CN100425722C - Method for improving property of TiAI intermetallic compound based composite material - Google Patents
Method for improving property of TiAI intermetallic compound based composite material Download PDFInfo
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- CN100425722C CN100425722C CNB2005100452813A CN200510045281A CN100425722C CN 100425722 C CN100425722 C CN 100425722C CN B2005100452813 A CNB2005100452813 A CN B2005100452813A CN 200510045281 A CN200510045281 A CN 200510045281A CN 100425722 C CN100425722 C CN 100425722C
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Abstract
The present invention relates to a method for improving the mechanical performance of a composite material using a TiAl intermetal compound as a base by thermal treatment and alloying. The method of the present invention comprises the following steps: using 35 to 55 mol% of Ti powder, 35 to 50 mol% of Al powder, 3 to 10 mol% of Nb powder and 0 to 5 mol% of B powder to prepare TiAl-based alloy powder by a thermal explosion method; adding 5 to 20 wt% of TiC ceramic particles to the TiAl-based alloy powder; preparing a Ti2 AlC/TiAl composite material by a spark plasma sintering method; carrying out thermal treatment to the Ti2 AlC/TiAl composite material. The processing method of the present invention can obviously improve the bending strength, the breaking tenacity and the mechanical performance of the composite material using the TiAl intermetal compound as the base.
Description
(1) technical field under
The present invention relates to a kind of method of utilizing thermal treatment and alloying to improve TiAl intermetallic compound based composite material mechanical property.
(2) background technology
The intermetallic compound structure material mainly is performances such as intensity, rigidity, hardness, thermotolerance and high temperature creep-resisting of utilizing intermetallic compound.Intermetallic compound is as Ni
3Al, NiAl, Ti
3Al, TiAl, Fe
3Al and FeAl etc. are high-temperature structural materials of new generation.Wherein the Ti-Al series intermetallic compound is because metallic bond and covalent linkage coexistence in the crystal, make the high-temperature behavior of its toughness that might have metal simultaneously concurrently and pottery, and consequent high specific tenacity, specific modulus, good oxidation-resistance, creep resistance and excellent high-temperature intensity, rigidity and low density or the like, making it to be better than present widely used metal and alloy thereof, is the very promising high-temperature structural material of a class.
There are multiple intermetallic compound, wherein TiAl in Ti-Al system
3, TiAl, Ti
3Al is three kinds of researchs Intermatallic Ti-Al compounds the most widely.Because TiAl has unique attractive over-all properties, be low density, high strength, high-melting-point and good creep resistance, antioxidant property and flame resistant performance, obtain concern widely aspect the high temperature aeronautic structure material, becoming the emphasis of people's research gradually.
Though the research about the TiAl intermetallic compound has obtained remarkable progress, it still has many stones of blocking the way need overcome with challenge on the road of practicability of marching toward.As: how to define optimum microstructure better, how to reach balance of ductility, creep property and other performance or the like.Improving the over-all properties of TiAl intermetallic compound can carry out from the following aspects: the one, to improve its intensity and ductility, can improve room temperature ductility by element alloyed as interpolation Mn, Cr, Si, Nb etc.; The 2nd, in TiAl, add the hard enhancing body of high-strength height, make the TiAl based composites to improve its hot strength and toughness; The 3rd, adopt advanced preparation method, and optimize microstructure by thermal treatment, improve the performance of TiAl intermetallic compound.
At present, aspect the over-all properties of improving the TiAl intermetallic compound, also do not satisfy the requirement of practicability, mechanical properties such as its flexural strength and fracture toughness property are not also brought up to the degree that is enough to substitute existing high-temperature structural material.Preparing the TiAl intermetallic compound based composite material is a kind of method of main raising intermetallic compound performance, in order further to improve composite property, optimize microstructure by thermal treatment and alloying, improve the performance of TiAl intermetallic compound based composite material.
(3) summary of the invention
The present invention provides a kind of method of utilizing thermal treatment and alloying to improve TiAl intermetallic compound based composite material mechanical property in order further to improve the mechanical property of TiAl intermetallic compound based composite material.
