: adopt nearly α high-temperature titanium alloy 86.25Ti-5.6Al-4.8Sn-2.0Zr-1.0Mo-0.35Si.2, determining of Al, Si constituent content: the weight percent of Al is 5.6, the weight percent of Si is 0.35.3, determining of smelting technology: use 0 grade of titanium sponge (Ti), zirconium sponge (Zr) and fine aluminium (Al) and master alloy Ti-Sn alloy, Al-Si alloy, Al-Mo alloy raw material, be pressed into electrode through hydropress, adopt vaccum consumable electrode electric arc furnace, through three meltings, be prepared into ingot casting, the excision rising head is so that further roll forming.4, determining of rolling deformation technology: with titan alloy casting ingot at the β phase region through water pressure engine cogging forging, finish forge, rolling bar, cutting processing process, be rolled into required bar at the alpha+beta two-phase region at last.5, determining of solid solution structure: adopt three sections tube furnaces that titanium alloy rod bar is carried out solution heat treatment, temperature is selected in following 10 ℃ of alpha+beta/beta transus temperature (1015 ℃), promptly 1005 ℃; Through 2 hours isothermal processes and in air naturally cooling, the solid solution structure of gained is the bifurcation tissue, that is, 20% the nascent bifurcation mixed structure that waits the β transformation lamellar structure of axle α tissue and 80%.6, the selection of aging thermal treating process: for guaranteeing α
2Fully separating out of phase and silicide grown up, and the plasticity of avoiding again causing thus reduces, and for alloy 86.25Ti-5.6Al-4.8Sn-2.0Zr-1.0Mo-0.35Si, selects lesser temps (700 ℃), long period (15 hours) to carry out timeliness.
α such as the process mentioned component is determined, thermal treatment process is determined
2The coordination control of phase and silicide obtains the 86.25Ti-5.6Al-4.8Sn-2.0Zr-1.0Mo-0.35Si alloy sample.Adopt transmission electron microscope that sample is observed, find α
2Wait axle α evenly to separate out in organizing to grow up nascent, size is at 5-10nm, and separates out hardly or less separating out in β transformation lamellar structure; Control separating out of silicide simultaneously and grow up more evenly along remaining β phase (the nascent interfacial phase that waits axle α tissue and β to change lamellar structure) distribution, do not produce obvious agglomeration, size is in the 150-220nm scope.
Under the standard test condition and standard test sample condition that adopt country to formulate, the 86.25Ti-5.6Al-4.8Sn-2.0Zr-1.0Mo-0.35Si alloy sample is carried out performance test, the result is as follows:
Tensile property: the tensile property after sample exposes through solid solution, timeliness thermal treatment and 600 ℃/100h blank heat is yield strength (σ
0.2) 985MPa, tensile strength (σ
b) 1060MPa, elongation after fracture (δ) 15.0% and relative reduction in area (Ψ) 26.0%;
Enduring quality: the enduring quality after the solid solution of sample process, the timeliness thermal treatment, rupture time by sample under 600 ℃ of temperature, the load 310MPa experiment condition is represented, lasting experiment is carried out on made in China RCL-3 creep equipment, and rupture time is 195 hours;
Creep property: the creep property after the solid solution of sample process, the timeliness thermal treatment, creep elongation (plastic elongation) by sample under 600 ℃ of temperature, load 160MPa, the time 100h experiment condition is represented, creep test also carries out on homemade RCL-3 creep equipment, and the creep property result who reaches is a plastic elongation 0.16%.
