CN103820675A - Novel V-contained beta-gamma TiAl intermetallic compound material with high Nb content and preparation method thereof - Google Patents
Novel V-contained beta-gamma TiAl intermetallic compound material with high Nb content and preparation method thereof Download PDFInfo
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Abstract
The invention provides a novel V-contained beta-gamma TiAl intermetallic compound material with high Nb content and a preparation method thereof, and belongs to an intermetallic compound material. The novel V-contained beta-gamma TiAl intermetallic compound material with the high Nb content comprises elements in a mole percentage as follows: 43%-45% of Al, 5%-15% of Nb, not higher than 1% of V and the balance of Ti and inevitable impurities. According to composition, the raw materials are subjected to briquetting forming by a metal briquetting machine, a briquette comprises a titanium sponge layer, a high-purity aluminum layer, an aluminum and Nb intermediate alloy layer, an aluminum and V intermediate alloy layer and a titanium sponge layer from bottom to top respectively; the briquette is placed in a water-cooling copper crucible vacuum induction suspension melting furnace, vacuum pumping is performed, smelting power is increased at a speed of 20-30 kW/min until the smelting power is increased to 160-180 kW, then smelting is performed under the constant power to obtain melts, and the melts are mixed uniformly; and the melts are cast into a preheated metal casting mold which centrifugally rotates, and are subjected to furnace cooling. Therefore, the TiAl alloy with high Nb content is obtained, is uniform and small in structure and has no obvious segregation.
Description
Technical field
The present invention relates to a kind of intermetallic compound and preparation technology thereof, relate in particular to a kind of novel β-γ of the high Nb of V TiAl inter-metallic compound material and preparation method thereof that contains, belong to inter-metallic compound material.
Background technology
TiAl intermetallic compound has low density, good mechanical behavior under high temperature and the feature such as oxidation-resistance property preferably, is considered to 21st century the most with potential applications and be expected to be widely used in the high-temperature structural material in the field such as Aeronautics and Astronautics and automobile.But, the drawbacks limit such as the low and hot workability of TiAl intermetallic compound temperature-room type plasticity is poor its widespread use.Recent decades, Chinese scholars is being done a large amount of explorations and research aspect the microstructure and property of TiAl intermetallic compound.Result demonstration, introducing β is the important means that improves TiAl intermetallic compound mechanical property and hot workability mutually.And in recent years, the high-niobium TiAl intermetallic compound rising both at home and abroad receives much concern because it has good over-all properties.But there is not yet report about preparation and the physical metallurgy behavior of V in high niobium Ti Al alloy of the high-niobium TiAl intermetallic compound material that contains β phase.
Summary of the invention
The object of this invention is to provide and a kind ofly obtain by adding β phase stable element V the tissue that contains β phase, so improve material property containing the high Nb of V novel β-γ TiAl inter-metallic compound material and preparation method.
One of the present invention containing the novel β-γ of the high niobium of V TiAl inter-metallic compound material, is characterized in that, the molar content of its element is: 43%～45% Al, 5～15%(preferably 8%) Nb, not higher than the Ti of 1% V and surplus and inevitable impurity.
Preparation method containing the novel β-γ of the high Nb of V TiAl intermetallic compound of the present invention, realizes by following step:
(1), take following raw material: titanium sponge, rafifinal, aluminium niobium master alloy and aluminium vanadium master alloy; The Al that the molar content of wherein controlling Al, Nb, V and Ti element is 43%～45%, 5～15% Nb, be not Ti and inevitable impurity higher than 1% V and surplus;
(2), by step (1) claim raw material carry out compound stalk forming by metallic briquette machine, when briquetting from bottom to top each layer be respectively sponge titanium layer, high-purity aluminium lamination, aluminium niobium master alloy layer, aluminium vanadium master alloy layer and sponge titanium layer;
(3) briquetting step (2) being obtained put into can the water jacketed copper crucible vacuum induction suspension smelting furnace of centrifugal casting in, before melting, metallic mould is preheated to 300～400 ℃, water jacketed copper crucible vacuum induction melting furnace is evacuated to 1.0～3.0 × 10
-3mbar, with the preferred 30kW/min of 20～30kW/min() rate of rise stops increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system is risen to 160～180kW, and then under firm power, melting 200～300s obtains melt, makes melt-mixing even;
(4) melt is cast in metallic mould after preheating and centrifugal rotation, centrifuge speed is preferably 140r/min, form containing V high-niobium TiAl intermetallic compound ingot casting, and furnace cooling.
