CN110239161A - A kind of Nb-TiAl laminar composite and preparation method thereof - Google Patents
A kind of Nb-TiAl laminar composite and preparation method thereof Download PDFInfo
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- CN110239161A CN110239161A CN201910636779.9A CN201910636779A CN110239161A CN 110239161 A CN110239161 A CN 110239161A CN 201910636779 A CN201910636779 A CN 201910636779A CN 110239161 A CN110239161 A CN 110239161A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/42—Alternating layers, e.g. ABAB(C), AABBAABB(C)
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Abstract
A kind of Nb-TiAl laminar composite and preparation method thereof, belongs to field of alloy preparation technology.The invention solves the intrinsic brittleness of TiAl alloy, the problem of ductility and toughness at room temperature is low, molding not easy to be processed.A kind of Nb-TiAl laminar composite is by periodic Nb/ high Nb containing TiAl based alloy structure composition.Method: the one, surface clean of Ti foil, Al foil and Nb foil；Two, washed Ti foil, Al foil and Nb foil are subjected to lamination, prepare prefabricated component；Three, Low Temperature Heat Treatment；Four, medium annealing；Five, consolidation to obtain the final product.The present invention is used to prepare Nb-TiAl laminar composite, can other complicated shapes such as nearly sheet forming Nb-TiAl laminar composite.
Description
Technical field
The invention belongs to technical field of composite preparation, and in particular to a kind of Nb-TiAl laminar composite and its system
Preparation Method.
Background technique
TiAl alloy has excellent high-temperature behavior, preferable inoxidizability, while having very high specific strength, specific modulus
The features such as, it is had broad application prospects in fields such as automobile manufacture, aerospaces.But TiAl alloy has intrinsic brittleness,
Disadvantages, these disadvantages such as low, room temperature moulding that there are damage tolerances and toughness are low make TiAl alloy difficult forming, are difficult to prepare shape
The structural member of shape complexity, using the modes such as isothermal forging, hot rolling to high Nb containing TiAl based alloy processed not only complex process but also
Cost is also higher.It, also can nearly sheet forming or other shapes how while improving the ductility and toughness at room temperature of TiAl alloy based on this
The structural member of shape complexity is that current needs urgently solve the problems, such as.
Summary of the invention
The purpose of the present invention is to solve at present can not be close to form system while improving TiAl alloy ductility and toughness at room temperature
The problem of slave board material or complex-shaped structural member, provides a kind of Nb-TiAl laminar composite and preparation method thereof, this method
While improving the ductility and toughness at room temperature of TiAl alloy, the structural member of the nearly sheet forming of energy or other shapes complexity.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of Nb-TiAl laminar composite, the Nb-TiAl laminar composite are by periodic Nb/
Ti3Al-TiAl/Nb structure composition, Nb be pure Nb, upper and lower two it is Nb layers pure between, be arranged alternately Ti3Al layers and TiAl layers, and structure
At a cycle laminated construction.
A kind of preparation method of above-mentioned Nb-TiAl laminar composite, the method follow the steps below:
Step 1: 5~10min successively is cleaned by ultrasonic to Ti foil, Al foil and Nb foil respectively using alcohol and acetone, removes table
Then the greasy dirt in face utilizes 5vol.%~15vol.%HF, 100vol.%HF and 5vol.%~15vol.%NaOH solution point
It is other that Ti foil, Nb foil and Al foil surface are cleaned, the oxide skin on surface is removed, after being finally cleaned by ultrasonic 2~5min with alcohol,
It dries up spare；
Step 2: Ti foil, Al foil and the Nb foil that step 1 is washed carry out lamination, when in order to guarantee to fill sample and hot pressing, institute
The section of foil be it is identical, the materials'use graphite paper folded is coated, and fix lamination using wire, is obtained
To Nb/ high Nb-TiAl laminar composite prefabricated component；The lamination is the upper layer and lower layer difference in each period laminated construction
Nb foil is placed, then by Ti foil and Al foil alternative stacked between upper layer and lower layer Nb foil；By adjusting lamination quantity from 1 period
Laminated construction can control the thickness of final material to multiple period laminated construction；
Step 3: prefabricated component prepared by step 2 being fitted into graphite jig, is then placed in vacuum hotpressing stove, and vacuum is taken out
To 1 × 10-3Pa applies 40~80MPa pressure hereinafter, in 520~550 DEG C of 10~30min of hot pressing；Then 600~660 are warming up to
DEG C heat preservation 2~8h, apply 10~30MPa pressure carry out low-temperature annealing, obtain by Nb, Ti and TiAl3The composite material of phase composition；
Step 4: by step 3 obtain by Nb, Ti and TiAl3The composite material of phase composition is warming up to 800~880 DEG C
10~30h is kept the temperature, 30~50MPa pressure is applied, acquisition periodic structure is Nb-Ti3The laminar composite of Al-TiAl-Nb；
Step 5: the laminar composite that step 4 is obtained is warming up to 1150~1250 DEG C of 10~60min of heat preservation, applies
50~80MPa pressure obtains Nb-TiAl laminar composite.
