CN105803283B - A kind of Nb Si Ti W Cr alloy bar materials and preparation method thereof - Google Patents
A kind of Nb Si Ti W Cr alloy bar materials and preparation method thereof Download PDFInfo
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- CN105803283B CN105803283B CN201610272566.9A CN201610272566A CN105803283B CN 105803283 B CN105803283 B CN 105803283B CN 201610272566 A CN201610272566 A CN 201610272566A CN 105803283 B CN105803283 B CN 105803283B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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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
Abstract
The invention provides a kind of Nb Si Ti W Cr alloy bar materials, it is made up of the composition of following mass percent：Si 2.4%~6.7%, Ti 5%~25%, W 5%~15%, Cr 2%~8%, surplus are Nb and inevitable impurity.Present invention also offers a kind of method for preparing the bar, comprise the following steps：First, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are well mixed using the method for wet ball grinding, mixed-powder is obtained after vacuum drying；2nd, vacuum-sintering is carried out, obtains sintered body；3rd, electronic torch melting 2~5 times, obtain ingot casting；4th, hot extrusion, semi-finished product bar stock is obtained；5th, hot extrusion, Nb Si Ti W Cr alloy bar materials are obtained.Nb Si Ti W Cr alloy bar materials of the present invention have low-density and good comprehensive mechanical property and antioxygenic property, can be used in 1400 DEG C of air ambients.
Description
Technical field
The invention belongs to alloy material preparing technical field, and in particular to a kind of Nb-Si-Ti-W-Cr alloy bar materials and its
Preparation method.
Background technology
Advanced aero engine needs a kind of new material more than the current nickel based super alloy temperature in use limit.This green wood
Material need to have the characteristics that high-melting-point, low-density, 1300~1400 DEG C of anti-oxidant and excellent elevated temperature strengths.Refractory metal has molten
The features such as point is high, elevated temperature strength is high and modulus of elasticity is big, people start to rethink refractory metal in aero-engine again
Using.In all refractory metals, niobium is most likely in aero-engine and is applied.Niobium and other intensified elements have
High solid solubility limit.Niobium has good ductility and relatively low density (8.56g/cm at room temperature3), but in single-phase situation
Under, greatly improve the limited promise that its mechanical property is applied to reach on high thrust-weight ratio engine, and the inoxidizability of niobium
Energy extreme difference, further limit its use range.But Nb5Si3Intermetallic compound has high-temperature oxidation resistance, and has
There is high elevated temperature strength.Nb-Si systems alloy by in-situ authigenic Nb5Si3Intermetallic compound phase and niobium solid solution (Nbss) phase
Compound composition, the material have high-melting-point, low-density, high intensity and preferable antioxygenic property, most possible as of future generation
The candidate material of advanced jet engine.However, a popular feature of these Nb-Si systems alloys is highly brittle at room temperature, this
It is due to be dissolved using Nb-Si systems alloy microstructure prepared by conventional method by compound between thick dendritic metal and niobium
Body (Nbss) forms.Compound phase and Nbss phases thermal coefficient of expansion and mechanical property mismatch between this dendritic metal, hold very much
Micro-crack is also easy to produce, makes Room-Temperature Fracture Toughness very low, at ambient temperature without plasticity, it is difficult to shape；Also reduce simultaneously
The Testing Tensile Strength at Elevated Temperature of alloy material, it is degrading the antioxygenic property of material.Therefore, it is necessary to pass through multicomponent alloying and work
Skill controls, and obtains with the alloy microscopic structure fine and close, uniform, particle is tiny to overcome Nb-Si systems Alloy At Room Temperature fragility etc. to lack
Point, Nb-Si systems Alloy At Room Temperature plasticity and toughness, elevated temperature strength and antioxygenic property is set to reach well balanced.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of Nb-Si-Ti-
W-Cr alloy bar materials, the density of the Nb-Si-Ti-W-Cr alloy bar materials is 6.8g/cm3~7.5g/cm3, oxygen content be 76ppm~
93ppm, room temperature tensile intensity is 573MPa~756MPa, elongation percentage is 2.1%~6.7%, and 1400 DEG C of tensile strength is
159MPa~315MPa, material loss is 0.27mg/cm after 100h is aoxidized in 1400 DEG C of air ambients2~0.12mg/cm2, should
Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can make in 1400 DEG C of air ambients
With.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of Nb-Si-Ti-W-Cr alloy bar materials,
Characterized in that, it is made up of the composition of following mass percent：Si 2.4%~6.7%, Ti 5%~25%, W 5%~
15%, Cr 2%~8%, surplus are Nb and inevitable impurity.
