CN104388753A - Smelting preparation method for titanium-aluminum intermetallic compounds - Google Patents

Smelting preparation method for titanium-aluminum intermetallic compounds Download PDF

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CN104388753A
CN104388753A CN201410608728.2A CN201410608728A CN104388753A CN 104388753 A CN104388753 A CN 104388753A CN 201410608728 A CN201410608728 A CN 201410608728A CN 104388753 A CN104388753 A CN 104388753A
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alloy
layer
raw material
melting
crucible
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朱郎平
李建崇
南海
黄东
罗倩
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BEIJING INSTITUTE OF AERONAUTICAL MATERIALS CHINA AVIATION INDUSTRY GROUP Corp
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BEIJING INSTITUTE OF AERONAUTICAL MATERIALS CHINA AVIATION INDUSTRY GROUP Corp
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Abstract

The invention discloses a smelting preparation method for titanium-aluminum intermetallic compounds. The method comprises the following steps: by taking titanium sponge, aluminum shot and other intermediate alloys as raw materials, layering and distributing materials in a crucible of a cold crucible vacuum induction suspension smelting furnace; vacuumizing, filling back inert gases, and smelting, the power is sequentially increased by stages in the smelting process; and finally, pouring the melt or cooling in the crucible, thereby obtaining the alloy with uniform composition. According to the smelting method, an electrode is not pressed, and the alloy with uniform composition and high purity can be obtained by virtue of an electromagnetic stirring function of induction smelting. The method is particularly suitable for smelting preparation of titanium-aluminum intermetallic compounds such as gamma-TiAl, Ti3Al and Ti2AlNb.