The present invention having the beneficial effect that compared with the existing technology
One, Nb-Ti is prepared by the way of foil metallurgy3Al-TiAl-Nb laminar composite utilizes the good room of foil
Warm deformation and mouldability feature, can nearly sheet forming and other complex-shaped structural members, avoid it is subsequent to material at
Type processing；
Two, Nb-Ti is prepared3Al-TiAl-Nb laminar composite simple process, without special equipment.
Three, tissue thickness is regulated and controled by the way of multiple step anneal heat treatment, it is matched is easily obtained optimum performance
Composite material.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of stacking material；
Fig. 2 is the microscopic appearance figure after 550 DEG C/30min/50MPa+860 DEG C/3h/30MPa heat treatment；
Fig. 3 is the microscopic appearance figure after 550 DEG C/30min/50MPa+860 DEG C/20h/30MPa heat treatment.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawings and examples, and however, it is not limited to this,
All to be modified to technical solution of the present invention or equivalent replacement, range without departing from the spirit of the technical scheme of the invention should all
Cover within the protection scope of the present invention.
Specific embodiment 1: that present embodiment record is a kind of Nb-TiAl laminar composite, the Nb-
TiAl laminar composite is by periodic Nb/Ti3Al-TiAl/Nb structure composition, Nb are pure Nb, and upper and lower two Nb layers pure
Between, it is arranged alternately Ti3Al layers and TiAl layers, and constitute a cycle laminated construction.
Specific embodiment 2: a kind of Nb-TiAl laminar composite described in specific embodiment one, described Nb layers pure
Single layer with a thickness of 20~50 μm, primarily as the ductile layers of composite material, while there is good heat-resisting quantity.
Specific embodiment 3: a kind of Nb-TiAl laminar composite, the Ti described in specific embodiment one3Al
Layer and TiAl layer thickness ratio be 1:1~2, can by preparation process adjustment raw material Ti foil and Al foil thickness ratio or
It is to be regulated and controled by controlling in 1150~1250 DEG C of soaking time.
Specific embodiment 4: a kind of Nb-TiAl laminar composite described in specific embodiment one, described Nb layers pure
Thick and TiAl thickness and Ti3The thickness ratio of Al thickness summation be 1:3.5~5, by control during the preparation process ductile layers Nb foil,
The original thickness of Ti foil and Al foil ratio, can control final Nb, TiAl and Ti3The thickness ratio of Al, to the close of laminar composite
Degree, plasticity and toughness are regulated and controled, and the best Nb-TiAl laminar composite of comprehensive performance is obtained.
Specific embodiment 5: Nb-TiAl layers described in a kind of any specific embodiment of specific embodiment one to four
The preparation method of shape composite material, the method follow the steps below:
Step 1: successively using alcohol and acetone respectively to Ti foil, Al foil and Nb foil ultrasonic (power 2000W) cleaning 5~
10min removes the greasy dirt on surface, then using 5vol.%~15vol.%HF, 100vol.%HF and 5vol.%~
15vol.%NaOH solution respectively cleans Ti foil, Nb foil and Al foil surface, removes the oxide skin on surface, finally uses alcohol
After ultrasonic (power 2000W) cleans 2~5min, hair dryer drying is spare；
Step 2: Ti foil, Al foil and the Nb foil that step 1 is washed carry out lamination, when in order to guarantee to fill sample and hot pressing, institute
The section of foil be it is identical, the materials'use graphite paper folded coated, and the use of diameter is 0.1~0.2mm
Wire fixes lamination, obtains Nb/ high Nb-TiAl laminar composite prefabricated component；The lamination is folded in each period
The upper layer and lower layer of layer structure place Nb foil respectively, then by Ti foil and Al foil alternative stacked between upper layer and lower layer Nb foil；Pass through
Lamination quantity is adjusted from 1 period laminated construction to multiple period laminated construction, can control the thickness of final material；
Step 3: prefabricated component prepared by step 2 being fitted into graphite jig, is then placed in vacuum hotpressing stove, and vacuum is taken out
To 1 × 10-3Pa applies 40~80MPa pressure hereinafter, in 520~550 DEG C of 10~30min of hot pressing；Then 600~660 are warming up to
DEG C heat preservation 2~8h, apply 10~30MPa pressure carry out low-temperature annealing, obtain by Nb, Ti and TiAl3The composite material of phase composition；
The shape of the graphite jig can be cuboid (the square bodily form), is also possible to other complicated shapes, thus reaches
The purpose of sheet forming or complex structural member；
Step 4: by step 3 obtain by Nb, Ti and TiAl3The composite material of phase composition is warming up to 800~880 DEG C
10~30h is kept the temperature, 30~50MPa pressure is applied, acquisition periodic structure is Nb-Ti3The laminar composite of Al-TiAl-Nb；
Step 5: the laminar composite that step 4 is obtained is warming up to 1150~1250 DEG C of 10~60min of heat preservation, applies
50~80MPa pressure obtains fine and close and does not have defective Nb-TiAl laminar composite.