Above-mentioned a kind of Nb-Si-Ti-W-Cr alloy bar materials, it is characterised in that by following mass percent into packet
Into：Si 3.1%~6.1%, Ti 10%~20%, W 7%~15%, Cr 3%~7%, surplus is for Nb and inevitably
Impurity.
Above-mentioned a kind of Nb-Si-Ti-W-Cr alloy bar materials, it is characterised in that by following mass percent into packet
Into：Si 3.7%, Ti 15%, W 15%, Cr 5%, surplus are Nb and inevitable impurity.
In addition, present invention also offers a kind of method for preparing above-mentioned Nb-Si-Ti-W-Cr alloy bar materials, its feature exists
In this method comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are well mixed using the method for wet ball grinding, vacuum drying
After obtain mixed-powder；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1Pa, insulation 2h~3h is burnt under conditions of temperature is 1500 DEG C~1600 DEG C
Knot processing, sintered body is obtained after furnace cooling；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 2~5 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The electric current of the electronic torch melting
For 1A~2A, the voltage of the electronic torch melting is 60kV~80kV；
Step 4: by ingot casting described in step 3 temperature be 1200 DEG C~1400 DEG C, extrusion ratio be 5~7 under conditions of
Extruded, the processing that strips off the skin is carried out after natural cooling, obtain semi-finished product bar stock；
Step 5: by semi-finished product bar stock described in step 4 extrusion temperature be 1100 DEG C~1300 DEG C, extrusion ratio be 4~
Extruded under conditions of 6, the processing that strips off the skin is carried out after natural cooling, obtain Nb-Si-Ti-W-Cr alloy bar materials.
Above-mentioned method, it is characterised in that niobium powder described in step 1, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder
It is not less than 99%.
Above-mentioned method, it is characterised in that the particle diameter of titanium valve described in step 1 is not more than 9 μm, the particle diameter of the tungsten powder
No more than 7 μm, for the particle diameter of the silica flour and chromium powder no more than 10 μm, the particle diameter of the niobium powder is not more than 20 μm.
Above-mentioned method, it is characterised in that it is scattered to use absolute ethyl alcohol described in step 1 during wet ball grinding
Agent, the volume of the absolute ethyl alcohol are 2~3 times of niobium powder, silica flour, titanium valve, tungsten powder and chromium powder quality sum, wherein the list of volume
Position is mL, and the unit of quality is g.
Above-mentioned method, it is characterised in that the speed of wet ball grinding described in step 1 is 200rpm~300rpm, ball material
Mass ratio is (5~10): 1, Ball-milling Time is 15h~25h.
Above-mentioned method, it is characterised in that extrusion temperature described in step 4 is 1250 DEG C~1350 DEG C, and extrusion ratio is
5.5~6.5.
Above-mentioned method, it is characterised in that extrusion temperature described in step 5 is 1150 DEG C~1250 DEG C, and extrusion ratio is
4.5~5.5.
The present invention has advantages below compared with prior art：
1st, the present invention prepares Nb-Si-Ti- using multicomponent mechanical alloying+electronic torch melting+secondary extrusion technical process
W-Cr alloy bar materials, the density of prepared Nb-Si-Ti-W-Cr alloy bar materials is 6.8g/cm3~7.5g/cm3, oxygen content is
76ppm~93ppm, room temperature tensile intensity is 573MPa~756MPa, elongation percentage is 2.1%~6.7%, and 1400 DEG C of tension is strong
Spend for 159MPa~315MPa, material loss is 0.12mg/cm after 100h is aoxidized in 1400 DEG C of air ambients2~0.27mg/
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have low-density and good comprehensive mechanical property and antioxygenic property, can
Used in 1400 DEG C of air ambients..