The present invention is achieved by the following measures:
The present invention relates to a kind of method of the TiAl of improvement intermetallic compound based composite material performance, may further comprise the steps,
Get the Ti powder of molar percentage 35-55%, the Al powder of 35-50%, the Nb powder of 3-10%, the B powder of 0-5%, after the mechanically mixing, be warming up to 1100-1200 ℃, adopt the thermal explosion reaction synthesis method to make TiAl, ground 325 mesh sieves, get the TiAl base alloy powder;
It is the TiC ceramic particle of 5%-20% that described TiAl base alloy powder adds weight percentage, adopts the discharge plasma sintering method, makes Ti
2The AlC/TiAl matrix material, the TiC ceramic particle accounts for Ti
2The 5%-20% weight of AlC/TiAl matrix material;
Described Ti
2The AlC/TiAl matrix material is heat-treated, and realizes by rapid thermal process or multistep thermal treatment.
In the method for the present invention, described quick heat treatment method is the discharge plasma sintering method, and rate of heating is 500 ℃/min, and treatment temp is 1100-1250 ℃, and soaking time is 5-30min, and pressure is 20-40Mpa.
In the method for the present invention, described multistep heat treating method adopts three step factures, is heated to 1050 ℃ from room temperature, and air cooling is to room temperature behind the insulation 24h; Reheat is to 1300-1400 ℃, and air cooling is to room temperature behind the insulation 5-45min; Be heated to 900 ℃ at last, stove is chilled to room temperature behind the insulation 6h.
In the method for the present invention, the particle diameter of described TiC ceramic particle is 0.1-5.0 μ m.
Now improved performance mechanism of the present invention and correlated phenomena are further described:
1, fracture mode changes
The cross-section morphology SEM figure before and after thermal treatment, we can find, Ti
2The fracture mode of AlC/TiAl matrix material is a mixed mode before thermal treatment, then is transcrystalline cleavage fracture after the thermal treatment.This is owing to after the thermal treatment, generated in-situ high rigidity ceramic phase Ti
2AlC combines well with the matrix phase interface, and the combination of TiAl matrix crystal boundary is tight, and forms more α
2/ γ synusia colony, so dislocation reaction takes place in the jack per line edge dislocation in the matrix material under stress, is merged into small cavity, this moment, dislocation plug collection was at crystal boundary or Ti
2Before the AlC particle.When the stress that applies reached certain value, the stress concentration that dislocation plug cluster causes made its front end produce cleavage crack, and in adjacent intragranular expansion.When the cleavage crack of intracrystalline and screw dislocation intersect, on cleavage surface, will form step, cause the river pattern on the fracture.Since transcrystalline cleavage fracture mass consumption the energy of material internal, suppressed the expansion of crackle, simultaneously, increased the extensions path of crackle because the high rigidity of himself impels crackle to change direction, disperseed the expansion energy needed.Therefore the flexural strength of material and fracture toughness property all obviously improve after the thermal treatment.
2, refined crystalline strengthening and malleableize
Generated in-situ Ti
2The AlC fine particle is distributed in the matrix material to even dispersion, so in heat treatment process, Ti
2The AlC wild phase can suppress the migration of matrix phase crystal boundary, refinement γ crystal grain and α
2/ γ synusia colony.
In heat treatment process, the needle-like boride TiB that the B element forms
2(as shown in figure 12) but pinning α crystal boundary and γ crystal boundary hinder crystal boundary migration, prevent grain growth, refinement layer sheet colony.
In heat treatment process, γ crystal grain can not only be from α crystal boundary forming core, also can be from TiB
2And Ti
2Forming core is separated out on the AlC interface, and γ crystal grain forming core position is increased greatly, improves nucleation rate, significantly refinement γ crystal grain.
According to the Hall-Petch relational expression:
σ
f＝σ
0+kd
-1/2
As can be seen, intensity reducing and improve with crystal grain effective diameter d value.Therefore, according to above-mentioned thin brilliant effect and phenomenon, Ti
2The flexural strength of AlC/TiAl matrix material is significantly improved.
