CN105803283A - Nb-Si-Ti-W-Cr alloy bar and production method thereof - Google Patents
Nb-Si-Ti-W-Cr alloy bar and production method thereof Download PDFInfo
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- CN105803283A CN105803283A CN201610272566.9A CN201610272566A CN105803283A CN 105803283 A CN105803283 A CN 105803283A CN 201610272566 A CN201610272566 A CN 201610272566A CN 105803283 A CN105803283 A CN 105803283A
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- 229910000599 Cr alloy Inorganic materials 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 62
- 239000010936 titanium Substances 0.000 claims abstract description 53
- 239000011812 mixed powder Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 238000010894 electron beam technology Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 101
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 72
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 50
- 229910052719 titanium Inorganic materials 0.000 claims description 50
- 239000010955 niobium Substances 0.000 claims description 41
- 238000001125 extrusion Methods 0.000 claims description 40
- 238000002844 melting Methods 0.000 claims description 37
- 230000008018 melting Effects 0.000 claims description 37
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 36
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 36
- 238000001816 cooling Methods 0.000 claims description 36
- 235000013312 flour Nutrition 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 36
- 239000000377 silicon dioxide Substances 0.000 claims description 36
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000011265 semifinished product Substances 0.000 claims description 18
- 239000011651 chromium Substances 0.000 claims description 17
- 229910052804 chromium Inorganic materials 0.000 claims description 14
- 238000005266 casting Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 abstract description 15
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 239000000843 powder Substances 0.000 abstract 4
- 238000001192 hot extrusion Methods 0.000 abstract 2
- 238000003723 Smelting Methods 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 19
- 229910052760 oxygen Inorganic materials 0.000 description 19
- 239000001301 oxygen Substances 0.000 description 19
- 239000006104 solid solution Substances 0.000 description 13
- 239000000956 alloy Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 230000003064 anti-oxidating effect Effects 0.000 description 9
- 230000003026 anti-oxygenic effect Effects 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 7
- 229910020010 Nb—Si Inorganic materials 0.000 description 6
- 229910000765 intermetallic Inorganic materials 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000003870 refractory metal Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides an Nb-Si-Ti-W-Cr alloy bar. The Nb-Si-Ti-W-Cr alloy bar is produced from components in percentage by mass as follows: 2.4%-6.7% of Si, 5%-25% of Ti, 5%-15% of W, 2%-8% of Cr and the balance Nb and inevitable impurities. The invention further provides a method for producing the bar. The method comprises steps as follows: I, Nb powder, Si powder, Ti powder, W powder and Cr powder are evenly mixed through a wet ball-milling method, and mixed powder is obtained after vacuum drying; II, vacuum sintering is performed, and a sintered body is obtained; III, smelting is performed for 2-5 times by the aid of an electron beam, and a cast ingot is obtained; IV, hot extrusion is performed, and a semi-finished bar blank is obtained; V, hot extrusion is performed, and the Nb-Si-Ti-W-Cr alloy bar is obtained. The Nb-Si-Ti-W-Cr alloy bar has the low density as well as good comprehensive mechanical properties and oxidation resistance and can be used in an air environment at 1,400 DEG C.
Description
Technical field
The invention belongs to alloy material preparing technical field, be specifically related to a kind of Nb-Si-Ti-W-Cr and close
Gold bar and preparation method thereof.
