CN110643874A - Nb-Si base multi-component alloy material for improving oxidation resistance in wide temperature range - Google Patents

Nb-Si base multi-component alloy material for improving oxidation resistance in wide temperature range Download PDF

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CN110643874A
CN110643874A CN201911005065.4A CN201911005065A CN110643874A CN 110643874 A CN110643874 A CN 110643874A CN 201911005065 A CN201911005065 A CN 201911005065A CN 110643874 A CN110643874 A CN 110643874A
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苏琳芬
卓冠群
杨建勇
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Huaqiao University
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Abstract

The invention discloses an Nb-Si-based multi-component alloy material for improving oxidation resistance in a wide temperature range, which consists of 40-50 at.% of Nb, 20-30 at.% of Ti, 10-18 at.% of Cr, 1-3 at.% of Al, 0-4 at.% of Hf, 13-19 at.% of Si, 0-4 at.% of Sn, 0-3 at.% of Ta, 0-6 at.% of Ge and 0-6 at.% of B, wherein the sum of the contents of Si and Ge is 16-20 at.%, the sum of the contents of B, Sn and Ta is 2-5 at.%, and the sum of the atomic percentages of the elements is 100%. The Nb-Si-based multielement alloy material prepared according to the component proportion and the preparation method in the scheme has greatly improved oxidation resistance in a medium-high temperature range.

Description

Nb-Si base multi-component alloy material for improving oxidation resistance in wide temperature range
Technical Field
The invention relates to the field of ultra-high temperature alloy materials, in particular to an Nb-Si based multi-component alloy material with improved oxidation resistance at medium temperature and high temperature.
Background
The Nb-Si base multicomponent alloy has high melting point (higher than 1750 ℃) and low density (6.6-7.2 g)/cm3) And the high-temperature-resistant high-performance gas turbine engine material has obvious advantages in the aspects of breaking strength, fatigue performance, processability and the like, becomes the most potential candidate of the future high-performance gas turbine engine material, and is expected to be applied to certain high-temperature fixed components and high-temperature rotating components in advanced aviation and aerospace gas turbine engines. Nb-Si based multi-component alloys rely primarily on a metallic solid solution phase (Nb)SS) To improve its room temperature toughness, by means of intermetallic compound phases (Nb)5Si3、Nb3Si and Cr2Nb, etc.) to improve the high-temperature strength and the high-temperature oxidation resistance, and the ultrahigh-temperature structural material with excellent obdurability matching performance is obtained through proper combination.
However, the Nb-Si based multicomponent alloy has serious oxidation phenomenon under the working environment of 600-1300 ℃, and the application of the Nb-Si based multicomponent alloy in the aerospace field is limited. The Nb-Si multi-component alloy can be subjected to pulverization and oxidation at the temperature of (600-800 ℃), and an oxide film generated at the high temperature of more than 1000 ℃ is loose and porous and cannot protect the matrix metal. Recent main research focuses on improving the high-temperature oxidation resistance of the Nb-Si-based multi-component alloy, and the high-temperature oxidation performance of the alloy is remarkably improved by adding elements such as Ti, V, Hf, Zr, Cr, Mn, Si, Be, B, Zr, Ce and the like. At present, there are few patents on medium temperature oxidation of Nb-Si based alloys. Therefore, there is a need to develop a method for improving the oxidation resistance of Nb-Si-based multi-component alloys in a wide temperature range to solve the problem of comprehensive oxidation performance, and to lay a solid foundation for the application of Nb-Si-based multi-component alloys in future aviation industry.
Disclosure of Invention
The present invention provides an Nb-Si based multi-component alloy material with improved oxidation resistance over a wide temperature range that overcomes the deficiencies of the prior art described in the background.