Description

A kind of smelting preparation method of Intermatallic Ti-Al compound
Technical field
The present invention is a kind of smelting preparation method of Intermatallic Ti-Al compound, relates to metal alloy compositions field of metallurgy.
Background technology
Intermatallic Ti-Al compound has that intensity is high, quality is light, good in oxidation resistance, and the advantage such as mechanical behavior under high temperature is good, be applied to aeroplane engine and aircraft component, can effectively reduce Flight Vehicle Structure weight, improve aircraft flying power and flight velocity, can also fuel efficiency be improved simultaneously, reduce flight cost, have great application prospect.But due to the type alloy each constituent element between the physical property difference such as fusing point, density large, cause the alloy being difficult to obtain uniform composition; The factor such as titanium, aluminium reactive behavior is high, and high to the susceptibility of interstitial element, is very easily polluted in fusion process; The reaction heat of alloying element dissolution process is high, and fusion process is wayward, and alloying constituent tolerance is little, and the trace change of composition often causes the greatest differences of performance.Such feature adds difficulty to the high-quality alloy melt of acquisition and ingot casting, proposes harsh requirement to the melting of such alloy.Therefore so select suitable melting technology, acquisition uniform composition, the Intermatallic Ti-Al compound that accurate, foreign matter content is low are melting urgent problems.
Vacuum induction skull melting technology (Induction Skull Melting, ISM) is one of method of melting hyperergy alloy advanced in the world at present.The method uses and forms crucible by the copper billet of several arc, external rings is around ruhmkorff coil, in fusion process, each copper billet of inserting in alternating electromagnetic field produces induced current, form a high-intensity magnetic field due to the annular effect in magnetic field in crucible inside, in metal charge, produce powerful induced current and furnace charge is melted rapidly.And in fusion process, furnace charge melt, owing to keeping non-contacting suspension tumbling state between electromagnetic repulsion force and crucible, produces strong stirring action, make that the overall composition of melt is consistent, the final content of homogeneous temperature, gas is less; Metal charge forms the very thin scull of one deck due to the chilling action of water jacketed copper crucible, the metal of melting and sidewall of crucible are separated, and has blocked the reaction between alloy melt and copper crucible, avoids the pollution of crucible material to metal melt.Therefore, the method is a kind of method of excellent melting Intermatallic Ti-Al compound.
But, adopt the method melting Intermatallic Ti-Al compound also to there are some technical problems.First, because the melting difference of the raw materials such as titanium sponge and aluminium simple substance reaches nearly 1000 degrees Celsius, in Vacuum Melting, during the melting sources such as titanium sponge, aluminium evaporates in a large number, causes element loss, accurately controls to bring certain difficulty to alloying constituent; On the other hand because the simple substance such as titanium, aluminium alloying is exothermic process, will produce a large amount of heat in fusion process, it is improper to control, and will cause splash that thermal explosion phenomenon even occurs, cause damage to equipment.Therefore, vacuum induction skull melting technology melting Intermatallic Ti-Al compound is utilized to have higher technical threshold.
Summary of the invention
The present invention designs for above-mentioned the deficiencies in the prior art the smelting preparation method providing a kind of Intermatallic Ti-Al compound just, its objective is the homogenizing degree in order to improve Intermatallic Ti-Al compound further, solving the problem of Intermatallic Ti-Al compound induction melting generation splash or thermal explosion.
The object of the invention is to be achieved through the following technical solutions:
The smelting preparation method of this kind of Intermatallic Ti-Al compound, described Intermatallic Ti-Al compound is TiAl alloy, Ti3Al alloy and Ti2AlNb alloy, it is characterized in that: the step of the method is as follows:
(1) weighing
According to the composition proportion of Intermatallic Ti-Al compound, take titanium sponge, aluminium shot or aluminium block, and simple substance element, master alloy or simple substance element add master alloy, are contained in different containers for future use respectively by kind;
The purity of titanium sponge is A level or 0A level;
In aluminium shot or aluminium block, the massfraction of fine aluminium is not less than 99.99%;
Simple substance element refers to one or more in Nb, Cr, W, Mo, Mn, Ta, Er, Ni or B;
Master alloy refers to one or more in AlNb alloy, AlMo alloy, AlMn alloy, AlSi alloy, AlV alloy, AlY alloy, AlEr alloy, TiSn alloy, TiNb alloy or TiB2 alloy;
(2) cloth
Raw material layering is put in the middle of water-cooled copper pincers pot vacuum induction melting furnace crucible by 2.1, and at crucible bottom paving sponge titanium layer I or placement scull, this thickness being positioned at the sponge titanium layer I of crucible bottom is 1 ~ 5 centimetre;
