CN106048356A - Multi-element Nb-Si-based super-high-temperature alloy material and preparing method thereof - Google Patents
Multi-element Nb-Si-based super-high-temperature alloy material and preparing method thereof Download PDFInfo
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Abstract
The invention discloses a multi-element Nb-Si-based super-high-temperature alloy material and a preparing method thereof to solve the technical problem that an existing Nb-Si-based super-high-temperature alloy material is poor in high-temperature oxidation resistance. According to the technical scheme, the multi-element Nb-Si-based super-high-temperature alloy material is composed of 30 at.% to 72 at.% of Nb, 10 at.% to 30 at.% of Ti, 12 at.% to 18 at.% of Si, 2 at.% to 5 at.% of Al, 2 at.% to 8 at.% of Hf, 1 at.%-10 at.% of B, 3 at.%-20 at.% of Cr, 0 at.% to 8 at.% of Zr, 0 at.%-8 at.% of Mo, 0 at.%-0.5 at.% of Ce and 0.03 at.% to 0.3 at.% of Y. The preparing method includes the step of adding Ti, Al, B, Cr, Zr and trace rare earth elements of Ce and Y into the alloy, and the high-temperature oxidization resistance of the multi-element Nb-Si-based super-high-temperature alloy material is improved.
Description
Technical field
The present invention relates to a kind of ultra high temperature alloy material, particularly to a kind of polynary Nb-Si based ultra-high temperature alloy material.Also
Relate to the preparation method of this polynary Nb-Si based ultra-high temperature alloy material.
Background technology
Nb-Si based ultra-high temperature alloy is owing to having fusing point high (more than 1700 DEG C), medium density (6.6～7.2g/cm3) and
Elevated temperature strength high and enjoy vast researcher to pay close attention to.The composition of such alloy is mainly niobio solid solution (Nb mutuallyss, tough
Property phase) and intermetallic compound ((Nb, X)5Si3、(Nb,X)3Si, or (Nb, X) Cr2Laves phase, hardening constituent, " X " represents
The atoms such as Ti, Hf, Cr and Zr of replacing Nb in lattice).Wherein, (Nb, X)5Si3Have three kinds of crystal formations, i.e. α (Nb, X)5Si3(four
Side D8lStructure), β (Nb, X)5Si3(four directions D8mStructure) and γ (Nb, X)5Si3(six side D88Structure).By above-mentioned toughness phase with strong
The in situ composites that change phase is constituted has reached preferable balance it is considered to be one has in high/low temperature mechanical property
Wish to replace the Ni based single-crystal high-temperature alloy high-temperature structural material that (1200～1400 DEG C) are applied at a higher temperature.
But, Room-Temperature Fracture Toughness and the high-temperature oxidation resistance of such alloy are poor, thus limit it in aviation, boat
The application in the field such as it and nuclear industry.Based on composition-tissue-property relationship, alloying, the microalloying including rare earth element is
Improve Nb-Si based ultra-high temperature alloy combination property (particularly permissible at the aspect such as room-temperature mechanical property and high-temperature oxidation resistance
Obtain preferably balance) effective means.Wherein, Ti, Al, Hf, B, Cr, Zr, Mo and Rare-Earth Ce, Y are several important alloys
Change element.Although the alloying research report of these elements existing, but still there are the following problems: (1) alloying research is main
Concentrate in the simple alloy system such as ternary, quaternary, and the research in multi-element alloy system is the most relatively fewer；(2) for certain
One system alloy, researcher is generally only concerned performance (mechanical property or antioxygenic property) in a certain respect, and do not rise to from
The combination property of alloy is considered every possible angle；(3) when studying the alloying action of a certain element, only choose a certain certain content and
A scope, can't this element of full appreciation on alloy structure and the impact of performance；(4) generally, researcher
Only focus on the alloying action of a certain element-specific, and the compound action between each element is mentioned less.