Crystal grain thinning not only can improve intensity, and can improve toughness.Reason is that crystal grain is thin more, the difficult more needed stress concentration of crack nucleation that causes; Simultaneously, crystal grain is thin more, crackle coordination not to each intragranular propagate also more difficult.Therefore, after the thermal treatment, Ti
2The fracture toughness property of AlC/TiAl matrix material also makes moderate progress.
3, phase boundary drives and changes
Ti
2The AlC/TiAl matrix material is through 1050 ℃ 24h ageing treatment, the TiAl matrix phase boundary can take place drives transformation: α melts mutually in the TiAl matrix, α is changed mutually, to reduce the free energy of chemistry of system at 1050 ℃ of definite equilibrium phase diagram compositions towards the Ti-Al binary phase diagram with γ composition mutually.And the melting of α phase, not only can on the γ crystal boundary, take place, also can be at Ti
2AlC and TiB
2The interface on take place, promptly the forming core position of γ phase is numerous, can obtain more tiny and uniform γ crystal grain.Therefore, after 1050 ℃ of ageing treatment, the microstructure of matrix material changes more tiny and uniform nearly γ tissue into, and its mechanical property is also improved therefore and greatly.
4, wild phase to the inhibition of α phase and to the also bigger improvement of the inhibition of discontinuous alligatoring Ti
2The mechanical property of AlC/TiAl matrix material.
In sum, adopt treatment process of the present invention, can significantly improve the flexural strength and the fracture toughness property of TiAl intermetallic compound based composite material, improve its mechanical property.
(4) description of drawings
Preparation technology's flow process of Fig. 1 TiAl base alloy powder
Fig. 2 is Ti
2The surface topography of AlC/TiAl matrix material
Fig. 3 (a) and (b) are Ti
2The cross-section morphology of AlC/TiAl matrix material
Fig. 4 Ti
2The DTA curve of AlC/TiAl matrix material
Fig. 5 (a) is Ti
2The AlC/TiAl flexural strength contrast after the thermal treatment that is rapidly heated
Fig. 5 (b) is Ti
2The AlC/TiAl fracture toughness property contrast after the thermal treatment that is rapidly heated
Fig. 6 Ti
2The AlC/TiAl matrix material cross-section morphology after the thermal treatment that is rapidly heated
Fig. 7 Ti
2The AlC/TiAl matrix material surface topography after the thermal treatment that is rapidly heated
Fig. 8 multistep thermal treatment process figure
Fig. 9 (a) is Ti
2The flexural strength of each sample after the thermal treatment of AlC/TiAl multistep
Fig. 9 (b) is Ti
2The fracture toughness property of each sample after the thermal treatment of AlC/TiAl multistep
Figure 10 is Ti
2The cross-section morphology of each sample after the thermal treatment of AlC/TiAl multistep
Figure 11 is the surface topography of each sample after the thermal treatment of Ti2AlC/TiAl multistep
Thin bar-shaped TiB among Figure 12 Ti2AlC/TiAl
2
(5) embodiment
Below the present invention is made specific description.
Choose the starting material of table 1, by the Ti powder of mole per-cent 49.45%, 48.30% Al powder, 2.25% Nb powder, in ratio of grinding media to material is that 10: 1 ratio adds in the ball mill, carry out mechanically mixing, then, be warming up to 1100-1200 ℃, adopt the thermal explosion reaction synthesis method to make TiAl, grind 325 mesh sieves, got TiAl base alloy powder Ti-48.30A1-2.25Nb, abbreviated TN as.Preparation technology such as Fig. 1.
Choose the starting material of table 1, by the Ti powder of mole per-cent 48.78%, 47.66% Al powder, 2.22% Nb powder, 1.34B powder, in ratio of grinding media to material is that 10: 1 ratio adds in the ball mill, carry out mechanically mixing, then, be warming up to 1100-1200 ℃, adopt the thermal explosion reaction synthesis method to make TiAl, grind 325 mesh sieves, got TiAl base alloy powder Ti-47.66Al-2.22Nb-1.34B, abbreviated TNB as.
Table 1 experiment starting material
Above-mentioned TiAl base alloy powder adds that weight percentage is 10%, granularity is the TiC ceramic particle of 0.5-2.0 μ m, adopts the discharge plasma sintering method, makes Ti
2The AlC/TiAl matrix material.