2.2 spread simple substance element layer, master alloy layer or simple substance element layer on the sponge titanium layer I or scull of bottom adds master alloy layer, sponge titanium layer II is repaved afterwards above, the thickness of simple substance element layer and master alloy layer is 0.1 ~ 5 centimetre, and the thickness of sponge titanium layer II is 1 ~ 5 centimetre;
2.3 repetition above-mentioned steps 2.2 to simple substance elements, master alloy raw material are used up, and then spread aluminium shot or aluminium block layer, finally on aluminium shot or aluminium block layer, repave sponge titanium layer III, the thickness of sponge titanium layer III is 1 ~ 5 centimetre;
The material of described scull is the alloy with prepared alloy with identical component, or pure titanium scull;
(3) vacuumize after closing fire door, vacuumize and complete by one of following two kinds of modes:
3.1 suctions reach below 1Pa, and backfill argon gas or helium to 300 ~ 30000Pa carry out melting;
3.2 suctions backfill argon gas or helium after reaching below 10Pa, and then backfill argon gas or helium after being evacuated down to below 10Pa, repeatedly carry out 1 ~ 5 time to reduce the elemental gas such as oxygen, nitrogen content in stove, backfill argon gas or helium to 300 ~ 30000Pa carry out melting;
(4) melting
After melting starts, first with the power of 20 ~ 100KW, raw material is toasted 1 ~ 5 minute, then improve after there is red heat around power to raw material and be incubated 2 ~ 10 minutes, until donor center position is popular in crucible, again improve after there is drop around power to raw material and be incubated 1 ~ 10 minute, now raw material melts gradually, power is improved after raw material melts completely, melt temperature is made to reach more than alloy melting point 20 ~ 100 DEG C, and being incubated 1 ~ 20 minute, the melt of suspension realizes uniform composition under function composite by electromagnetic stirring;
(5) shaping ingot casting
Again by power raising 1% ~ 20%, improve melt overheat degree, reduce the viscosity of melt further, cool in crucible after insulation 0.5 ~ 5min or pour into ingot casting.
The present invention relates to Intermatallic Ti-Al compound preparation method, bulk cargo is adopted to carry out induction melting, the vacuum consumable smelting method that smelting titanium alloy is conventional relatively at present, decreases piezoelectricity polar ring joint, is conducive to this kind of preparation being difficult to press electrode metal of Intermatallic Ti-Al compound; The melt of load melting rear formation, in strong electromagnetic force current downflow, accelerates high-melting-point melting sources and diffusion, can eliminate high-density and be mingled with, the alloying constituent uniformity prepared; Physical characteristics according to different material carries out layer-by-layer distribution, solves splash, thermal explosion phenomenon appear in this type alloy problem in induction melting process; And by controlling melting vacuum tightness, reduce the volatilization of low melting point element, improve the accuracy of molten alloy composition, effectively can realize the accurate control of alloy composition.
The present invention, mainly for the preparation of the Intermatallic Ti-Al compound such as γ-TiAl, Ti3Al and Ti2AlNb of uniform composition, has very important using value and wide application market.
Embodiment
Below with reference to embodiment, technical solution of the present invention is further described:
Embodiment 1
The Intermatallic Ti-Al compound of preparation is TiAl alloy, and equipment adopts 20 kilograms of water-cooled copper pincers pot vacuum induction melting furnaces, and the step of the method is as follows:
(1) weighing
According to the composition proportion of Intermatallic Ti-Al compound, take 0A level titanium sponge 5.86kg, aluminium shot 3.24kg, AlNb75 alloying pellet 0.63kg, chromium powder 0.27kg, and be contained in different containers for future use respectively;
The massfraction 99.99% of fine aluminium in aluminium shot or aluminium block;
(2) cloth
2.1 place TiAl alloy scull in crucible bottom;
2.2 spread sponge titanium layer II on scull, and thickness is 2 centimetres, and then spread AlNb75 alloying pellet layer, thickness 1 centimetre, repaves chromium powder layer, thickness 0.5 centimetre;
2.3 repeat above-mentioned steps 2.2 process uses up AlNb75 alloying pellet and chromium powder for 4 times, and then spread aluminum bean layer, finally on aluminium shot or aluminium block layer, repave sponge titanium layer III, the thickness of sponge titanium layer III is 5 centimetres;
(3) vacuumize after closing fire door:
Suction reaches below 3Pa, then backfills argon gas to 300Pa, then carries out melting;
(4) melting
After melting starts, first with the power of 20 ~ 100KW, 2 minutes are toasted to raw material, then improve after there is red heat around power to raw material and be incubated 10 minutes, until donor center position is popular in crucible, again improve after there is drop around power to raw material and be incubated 8 minutes, now raw material melts gradually, power is improved after raw material melts completely, make melt temperature reach 1800 DEG C, and be incubated 10 minutes, the melt of suspension realizes uniform composition under function composite by electromagnetic stirring;
(5) shaping ingot casting
Again power is improved 20%, improve melt overheat degree, reduce the viscosity of melt further, after insulation 0.5min, pour into the ingot casting of diameter 120mm.
On ingot casting top, centre and bottom sampling carry out composition analysis, different element mass percentage is as shown in the table:
Element Ti Al Nb Cr O
Top More than 33.35 4.78 2.68 0.042
Middle part More than 33.34 4.79 2.67 0.045
Bottom More than 33.35 4.79 2.69 0.041
Embodiment 2
The Intermatallic Ti-Al compound of preparation is Ti2AlNb alloy, and equipment adopts 20 kilograms of water-cooled copper pincers pot vacuum induction melting furnaces, and the step of the method is as follows:
(1) weighing
According to the composition proportion of Intermatallic Ti-Al compound, take titanium sponge 4.64kg, aluminium block 1.11kg, niobium bits 4.25kg, and be contained in different containers for future use respectively;
The massfraction 99.99% of fine aluminium in aluminium shot or aluminium block;
(2) cloth
2.1 place Ti2AlNb alloy skull in crucible bottom;
2.2 spread sponge titanium layer II on scull, and thickness is 2 centimetres, then spread niobium bits, thickness 1 centimetre;
2.3 repeat above-mentioned steps 2.2 process uses up AlNb75 alloying pellet and chromium powder for 7 times, and then spread aluminum bean layer, finally on aluminium shot or aluminium block layer, repave sponge titanium layer III, the thickness of sponge titanium layer III is 5 centimetres;
(3) vacuumize after closing fire door:
Suction reaches 3Pa, then backfills argon gas to 5000Pa, then closes vacuum pump valve;
(4) melting
After melting starts, first with the power of 20 ~ 100KW, 1 minute is toasted to raw material, then improve after there is red heat around power to raw material and be incubated 2 minutes, until donor center position is popular in crucible, again improve after there is drop around power to raw material and be incubated 20 minutes, now raw material melts gradually, power is improved after raw material melts completely, make melt temperature reach 1850 DEG C, and be incubated 1 minute, the melt of suspension realizes uniform composition under function composite by electromagnetic stirring;
(5) shaping ingot casting
Again power is improved 20%, improve melt overheat degree, reduce the viscosity of melt further, after insulation 0.5min, in crucible, cooling obtains Ti2AlNb alloy cast ingot.
On ingot casting top, centre and bottom sampling carry out composition analysis, different element mass percentage is as shown in the table:
Element Ti Al Nb O
Top More than 27.10 42.85 0.039
Middle part More than 27.05 42.83 0.040
Bottom More than 27.11 42.84 0.040
Embodiment 3
The Intermatallic Ti-Al compound of preparation is Ti3Al alloy, and equipment adopts 20 kilograms of water-cooled copper pincers pot vacuum induction melting furnaces, and the step of the method is as follows:
(1) weighing
According to the composition proportion of Intermatallic Ti-Al compound, take titanium sponge 5.67kg, aluminium block 1.12kg, niobium block 2.77kg, AlMo50 alloying pellet 0.37kg, AlV50 alloying pellet 0.15kg, and be contained in different containers for future use respectively;
The massfraction 99.99% of fine aluminium in aluminium shot or aluminium block;
(2) cloth
2.1 at crucible bottom paving sponge titanium layer I, and thickness is 5 centimetres;
2.2 on sponge titanium layer I upper berth, and thickness is 2 centimetres, and then spread niobium bits layer, AlMo50 alloy layer and AlV50 alloy layer successively, thickness is respectively 1 centimetre, 0.2 centimetre and 0.1 centimetre;
2.3 repeat above-mentioned steps 2.2 process uses up niobium bits, AlMo50 alloy and AlV50 alloy for 6 times, and then spread aluminum bean layer, finally on aluminium shot or aluminium block layer, repave sponge titanium layer III, the thickness of sponge titanium layer III is 1 centimetre;
(3) vacuumize after closing fire door:
Suction reaches 3Pa, then backfills argon gas to 30000Pa, then closes vacuum pump valve;
(4) melting
After melting starts, first with the power of 20 ~ 100KW, 5 minutes are toasted to raw material, then improve after there is red heat around power to raw material and be incubated 5 minutes, until donor center position is popular in crucible, again improve after there is drop around power to raw material and be incubated 10 minutes, now raw material melts gradually, power is improved after raw material melts completely, make melt temperature reach 1850 DEG C, and be incubated 20 minutes, the melt of suspension realizes uniform composition under function composite by electromagnetic stirring;
(5) shaping ingot casting
Again power is improved 20%, improve melt overheat degree, reduce the viscosity of melt further, after insulation 0.5min, pour into the ingot casting of diameter 120mm.
On ingot casting top, centre and bottom sampling carry out composition analysis, different element mass percentage is as shown in the table:
Element Ti Al Nb Mo V O
Top More than 12.91 27.82 1.92 0.52 0.045
Middle part More than 12.89 27.84 1.91 0.50 0.043
Bottom More than 12.90 27.83 1.93 0.51 0.041
Technical solution of the present invention adopts titanium sponge, aluminium shot and other master alloy to be raw material, in cold crucible vacuum induction suspension smelting furnace crucible, carry out layer-by-layer distribution; Vacuumize rear backfilled with inert gas and carry out melting, in fusion process, heightening power successively stage by stage, the most at last melt cast or cool in crucible, obtaining the alloy of uniform composition.This melting method, without electrode pressing, can obtain uniform composition, alloy that purity is high by the induction stirring function of induction melting.The method is specially adapted to the melting preparation of the Intermatallic Ti-Al compounds such as γ-TiAl, Ti3Al and Ti2AlNb.