2nd, the present invention adds Ti elements in Nb-Si systems alloy material, improves the ductility and toughness at room temperature of material, and reduce
Density；Addition W elements significantly improve Nb-Si-Ti-W-Cr alloy bar material mechanical properties；Addition Cr elements reduce material
Density and improve the antioxygenic properties of Nb-Si-Ti-W-Cr alloy bar materials.
3rd, the present invention using the technical process of electronic torch melting prepare Nb-Si-Ti-W-Cr alloy bar materials have purity it is high,
The advantages such as oxygen content is low, be advantageous to improve the ductility and toughness at room temperature of material.
4th, the present invention prepares Nb-Si-Ti-W-Cr alloy bar materials by secondary extrusion technical process, on the one hand reduces crowded
Temperature and extrusion ratio are pressed, reduces the requirement to extrusion equipment；On the other hand, crush and liked dendritic structure, and make
Tiny Nb5Si3Intermetallic compound phase is distributed in thick niobium solid solution phase, and this tissue causes Nb-Si-Ti-W-Cr to close
Golden bar has preferable plasticity at room temperature, is advantageous to shape, and add the reliability of materials'use.
The present invention is described in further detail with reference to the accompanying drawings and examples.
Brief description of the drawings
Fig. 1 is the micro-organization chart of 1Nb-Si-Ti-W-Cr alloy bar materials of the embodiment of the present invention.
Embodiment
Embodiment 1
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：Si 3.7%, Ti
15%, W 15%, Cr 5%, surplus are Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 250rpm, and ball material mass ratio is 7.5:Wet ball grinding 20h under conditions of 1, dry after ball milling, obtain under vacuum
Mixed-powder；The volume of the absolute ethyl alcohol is 2.5 times of niobium powder, silica flour, titanium valve, tungsten powder and chromium powder quality sum, wherein body
Long-pending unit is mL, and the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than
99%, the particle diameter of the silica flour and chromium powder is no more than 10 μm, and the particle diameter of the titanium valve is not more than 9 μm, the particle diameter of the tungsten powder
No more than 7 μm, the particle diameter of the niobium powder is not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1550 DEG C, soaking time 2.5h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 5 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 70kV to flow for 1.5A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1300 DEG C, extrusion ratio be 6 under conditions of extruded,
The processing that strips off the skin is carried out after natural cooling, obtains semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1200 DEG C,
Extrusion ratio is extruded under conditions of being 5, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
The microscopic structure of Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment is as shown in Figure 1.Can from Fig. 1
Go out, the microscopic structures of Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment by niobium solid solution (Nbss) mutually with it is tiny
Nb5Si3Intermetallic compound phase forms, and without visible both macro and micro crackle, dendritic structure is broken and refined completely,
The Nb of this fine uniform5Si3Intermetallic compound phase drastically increases the Testing Tensile Strength at Elevated Temperature of material.
Because Nb-Si-Ti-W-Cr alloy bar materials pass through 5 electronic torch meltings, make oxygen content and impurity content pole in material
It is low, improve the plasticity of niobium solid solution (Nbss) phase；In addition, by secondary extrusion make part niobium solid solution (Nbss) tissue along squeeze
Pressure direction is elongated to form streaky structure, and tiny Nb5Si3Intermetallic compound phase is distributed in continuous niobium solid solution
(Nbss) in phase, this continuously distributed niobium solid solution (Nbss) mutually substantially improves material with strip niobium solid solution (Nbss) tissue
The ductility and toughness at room temperature of material, make Nb-Si-Ti-W-Cr alloy bar materials that there is preferable plasticity in room temperature.Further test the present embodiment
Niobium solid solution phase (Nbss) and Nb in the Nb-Si-Ti-W-Cr alloy bar materials of preparation5Si3The chemical composition of intermetallic compound phase,
It the results are shown in Table 1.