Document 1 " application publication number is the Chinese invention patent of CN102021458A ", " application publication number is document 2
The Chinese invention patent of CN101974712A " and document 3 " application publication number is the Chinese invention patent of CN101792879A " point
Do not disclose Nb-Ti-Si-Zn, Nb-Ti-Si-Sr and Nb-Mo-Si-B/Ge alloy system, but these systems all exist comprehensive
Can not be good, the problem that especially high-temperature oxidation resistance is poor.At present, the China about polynary Nb-Si based ultra-high temperature alloy is special
Profit is actually rare.From the combination property of alloy, i.e. Room-Temperature Fracture Toughness and ductility, elevated temperature strength, high-temperature creep resistance and
The aspects such as antioxygenic property consider, and it is very important for developing polynary Nb-Si based ultra-high temperature alloy material.
Summary of the invention
In order to overcome the deficiency of existing Nb-Si based ultra-high temperature alloy material high-temperature oxidation resistance difference, the present invention provides one
Plant polynary Nb-Si based ultra-high temperature alloy material and preparation method thereof.Described polynary Nb-Si based ultra-high temperature alloy material by 30～
The Hf of the Al of the Si of the Ti of the Nb of 72at.%, 10～30at.%, 12～18at.%, 2～5at.%, 2～8at.%, 1～
The Ce and 0.03 of the Mo of the Zr of the Cr of the B of 10at.%, 3～20at.%, 0～8at.%, 0～8at.%, 0～0.5at.%～
The Y composition of 0.3at.%.The preparation method of described polynary Nb-Si based ultra-high temperature alloy material be in alloy add Ti, Al, B,
Cr, Zr and trace rare-earth Ce, Y element, improve the high-temperature oxidation resistance of polynary Nb-Si based ultra-high temperature alloy material.
The technical solution adopted for the present invention to solve the technical problems is: a kind of polynary Nb-Si based ultra-high temperature alloy material,
Be characterized in: the Al of the Si of the Ti of Nb, 10～30at.%, 12～18at.%, 2～5at.% by 30～72at.%, 2～
The Mo of the Zr of the Cr of the B of the Hf of 8at.%, 1～10at.%, 3～20at.%, 0～8at.%, 0～8at.%, 0～
The Y of the Ce and 0.03～0.3at.% of 0.5at.% forms, and the atomic percentage conc sum of above-mentioned each element is 100%.
The preparation method of a kind of above-mentioned polynary Nb-Si based ultra-high temperature alloy material, is characterized in comprising the following steps:
The first step, choose material N b block, sponge Ti or Ti paper tinsel, Si block, Al block, Hf block, B grain, Cr block, Zr grain, Mo block,
Ce block and Y block, its purity is 99.97wt.%, removes raw material surface irregularities and oxide with standby；
Second step, weighs each former material respectively according to Nb-Ti-Si-Al-Hf-B-Cr-Zr-Mo-Ce-Y target component proportioning
Material, in terms of 200～250 grams/ingot, and puts it in vacuum non-consumable arc-melting furnace, depends on by fusing point order from low to high
Secondary stack, and B grain, Ce block and Y block Ti paper tinsel are wrapped, compacting；
Described Nb-Ti-Si-Al-Hf-B-Cr-Zr-Mo-Ce-Y target component by 30～72at.% Nb, 10～
The B of the Hf of the Al of the Si of the Ti of 30at.%, 12～18at.%, 2～5at.%, 2～8at.%, 1～10at.%, 3～
The Y group of the Ce and 0.03～0.3at.% of the Mo of the Zr of the Cr of 20at.%, 0～8at.%, 0～8at.%, 0～0.5at.%
Become, and the atomic percentage conc sum of above-mentioned each element is 100%；
3rd step, is first evacuated to 1～3 × 10-3Pa, is then filled with the argon that purity is 99.999wt.% in stove and enters
Row melting, electric current during melting controls 1000～1150A.Electromagnetic agitation power supply, electric current is opened after alloy material is completely melt
Control 10～20A, melt back 5～6 times, it is thus achieved that the uniform alloy pig of composition；
4th step, puts into superhigh temperature hypertonic solutions stove by the alloy pig prepared in the 3rd step, simultaneously at alloy pig
Around put some sponge Ti to reach the purpose of oxygen uptake；
5th step, is evacuated to 1～3 × 10-3Beginning to warm up during Pa, heating rate is about 15～17 DEG C/min.When in stove
Stop evacuation when temperature reaches 950～1050 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.