In step of the present invention (1), the quality purity of titanium sponge is 99.7%, and the quality purity of rafifinal is 99.99%, and the quality purity of aluminium niobium master alloy is 99.8%, and the quality purity of aluminium vanadium master alloy is 99.6%; Each raw material is commercially available prod.
The present invention has determined the optimal addn scope of V, in Material Coagulating Process, V adds the route that solidifies that has changed alloy, by traditional L → L+ β → α → ... become L → L+ β → β → ... the high-niobium TiAl intermetallic compound material microstructure obtaining is very tiny, and without obviously segregation appearance, the β of formation mainly appears at lamella colony grain boundaries mutually, and is net distribution.Tiny tissue even, the obvious segregation of nothing is conducive to the hot workability of alloy, improves the over-all properties of alloy.
The present invention obtained even tiny and without obvious segregation TiAl alloy structure, and adopt the melting of water jacketed copper crucible vacuum induction suspension smelting furnace, technological process is simple to operation.
Accompanying drawing explanation
Fig. 1 embodiment 1 schemes containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-43Al-8Nb-0.1V cast alloy optical microstructure;
Fig. 2 embodiment 1 containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-43Al-8Nb-0.1V cast alloy X-ray diffraction spectrogram;
Fig. 3 embodiment 1 containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-43Al-8Nb-0.1V cast alloy scanning electron microscopy;
Fig. 4 embodiment 2 schemes containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-45Al-8Nb-1V cast alloy optical microstructure;
Fig. 5 embodiment 2 containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-45Al-8Nb-1V cast alloy X-ray diffraction spectrogram;
Fig. 6 embodiment 2 containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-45Al-8Nb-1V cast alloy scanning electron microscopy.
Fig. 7 embodiment 3 schemes containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-44Al-8Nb-0.5V cast alloy optical microstructure;
Fig. 8 embodiment 3 containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-44Al-8Nb-0.5V cast alloy X-ray diffraction spectrogram;
Fig. 9 embodiment 3 containing the novel β-γ of the high Nb of V TiAl intermetallic compound Ti-44Al-8Nb-0.5V cast alloy scanning electron microscopy.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
Realizing by following step containing the preparation of the novel β-γ of the high Nb of V TiAl inter-metallic compound material of the present embodiment: one, take following raw material: titanium sponge, rafifinal, aluminium niobium master alloy and aluminium vanadium master alloy, wherein Ti48.9at.%, Al43at.%, Nb8at.%, V0.1at.%; Two, step 1 is claimed raw material carry out compound stalk forming by metallic briquette machine, when briquetting from bottom to top each layer be respectively sponge titanium layer, high-purity aluminium lamination, aluminium niobium master alloy layer, aluminium vanadium master alloy layer and sponge titanium layer; Three, briquetting step 2 being obtained put into can the water jacketed copper crucible vacuum induction suspension smelting furnace of centrifugal casting in, before melting, metallic mould is preheated to 350 ℃, water jacketed copper crucible vacuum induction melting furnace is evacuated to 1.0 × 10
-3mbar; Four, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system being risen to 180kW with 30kW/min rate of rise, then under firm power, melting 200s obtains melt, makes melt-mixing even; Five, melt is cast in metallic mould after preheating and centrifugal rotation, centrifuge speed is preferably 140r/min, and ingot casting is of a size of φ 50 × 180mm, and furnace cooling, obtains Ti-43Al-8Nb-0.1V compound ingot casting.
Adopt electric spark wire cutting method to cut 15 × 15 × 10mm sample from ingot casting, metallographic and scanned sample are ground to 2000 orders through abrasive paper for metallograph from 180 orders, then throw with electropolisher, is smart; X-ray diffraction sample is ground to 1000 orders through washing sand paper from 180 orders, then uses dehydrated alcohol clean surface; Transmission sample is the thin slice of 0.5mm, is ground to 40um thick with sand paper, then adopts the preparation of two spray thinning technique.Utilize the microstructure of metallography microscope sem observation Ti-43Al-8Nb-0.1V to find, the tissue of TiAl alloy is tiny equiaxed grain structure, sees Fig. 1; Utilize XRD (X-ray diffractometer) to analyze discovery, in alloy except α
2outside γ phase, also have β to occur mutually, see Fig. 2; Utilize scanning electronic microscope and electronic probe to analyze discovery, white exposes and is mainly distributed in lamella colony grain boundaries, sees Fig. 3.