Hot pressing in the present invention is divided into three phases, the first stage: 520~550 DEG C/10~30min+600~660 DEG C/2
~8h makes Al foil be completely converted into TiAl3, Al liquid stream when high temperature is avoided to go out；Second stage: 800~880 DEG C of annealing guarantee
TiAl based compound TiAl2、TiAl3、Ti2Al5、Ti3Al, γ-TiAl etc. is substantially transitioned to α2-Ti3Al and γ-TiAl chemical combination
Object, while controlling Nb layers of reaction；Phase III: being warming up to 1150~1250 heat treatments, eliminates existing hole when medium annealing
The defects of hole, carries out densification to material, while can also regulate and control to each phase thickness degree of material.
The Nb-Ti of in-situ authigenic method preparation is utilized in the present invention3The laminar composite of Al-TiAl-Nb, Nb layers are located at
Nb-Ti3Two layers of the outermost of Al-TiAl-Nb periodic structure, Nb layers, Ti3Al, TiAl thickness degree are controllable, and interface is straight and connects
It connects very well；TiAl layers of elevated temperature strength with higher, Ti3Al layers have higher hardness, Ti3Al layers can further strengthen
The multilayered structure of the performance of TiAl, the preferable Nb of plasticity and toughness and material can be further improved the plasticity and toughness of material, obtain tough
The material of property best fit；The institutional framework needed is obtained using medium temperature, the mode of high annealing densification can be controlled effectively
The diffusion of Nb processed guarantees that the thickness of Nb is controllable.
The material interface that the present invention is formed is clearly smooth, material densification zero defect.Preparation process is pollution-free, and process advantage is bright
It is aobvious.
Specific embodiment 6: a kind of preparation method of Nb-TiAl laminar composite described in specific embodiment five,
In step 1, the Ti foil is TC4Or the common foil such as TA1, thickness in monolayer are 20~50 μm；The Al foil is pure Al foil, single
Layer is with a thickness of 10~50 μm.
Specific embodiment 7: a kind of preparation method of Nb-TiAl laminar composite described in specific embodiment five,
In step 1, Ti foil and Al foil surface magnetic control sputtering Nb film or Nb alloy film after drying, coating single side, with a thickness of 0~4 μ
M prepares Nb/Ti using the foil of plated film3Al-TiAl/Nb laminar composite, Ti at this time3Al and TiAl layers is just able to achieve Nb
Etc. alloyings, further increase Ti3Al and TiAl layers of mechanical property.
Specific embodiment 8: a kind of preparation method of Nb-TiAl laminar composite described in specific embodiment five,
In step 3, specifically: prefabricated component prepared by step 2 is fitted into graphite jig, is then placed in vacuum hotpressing stove, vacuum
It is evacuated to 1 × 10-3Pa applies 50~60MPa pressure hereinafter, in 540~550 DEG C of 10~20min of hot pressing；Then it is warming up to 630~
645 DEG C of 4~6h of heat preservation apply 10~15MPa pressure and carry out low-temperature annealing, obtain by Nb, Ti and TiAl3The composite wood of phase composition
Material.
Specific embodiment 9: a kind of preparation method of Nb-TiAl laminar composite described in specific embodiment five,
In step 4, specifically: by step 3 obtain by Nb, Ti and TiAl3The composite material of phase composition is warming up to 850~880 DEG C
Heat preservation 18~for 24 hours, apply 30~40MPa pressure, acquisition periodic structure is Nb-Ti3The layer structure material of Al-TiAl-Nb.