Continue heating and will heat up rate controlled at 14～16 DEG C/min, be incubated after in-furnace temperature reaches 1400～1500 DEG C 45～
55h carries out Homogenization Treatments.After insulation terminates, cool to room temperature with the furnace；
6th step, is evacuated to 1～3 × 10-3Beginning to warm up during Pa, heating rate is about 15～17 DEG C/min.When in stove
Stop evacuation when temperature reaches 950～1050 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.
Continue heating and will heat up rate controlled at 14～16 DEG C/min, be incubated after in-furnace temperature reaches 1000～1150 DEG C 45～
55h carries out Ageing Treatment.After insulation terminates, cool to room temperature with the furnace.
The invention has the beneficial effects as follows: the present invention polynary Nb-Si based ultra-high temperature alloy material by 30～72at.% Nb,
The B of the Hf of the Al of the Si of Ti, 12～18at.%, 2～5at.%, 2～8at.%, 1～10at.% of 10～30at.%, 3～
The Y group of the Ce and 0.03～0.3at.% of the Mo of the Zr of the Cr of 20at.%, 0～8at.%, 0～8at.%, 0～0.5at.%
Become.The preparation method of described polynary Nb-Si based ultra-high temperature alloy material is interpolation Ti, Hf, B and Zr element in alloy, to carry
Its Room-Temperature Fracture Toughness high.Add Hf, B, Zr and Mo element, to improve its elevated temperature strength.Add Ti, Al, B, Cr, Zr and trace
Rare-Earth Ce, Y element, to improve its high-temperature oxidation resistance, thus obtain the combination property relatively balanced.The present invention's is polynary
Nb-Si based ultra-high temperature alloy material is by toughness phase NbssWith hardening constituent (Nb, X)5Si3、(Nb,X)3Si or (Nb, X) Cr2Constitute, its
Room-Temperature Fracture Toughness KQValue is 9.2～23.8MPa m1/2, at 1250 DEG C/0.005s-1Under the conditions of compressive strength σpIt is 192.6
～520.1MPa, the unit are weightening finish after 1250 DEG C/50h aoxidizes is 18.3～156.5mg/cm2。
The present invention is described in detail below in conjunction with drawings and Examples.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) spectrum of the polynary Nb-Si based ultra-high temperature alloy that embodiment 1 prepares.
Fig. 2 be the polynary Nb-Si based ultra-high temperature alloy that embodiment 1 prepares backscattered electron (BSE) as.
Fig. 3 is that the prepared polynary Nb-Si based ultra-high temperature alloy of embodiment 1 is through 1250 DEG C/0.005s-1Stress after compression-
Strain curve.
Fig. 4 is that the prepared polynary Nb-Si based ultra-high temperature alloy of embodiment 1 is through 1250 DEG C/0.005s-1The back of the body of tissue after compression
Scattered electron (BSE) as.
Fig. 5 is that the polynary Nb-Si based ultra-high temperature alloy that embodiment 1 prepares dissipates through the back of the body of 1250 DEG C/50h oxidation rear oxidation film
Radio (BSE) as.
Detailed description of the invention
Following example are with reference to Fig. 1-5.
The present invention relates to a kind of polynary Nb-Si based ultra-high temperature alloy material can applied at a temperature of 1200 DEG C of environment above
Material, its by 30～72at.% the Al of the Si of the Ti of Nb, 10～30at.%, 12～18at.%, 2～5at.%, 2～
The Mo of the Zr of the Cr of the B of the Hf of 8at.%, 1～10at.%, 3～20at.%, 0～8at.%, 0～8at.%, 0～
The Y of the Ce and 0.03～0.3at.% of 0.5at.% forms, and the atomic percentage conc sum of above-mentioned each element is 100%.