Background technology
Advanced aero engine needs a kind of green wood exceeding current nickel based super alloy use temperature extremes
Material.This new material need to have high-melting-point, low-density, 1300～1400 DEG C of antioxidation and the height of excellence
The features such as temperature intensity.Refractory metal has the features such as fusing point height, elevated temperature strength height and elastic modelling quantity are big,
People start again the application rethinking refractory metal in aero-engine.At all of refractory metal
In, niobium is most likely in aero-engine and is applied.Niobium and other intensified element have high consolidating
The molten limit.Niobium at room temperature has good ductility and relatively low density (8.56g/cm3), but
In the case of single-phase, its mechanical property is greatly improved to reach the prospect of application on high thrust-weight ratio engine
Limited, and the antioxygenic property extreme difference of niobium, further limit its range.But Nb5Si3
Intermetallic compound has high-temperature oxidation resistance, and has high elevated temperature strength.Nb-Si system
Alloy is by the Nb of in-situ authigenic5Si3Intermetallic compound phase is compound mutually with niobium solid solution (Nbss) to be constituted,
This material has high-melting-point, low-density, high intensity and preferably antioxygenic property, most possible conduct
The candidate material of advanced jet engine of future generation.But, of these Nb-Si system alloys is universal
Feature is to be highly brittle under room temperature, and this is the Nb-Si system alloy microcosmic group owing to using traditional method to prepare
Knit and be made up of compound between thick dendritic metal and niobium solid solution (Nbss).This dendritic metal
Between compound phase and Nbss phase thermal coefficient of expansion and mechanical property do not mate, it is easy to produce micro-crack,
Make Room-Temperature Fracture Toughness the lowest, there is no plasticity at ambient temperature, it is difficult to shape；Also drop simultaneously
The low Testing Tensile Strength at Elevated Temperature of alloy material, is degrading the antioxygenic property of material.Therefore, it is necessary to it is logical
Too much composition alloy and technology controlling and process, it is thus achieved that have densification, uniformly, alloy that granule is tiny micro-
Tissue overcome the shortcomings such as Nb-Si system Alloy At Room Temperature fragility, make Nb-Si system Alloy At Room Temperature plasticity and toughness,
Elevated temperature strength and antioxygenic property reach well balanced.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that a kind of
Nb-Si-Ti-W-Cr alloy bar material, the density of this Nb-Si-Ti-W-Cr alloy bar material is
6.8g/cm3～7.5g/cm3, oxygen content is 76ppm～93ppm, and room temperature tensile intensity is
573MPa～756MPa, elongation percentage are 2.1%～6.7%, and the tensile strength of 1400 DEG C is
159MPa～315MPa, after aoxidizing 100h in 1400 DEG C of air ambients, material unaccounted-for (MUF) is
0.27mg/cm2～0.12mg/cm2, this Nb-Si-Ti-W-Cr alloy bar material has that density is low, intensity is high
With the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of Nb-Si-Ti-W-Cr
Alloy bar material, it is characterised in that be grouped into by the one-tenth of following mass percent: Si 2.4%～6.7%,
Ti 5%～25%, W 5%～15%, Cr 2%～8%, surplus is Nb and inevitable impurity.
Above-mentioned a kind of Nb-Si-Ti-W-Cr alloy bar material, it is characterised in that by following percent mass
The one-tenth of ratio is grouped into: Si 3.1%～6.1%, Ti 10%～20%, W 7%～15%, Cr 3%～7%,
Surplus is Nb and inevitable impurity.
Above-mentioned a kind of Nb-Si-Ti-W-Cr alloy bar material, it is characterised in that by following percent mass
The one-tenth of ratio is grouped into: Si 3.7%, Ti 15%, W 15%, Cr 5%, and surplus is Nb and can not keep away
The impurity exempted from.
It addition, present invention also offers a kind of method preparing above-mentioned Nb-Si-Ti-W-Cr alloy bar material,
It is characterized in that, the method comprises the following steps:
Niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are mixed by step one, the method for employing wet ball grinding
Uniformly, mixed-powder is obtained after vacuum drying；
Step 2, by compressing for mixed-powder described in step one, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Pa, temperature is 1500 DEG C～1600
It is incubated 2h～3h under conditions of DEG C to be sintered, after furnace cooling, obtains sintered body；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 2～5 times under conditions of Pa, carry out the process that strips off the skin after natural cooling,
To ingot casting；The electric current of described electronic torch melting is 1A～2A, and the voltage of described electronic torch melting is 60kV
～80kV；
Step 4, being 1200 DEG C～1400 DEG C by ingot casting described in step 3 in temperature, extrusion ratio is 5～7
Under conditions of extrude, carry out the process that strips off the skin after natural cooling, obtain semi-finished product rod base；
Step 5, it is 1100 DEG C～1300 DEG C by the base of semi-finished product rod described in step 4 at extrusion temperature,
Extrusion ratio is to extrude under conditions of 4～6, carries out the process that strips off the skin, obtain after natural cooling
Nb-Si-Ti-W-Cr alloy bar material.
Above-mentioned method, it is characterised in that niobium powder described in step one, silica flour, titanium valve, tungsten powder and
The quality purity of chromium powder is all not less than 99%.