Ti
2The Mechanics Performance Testing result of AlC/TiAl matrix material is as shown in table 2.
Table 2:Ti
2The mechanical property of AlC/TiAl matrix material
Fig. 2 is Ti
2The surface topography of AlC/TiAl matrix material can be found Ti
2The AlC wild phase is evenly distributed on around the TiAl matrix.Fig. 3 is Ti
2The cross-section morphology of AlC/TiAl matrix material can be found the existing transcrystalline cleavage fracture of fracture mode of matrix material, also has along brilliant fracture, can be described as mixed mode.
In order further to improve Ti
2AlC/TiAl performance of composites or reach certain requirement is to Ti
2The AlC/TiAl matrix material is heat-treated to realize improving Ti
2The purpose of AlC/TiAl composite materials property.Adopt differential thermal analysis to determine the transformation temperature of TiAl intermetallic compound based composite material earlier, determine Ti as adopting differential thermal analysis
2Two phase transformation temperature points (eutectoid transformation T of AlC/TiAl matrix material
eWith peritectic transformation T
α), the result as shown in Figure 5, eutectoid transformation T
e1200 ℃ of ≈, peritectic transformation T
α1370 ℃ of ≈.As seen Ti
2The transformation temperature of AlC/TiAl matrix material is than the transformation temperature (T of general T iAl alloy
e1125 ℃ of ≈, T
α1360 ℃ of ≈) want high many.
The present invention has adopted two kinds of heat treatment modes to improve Ti
2The mechanical property of AlC/TiAl matrix material, a kind of is the thermal treatment that is rapidly heated; Another kind is to Ti
2The AlC/TiAl matrix material carries out multistep thermal treatment, comprises homogenizing processing, anneal and three steps of ageing treatment.
Thermal treatment is rapidly heated: have the advantages that as adopting discharge plasma sintering (SPS) technology sintering heat-up rate is fast, sintering temperature is low, for the body series matrix material, compare with other conventional sintering methods, low 150 ℃ approximately of SPS sintering temperatures.It is as shown in table 3 to formulate 2 kinds of heat-treatment protocol.
Table 3: heat-treatment protocol is rapidly heated
Ti
2The AlC/TiAl matrix material be rapidly heated after the thermal treatment the Mechanics Performance Testing result as shown in Figure 5.After can finding thermal treatment, flexural strength and fracture toughness property all are significantly improved, and the composite property of admixture B element is better.
Ti
2The AlC/TiAl matrix material be rapidly heated after the thermal treatment cross-section morphology as shown in Figure 6.The fracture mode that can find matrix material is a transcrystalline cleavage fracture entirely almost, has a large amount of cleavage step and river pattern.Ti
2The AlC/TiAl matrix material be rapidly heated after the thermal treatment surface topography as shown in Figure 7.The matrix that can find matrix material has formed more synusia colony, and the matrix grain and the synusia colony size of the matrix material of admixture trace element B are more tiny.
Multistep thermal treatment: matrix material is carried out multistep thermal treatment, and formulate thermal treatment process.As adopt high temperature box type resistance furnace that matrix material is carried out multistep thermal treatment.Its thermal treatment process figure as shown in Figure 8.4 kinds of heat-treatment protocol of specific design are as follows:
T1: sample is heated to 1050 ℃ from room temperature, and air cooling is to room temperature behind the insulation 24h; Reheat to 1390 ℃, air cooling is to room temperature behind the insulation 5min; Be heated to 900 ℃ at last, stove is chilled to room temperature behind the insulation 6h.
T2: sample is heated to 1050 ℃ from room temperature, and air cooling is to room temperature behind the insulation 24h; Reheat to 1320 ℃, air cooling is to room temperature behind the insulation 45min; Be heated to 900 ℃ at last, stove is chilled to room temperature behind the insulation 6h.
T3: sample is heated to 1050 ℃ from room temperature, and air cooling is to room temperature behind the insulation 24h; Reheat to 1250 ℃, air cooling is to room temperature behind the insulation 2h; Be heated to 900 ℃ at last, stove is chilled to room temperature behind the insulation 6h.