The present invention use have the vacuum non-consumable electric arc melting technology of electromagnetic agitation function and 1450 DEG C/50h+1100 DEG C/
50h heat treatment method prepares this polynary Nb-Si based ultra-high temperature alloy material, and it includes the following step:
The first step, choose Nb block, sponge Ti or Ti paper tinsel, Si block, Al block, Hf block, B grain, Cr block, Zr grain, Mo block, Ce block and
Y block, its purity, all at more than 99.97wt.%, removes raw material surface irregularities and oxide with standby；
Second step, weighs each former material respectively according to Nb-Ti-Si-Al-Hf-B-Cr-Zr-Mo-Ce-Y target component proportioning
Material, in terms of 200～250 grams/ingot, and puts it in vacuum non-consumable arc-melting furnace, depends on by fusing point order from low to high
Secondary stack, and B grain, Ce block and Y block need to be wrapped with Ti paper tinsel, compacting；
Described Nb-Ti-Si-Al-Hf-B-Cr-Zr-Mo-Ce-Y target component by 30～72at.% Nb, 10～
The B of the Hf of the Al of the Si of the Ti of 30at.%, 12～18at.%, 2～5at.%, 2～8at.%, 1～10at.%, 3～
The Y group of the Ce and 0.03～0.3at.% of the Mo of the Zr of the Cr of 20at.%, 0～8at.%, 0～8at.%, 0～0.5at.%
Become, and the atomic percentage conc sum of above-mentioned each element is 100%；
3rd step, is first evacuated to 1 × 10-3Pa, is then filled with the argon that purity is 99.999wt.% in stove and melts
Refining, electric current during melting controls 1000～1150A.Opening electromagnetic agitation power supply after alloy material is completely melt, electric current controls
10～20A, melt back 5～6 times, to obtain the uniform alloy pig of composition；
4th step, puts into superhigh temperature hypertonic solutions stove by the alloy pig prepared in the 3rd step, simultaneously at alloy pig
Around put some sponge Ti to reach the purpose of oxygen uptake；
5th step, is evacuated to 1 × 10-3Beginning to warm up during Pa, heating rate is about 16 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 1000 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 15 DEG C/min, is incubated 50h after in-furnace temperature reaches 1450 DEG C and carries out Homogenization Treatments.After insulation terminates,
Sample cools to room temperature with the furnace；
6th step, is evacuated to 1 × 10-3Beginning to warm up during Pa, heating rate is about 16 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 1000 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 15 DEG C/min, is incubated 50h after in-furnace temperature reaches 1100 DEG C and carries out Ageing Treatment.After insulation terminates, examination
Sample cools to room temperature with the furnace.
Use X-ray diffractometer (XRD) and scanning electron microscope (SEM) respectively to polynary Nb-Si based ultra-high temperature alloy
Sample carries out crystal species analysis and microstructure observation, and alloy structure includes toughness phase NbssWith hardening constituent (Nb, X)5Si3、
(Nb,X)3Si or (Nb, X) Cr2。
Use Instron3383 type electronic universal mechanics machine that polynary Nb-Si based ultra-high temperature alloy sample is carried out room
Temperature fracture toughness test, its KQValue is 9.2～23.8MPa m1/2。
Use Gleeble 3500 type heat/power simulated experiment machine that polynary Nb-Si based ultra-high temperature alloy sample is carried out high temperature
Compression performance is tested, and test condition is 1250 DEG C/0.005s-1, its compressive strength σpIt is 192.6～520.1MPa.
Use homemade drawing by high temperature oxidation furnace that polynary Nb-Si based ultra-high temperature alloy sample is carried out high-temperature oxidation resistance
Test, test condition is 1250 DEG C/50h, and its unit are oxidation weight gain is 18.3～156.5mg/cm2。
Embodiment 1:
Use and have at vacuum non-consumable electric arc melting technology and 1450 DEG C/50h+1100 DEG C/50h heat of electromagnetic agitation function
Reason method prepares polynary Nb-Si based ultra-high temperature alloy material, and it includes the following step:
The first step, chooses Nb block, sponge Ti or Ti paper tinsel, Si block, Al block, Hf block, B grain, Cr block, Zr grain and Y block, its purity
All at more than 99.97wt.%, remove raw material surface irregularities and oxide with standby；
Second step, according to Nb-22Ti-15Si-5Cr-4Zr-3Al-3Hf-1.5B-0.06Y (at.%) composition proportion respectively
Weigh each raw material, in terms of 200 grams/ingot, and put it in vacuum non-consumable arc-melting furnace, by fusing point from low to high suitable
Sequence stacks successively, and B grain and Y block need to be wrapped with Ti paper tinsel, compacting；
3rd step, is first evacuated to 1 × 10-3Pa, is then filled with the argon that purity is 99.999wt.% in stove and melts
Refining, electric current during melting controls at 1100A.Opening electromagnetic agitation power supply after alloy material is completely melt, electric current controls at 15A,
Melt back 6 times, to obtain the uniform alloy pig of composition；
4th step, puts into superhigh temperature hypertonic solutions stove by the alloy pig prepared in the 3rd step, simultaneously at alloy pig
Around put some sponge Ti to reach the purpose of oxygen uptake；
5th step, is evacuated to 1 × 10-3Beginning to warm up during Pa, heating rate is about 16 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 1000 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 15 DEG C/min, is incubated 50h after in-furnace temperature reaches 1450 DEG C and carries out Homogenization Treatments.After insulation terminates,
Sample cools to room temperature with the furnace；
6th step, is evacuated to 1 × 10-3Beginning to warm up during Pa, heating rate is about 16 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 1000 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 15 DEG C/min, is incubated 50h after in-furnace temperature reaches 1100 DEG C and carries out Ageing Treatment.After insulation terminates, examination
Sample cools to room temperature with the furnace.