Above-mentioned method, it is characterised in that the particle diameter of titanium valve described in step one is not more than 9 μm,
The particle diameter of described tungsten powder is not more than 7 μm, and the particle diameter of described silica flour and chromium powder is no more than 10 μm, institute
The particle diameter stating niobium powder is not more than 20 μm.
Above-mentioned method, it is characterised in that use anhydrous described in step one during wet ball grinding
Ethanol is dispersant, and the volume of described dehydrated alcohol is niobium powder, silica flour, titanium valve, tungsten powder and chromium powder matter
2～3 times of amount sum, wherein the unit of volume 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 one is
200rpm～300rpm, ball material mass ratio is (5～10): 1, and 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,
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,
Extrusion ratio is 4.5～5.5.
The present invention compared with prior art has the advantage that
1, the present invention uses multicomponent mechanical alloying+electronic torch melting+secondary extrusion technical process system
Standby Nb-Si-Ti-W-Cr alloy bar material, the density of prepared Nb-Si-Ti-W-Cr alloy bar material is
6.8g/cm3～7.5g/cm3, oxygen content is 76ppm～93ppm, and room temperature tensile intensity is
573MPa～756MPa, elongation percentage are 2.1%～6.7%, and the tensile strength of 1400 DEG C is
159MPa～315MPa, after aoxidizing 100h in 1400 DEG C of air ambients, material unaccounted-for (MUF) is
0.12mg/cm2～0.27mg/cm2, this Nb-Si-Ti-W-Cr alloy bar material has low-density and good
Comprehensive mechanical property and antioxygenic property, it is possible in 1400 DEG C of air ambients use..
2, the present invention adds Ti element in Nb-Si system alloy material, and the room temperature that improve material is moulded
Toughness, and reduce density；Add W element and significantly improve Nb-Si-Ti-W-Cr alloy bar material
Mechanical property；Add Cr element reduce the density of material and improve Nb-Si-Ti-W-Cr alloy bar
The antioxygenic property of material.
3, the present invention uses the technical process of electronic torch melting to prepare Nb-Si-Ti-W-Cr alloy bar material tool
There are the advantages such as purity is high, oxygen content is low, are conducive to improving the ductility and toughness at room temperature of material.
4, the present invention prepares Nb-Si-Ti-W-Cr alloy bar material, a side by secondary extrusion technical process
Face decreases extrusion temperature and extrusion ratio, reduces the requirement to extrusion equipment；On the other hand, broken
With liked dendritic structure, and make tiny Nb5Si3Intermetallic compound is distributed in thick mutually
In niobium solid solution phase, this tissue makes Nb-Si-Ti-W-Cr alloy bar material at room temperature have preferably
Plasticity, be conducive to shaping, and add the reliability of materials'use.
With embodiment, the present invention is described in further detail below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the micro-organization chart of embodiment of the present invention 1Nb-Si-Ti-W-Cr alloy bar material.
Detailed description of the invention
Embodiment 1
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent: Si
3.7%, Ti 15%, W 15%, Cr 5%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 250rpm at rotating speed, and ball material mass ratio is wet ball grinding under conditions of 7.5:1
20h, dries after ball milling under vacuum, obtains mixed-powder；The volume of described dehydrated alcohol is
Niobium powder, silica flour, titanium valve, tungsten powder and 2.5 times of chromium powder quality sum, wherein the unit of volume is mL,
The unit of quality is g, and the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder is the least
In 99%, the particle diameter of described silica flour and chromium powder is not more than no more than 10 μm, the particle diameter of described titanium valve
9 μm, the particle diameter of described tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1550 DEG C, and temperature retention time is
2.5h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 5 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 1.5A, and melting voltage is 70kV；
Step 4, being 1300 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the condition of 6
Under extrude, carry out the process that strips off the skin after natural cooling, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1200 DEG C, and extrusion ratio is to extrude under conditions of 5, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
The microscopic structure of Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment is as shown in Figure 1.From
It can be seen that the microscopic structure of Nb-Si-Ti-W-Cr alloy bar material prepared of the present embodiment is by niobium in Fig. 1
Solid solution (Nbss) phase and tiny Nb5Si3Intermetallic compound phase composition, do not have visible macroscopic view and
Microfissure, dendritic structure is broken completely and refines, the Nb of this fine uniform5Si3Between metal
Compound drastically increases the Testing Tensile Strength at Elevated Temperature of material mutually.