Embodiment 2: α among the nearly α high-temperature titanium alloy 85.95Ti-6.0Al-4.8Sn-2.0Zr-1.0Mo-0.25Si
2Phase and silicide separate out control.Its method is: 1, determining of alloy system: adopt nearly α high-temperature titanium alloy 85.95Ti-6.0Al-4.8Sn-2.0Zr-1.0Mo-0.25Si.2, determining of Al, Si constituent content: the weight percent of Al is 6.0, the weight percent of Si is 0.25.3, determining of smelting technology: use 0 grade of titanium sponge (Ti), zirconium sponge (Zr) and fine aluminium (Al) and master alloy Ti-Sn alloy, Al-Si alloy, Al-Mo alloy raw material, be pressed into electrode through hydropress, adopt vaccum consumable electrode electric arc furnace, through three meltings, be prepared into ingot casting, the excision rising head is so that further roll forming.4, determining of rolling deformation technology: with titan alloy casting ingot at the β phase region through water pressure engine cogging forging, finish forge, rolling bar, cutting processing process, be rolled into required bar at the alpha+beta two-phase region at last.5, determining of solid solution structure: adopt three sections tube furnaces that titanium alloy rod bar is carried out solution heat treatment, temperature is selected in following 12 ℃ of alpha+beta/beta transus temperature (1027 ℃), that is, and and 1015 ℃; Through 2 hours isothermal processes and in air naturally cooling, the solid solution structure of gained is the bifurcation tissue, that is, about 20% the nascent β that waits axle α tissue and about 80% changes the bifurcation mixed structure of lamellar structure.6, the selection of aging thermal treating process: for guaranteeing α
2Fully separating out of phase and silicide grown up, and the plasticity of avoiding again causing thus reduces, and for alloy 85.95Ti-6.0Al-4.8Sn-2.0Zr-1.0Mo-0.25Si, selects comparatively high temps (760 ℃), short period (10 hours) to carry out timeliness.
α such as the process mentioned component is determined, thermal treatment process is determined
2The control method for coordinating of phase and silicide obtains the 85.95Ti-6.0Al-4.8Sn-2.0Zr-1.0Mo-0.25Si alloy sample.Adopt transmission electron microscope that sample is observed, find α
2Wait axle α evenly to separate out in organizing to grow up nascent, size is at 5-10nm, and in β transformation lamellar structure less separating out arranged; Control simultaneously separating out of silicide grow up more even along remaining β phase (the nascent interfacial phase that waits axle α tissue and β to change lamellar structure) distribution, no agglomeration, size is in the 180-220nm scope.
Under the standard test condition and standard test sample condition that adopt country to formulate, the 85.95Ti-6.0Al-4.8Sn-2.0Zr-1.0Mo-0.25Si alloy sample is carried out performance test, the result is as follows:
Tensile property: the tensile property after sample exposes through solid solution, timeliness thermal treatment and 600 ℃/100h blank heat is yield strength (σ
0.2) 1000MPa, tensile strength (σ
b) 1060MPa, elongation after fracture (δ) 16.5% and relative reduction in area (Ψ) 28.0%;
Enduring quality: the enduring quality after the solid solution of sample process, the timeliness thermal treatment, rupture time by sample under 600 ℃ of temperature, the load 310MPa experiment condition is represented, lasting experiment is carried out on made in China RCL-3 creep equipment, and rupture time is 150 hours;
Creep property: the creep property after the solid solution of sample process, the timeliness thermal treatment, creep elongation (plastic elongation) by sample under 600 ℃ of temperature, load 160MPa, the time 100h experiment condition is represented, creep test also carries out on homemade RCL-3 creep equipment, and the creep property result who reaches is a plastic elongation 0.28%.