Use X-ray diffractometer (XRD) and scanning electron microscope (SEM) respectively to Nb-22Ti-15Si-5Cr-4Zr-
3Al-3Hf-1.5B-0.06Y (at.%) supertherm sample (a size of 8mm × 8mm × 8mm) carry out crystal species analysis and
Microstructure observation.Seeing figures.1.and.2, alloy structure is by toughness phase Nbss and hardening constituent γ (Nb, X)5Si3Constitute, and γ
(Nb,X)5Si3It is evenly distributed on continuous print Nbss matrix.
Use Instron3383 type electronic universal mechanics machine to Nb-22Ti-15Si-5Cr-4Zr-3Al-3Hf-
1.5B-0.06Y (at.%) supertherm sample (a size of 30mm × 5mm × 2.5mm) carries out Room-Temperature Fracture Toughness test,
Its KQValue is 14.1MPa m1/2。
Use Gleeble 3500 type heat/power simulated experiment machine to Nb-22Ti-15Si-5Cr-4Zr-3Al-3Hf-1.5B-
0.06Y (at.%) supertherm sample (a size of Φ 6mm × 9mm) carries out compressive property test, and test condition is
1250℃/0.005s-1.With reference to Fig. 3 and Fig. 4, alloy compressive strength σpFor 345.2MPa, in compression process, Nbss occurs to become continuously
Shape, γ (Nb, X)5Si3Particle surface bends, and is evenly distributed on Nbss matrix.
Use homemade drawing by high temperature oxidation furnace to Nb-22Ti-15Si-5Cr-4Zr-3Al-3Hf-1.5B-0.06Y
(at.%) supertherm sample (a size of 8mm × 8mm × 8mm) carries out high-temperature oxidation resistance test, and test condition is
1250 DEG C/50h, its unit are oxidation weight gain is 58.9mg/cm2.With reference to Fig. 5, alloy oxide film is comparatively dense, can effectively hinder
Block is to internal diffusion, thus makes it have preferable high-temperature oxidation resistance.
Embodiment 2:
Use and have at vacuum non-consumable electric arc melting technology and 1450 DEG C/50h+1100 DEG C/50h heat of electromagnetic agitation function
Reason method prepares polynary Nb-Si based ultra-high temperature alloy material, and it includes the following step:
The first step, chooses Nb block, sponge Ti or Ti paper tinsel, Si block, Al block, Hf block, B grain, Cr block and Y block, and its purity all exists
More than 99.97wt.%, removes raw material surface irregularities and oxide with standby；
Second step, weighs respectively respectively according to Nb-22Ti-16Si-8Hf-3Cr-3Al-2B-0.06Y (at.%) composition proportion
Raw material, in terms of 250 grams/ingot, and puts it in vacuum non-consumable arc-melting furnace, by fusing point order from low to high successively
Stack, and B grain and Y block need to be wrapped with Ti paper tinsel, compacting；
3rd step, is first evacuated to 2 × 10-3Pa, is then filled with the argon that purity is 99.999wt.% in stove and melts
Refining, electric current during melting controls at 1000A.Opening electromagnetic agitation power supply after alloy material is completely melt, electric current controls at 10A,
Melt back 5 times, to obtain the uniform alloy pig of composition；
4th step, puts into superhigh temperature hypertonic solutions stove by the alloy pig prepared in the 3rd step, simultaneously at alloy pig
Around put some sponge Ti to reach the purpose of oxygen uptake；
5th step, is evacuated to 2 × 10-3Beginning to warm up during Pa, heating rate is about 15 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 950 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 14 DEG C/min, is incubated 45h after in-furnace temperature reaches 1400 DEG C and carries out Homogenization Treatments.After insulation terminates,
Sample cools to room temperature with the furnace；
6th step, is evacuated to 2 × 10-3Beginning to warm up during Pa, heating rate is about 15 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 950 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 14 DEG C/min, is incubated 45h after in-furnace temperature reaches 1000 DEG C and carries out Ageing Treatment.After insulation terminates, examination
Sample cools to room temperature with the furnace.