Owing to Nb-Si-Ti-W-Cr alloy bar material is through 5 electronic torch meltings, make oxygen content in material
Extremely low with impurity content, improve the plasticity of niobium solid solution (Nbss) phase；It addition, pass through secondary extrusion
Part niobium solid solution (Nbss) tissue is made to be elongated formation streaky structure along the direction of extrusion, and tiny
Nb5Si3Intermetallic compound be distributed in mutually continuous print niobium solid solution (Nbss) mutually in, this continuous distribution
Niobium solid solution (Nbss) mutually substantially improve the room temperature of material mould with strip niobium solid solution (Nbss) tissue
Toughness, makes Nb-Si-Ti-W-Cr alloy bar material have preferable plasticity in room temperature.Test this further
Niobium solid solution phase (Nbss) and Nb in Nb-Si-Ti-W-Cr alloy bar material prepared by embodiment5Si3Metal
Between the chemical composition of compound phase, the results are shown in Table 1.
The chemical composition of the Nb-Si-Ti-W-Cr alloy bar material of table 1 embodiment 1 preparation
As shown in table 1, Ti element is mainly solid-solubilized in Nb, forms solid solution with Nb, reduces
The density of material and the ductility and toughness at room temperature that improve Nb-Si-Ti-W-Cr alloy bar material, and improve material
The antioxygenic property of material；W element and Nb and Nb5Si3Formation solid solution greatly improves
The elevated temperature strength of Nb-Si-Ti-W-Cr alloy bar material；Cr element solid solution is at Nb and Nb5Si3In,
High temperature oxidative atmosphere is formed one layer of fine and close oxide-film, stops the intrusion of oxygen, protect material
Surface, improves the antioxygenic property of Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 7.1g/cm3, oxygen content is 76ppm, and room temperature resists
Tensile strength is 756MPa, elongation percentage is 5.9%, and the tensile strength of 1400 DEG C is 315MPa, at 1400 DEG C
In air ambient, after oxidation 100h, material unaccounted-for (MUF) is 0.12mg/cm2, this Nb-Si-Ti-W-Cr alloy bar
Material has that density is low, intensity is high and the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
Embodiment 2
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent: Si
3.1%, Ti 20%, W 7%, Cr 7%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 200rpm at rotating speed, and ball material mass ratio is wet ball grinding 15h under conditions of 5:1,
Dry under vacuum after ball milling, obtain mixed-powder；The volume of described dehydrated alcohol be niobium powder,
Silica flour, titanium valve, tungsten powder and 2 times of chromium powder quality sum, wherein the unit of volume is mL, quality
Unit be g, the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder all not less than 99%,
The particle diameter of described silica flour and chromium powder is no more than 10 μm, and the particle diameter of described titanium valve is not more than 9 μm, institute
The particle diameter stating tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1500 DEG C, and temperature retention time is
2h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 2 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 1A, and melting voltage is 60kV；
Step 4, being 1200 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the condition of 5
Under extrude, carry out the process that strips off the skin after natural cooling, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1100 DEG C, and extrusion ratio is to extrude under conditions of 4, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 6.9g/cm3, oxygen content is 93ppm, and room temperature resists
Tensile strength is 573MPa, elongation percentage is 6.7%, and the tensile strength of 1400 DEG C is 159MPa, at 1400 DEG C
In air ambient, after oxidation 100h, material unaccounted-for (MUF) is 0.27mg/cm2, this Nb-Si-Ti-W-Cr alloy bar
Material has that density is low, intensity is high and the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
Embodiment 3
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent:
6.1%, Ti 10%, W 13%, Cr 3%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 300rpm at rotating speed, and ball material mass ratio is wet ball grinding 25h under conditions of 10:1,
Dry under vacuum after ball milling, obtain mixed-powder；The volume of described dehydrated alcohol be niobium powder,
Silica flour, titanium valve, tungsten powder and 3 times of chromium powder quality sum, wherein the unit of volume is mL, quality
Unit be g, the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder all not less than 99%,
The particle diameter of described silica flour and chromium powder is no more than 10 μm, and the particle diameter of described titanium valve is not more than 9 μm, institute