Claims (1)
1. α in the nearly α high-temperature titanium alloy
2The control method for coordinating of phase and silicide is characterized in that: α in a kind of nearly α high-temperature titanium alloy
2The control method for coordinating of phase and silicide comprises successively:
(1), the determining of alloy system: the nearly α high-temperature titanium alloy of determining is that Ti-Al-Sn-Zr-Mo-Si is an alloy, and wherein the content of Sn, Zr, Mo is respectively: the Sn weight percent is 4.8, the Zr weight percent is 2.0, and the Mo weight percent is 1.0; The Ti weight percent is 85.95-86.25, and all the other are the content of Al, Si;
(2), determining of the variation range of Al, Si constituent content: determine that Ti-Al-Sn-Zr-Mo-Si is the variation range of Al in the alloy, Si constituent content, wherein the variation range of the weight percent of Al is that the variation range of the weight percent of 5.6-6.0, Si is 0.25-0.35; And when the Al constituent content takes off in limited time the content capping of Si element; During Al constituent content capping, the content of Si element takes off limit;
(3), determining of smelting technology: determined to use 0 grade of titanium sponge (Ti), zirconium sponge (Zr) and fine aluminium (Al) and master alloy Ti-Sn alloy, Al-Si alloy, Al-Mo alloy raw material, be pressed into electrode through hydropress, adopt vaccum consumable electrode electric arc furnace, through three meltings, be prepared into ingot casting, the excision rising head is so that further roll forming;
(4), the determining of rolling deformation technology: with titan alloy casting ingot at the β phase region through water pressure engine cogging forging, finish forge, rolling bar, cutting processing process, be rolled into required bar at the alpha+beta two-phase region at last;
(5), determining of solid solution structure: titanium alloy rod bar is carried out solution heat treatment, temperature is selected in the following 10-12 of alpha+beta/beta transus temperature ℃, through 2 hours isothermal processes and in air naturally cooling, the solid solution structure of gained is the bifurcation tissue, that is 20% the nascent bifurcation mixed structure that waits the β transformation lamellar structure of axle α tissue and 80%;
(6), the selection of aging thermal treating process: refer to the selection of aging temp and aging time, should guarantee α
2Fully separating out of phase and silicide grown up, and the plasticity of avoiding again causing thus reduces; For Ti-Al-Sn-Zr-Mo-Si is alloy, and when Al content took off limit, Si content capping, selecting temperature was that 700 ℃, time are to carry out timeliness in 10-15 hour; When Al content capping, Si content take off in limited time, selecting temperature is that 760 ℃, time are to carry out timeliness in 5-10 hour.
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| CN101850503B (en) * | 2010-05-21 | 2011-11-02 | 哈尔滨工业大学 | Preparation method of TiC granule reinforcing Ti-Al-Sn-Zr-Mo-Si high-temperature titanium alloy composite material plate |
| CN102051493A (en) * | 2011-01-26 | 2011-05-11 | 西北有色金属研究院 | Preparation method of multielement titanium alloy |
| CN104694863B (en) * | 2013-12-10 | 2016-09-14 | 陕西宏远航空锻造有限责任公司 | A kind of heat treatment method of titanium alloy |
| CN108754371B (en) * | 2018-05-24 | 2020-07-17 | 太原理工大学 | Preparation method of refined α -close high-temperature titanium alloy grains |
| CN110923589B (en) * | 2019-11-26 | 2021-12-17 | 中国科学院金属研究所 | Short fiber reinforced high-temperature titanium alloy Ti-101AM for 700-750 DEG C |
| CN111020414B (en) * | 2019-11-26 | 2021-11-09 | 中国科学院金属研究所 | Preparation method of short fiber reinforced high-temperature titanium alloy bar for 700-750 DEG C |
| CN111500959B (en) * | 2020-06-09 | 2021-06-25 | 北京工业大学 | Thermal processing and heat treatment process for preparing near-alpha type high-temperature titanium alloy layered structure |
| CN114150242B (en) * | 2021-11-25 | 2023-07-18 | 南京理工大学 | Method for inhibiting coarsening of light high-strength TiAl alloy sheet |
| CN114959525B (en) * | 2022-04-29 | 2023-11-10 | 中国科学院金属研究所 | High-temperature titanium alloy hot working preparation method with mixed structure and high strength characteristics |
| CN116145064A (en) * | 2023-02-02 | 2023-05-23 | 中国科学院金属研究所 | Method for improving creep property of titanium alloy |
| CN116144980A (en) * | 2023-02-02 | 2023-05-23 | 中国科学院金属研究所 | Silicide of high-temperature titanium alloy and control method for precipitation growth of silicide |
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