Embodiment 2
Realizing by following step containing the preparation of the novel β-γ of the high Nb of V TiAl inter-metallic compound material of present embodiment: one, take following raw material: titanium sponge, rafifinal, aluminium niobium master alloy and aluminium vanadium master alloy, wherein Ti46at.%, Al45at.%, Nb8at.%, V1.0at.%; Two, step 1 is claimed raw material carry out compound stalk forming by metallic briquette machine, when briquetting from bottom to top each layer be respectively sponge titanium layer, high-purity aluminium lamination, aluminium niobium master alloy layer, aluminium vanadium master alloy layer and sponge titanium layer; Three, briquetting step 2 being obtained put into can the water jacketed copper crucible vacuum induction suspension smelting furnace of centrifugal casting in, before melting, metallic mould is preheated to 380 ℃, water jacketed copper crucible vacuum induction melting furnace is evacuated to 2.6 × 10
-3mbar; Four, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system being risen to 170kW with 30kW/min rate of rise, then under firm power, melting 220s obtains melt, makes melt-mixing even; Five, melt is cast in metallic mould after preheating and centrifugal rotation, centrifuge speed is preferably 140r/min, and ingot casting is of a size of φ 50 × 180mm, and furnace cooling, obtains Ti-45Al-8Nb-1V compound ingot casting.
Adopt electric spark wire cutting method to cut 15 × 15 × 10mm sample from ingot casting, metallographic and scanned sample are ground to 2000 orders through abrasive paper for metallograph from 180 orders, then throw with electropolisher, is smart; X-ray diffraction sample is ground to 1000 orders through washing sand paper from 140 orders, then uses ultrasonic oscillator clean surface; Transmission sample is the thin slice of 0.5mm, is ground to 40um thick with sand paper, then adopts the preparation of two spray thinning technique.Utilize the microstructure of metallography microscope sem observation Ti-45Al-8Nb-1V to find, the tissue of TiAl alloy is tiny equiaxed grain structure, sees Fig. 4; Utilize XRD (X-ray diffractometer) to analyze discovery, in alloy except α
2outside γ phase, also have β to occur mutually, see Fig. 5; Utilize scanning electronic microscope and electronic probe to analyze discovery, white exposes and is mainly distributed in lamella colony grain boundaries and is net distribution, sees Fig. 6.
Embodiment 3
Realizing by following step containing the preparation of the novel β-γ of the high Nb of V TiAl inter-metallic compound material of present embodiment: one, take following raw material: titanium sponge, rafifinal, aluminium niobium master alloy and aluminium vanadium master alloy, wherein Ti47.5at.%, Al44at.%, Nb8at.%, V0.5at.%; Two, step 1 is claimed raw material carry out compound stalk forming by metallic briquette machine, when briquetting from bottom to top each layer be respectively sponge titanium layer, high-purity aluminium lamination, aluminium niobium master alloy layer, aluminium vanadium master alloy layer and sponge titanium layer; Three, briquetting step 2 being obtained put into can the water jacketed copper crucible vacuum induction suspension smelting furnace of centrifugal casting in, before melting, metallic mould is preheated to 320 ℃, water jacketed copper crucible vacuum induction melting furnace is evacuated to 1.8 × 10
-3mbar; Four, stop increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system being risen to 165kW with 30kW/min rate of rise, then under firm power, melting 250s obtains melt, makes melt-mixing even; Five, melt is cast in metallic mould after preheating and centrifugal rotation, centrifuge speed is preferably 140r/min, and ingot casting is of a size of φ 50 × 180mm, and furnace cooling, obtains Ti-44Al-8Nb-0.5V compound ingot casting.
Adopt electric spark wire cutting method to cut 15 × 15 × 10mm sample from ingot casting, metallographic and scanned sample are ground to 2000 orders through abrasive paper for metallograph from 180 orders, then throw with electropolisher, is smart; X-ray diffraction sample is ground to 1000 orders through washing sand paper from 140 orders, then uses ultrasonic oscillator clean surface; Transmission sample is the thin slice of 0.5mm, is ground to 40um thick with sand paper, then adopts the preparation of two spray thinning technique.Utilize the microstructure of metallography microscope sem observation Ti-44Al-8Nb-0.5V to find, the tissue of TiAl alloy is tiny equiaxed grain structure, sees Fig. 7; Utilize XRD (X-ray diffractometer) to analyze discovery, in alloy except α
2outside γ phase, also have β to occur mutually, see Fig. 8; Utilize scanning electronic microscope and electronic probe to analyze discovery, white exposes and is mainly distributed in lamella colony grain boundaries and is net distribution, sees Fig. 9.