The particle diameter stating tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1600 DEG C, and temperature retention time is
3h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 3 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 2A, and melting voltage is 80kV；
Step 4, being 1400 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the condition of 7
Under extrude, carry out the process that strips off the skin after natural cooling, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1300 DEG C, and extrusion ratio is to extrude under conditions of 6.5, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 7.2g/cm3, oxygen content is 82ppm, and room temperature resists
Tensile strength is 617MPa, elongation percentage is 3.2%, and the tensile strength of 1400 DEG C is 187MPa, at 1400 DEG C
In air ambient, after oxidation 100h, material unaccounted-for (MUF) is 0.21mg/cm2, this Nb-Si-Ti-W-Cr alloy bar
Material has that density is low, intensity is high and the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
Embodiment 4
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent: Si
6.7%, Ti 25%, W 5%, Cr 8%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 260rpm at rotating speed, and ball material mass ratio is wet ball grinding 25h under conditions of 8:1,
Dry under vacuum after ball milling, obtain mixed-powder；The volume of described dehydrated alcohol be niobium powder,
Silica flour, titanium valve, tungsten powder and 3 times of chromium powder quality sum, wherein the unit of volume is mL, quality
Unit be g, the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder all not less than 99%,
The particle diameter of described silica flour and chromium powder is no more than 10 μm, and the particle diameter of described titanium valve is not more than 9 μm, institute
The particle diameter stating tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1600 DEG C, and temperature retention time is
3h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 4 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 2A, and melting voltage is 75kV；
Step 4, being 1400 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the bar of 5.5
Extrude under part, after natural cooling, carry out the process that strips off the skin, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1300 DEG C, and extrusion ratio is to extrude under conditions of 5.5, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 6.8g/cm3, oxygen content is 79ppm, and room temperature resists
Tensile strength is 612MPa, elongation percentage is 2.1%, and the tensile strength of 1400 DEG C is 295MPa, at 1400 DEG C
In air ambient, after oxidation 100h, material unaccounted-for (MUF) is 0.12mg/cm2, this Nb-Si-Ti-W-Cr alloy bar
Material has that density is low, intensity is high and the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
Embodiment 5
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent: Si
2.4%, Ti 5%, W 15%, Cr 2%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 300rpm at rotating speed, and ball material mass ratio is wet ball grinding 15h under conditions of 10:1,
Dry under vacuum after ball milling, obtain mixed-powder；The volume of described dehydrated alcohol be niobium powder,
Silica flour, titanium valve, tungsten powder and 2 times of chromium powder quality sum, wherein the unit of volume is mL, quality
Unit be g, the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder all not less than 99%,
The particle diameter of described silica flour and chromium powder is no more than 10 μm, and the particle diameter of described titanium valve is not more than 9 μm, institute
The particle diameter stating tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1500 DEG C, and temperature retention time is
2h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 3 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 1A, and melting voltage is 80kV；
Step 4, being 1400 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the condition of 5
Under extrude, carry out the process that strips off the skin after natural cooling, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1300 DEG C, and extrusion ratio is to extrude under conditions of 4, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 6.8g/cm3, oxygen content is 79ppm, and room temperature resists
Tensile strength is 612MPa, elongation percentage is 2.1%, and the tensile strength of 1400 DEG C is 159MPa～315MPa,
In 1400 DEG C of air ambients, after oxidation 100h, material unaccounted-for (MUF) is 0.27mg/cm2, should
Nb-Si-Ti-W-Cr alloy bar material has that density is low, intensity is high and the feature such as antioxidation, it is possible to