The technical scheme adopted by the invention for solving the technical problems is as follows:
an Nb-Si based multicomponent alloy material for improving oxidation resistance in a wide temperature range comprises 40-50 at.% of Nb, 20-30 at.% of Ti, 10-18 at.% of Cr, 1-3 at.% of Al, 0-4 at.% of Hf, 13-19 at.% of Si, 0-4 at.% of Sn, 0-3 at.% of Ta, 0-6 at.% of Ge and 0-6 at.% of B, wherein the sum of the contents of Si and Ge is 16-20 at.%, the sum of the contents of B, Sn and Ta is 2-5 at.%, and the sum of the atomic percentages of the elements is 100%.
In one embodiment: the preparation method comprises the following steps:
1) selecting raw materials of Nb blocks, sponge Ti, Si blocks, Al blocks, Hf grains, B grains, Cr blocks, Ge blocks, Ta foil, Sn blocks and B grains, wherein the purities of the Nb blocks, the sponge Ti, the Si blocks, the Al blocks, the Hf grains, the B grains, the Cr blocks, the Ge blocks, the Ta foil, the Sn blocks and the B grains are all 99.97 wt%, and removing impurities and oxides on the surfaces of the;
2) weighing the raw materials according to the target component proportion of Nb-Ti-Si-Al-Hf-B-Cr-Ge-Sn-Ta, respectively, weighing the raw materials by 200-300 g/ingot, putting the raw materials into a vacuum non-consumable arc melting furnace, and stacking the raw materials in sequence from low melting point to high melting point;
3) in a non-consumable vacuum arc furnace, vacuum pumping is carried out to 1 × 10-3-5×10-3Pa, filling high-purity argon to 1.01 multiplied by 105Pa, then repeatedly smelting under the protection of argon to ensure the uniformity of the components of the arc ingot;
4) putting the alloy ingot prepared in the step 3) into an ultrahigh-temperature high-vacuum heat treatment furnace, and simultaneously putting a plurality of sponge Ti around the alloy ingot to achieve the purpose of oxygen absorption;
5) vacuum pumping to 3 × 10-3-6×10-3Heating is started when the temperature is Pa, and the heating rate is about 12-15 ℃/min; stopping vacuumizing when the temperature in the furnace reaches 1000 ℃, and introducing argon for protection; continuing heating, controlling the heating rate at 14-16 ℃/min, and preserving heat for 10-50 h after the temperature in the furnace reaches 1300-1500 ℃ to carry out homogenization and metastable phase decomposition treatment; and after the heat preservation is finished, cooling to room temperature along with the furnace.
In one embodiment: in the step 3), the raw material is repeatedly smelted for four times under the protection of argon gas to ensure the uniformity of the components of the electric arc ingot.
In one embodiment: the alloy structure comprises room temperature toughness NbSSPhase, oxidation resistant Nb5Si3Phase in which NbSS30-60% of phase, Nb5Si3The phase content is 30-50%.
In one embodiment: the alloy structure also comprises 0-25% of high-temperature oxidation resistant Cr2And (4) a Nb phase.
In one embodiment: the oxidation weight gain of the alloy is less than 10mg/cm at 800 ℃/100h2The weight gain is less than 40mg/cm at 1000 ℃/100h through oxidation2The oxidation weight gain of 1200 ℃/100h is less than 72mg/cm2The oxidation weight gain is less than 200mg/cm at 1300 ℃/100h2。
In one embodiment: adopting an Instron universal mechanical testing machine to carry out room temperature fracture toughness test on the Nb-Si base multicomponent alloy material, wherein the fracture toughness K isQThe value is 8.3 to 12 MPa.m1/2。
Compared with the background technology, the technical scheme has the following advantages:
the Nb-Si-based multielement alloy material prepared according to the component proportion and the preparation method in the scheme has greatly improved oxidation resistance in a medium-high temperature range.
Drawings
The invention is further illustrated by the following figures and examples.
FIG. 1 is a graph showing the oxidation resistance test curves at 800 deg.C, 1000 deg.C, 1200 deg.C, and 1300 deg.C in examples 1 and 2.
FIG. 2 is an X-ray diffraction (XRD) spectrum of the Nb-Si based multi-component alloy prepared in example 2.
FIG. 3 is a back-scattered electron (BSE) image of the Nb-Si based multi-component alloy prepared in example 2.