The mode using embodiment 1 carries out crystal species analysis and microstructure observation understands, Nb-22Ti-16Si-8Hf-
The tissue of 3Cr-3Al-2B-0.06Y (at.%) supertherm sample is by toughness phase Nbss, hardening constituent γ (Nb, X)5Si3With
(Nb,X)3Si is constituted, and γ (Nb, X)5Si3(Nb, X)3Si is evenly distributed on continuous print Nbss matrix.
The mode using embodiment 1 carries out Room-Temperature Fracture Toughness test and understands, Nb-22Ti-16Si-8Hf-3Cr-3Al-
The K of 2B-0.06Y (at.%) supertherm sampleQValue is 16.3MPa m1/2。
The mode using embodiment 1 carries out compressive property test and understands, Nb-22Ti-16Si-8Hf-3Cr-3Al-
Compressive strength σ of 2B-0.06Y (at.%) supertherm samplepFor 383.7MPa, in compression process, Nbss occurs to become continuously
Shape, γ (Nb, X)5Si3(Nb, X)3Si particle surface bends, and is evenly distributed on Nbss matrix.
The mode using embodiment 1 carries out high-temperature oxidation resistance test and understands, Nb-22Ti-16Si-8Hf-3Cr-3Al-
2B-0.06Y (at.%) the unit are oxidation weight gain of supertherm sample is 96.6mg/cm2, alloy oxide film causes relatively
Close, oxygen can be stoped to internal diffusion, thus make it have preferable high-temperature oxidation resistance.
Embodiment 3:
Use and have at vacuum non-consumable electric arc melting technology and 1450 DEG C/50h+1100 DEG C/50h heat of electromagnetic agitation function
Reason method prepares polynary Nb-Si based ultra-high temperature alloy material, and it includes the following step:
The first step, chooses Nb block, sponge Ti or Ti paper tinsel, Si block, Al block, Hf block, B grain, Cr block and Y block, and its purity all exists
More than 99.97wt.%, removes raw material surface irregularities and oxide with standby；
Second step, weighs respectively respectively according to Nb-22Ti-16Si-8Hf-3Cr-3Al-2B-0.06Y (at.%) composition proportion
Raw material, in terms of 200 grams/ingot, and puts it in vacuum non-consumable arc-melting furnace, by fusing point order from low to high successively
Stack, and B grain and Y block need to be wrapped with Ti paper tinsel, compacting；
3rd step, is first evacuated to 3 × 10-3Pa, is then filled with the argon that purity is 99.999wt.% in stove and melts
Refining, electric current during melting controls at 1150A.Opening electromagnetic agitation power supply after alloy material is completely melt, electric current controls at 20A,
Melt back 5 times, to obtain the uniform alloy pig of composition；
4th step, puts into superhigh temperature hypertonic solutions stove by the alloy pig prepared in the 3rd step, simultaneously at alloy pig
Around put some sponge Ti to reach the purpose of oxygen uptake；
5th step, is evacuated to 3 × 10-3Beginning to warm up during Pa, heating rate is about 17 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 1050 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 16 DEG C/min, is incubated 55h after in-furnace temperature reaches 1400 DEG C and carries out Homogenization Treatments.After insulation terminates,
Sample cools to room temperature with the furnace；
6th step, is evacuated to 3 × 10-3Beginning to warm up during Pa, heating rate is about 17 DEG C/min.When in-furnace temperature reaches
Stop evacuation when 1050 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect.Continue heating and will rise
Temperature rate controlled, at 16 DEG C/min, is incubated 55h after in-furnace temperature reaches 1150 DEG C and carries out Ageing Treatment.After insulation terminates, examination
Sample cools to room temperature with the furnace.