T4: sample is heated to 1050 ℃ from room temperature, and stove is chilled to room temperature behind the insulation 24h, and sample only carries out long ageing treatment.
Ti
2Mechanics Performance Testing result after the thermal treatment of AlC/TiAl matrix material multistep as shown in Figure 9.After can finding thermal treatment, various aspects of performance all makes moderate progress.
The cross-section morphology of each sample such as Figure 10 after the multistep thermal treatment, fracture mode is mainly transcrystalline cleavage fracture; Its surface topography such as Figure 11 can find at T
3And T
4In the heat-treatment protocol, promptly when 1250 ℃ of anneal and 1050 ℃ of ageing treatment, do not obtain the synusia colony, and at T
1And T
2In the heat-treatment protocol, promptly when 1390 ℃ and 1320 ℃ of anneal, obtain more synusia colony.
Claims (2)
1. method of improving TiAl intermetallic compound based composite material performance is characterized in that: may further comprise the steps,
Get the Ti powder of molar percentage 35-55%, the Al powder of 35-50%, the Nb powder of 3-10%, the B powder of 0-5%, after the mechanically mixing, be warming up to 1100-1200 ℃, adopt the thermal explosion reaction synthesis method to make TiAl, ground 325 mesh sieves, get the TiAl base alloy powder;
It is the TiC ceramic particle of 5%-20% that described TiAl base alloy powder adds weight percentage, adopts the discharge plasma sintering method, makes Ti
2The AlC/TiAl matrix material;
Described Ti
2The AlC/TiAl matrix material is heat-treated, and realizes by following multistep thermal treatment: described multistep heat treating method is three step factures, is heated to 1050 ℃ from room temperature, and air cooling is to room temperature behind the insulation 24h; Reheat is to 1300-1400 ℃, and air cooling is to room temperature behind the insulation 5-45min; Be heated to 900 ℃ at last, stove is chilled to room temperature behind the insulation 6h.
2. method according to claim 1 is characterized in that: described TiC ceramic particle particle diameter is 0.1-5.0 μ m.
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| EP3974082A4 (en) * | 2019-05-23 | 2023-05-31 | IHI Corporation | Tial alloy and production method therefor |
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| CN102501457A (en) * | 2011-09-30 | 2012-06-20 | 哈尔滨工业大学 | Ceramic-TiAl micro-laminated composite material board and preparation method thereof |
| FR3006696B1 (en) * | 2013-06-11 | 2015-06-26 | Centre Nat Rech Scient | PROCESS FOR MANUFACTURING A TITANIUM ALUMINUM ALLOY PIECE |
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| CN104961467B (en) * | 2015-06-12 | 2018-01-16 | 华南理工大学 | A kind of high tenacity ceramic matric composite and preparation method and application |
| CN108165865A (en) * | 2017-12-27 | 2018-06-15 | 济南大学 | A kind of novel TiAl-base alloy material and preparation method |
| CN109694971B (en) * | 2019-01-24 | 2021-02-26 | 重庆大学 | Powder metallurgy titanium-aluminum-based composite material and preparation method thereof |
| CN111961900A (en) * | 2020-09-07 | 2020-11-20 | 济南大学 | Novel titanium-aluminum-based composite material and preparation method thereof |
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| CN1337377A (en) * | 2001-09-20 | 2002-02-27 | 山东大学 | Intermatallic Ti-Al compound/alumina ceramic composite material and its prepn process |
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| CN1337377A (en) * | 2001-09-20 | 2002-02-27 | 山东大学 | Intermatallic Ti-Al compound/alumina ceramic composite material and its prepn process |
Non-Patent Citations (2)
| Title |
|---|
| TiC/TiAl复合材料微观结构观察及强韧化机理分析. 岳云龙，吴海涛，王志杰，王传彬，张联盟.济南大学学报（自然科学版），第18卷第2期. 2004 |
| TiC/TiAl复合材料微观结构观察及强韧化机理分析. 岳云龙，吴海涛，王志杰，王传彬，张联盟.济南大学学报（自然科学版），第18卷第2期. 2004 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3974082A4 (en) * | 2019-05-23 | 2023-05-31 | IHI Corporation | Tial alloy and production method therefor |
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