The chemical composition of Nb-Si-Ti-W-Cr alloy bar materials prepared by the embodiment 1 of table 1
As shown in table 1, Ti elements are mainly solid-solubilized in Nb, are formed solid solution with Nb, are reduced density and the raising of material
The ductility and toughness at room temperature of Nb-Si-Ti-W-Cr alloy bar materials, and improve the antioxygenic property of material；W elements and Nb and Nb5Si3
Form the elevated temperature strength that solid solution greatly improves Nb-Si-Ti-W-Cr alloy bar materials；Cr element solid solutions are in Nb and Nb5Si3In,
One layer of fine and close oxide-film is formed in high temperature oxidative atmosphere, the intrusion of oxygen is prevented, protects the surface of material, improve
The antioxygenic property of Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 7.1g/cm3, oxygen content 76ppm, room temperature tensile intensity is 756MPa, elongation percentage is
5.9%, 1400 DEG C of tensile strength is 315MPa, and material loss is 0.12mg/ after 100h is aoxidized in 1400 DEG C of air ambients
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be in 1400 DEG C of air rings
Used in border.
Embodiment 2
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：Si 3.1%, Ti
20%, W 7%, Cr 7%, surplus are Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 200rpm, and ball material mass ratio is 5:Wet ball grinding 15h under conditions of 1, dry after ball milling, mixed under vacuum
Close powder；The volume of the absolute ethyl alcohol is niobium powder, silica flour, titanium valve, wherein 2 times of tungsten powder and chromium powder quality sum, volume
Unit is mL, and the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than 99%, institute
The particle diameter of silica flour and chromium powder is stated no more than 10 μm, the particle diameter of the titanium valve is not more than 9 μm, and the particle diameter of the tungsten powder is not more than 7 μ
M, the particle diameter of the niobium powder are not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1500 DEG C, soaking time 2h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 2 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 60kV to flow for 1A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1200 DEG C, extrusion ratio be 5 under conditions of extruded,
The processing that strips off the skin is carried out after natural cooling, obtains semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1100 DEG C,
Extrusion ratio is extruded under conditions of being 4, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 6.9g/cm3, oxygen content 93ppm, room temperature tensile intensity is 573MPa, elongation percentage is
6.7%, 1400 DEG C of tensile strength is 159MPa, and material loss is 0.27mg/ after 100h is aoxidized in 1400 DEG C of air ambients
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be in 1400 DEG C of air rings
Used in border.
Embodiment 3
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：6.1%, Ti
10%, W 13%, Cr 3%, surplus are Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 300rpm, and ball material mass ratio is 10:Wet ball grinding 25h under conditions of 1, dry after ball milling, obtain under vacuum
Mixed-powder；The volume of the absolute ethyl alcohol is 3 times of niobium powder, silica flour, titanium valve, tungsten powder and chromium powder quality sum, wherein volume
Unit be mL, the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than 99%,
The particle diameter of the silica flour and chromium powder is no more than 10 μm, and the particle diameter of the titanium valve is not more than 9 μm, and the particle diameter of the tungsten powder is not more than
7 μm, the particle diameter of the niobium powder is not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1600 DEG C, soaking time 3h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 3 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 80kV to flow for 2A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1400 DEG C, extrusion ratio be 7 under conditions of extruded,
The processing that strips off the skin is carried out after natural cooling, obtains semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1300 DEG C,
Extrusion ratio is extruded under conditions of being 6.5, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 7.2g/cm3, oxygen content 82ppm, room temperature tensile intensity is 617MPa, elongation percentage is
3.2%, 1400 DEG C of tensile strength is 187MPa, and material loss is 0.21mg/ after 100h is aoxidized in 1400 DEG C of air ambients
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be in 1400 DEG C of air rings
Used in border.