Specific embodiment 10: a kind of preparation method of Nb-TiAl laminar composite described in specific embodiment five,
In step 5, specifically: the laminar composite for obtaining step 4 is warming up to 1200~1250 DEG C of 10~30min of heat preservation, applies
Add 50~60MPa pressure, obtains fine and close Nb-TiAl laminar composite.
Embodiment 1:
One, first Ti foil, Al foil and Nb foil are cleaned by ultrasonic with alcohol and acetone respectively, scavenging period 5min, are removed
The greasy dirt on surface, then using 10vol.%HF, 100vol.%HF and 10vol.%NaOH solution respectively to Ti foil, Nb foil and
Al foil carries out surface clean, removes the oxide skin on surface, and after being finally cleaned by ultrasonic 5min with alcohol, hair dryer drying is spare；Its
Described in Ti foil with a thickness of 20 μm, Al foil with a thickness of 17 μm, Nb foil with a thickness of 25 μm；
Two, Ti foil, Al foil and the Nb foil washed step 1 carries out lamination, and folding sequence is Nb foil respectively in a cycle
The top and bottom of lamination, middle layer are alternate Ti foil and Al foil；When in order to guarantee to fill sample and hot pressing, all foils begin
Eventually in a plane, graphite coat is carried out to the material folded, fixes lamination using the wire that diameter is 0.15mm, makes
Standby Nb/ high Nb-TiAl laminar composite prefabricated component；
Three, prefabricated component prepared by step 2 is fitted into graphite jig, is then placed in vacuum hotpressing stove, vacuum is evacuated to 1
×10-3Pa applies 50MPa pressure hereinafter, in 550 DEG C of hot pressing 15min；Then 640 DEG C of heat preservation 4h are warming up to, 15MPa pressure is applied
Power carries out low-temperature annealing, obtains by Nb, Ti and TiAl3The low-temperature annealing tissue of phase composition；
Four, by step 3 obtain by Nb, Ti and TiAl3The low-temperature annealing tissue of phase composition is warming up to 865 DEG C of heat preservations
20h, applies 40MPa pressure, and acquisition periodic structure is Nb-Ti3The layer structure material of Al-TiAl-Nb；
Five, the laminar composite that the periodic structure that step 4 obtains is Nb-Ti3Al-TiAl-Nb is warming up to 1200
DEG C, 30min is kept the temperature, 60MPa pressure is applied, obtains fine and close and does not have defective Nb-TiAl laminar composite.
The structure of precast body described in the present embodiment step 4 is as shown in Figure 1, as can be seen from the figure Nb-Ti3Al-
The laminar composite a cycle layer of TiAl-Nb folds sequence and using the fixed foil of wire after graphite paper cladding.
In Fig. 2 step 4, SEM-BSE organization chart of the composite material after 865 DEG C of heat preservation 10h, as seen from the figure, at this moment material is main
By Nb, γ-TiAl, Ti3Al、TiAl3、TiAl2Deng composition；Fig. 3 is in step 4, and composite material is after 865 DEG C of heat preservation 20h
SEM-BSE tissue, as seen from the figure, after the reaction of 20h, material is by Nb, Ti3Al, γ-TiAl composition.
Claims (10)
1. a kind of Nb-TiAl laminar composite, it is characterised in that: the Nb-TiAl laminar composite is by periodicity
Nb/Ti3Al-TiAl/Nb structure composition, Nb be pure Nb, upper and lower two it is Nb layers pure between, be arranged alternately Ti3Al layers and TiAl
Layer, and constitute a cycle laminated construction.
2. a kind of Nb-TiAl laminar composite according to claim 1, it is characterised in that: the pure Nb layers of single layer
With a thickness of 20~50 μm.
3. a kind of Nb-TiAl laminar composite according to claim 1, it is characterised in that: the Ti3Al layers and TiAl
The thickness ratio of layer is 1:1~2.
4. a kind of Nb-TiAl laminar composite according to claim 1, it is characterised in that: the pure Nb thickness with
TiAl thickness and Ti3The thickness ratio of Al thickness summation is 1:3.5~5.