FIG. 4 is a secondary electron image of an oxide film of the Nb-Si based multicomponent alloy prepared in example 2 after oxidation at 800 deg.C/100 h, 1000 deg.C/100 h, 1200 deg.C/100 h, and 1300 deg.C/100 h.
Detailed Description
The invention relates to an Nb-Si based multi-component alloy material capable of being applied at the environment temperature of 800-1300 ℃, which comprises 40-50 at.% of Nb, 20-30 at.% of Ti, 10-18 at.% of Cr, 1-3 at.% of Al, 0-4 at.% of Hf, 13-19 at.% of Si, 0-4 at.% of Sn, 0-3 at.% of Ta, 0-6 at.% of Ge and 0-6 at.% of B, wherein in order to ensure the high-temperature oxidation performance of the alloy, the sum of the contents of Si and Ge is 16-20 at.%, in order to ensure that the alloy cannot be subjected to medium-temperature pulverization oxidation, the sum of the contents of B, Sn and Ta is 2-5 at.%, and the sum of the atomic percentages of the elements is 100%.
The Nb-Si-based multielement alloy material can be prepared by adopting a vacuum non-consumable arc melting technology with an electromagnetic stirring function and a heat treatment method, and comprises the following preparation steps:
1) selecting raw materials of Nb blocks, sponge Ti, Si blocks, Al blocks, Hf grains, B grains, Cr blocks, Ge blocks, Ta foil, Sn blocks and B grains, wherein the purities of the Nb blocks, the sponge Ti, the Si blocks, the Al blocks, the Hf grains, the B grains, the Cr blocks, the Ge blocks, the Ta foil, the Sn blocks and the B grains are all 99.97 wt%, and removing impurities and oxides on the surfaces of the;
2) weighing the raw materials according to the target component proportion of Nb-Ti-Si-Al-Hf-B-Cr-Ge-Sn-Ta, respectively, weighing the raw materials by 200-300 g/ingot, putting the raw materials into a vacuum non-consumable arc melting furnace, and stacking the raw materials in sequence from low melting point to high melting point; the Nb-Ti-Si-Al-Hf-B-Cr-Ge-Sn-Ta target component comprises 40-50 at.% of Nb, 20-30 at.% of Ti, 10-15 at.% of Cr, 1-3 at.% of Al, 0-4 at.% of Hf, 13-19 at.% of Si, 0-4 at.% of Sn, 0-3 at.% of Ta, 0-5 at.% of Ge and 0-6 at.% of B, and the sum of the atomic percentages of the elements is 100%;
3) in a non-consumable vacuum arc furnace, vacuum pumping is carried out to 1 × 10-3-5×10-3Pa, filling high-purity argon to 1.01 multiplied by 105Pa, repeatedly smelting for multiple times (at least repeatedly smelting for four times) under the protection of argon to ensure the uniformity of the components of the arc ingot;
4) putting the alloy ingot prepared in the step 3) into an ultrahigh-temperature high-vacuum heat treatment furnace, and simultaneously putting a plurality of sponge Ti around the alloy ingot to achieve the purpose of oxygen absorption;
5) vacuum pumping to 3 × 10-3-6×10-3Heating is started when the temperature is Pa, and the heating rate is about 12-15 ℃/min; stopping vacuumizing when the temperature in the furnace reaches 1000 ℃, and introducing argon for protection; continuing heating, controlling the heating rate at 14-16 ℃/min, and preserving heat for 10-50 h after the temperature in the furnace reaches 1300-1500 ℃ to carry out homogenization and metastable phase decomposition treatment; and after the heat preservation is finished, cooling to room temperature along with the furnace.