Embodiment 4
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：Si 6.7%, Ti
25%, W 5%, Cr 8%, surplus are Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 260rpm, and ball material mass ratio is 8:Wet ball grinding 25h under conditions of 1, dry after ball milling, mixed under vacuum
Close powder；The volume of the absolute ethyl alcohol is niobium powder, silica flour, titanium valve, wherein 3 times of tungsten powder and chromium powder quality sum, volume
Unit is mL, and the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than 99%, institute
The particle diameter of silica flour and chromium powder is stated no more than 10 μm, the particle diameter of the titanium valve is not more than 9 μm, and the particle diameter of the tungsten powder is not more than 7 μ
M, the particle diameter of the niobium powder are not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1600 DEG C, soaking time 3h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 4 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 75kV to flow for 2A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1400 DEG C, extrusion ratio be 5.5 under conditions of squeezed
Press, carry out the processing that strips off the skin after natural cooling, obtain semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1300 DEG C,
Extrusion ratio is extruded under conditions of being 5.5, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 6.8g/cm3, oxygen content 79ppm, room temperature tensile intensity is 612MPa, elongation percentage is
2.1%, 1400 DEG C of tensile strength is 295MPa, and material loss is 0.12mg/ after 100h is aoxidized in 1400 DEG C of air ambients
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be in 1400 DEG C of air rings
Used in border.
Embodiment 5
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：Si 2.4%, Ti
5%, W 15%, Cr 2%, surplus are Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 300rpm, and ball material mass ratio is 10:Wet ball grinding 15h under conditions of 1, dry after ball milling, obtain under vacuum
Mixed-powder；The volume of the absolute ethyl alcohol is 2 times of niobium powder, silica flour, titanium valve, tungsten powder and chromium powder quality sum, wherein volume
Unit be mL, the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than 99%,
The particle diameter of the silica flour and chromium powder is no more than 10 μm, and the particle diameter of the titanium valve is not more than 9 μm, and the particle diameter of the tungsten powder is not more than
7 μm, the particle diameter of the niobium powder is not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1500 DEG C, soaking time 2h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 3 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 80kV to flow for 1A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1400 DEG C, extrusion ratio be 5 under conditions of extruded,
The processing that strips off the skin is carried out after natural cooling, obtains semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1300 DEG C,
Extrusion ratio is extruded under conditions of being 4, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 6.8g/cm3, oxygen content 79ppm, room temperature tensile intensity is 612MPa, elongation percentage is
2.1%, 1400 DEG C of tensile strength is 159MPa~315MPa, and material loss is after oxidation 100h in 1400 DEG C of air ambients
0.27mg/cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be 1400
Used in DEG C air ambient.
Embodiment 6
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：Si 2.4%, Ti
5%, W 5%, Cr 2%, surplus are Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 300rpm, and ball material mass ratio is 5:Wet ball grinding 20h under conditions of 1, dry after ball milling, mixed under vacuum
Close powder；The volume of the absolute ethyl alcohol is niobium powder, silica flour, titanium valve, wherein 3 times of tungsten powder and chromium powder quality sum, volume
Unit is mL, and the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than 99%, institute
The particle diameter of silica flour and chromium powder is stated no more than 10 μm, the particle diameter of the titanium valve is not more than 9 μm, and the particle diameter of the tungsten powder is not more than 7 μ
M, the particle diameter of the niobium powder are not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1550 DEG C, soaking time 2h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 5 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 60kV to flow for 2A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1200 DEG C, extrusion ratio be 5.5 under conditions of squeezed
Press, carry out the processing that strips off the skin after natural cooling, obtain semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1100 DEG C,
Extrusion ratio is extruded under conditions of being 5.5, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 6.8g/cm3, oxygen content 76ppm, room temperature tensile intensity is 573MPa, elongation percentage is
6.7%, 1400 DEG C of tensile strength is 159MPa, and material loss is 0.27mg/ after 100h is aoxidized in 1400 DEG C of air ambients
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be in 1400 DEG C of air rings
Used in border.