Embodiment 4
(1), take following raw material: titanium sponge, rafifinal, aluminium niobium master alloy and aluminium vanadium master alloy; The Al that the molar content of wherein controlling Al, Nb, V and Ti element is 43%～45%, 8～10% the V of Nb, 0.1-1% and the Ti of surplus and impurity;
(2), by step (1) claim raw material carry out compound stalk forming by metallic briquette machine, when briquetting from bottom to top each layer be respectively sponge titanium layer, high-purity aluminium lamination, aluminium niobium master alloy layer, aluminium vanadium master alloy layer and sponge titanium layer;
(3) briquetting step (2) being obtained put into can the water jacketed copper crucible vacuum induction suspension smelting furnace of centrifugal casting in, before melting, metallic mould is preheated to 300～400 ℃, water jacketed copper crucible vacuum induction melting furnace is evacuated to 1.0～3.0 × 10
-3mbar, with the preferred 30kV/min of 20～30kW/min() rate of rise stops increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system is risen to 160～180kW, and then under firm power, melting 200～300s obtains melt, makes melt-mixing even;
(4) melt is cast in metallic mould after preheating and centrifugal rotation, centrifuge speed is preferably 140r/min, form containing the high Nb TiAl of V intermetallic compound ingot casting, and furnace cooling.
What adopt that the sign identical with embodiment 3 with embodiment 1, embodiment 2 obtain is tiny evenly and without obviously segregation containing V high-niobium TiAl intermetallic compound material microstructure, in tissue, there is the β phase of brilliant white, be mainly distributed in lamella colony grain boundaries and be net distribution.
Claims (7)
1. containing the novel β-γ of the high Nb of a V TiAl inter-metallic compound material, it is characterized in that the molar content of its element: 43%～45% Al, 5～15% Nb, not higher than the Ti of 1% V and surplus and inevitable impurity.
2. contain the novel β-γ of the high Nb of V TiAl inter-metallic compound material according to the one of claim 1, it is characterized in that, the molar content 8% of Nb, the molar content of V is not higher than 1%.
3. contain the novel β-γ of the high Nb of V TiAl inter-metallic compound material according to the one of claim 1, it is characterized in that the molar content 8% of Nb, the molar content 0.1～1% of V.
4. containing the preparation method of the novel β-γ of the high Nb of V TiAl intermetallic compound, it is characterized in that, comprise the steps:
(1), take following raw material: titanium sponge, rafifinal, aluminium niobium master alloy and aluminium vanadium master alloy; The Al that the molar content of wherein controlling Al, Nb, V and Ti element is 43%～45%, 5～15% Nb, not higher than 1% V and Ti and the impurity of surplus;
(2), by step (1) claim raw material carry out compound stalk forming by metallic briquette machine, when briquetting from bottom to top each layer be respectively sponge titanium layer, high-purity aluminium lamination, aluminium niobium master alloy layer, aluminium vanadium master alloy layer and sponge titanium layer;
(3), briquetting that step (2) is obtained put into can the water jacketed copper crucible vacuum induction suspension smelting furnace of centrifugal casting in, before melting, metallic mould is preheated to 300～400 ℃, water jacketed copper crucible vacuum induction melting furnace is evacuated to 1.0～3.0 × 10
-3mbar, stops increasing power after water jacketed copper crucible vacuum induction melting furnace monitor system being risen to 160～180kW with 20～30kW/min rate of rise, and then under firm power, melting 200～300s obtains melt, makes melt-mixing even;
(4), melt is cast in metallic mould after preheating and centrifugal rotation, form containing V high-niobium TiAl intermetallic compound ingot casting, and furnace cooling.
5. according to the method for claim 4, it is characterized in that, with 30kW/min rate of rise, water jacketed copper crucible vacuum induction suspension smelting furnace monitor system is risen to 160～180kW and carries out centrifugal casting forming.
6. according to the method for claim 4, it is characterized in that, centrifuge speed is preferably 140r/min.
7. according to the method for claim 4, it is characterized in that, in (1), the quality purity of titanium sponge is 99.7%, and the quality purity of rafifinal is 99.99%, and the quality purity of aluminium niobium master alloy is 99.8%, and the quality purity of aluminium vanadium master alloy is 99.6%.
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Cited By (2)
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| CN104928531A (en) * | 2015-05-12 | 2015-09-23 | 哈尔滨工业大学 | Uniform TiAl alloy lamellar structure and preparation method thereof |
| CN106702211A (en) * | 2016-12-30 | 2017-05-24 | 哈尔滨工业大学 | Method for optimizing beta-gamma TiAl alloy heat processing performance |
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| CN106702211A (en) * | 2016-12-30 | 2017-05-24 | 哈尔滨工业大学 | Method for optimizing beta-gamma TiAl alloy heat processing performance |
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Application publication date: 20140528 |