Respectively carrying out phase composition analysis and microstructure observation on Nb-Si based multicomponent alloy samples by using an X-ray diffractometer (XRD) and a Scanning Electron Microscope (SEM), and combiningThe gold structure comprises a ductile phase Nb with the content of 30-60 percentssAnd a strengthening phase Nb with the content of 30-50%5Si3Or, the alloy structure comprises a toughness phase Nb with the content of 30-60 percentss30-50% of strengthening phase Nb5Si30-25% of Cr2Nb。
The high-temperature tube furnace is adopted to carry out high-temperature oxidation resistance test on the Nb-Si-based multicomponent alloy sample to obtain the product with the oxidation weight gain of less than 10mg/cm at 800 ℃/100h2The weight gain is less than 10mg/cm at 1000 ℃/100h through oxidation2The oxidation weight gain of 1200 ℃/100h is less than 10mg/cm2The oxidation weight gain is less than 200mg/cm at 1300 ℃/100h2。
An Instron universal mechanical testing machine is adopted to carry out room temperature fracture toughness test on the Nb-Si base multicomponent alloy sample, and the fracture toughness K of the Nb-Si base multicomponent alloy sampleQThe value is 8.3 to 12 MPa.m1/2。
Example 1:
the Nb-Si based multicomponent alloy material is prepared by adopting a vacuum non-consumable arc melting technology and a 1400 ℃/10h heat treatment method, and comprises the following steps:
1) selecting raw materials of Nb blocks, sponge Ti, Si blocks, Al blocks, Hf grains, B grains, Cr blocks, Ge blocks, Ta foil, Sn blocks and B grains, wherein the purities of the Nb blocks, the sponge Ti, the Si blocks, the Al blocks, the Hf grains, the B grains, the Cr blocks, the Ge blocks, the Ta foil, the Sn blocks and the B grains are all 99.97 wt%, and removing impurities and oxides on the surfaces of the;
2) weighing raw materials respectively according to Nb-24Ti-15Si-13Cr-2Al-2Hf-2Ge-2B (in at.%), weighing 200 g/ingot, putting the raw materials into a vacuum non-consumable arc melting furnace, and stacking the raw materials in sequence from low melting point to high melting point;
3) in a non-consumable vacuum arc furnace, vacuum pumping is carried out to 1 × 10-3-5×10-3Pa, filling high-purity argon to 1.01 multiplied by 105Pa, and then repeatedly smelting for four times under the protection of argon to ensure the uniformity of the components of the arc ingot.
4) Putting the alloy ingot prepared in the step 3) into an ultrahigh-temperature high-vacuum heat treatment furnace, and simultaneously putting a plurality of sponge Ti around the alloy ingot to achieve the purpose of oxygen absorption;
5) vacuum pumping to 3 × 10-3-6×10-3Heating is started when the temperature is Pa, and the heating rate is about 12-15 ℃/min;when the temperature in the furnace reaches 1000 ℃, the vacuumizing is stopped, and argon is filled for protection. (ii) a Continuing heating, controlling the heating rate at 14-16 ℃/min, and preserving heat for 10 hours after the temperature in the furnace reaches 1400 ℃ for homogenization treatment; after the heat preservation is finished, cooling to room temperature along with the furnace;
phase composition analysis and microstructure observation were performed using an X-ray diffractometer (XRD) and a Scanning Electron Microscope (SEM) with Nb-24Ti-15Si-13Cr-2Al-2Hf-2Ge-2B (at.%) alloy specimens (dimensions 8mm × 8mm × 5mm), respectively. The alloy structure consists of a tough phase NbSS、Nb5Si3And Cr2And Nb.