Embodiment 7
The present embodiment Nb-Si-Ti-W-Cr alloy bar materials are made up of the composition of following mass percent：Si 2.4%, Ti
5%, W 5%, Cr 2%, surplus are Nb and inevitable impurity.Si 6.7%, Ti 25%, W 15%, Cr 8%, surplus
For Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, using absolute ethyl alcohol as dispersant,
Rotating speed is 200rpm, and ball material mass ratio is 10:Wet ball grinding 25h under conditions of 1, dry after ball milling, obtain under vacuum
Mixed-powder；The volume of the absolute ethyl alcohol is 3 times of niobium powder, silica flour, titanium valve, tungsten powder and chromium powder quality sum, wherein volume
Unit be mL, the unit of quality is g, and the niobium powder, silica flour, titanium valve, the quality purity of tungsten powder and chromium powder are not less than 99%,
The particle diameter of the silica flour and chromium powder is no more than 10 μm, and the particle diameter of the titanium valve is not more than 9 μm, and the particle diameter of the tungsten powder is not more than
7 μm, the particle diameter of the niobium powder is not more than 20 μm；
Step 2: a kind of mixed-powder of step is compressing, blank is obtained, the blank is then placed in vacuum
In sintering furnace, it is not more than 5 × 10 in vacuum-1It is sintered under conditions of Pa, sintered body is obtained after furnace cooling；It is described
The temperature of sintering processes is 1600 DEG C, soaking time 3h；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa
Under conditions of electronic torch melting 2 times, the processing that strips off the skin is carried out after natural cooling, obtains ingot casting；The melting electricity of the electronic torch melting
It is 60kV to flow for 2A, melting voltage；
Step 4: by institute's ingot casting in step 3 extrusion temperature be 1250 DEG C, extrusion ratio be 6.5 under conditions of squeezed
Press, carry out the processing that strips off the skin after natural cooling, obtain semi-finished product bar stock；
Step 5: by the Nb-Si-Ti-W-Cr alloy semi-finished product bar stocks described in step 4 extrusion temperature be 1150 DEG C,
Extrusion ratio is extruded under conditions of being 4.5, and the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
Nb-Si-Ti-W-Cr alloy bar materials manufactured in the present embodiment have quality purity height, oxygen content low and microstructure
The characteristics of fine uniform, density 7.5g/cm3, oxygen content 93ppm, room temperature tensile intensity is 657MPa, elongation percentage is
2.1%, 1400 DEG C of tensile strength is 273MPa, and material loss is 0.27mg/ after 100h is aoxidized in 1400 DEG C of air ambients
cm2, the Nb-Si-Ti-W-Cr alloy bar materials have the characteristics that density is low, intensity is high and anti-oxidant, can be in 1400 DEG C of air rings
Used in border.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention
Protection domain in.
Claims (10)
1. a kind of Nb-Si-Ti-W-Cr alloy bar materials, it is characterised in that be made up of the composition of following mass percent：Si
2.4%~6.7%, Ti 5%~25%, W 5%~15%, Cr 2%~8%, surplus are Nb and inevitable impurity；
The method for preparing the Nb-Si-Ti-W-Cr alloy bar materials comprises the following steps：
Step 1: be well mixed niobium powder, silica flour, titanium valve, tungsten powder and chromium powder using the method for wet ball grinding, after vacuum drying
To mixed-powder；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in vacuum-sintering
In stove, it is not more than 5 × 10 in vacuum-1Pa, insulation 2h~3h is sintered place under conditions of temperature is 1500 DEG C~1600 DEG C
Reason, sintered body is obtained after furnace cooling；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa bar
Electronic torch melting 2~5 times under part, carry out the processing that strips off the skin, obtain ingot casting after natural cooling；The electric current of the electronic torch melting is 1A
~3A, the voltage of the electronic torch melting is 60kV~80kV；
Step 4: by ingot casting described in step 3 temperature be 1200 DEG C~1400 DEG C, extrusion ratio be 5~7 under conditions of carry out
Extrude, carry out the processing that strips off the skin after natural cooling, obtain semi-finished product bar stock；
Step 5: in extrusion temperature it is 1100 DEG C~1300 DEG C by semi-finished product bar stock described in step 4, extrusion ratio is 4~6
Under the conditions of extruded, the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
2. a kind of Nb-Si-Ti-W-Cr alloy bar materials according to claim 1, it is characterised in that by following quality percentage
The composition composition of ratio：Si 3.1%~6.1%, Ti 10%~20%, W 7%~15%, Cr 3%~7%, surplus be Nb and
Inevitable impurity.
3. a kind of Nb-Si-Ti-W-Cr alloy bar materials according to claim 2, it is characterised in that by following quality percentage
The composition composition of ratio：Si 3.7%, Ti 15%, W 15%, Cr 5%, surplus are Nb and inevitable impurity.