Claims (1)

1. a smelting preparation method for Intermatallic Ti-Al compound, described Intermatallic Ti-Al compound is TiAl alloy, Ti3Al alloy and Ti2AlNb alloy, it is characterized in that: the step of the method is as follows:
(1) weighing
According to the composition proportion of Intermatallic Ti-Al compound, take titanium sponge, aluminium shot or aluminium block, and simple substance element, master alloy or simple substance element add master alloy, are contained in different containers for future use respectively by kind;
The purity of titanium sponge is A level or 0A level;
In aluminium shot or aluminium block, the massfraction of fine aluminium is not less than 99.99%;
Simple substance element refers to one or more in Nb, Cr, W, Mo, Mn, Ta, Er, Ni or B;
Master alloy refers to one or more in AlNb alloy, AlMo alloy, AlMn alloy, AlSi alloy, AlV alloy, AlY alloy, AlEr alloy, TiSn alloy, TiNb alloy or TiB2 alloy;
(2) cloth
Raw material layering is put in the middle of water-cooled copper pincers pot vacuum induction melting furnace crucible by 2.1, and at crucible bottom paving sponge titanium layer I or placement scull, this thickness being positioned at the sponge titanium layer I of crucible bottom is 1 ~ 5 centimetre;
2.2 spread simple substance element layer, master alloy layer or simple substance element layer on the sponge titanium layer I or scull of bottom adds master alloy layer, sponge titanium layer II is repaved afterwards above, the thickness of simple substance element layer and master alloy layer is 0.1 ~ 5 centimetre, and the thickness of sponge titanium layer II is 1 ~ 5 centimetre;
2.3 repetition above-mentioned steps 2.2 to simple substance elements, master alloy raw material are used up, and then spread aluminium shot or aluminium block layer, finally on aluminium shot or aluminium block layer, repave sponge titanium layer III, the thickness of sponge titanium layer III is 1 ~ 5 centimetre;
The material of described scull is the alloy with prepared alloy with identical component, or pure titanium scull;
(3) vacuumize after closing fire door, vacuumize and complete by one of following two kinds of modes:
3.1 suctions reach below 1Pa, and backfill argon gas or helium to 300 ~ 30000Pa carry out melting;
3.2 suctions backfill argon gas or helium after reaching below 10Pa, and then backfill argon gas or helium after being evacuated down to below 10Pa, repeatedly carry out 1 ~ 5 time to reduce the elemental gas such as oxygen, nitrogen content in stove, backfill argon gas or helium to 300 ~ 30000Pa carry out melting;
(4) melting
After melting starts, first with the power of 20 ~ 100KW, raw material is toasted 1 ~ 5 minute, then improve after there is red heat around power to raw material and be incubated 2 ~ 10 minutes, until donor center position is popular in crucible, again improve after there is drop around power to raw material and be incubated 1 ~ 10 minute, now raw material melts gradually, power is improved after raw material melts completely, melt temperature is made to reach more than alloy melting point 20 ~ 100 DEG C, and being incubated 1 ~ 20 minute, the melt of suspension realizes uniform composition under function composite by electromagnetic stirring;
(5) shaping ingot casting
Again by power raising 1% ~ 20%, improve melt overheat degree, reduce the viscosity of melt further, cool in crucible after insulation 0.5 ~ 5min or pour into ingot casting.
CN201410608728.2A 2014-11-03 2014-11-03 Smelting preparation method for titanium-aluminum intermetallic compounds Pending CN104388753A (en)

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CN106148739A (en) * 2016-06-29 2016-11-23 西安西工大超晶科技发展有限责任公司 A kind of preparation method containing niobium Ti3Al alloy cast ingot
CN107299250A (en) * 2017-05-26 2017-10-27 中国科学院金属研究所 As cast condition is tough Ti3Al intermetallic compounds and its manufacture method and application
CN107881354A (en) * 2017-12-21 2018-04-06 清远先导材料有限公司 Preparation method of nickel-platinum alloy
CN109666813A (en) * 2019-03-05 2019-04-23 西安斯塔克材料科技有限公司 A kind of preparation method of high purity titanium ambrose alloy marmem ingot casting
CN112111658A (en) * 2020-08-27 2020-12-22 宁波创润新材料有限公司 Smelting method of granular material

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CN106148739A (en) * 2016-06-29 2016-11-23 西安西工大超晶科技发展有限责任公司 A kind of preparation method containing niobium Ti3Al alloy cast ingot
CN106148739B (en) * 2016-06-29 2018-02-06 西安西工大超晶科技发展有限责任公司 A kind of preparation method of the alloy cast ingots of Ti3Al containing niobium
CN107299250A (en) * 2017-05-26 2017-10-27 中国科学院金属研究所 As cast condition is tough Ti3Al intermetallic compounds and its manufacture method and application
CN107881354A (en) * 2017-12-21 2018-04-06 清远先导材料有限公司 Preparation method of nickel-platinum alloy
CN109666813A (en) * 2019-03-05 2019-04-23 西安斯塔克材料科技有限公司 A kind of preparation method of high purity titanium ambrose alloy marmem ingot casting
CN112111658A (en) * 2020-08-27 2020-12-22 宁波创润新材料有限公司 Smelting method of granular material
CN112111658B (en) * 2020-08-27 2022-07-05 宁波创润新材料有限公司 Smelting method of granular material

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Application publication date: 20150304