Respectively carrying out phase composition analysis and microstructure observation on a multi-element Nb-Si-based alloy sample by using an X-ray diffractometer (XRD) and a Scanning Electron Microscope (SEM), wherein the alloy structure comprises a toughness phase NbSSAnd a strengthening phase Nb5Si3Or Cr2Nb。
Referring to FIG. 1, a high-temperature tube furnace is adopted to carry out a high-temperature oxidation resistance test on a multielement Nb-Si-based alloy sample, and the 800 ℃/100h oxidation weight gain of the alloy is 8.19mg/cm2The weight of the powder is increased by 15.56mg/cm at 1000 ℃/100h through oxidation2The oxidation weight gain of 1200 ℃/100h is 58.40mg/cm2High-temperature oxidation weight gain of 143.78mg/cm at 1300 ℃/100h2。
Room temperature fracture toughness testing was performed using an Instron universal mechanical tester Nb-24Ti-15Si-13Cr-2Al-2Hf-2Ge-2B (at.%) alloy specimen (dimensions 30mm x 6mm x 3mm), whose K isQA value of 11.6MPa · m1/2。
Example 2:
the method for preparing the multi-element Nb-Si-based alloy material by adopting a vacuum non-consumable arc melting technology and a 1400 ℃/10h heat treatment method comprises the following steps:
1) selecting raw materials of Nb blocks, sponge Ti, Si blocks, Al blocks, Hf grains, B grains, Cr blocks, Ge blocks, Ta foil, Sn blocks and B grains, wherein the purities of the Nb blocks, the sponge Ti, the Si blocks, the Al blocks, the Hf grains, the B grains, the Cr blocks, the Ge blocks, the Ta foil, the Sn blocks and the B grains are all 99.97 wt%, and removing impurities and oxides on the surfaces of the;
2) weighing raw materials respectively according to Nb-24Ti-15Si-13Cr-2Al-2Hf-2Ge-2B-2Sn (in at.%), weighing 200 g/ingot, putting the raw materials into a vacuum non-consumable arc melting furnace, and stacking the raw materials in sequence from low melting point to high melting point;
3) in a non-consumable vacuum arc furnace, vacuum pumping is carried out to 1 × 10-3-5×10-3Pa, filling high-purity argon to 1.01 multiplied by 105Pa, and then repeatedly smelting for four times under the protection of argon to ensure the uniformity of the components of the arc ingot.
4) Putting the alloy ingot prepared in the step 3) into an ultrahigh-temperature high-vacuum heat treatment furnace, and simultaneously putting a plurality of sponge Ti around the alloy ingot to achieve the purpose of oxygen absorption;
5) vacuum pumping to 3 × 10-3-6×10-3Heating is started when the temperature is Pa, and the heating rate is about 12-15 ℃/min; stopping vacuumizing when the temperature in the furnace reaches 1000 ℃, and introducing argon for protection; continuing heating, controlling the heating rate at 14-16 ℃/min, and preserving heat for 10 hours after the temperature in the furnace reaches 1400 ℃ for homogenization treatment; after the heat preservation is finished, cooling to room temperature along with the furnace;
phase composition analysis and microstructure observation were performed using an X-ray diffractometer (XRD) and a Scanning Electron Microscope (SEM) on Nb-24Ti-15Si-13Cr-2Al-2Hf-2Ge-2B-2Sn (at.%) alloy specimens (dimensions 8mm × 8mm × 5mm), respectively. Referring to FIGS. 2 and 3, the alloy structure is composed of a ductile phase Nbss and a strengthening phase Nb5Si3And Cr2And Nb.
Referring to FIG. 1, a high-temperature tube furnace is adopted to carry out a high-temperature oxidation resistance test on a Nb-Si-based multicomponent alloy sample, and the oxidation weight of the alloy is increased by 2.36mg/cm at 800 ℃/100h2The weight is increased by 10.97mg/cm at 1000 ℃/100h through oxidation2The oxidation weight gain of 1200 ℃/100h is 88.26mg/cm2High-temperature oxidation weight gain of 166.60mg/cm at 1300 ℃/100h2. Referring to fig. 4, the alloy oxide film is dense, so that the alloy oxide film has good oxidation resistance at medium and high temperatures.
Room temperature fracture toughness testing was performed using an Instron universal mechanical tester Nb-24Ti-15Si-13Cr-2Al-2Hf-2Ge-2B-2Sn (at.%) alloy coupon (dimensions 30mm x 6mm x 3mm), whose K isQA value of 8.3MPa · m1/2。
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.