A kind of 4. method for preparing the Nb-Si-Ti-W-Cr alloy bar materials as described in claim 1,2 or 3, it is characterised in that the party
Method comprises the following steps：
Step 1: be well mixed niobium powder, silica flour, titanium valve, tungsten powder and chromium powder using the method for wet ball grinding, after vacuum drying
To mixed-powder；
Step 2: mixed-powder described in step 1 is compressing, blank is obtained, the blank is then placed in vacuum-sintering
In stove, it is not more than 5 × 10 in vacuum-1Pa, insulation 2h~3h is sintered place under conditions of temperature is 1500 DEG C~1600 DEG C
Reason, sintered body is obtained after furnace cooling；
Step 3: sintered body described in step 2 is placed in electron beam furnace, it is not more than 1 × 10 in vacuum-2Pa bar
Electronic torch melting 2~5 times under part, carry out the processing that strips off the skin, obtain ingot casting after natural cooling；The electric current of the electronic torch melting is 1A
~3A, the voltage of the electronic torch melting is 60kV~80kV；
Step 4: by ingot casting described in step 3 temperature be 1200 DEG C~1400 DEG C, extrusion ratio be 5~7 under conditions of carry out
Extrude, carry out the processing that strips off the skin after natural cooling, obtain semi-finished product bar stock；
Step 5: in extrusion temperature it is 1100 DEG C~1300 DEG C by semi-finished product bar stock described in step 4, extrusion ratio is 4~6
Under the conditions of extruded, the processing that strips off the skin is carried out after natural cooling, obtains Nb-Si-Ti-W-Cr alloy bar materials.
5. according to the method for claim 4, it is characterised in that niobium powder described in step 1, silica flour, titanium valve, tungsten powder and chromium
The quality purity of powder is not less than 99%.
6. according to the method for claim 4, it is characterised in that the particle diameter of titanium valve described in step 1 is described no more than 9 μm
The particle diameter of tungsten powder is not more than 7 μm, and for the particle diameter of the silica flour and chromium powder no more than 10 μm, the particle diameter of the niobium powder is not more than 20 μ
m。
7. according to the method for claim 4, it is characterised in that using anhydrous during wet ball grinding described in step 1
Ethanol is dispersant, and the volume of the absolute ethyl alcohol is 2~3 times of niobium powder, silica flour, titanium valve, tungsten powder and chromium powder quality sum, its
The unit of middle volume is mL, and the unit of quality is g.
8. according to the method for claim 4, it is characterised in that the speed of wet ball grinding described in step 1 be 200rpm~
300rpm, ball material mass ratio are (5~10): 1, Ball-milling Time is 15h~25h.
9. according to the method for claim 4, it is characterised in that extrusion temperature described in step 4 is 1250 DEG C~1350
DEG C, extrusion ratio is 5.5~6.5.
10. according to the method for claim 4, it is characterised in that extrusion temperature described in step 5 is 1150 DEG C~1250
DEG C, extrusion ratio is 4.5~5.5.
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| CN110565169B (en) * | 2019-10-28 | 2021-01-26 | 西北有色金属研究院 | Method for cultivating Mo-Nb-W-Zr alloy single crystal seed crystal |
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| GB889099A (en) * | 1959-06-11 | 1962-02-07 | Gen Electric | Improvements in columbium-tungsten-titanium alloys |
| GB970362A (en) * | 1959-10-17 | 1964-09-23 | Birmingham Small Arms Co Ltd | Improvements in or relating to niobium-base alloys |
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| CN101235460A (en) * | 2008-03-10 | 2008-08-06 | 北京航空航天大学 | Niobium-silicon-hafnium-titanium-aluminum-chromium ultra-high temperature alloy and preparation method thereof |
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| GB970362A (en) * | 1959-10-17 | 1964-09-23 | Birmingham Small Arms Co Ltd | Improvements in or relating to niobium-base alloys |
| CN101235455A (en) * | 2008-03-10 | 2008-08-06 | 北京航空航天大学 | Niobium-titanium-silicon-zirconium-hafnium-boron alloy and preparation method thereof |
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