1400 DEG C of air ambients use.
Embodiment 6
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent: Si
2.4%, Ti 5%, W 5%, Cr 2%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 300rpm at rotating speed, and ball material mass ratio is wet ball grinding 20h under conditions of 5:1,
Dry under vacuum after ball milling, obtain mixed-powder；The volume of described dehydrated alcohol be niobium powder,
Silica flour, titanium valve, tungsten powder and 3 times of chromium powder quality sum, wherein the unit of volume is mL, quality
Unit be g, the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder all not less than 99%,
The particle diameter of described silica flour and chromium powder is no more than 10 μm, and the particle diameter of described titanium valve is not more than 9 μm, institute
The particle diameter stating tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1550 DEG C, and temperature retention time is
2h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 5 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 2A, and melting voltage is 60kV；
Step 4, being 1200 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the bar of 5.5
Extrude under part, after natural cooling, carry out the process that strips off the skin, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1100 DEG C, and extrusion ratio is to extrude under conditions of 5.5, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 6.8g/cm3, oxygen content is 76ppm, and room temperature resists
Tensile strength is 573MPa, elongation percentage is 6.7%, and the tensile strength of 1400 DEG C is 159MPa, at 1400 DEG C
In air ambient, after oxidation 100h, material unaccounted-for (MUF) is 0.27mg/cm2, this Nb-Si-Ti-W-Cr alloy bar
Material has that density is low, intensity is high and the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
Embodiment 7
The present embodiment Nb-Si-Ti-W-Cr alloy bar material is grouped into by the one-tenth of following mass percent: Si
2.4%, Ti 5%, W 5%, Cr 2%, surplus is Nb and inevitable impurity.Si 6.7%,
Ti 25%, W 15%, Cr 8%, surplus is Nb and inevitable impurity.
The preparation method of the present embodiment Nb-Si-Ti-W-Cr alloy bar material comprises the following steps:
Step one, niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are placed in ball mill, with anhydrous second
Alcohol is dispersant, is 200rpm at rotating speed, and ball material mass ratio is wet ball grinding 25h under conditions of 10:1,
Dry under vacuum after ball milling, obtain mixed-powder；The volume of described dehydrated alcohol be niobium powder,
Silica flour, titanium valve, tungsten powder and 3 times of chromium powder quality sum, wherein the unit of volume is mL, quality
Unit be g, the quality purity of described niobium powder, silica flour, titanium valve, tungsten powder and chromium powder all not less than 99%,
The particle diameter of described silica flour and chromium powder is no more than 10 μm, and the particle diameter of described titanium valve is not more than 9 μm, institute
The particle diameter stating tungsten powder is not more than 7 μm, and the particle diameter of described niobium powder is not more than 20 μm；
Step 2, by compressing for a kind of for step described mixed-powder, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Place it is sintered under conditions of Pa
Reason, obtains sintered body after furnace cooling；The temperature of described sintering processes is 1600 DEG C, and temperature retention time is
3h；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 2 times under conditions of Pa, carry out the process that strips off the skin, are cast after natural cooling
Ingot；The melting electric current of described electronic torch melting is 2A, and melting voltage is 60kV；
Step 4, being 1250 DEG C by institute's ingot casting in step 3 at extrusion temperature, extrusion ratio is the bar of 6.5
Extrude under part, after natural cooling, carry out the process that strips off the skin, obtain semi-finished product rod base；
Step 5, by the Nb-Si-Ti-W-Cr alloy semi-finished product rod base described in step 4 extruding temperature
Degree is 1150 DEG C, and extrusion ratio is to extrude under conditions of 4.5, carries out the process that strips off the skin after natural cooling,
Obtain Nb-Si-Ti-W-Cr alloy bar material.
Nb-Si-Ti-W-Cr alloy bar material prepared by the present embodiment has that quality purity is high, oxygen content is low
With the feature of microstructure fine uniform, density is 7.5g/cm3, oxygen content is 93ppm, and room temperature resists
Tensile strength is 657MPa, elongation percentage is 2.1%, and the tensile strength of 1400 DEG C is 273MPa, at 1400 DEG C
In air ambient, after oxidation 100h, material unaccounted-for (MUF) is 0.27mg/cm2, this Nb-Si-Ti-W-Cr alloy bar
Material has that density is low, intensity is high and the feature such as antioxidation, it is possible to use in 1400 DEG C of air ambients.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention.All
It is that any simple modification, change and the equivalence made above example according to inventive technique essence becomes
Change, all still fall within the protection domain of technical solution of the present invention.
Claims (10)
1. a Nb-Si-Ti-W-Cr alloy bar material, it is characterised in that by following mass percent
One-tenth is grouped into: Si 2.4%～6.7%, Ti 5%～25%, W 5%～15%, Cr 2%～8%, and surplus is
Nb and inevitable impurity.