Claims (2)
1. a polynary Nb-Si based ultra-high temperature alloy material, it is characterised in that: Nb, 10～the 30at.% by 30～72at.%
The B of the Hf of the Al of the Si of Ti, 12～18at.%, 2～5at.%, 2～8at.%, 1～10at.%, 3～20at.%
The Y composition of the Ce and 0.03～0.3at.% of the Mo of the Zr of Cr, 0～8at.%, 0～8at.%, 0～0.5at.%, and above-mentioned
The atomic percentage conc sum of each element is 100%.
2. the preparation method of polynary Nb-Si based ultra-high temperature alloy material described in a claim 1, it is characterised in that include following
Step:
The first step, chooses material N b block, sponge Ti or Ti paper tinsel, Si block, Al block, Hf block, B grain, Cr block, Zr grain, Mo block, Ce block
With Y block, its purity is 99.97wt.%, removes raw material surface irregularities and oxide；
Second step, weighs each raw material respectively according to Nb-Ti-Si-Al-Hf-B-Cr-Zr-Mo-Ce-Y target component proportioning, with
200～250 grams/ingot meter, and put it in vacuum non-consumable arc-melting furnace, fold successively by fusing point order from low to high
Put, and B grain, Ce block and Y block Ti paper tinsel are wrapped, compacting；
Described Nb-Ti-Si-Al-Hf-B-Cr-Zr-Mo-Ce-Y target component by 30～72at.% Nb, 10～30at.%
The Cr of the B of the Hf of the Al of the Si of Ti, 12～18at.%, 2～5at.%, 2～8at.%, 1～10at.%, 3～20at.%, 0
～the Y composition of the Ce of the Mo of the Zr of 8at.%, 0～8at.%, 0～0.5at.% and 0.03～0.3at.%, and above-mentioned each unit
The atomic percentage conc sum of element is 100%；
3rd step, is first evacuated to 1～3 × 10-3Pa, is then filled with the argon that purity is 99.999wt.% in stove and melts
Refining, electric current during melting controls 1000～1150A；Opening electromagnetic agitation power supply after alloy material is completely melt, electric current controls
10～20A, melt back 5～6 times, it is thus achieved that the uniform alloy pig of composition；
4th step, puts into superhigh temperature hypertonic solutions stove by the alloy pig prepared in the 3rd step, simultaneously around alloy pig
Put some sponge Ti to reach the purpose of oxygen uptake；
5th step, is evacuated to 1～3 × 10-3Beginning to warm up during Pa, heating rate is about 15～17 DEG C/min；Work as in-furnace temperature
Stop evacuation when reaching 950～1050 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect；Continue
Heat and will heat up rate controlled at 14～16 DEG C/min, after in-furnace temperature reaches 1400～1500 DEG C, being incubated 45～55h enter
Row Homogenization Treatments；After insulation terminates, cool to room temperature with the furnace；
6th step, is evacuated to 1～3 × 10-3Beginning to warm up during Pa, heating rate is about 15～17 DEG C/min；Work as in-furnace temperature
Stop evacuation when reaching 950～1050 DEG C, and in stove, be filled with the argon that purity is 99.999wt.% protect；Continue
Heat and will heat up rate controlled at 14～16 DEG C/min, after in-furnace temperature reaches 1000～1150 DEG C, being incubated 45～55h enter
Row Ageing Treatment；After insulation terminates, cool to room temperature with the furnace.
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| CN107326239A (en) * | 2017-09-04 | 2017-11-07 | 北京航空航天大学 | A kind of Nb Si based multicomponent alloys of rapid solidification containing Sc |
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| CN110643874A (en) * | 2019-10-22 | 2020-01-03 | 华侨大学 | Nb-Si base multi-component alloy material for improving oxidation resistance in wide temperature range |
| CN112191802A (en) * | 2020-09-23 | 2021-01-08 | 西北工业大学 | Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece |
| CN112191802B (en) * | 2020-09-23 | 2022-04-12 | 西北工业大学 | Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece |
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