5. a kind of preparation method of Nb-TiAl laminar composite described in Claims 1 to 4 any claim, feature
Be: the method follows the steps below:
Step 1: 5~10min successively is cleaned by ultrasonic to Ti foil, Al foil and Nb foil respectively using alcohol and acetone, removes surface
Greasy dirt, it is then right respectively using 5vol.%~15vol.%HF, 100vol.%HF and 5vol.%~15vol.%NaOH solution
Ti foil, Nb foil and Al foil surface are cleaned, and the oxide skin on surface is removed, after being finally cleaned by ultrasonic 2~5min with alcohol, drying
It is spare；
Step 2: Ti foil, Al foil and the Nb foil that step 1 is washed carry out lamination, when in order to guarantee to fill sample and hot pressing, all foils
The section of material be it is identical, the materials'use graphite paper folded is coated, and fix lamination using wire, is obtained
Nb/ high Nb-TiAl laminar composite prefabricated component；The lamination is put respectively for the upper layer and lower layer in each period laminated construction
Nb foil is set, then by Ti foil and Al foil alternative stacked between upper layer and lower layer Nb foil；
Step 3: prefabricated component prepared by step 2 is fitted into graphite jig, is then placed in vacuum hotpressing stove, vacuum is evacuated to 1
×10-3Pa applies 40~80MPa pressure hereinafter, in 520~550 DEG C of 10~30min of hot pressing；Then 600~660 DEG C are warming up to
2~8h is kept the temperature, applies 10~30MPa pressure and carries out low-temperature annealing, obtain by Nb, Ti and TiAl3The composite material of phase composition；
Step 4: by step 3 obtain by Nb, Ti and TiAl3The composite material of phase composition is warming up to 800~880 DEG C of heat preservations 10
~30h, applies 30~50MPa pressure, and acquisition periodic structure is Nb-Ti3The laminar composite of Al-TiAl-Nb；
Step 5: the laminar composite that step 4 is obtained is warming up to 1150~1250 DEG C of 10~60min of heat preservation, apply 50~
80MPa pressure obtains Nb-TiAl laminar composite.
6. a kind of preparation method of Nb-TiAl laminar composite according to claim 5, it is characterised in that: step 1
In, the Ti foil is TC4Or TA1, thickness in monolayer are 20~50 μm；The Al foil is pure Al foil, and thickness in monolayer is 10~50 μm.
7. a kind of preparation method of Nb-TiAl laminar composite according to claim 5, it is characterised in that: step 1
In, Ti foil and Al foil surface magnetic control sputtering Nb film or Nb alloy film after drying, coating single side, with a thickness of 0~4 μm.
8. a kind of preparation method of Nb-TiAl laminar composite according to claim 5, it is characterised in that: step 3
In, specifically: prefabricated component prepared by step 2 is fitted into graphite jig, is then placed in vacuum hotpressing stove, vacuum is evacuated to 1 ×
10-3Pa applies 50~60MPa pressure hereinafter, in 540~550 DEG C of 10~20min of hot pressing；Then 630~645 DEG C of guarantors are warming up to
4~6h of temperature applies 10~15MPa pressure and carries out low-temperature annealing, obtains by Nb, Ti and TiAl3The composite material of phase composition.
9. a kind of preparation method of Nb-TiAl laminar composite according to claim 5, it is characterised in that: step 4
In, specifically: by step 3 obtain by Nb, Ti and TiAl3The composite material of phase composition is warming up to 850~880 DEG C of heat preservations 18
~for 24 hours, apply 30~40MPa pressure, acquisition periodic structure is Nb-Ti3The layer structure material of Al-TiAl-Nb.
10. a kind of preparation method of Nb-TiAl laminar composite according to claim 5, it is characterised in that: step 5
In, specifically: the laminar composite for obtaining step 4 is warming up to 1200~1250 DEG C of 10~30min of heat preservation, apply 50~
60MPa pressure obtains Nb-TiAl laminar composite.
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| CN111187945A (en) * | 2020-01-15 | 2020-05-22 | 江苏大学 | TiNb/NiTi memory material containing Nb layer and preparation method |
| CN115319268A (en) * | 2022-08-22 | 2022-11-11 | 中国航发北京航空材料研究院 | For TiAl alloys/Ti 2 AlNb alloy or Ti 3 Intermediate layer for Al-based alloy connection and diffusion welding method |
| CN115319261A (en) * | 2022-08-22 | 2022-11-11 | 中国航发北京航空材料研究院 | Ti/Al + X composite intermediate layer for TiAl/nickel-based superalloy connection and diffusion welding method |
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Cited By (4)
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| CN115319261A (en) * | 2022-08-22 | 2022-11-11 | 中国航发北京航空材料研究院 | Ti/Al + X composite intermediate layer for TiAl/nickel-based superalloy connection and diffusion welding method |
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| Publication number | Publication date |
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| CN110239161B (en) | 2021-06-22 |
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