A kind of Nb-Si-Ti-W-Cr alloy bar material the most according to claim 1, it is characterised in that
It is grouped into by the one-tenth of following mass percent: Si 3.1%～6.1%, Ti 10%～20%, W 7%～15%,
Cr 3%～7%, surplus is Nb and inevitable impurity.
A kind of Nb-Si-Ti-W-Cr alloy bar material the most according to claim 2, it is characterised in that
It is grouped into by the one-tenth of following mass percent: Si 3.7%, Ti 15%, W 15%, Cr 5%, surplus
For Nb and inevitable impurity.
4. prepare the side of Nb-Si-Ti-W-Cr alloy bar material as described in claim 1,2 or 3 for one kind
Method, it is characterised in that the method comprises the following steps:
Niobium powder, silica flour, titanium valve, tungsten powder and chromium powder are mixed by step one, the method for employing wet ball grinding
Uniformly, mixed-powder is obtained after vacuum drying；
Step 2, by compressing for mixed-powder described in step one, obtain blank, then by described
Blank is placed in vacuum sintering furnace, is not more than 5 × 10 in vacuum-1Pa, temperature is 1500 DEG C～1600
It is incubated 2h～3h under conditions of DEG C to be sintered, after furnace cooling, obtains sintered body；
Step 3, sintered body described in step 2 is placed in electron beam furnace, little in vacuum
In 1 × 10-2Electronic torch melting 2～5 times under conditions of Pa, carry out the process that strips off the skin after natural cooling,
To ingot casting；The electric current of described electronic torch melting is 1A～3A, and the voltage of described electronic torch melting is 60kV
～80kV；
Step 4, being 1200 DEG C～1400 DEG C by ingot casting described in step 3 in temperature, extrusion ratio is 5～7
Under conditions of extrude, carry out the process that strips off the skin after natural cooling, obtain semi-finished product rod base；
Step 5, it is 1100 DEG C～1300 DEG C by the base of semi-finished product rod described in step 4 at extrusion temperature,
Extrusion ratio is to extrude under conditions of 4～6, carries out the process that strips off the skin, obtain after natural cooling
Nb-Si-Ti-W-Cr alloy bar material.
Method the most according to claim 4, it is characterised in that niobium powder described in step one,
The quality purity of silica flour, titanium valve, tungsten powder and chromium powder is all not less than 99%.
Method the most according to claim 4, it is characterised in that titanium valve described in step one
Particle diameter is not more than 9 μm, and the particle diameter of described tungsten powder is not more than 7 μm, described silica flour and the particle diameter of chromium powder
No more than 10 μm, the particle diameter of described niobium powder is not more than 20 μm.
Method the most according to claim 4, it is characterised in that wet method ball described in step one
During mill use dehydrated alcohol be dispersant, the volume of described dehydrated alcohol be niobium powder, silica flour,
Titanium valve, tungsten powder and 2～3 times of chromium powder quality sum, wherein the unit of volume is mL, the list of quality
Position is g.
Method the most according to claim 4, it is characterised in that wet method ball described in step one
The speed of mill is 200rpm～300rpm, and ball material mass ratio is (5～10): 1, and Ball-milling Time is
15h～25h.
Method the most according to claim 4, it is characterised in that extruding temperature described in step 4
Degree is 1250 DEG C～1350 DEG C, and extrusion ratio is 5.5～6.5.
Method the most according to claim 4, it is characterised in that extruding temperature described in step 5
Degree is 1150 DEG C～1250 DEG C, and extrusion ratio is 4.5～5.5.
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| CN109402476A (en) * | 2018-12-13 | 2019-03-01 | 西北有色金属研究院 | A kind of low-density high-strength niobium alloy bar material and preparation method thereof |
| CN110565169A (en) * | 2019-10-28 | 2019-12-13 | 西北有色金属研究院 | Method for cultivating Mo-Nb-W-Zr alloy single crystal seed crystal |
| CN110607562A (en) * | 2019-10-28 | 2019-12-24 | 西北有色金属研究院 | Preparation method of Mo-Nb-W-Zr alloy single crystal bar |
| CN114908261A (en) * | 2022-05-20 | 2022-08-16 | 西北有色金属研究院 | Preparation method of niobium-zirconium-carbon alloy cast ingot |
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| CN110565169A (en) * | 2019-10-28 | 2019-12-13 | 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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