Claims (7)

1. An Nb-Si base multielement alloy material for improving the oxidation resistance in a wide temperature range is characterized in that: the alloy consists of 40-50 at.% of Nb, 20-30 at.% of Ti, 10-18 at.% of Cr, 1-3 at.% of Al, 0-4 at.% of Hf, 13-19 at.% of Si, 0-4 at.% of Sn, 0-3 at.% of Ta, 0-6 at.% of Ge and 0-6 at.% of B, wherein the sum of the contents of Si and Ge is 16-20 at.%, the sum of the contents of B, Sn and Ta is 2-5 at.%, and the sum of the atomic percentages of the elements is 100%.
2. The Nb-Si based multi-component alloy material for improving oxidation resistance over a wide temperature range as claimed in claim 1, wherein: the preparation method comprises the following steps:
1) selecting raw materials of Nb blocks, sponge Ti, Si blocks, Al blocks, Hf grains, B grains, Cr blocks, Ge blocks, Ta foil, Sn blocks and B grains, wherein the purities of the Nb blocks, the sponge Ti, the Si blocks, the Al blocks, the Hf grains, the B grains, the Cr blocks, the Ge blocks, the Ta foil, the Sn blocks and the B grains are all 99.97 wt%, and removing impurities and oxides on the surfaces of the;
2) weighing the raw materials according to the target component proportion of Nb-Ti-Si-Al-Hf-B-Cr-Ge-Sn-Ta, respectively, weighing the raw materials by 200-300 g/ingot, putting the raw materials into a vacuum non-consumable arc melting furnace, and stacking the raw materials in sequence from low melting point to high melting point;
3) in a non-consumable vacuum arc furnace, vacuum pumping is carried out to 1 × 10-3-5×10-3Pa, filling high-purity argon to 1.01 multiplied by 105Pa, then repeatedly smelting under the protection of argon to ensure the uniformity of the components of the arc ingot;
4) putting the alloy ingot prepared in the step 3) into an ultrahigh-temperature high-vacuum heat treatment furnace, and simultaneously putting a plurality of sponge Ti around the alloy ingot to achieve the purpose of oxygen absorption;
5) vacuum pumping to 3 × 10-3-6×10-3Heating is started when the temperature is Pa, and the heating rate is 12-15 ℃/min; stopping vacuumizing when the temperature in the furnace reaches 1000 ℃, and introducing argon for protection; continuously heating, controlling the heating rate at 14-16 ℃/min, and after the temperature in the furnace reaches 1300-1500 ℃, preserving the heat for 10-50 h for homogenizationAnd decomposing the metastable phase; and after the heat preservation is finished, cooling to room temperature along with the furnace.
3. The Nb-Si based multi-component alloy material with improved oxidation resistance over a wide temperature range as claimed in claim 2, wherein: in the step 3), the raw material is repeatedly smelted at least four times under the protection of argon gas to ensure the uniformity of the components of the electric arc ingot.
4. An Nb-Si based multi-component alloy material with improved oxidation resistance over a wide temperature range as claimed in claim 1 or 2 or 3, characterized in that: the alloy structure contains NbSSPhase, Nb5Si3Phase in which NbSS30-60% of phase, Nb5Si3The phase content is 30-50%.
5. An Nb-Si based multi-component alloy material with improved oxidation resistance over a wide temperature range as claimed in claim 1 or 2 or 3, characterized in that: the alloy structure also comprises 0-25% Cr2And (4) a Nb phase.
6. An Nb-Si based multi-component alloy material with improved oxidation resistance over a wide temperature range as claimed in claim 1 or 2 or 3, characterized in that: the oxidation weight gain of the alloy material is less than 10mg/cm at 800 ℃/100h2The weight gain is less than 40mg/cm at 1000 ℃/100h through oxidation2The oxidation weight gain of 1200 ℃/100h is less than 72mg/cm2The oxidation weight gain is less than 200mg/cm at 1300 ℃/100h2。
7. An Nb-Si based multi-component alloy material with improved oxidation resistance over a wide temperature range as claimed in claim 1 or 2 or 3, characterized in that: adopting an Instron universal mechanical testing machine to carry out room temperature fracture toughness test on the Nb-Si base multicomponent alloy material, wherein the fracture toughness K isQThe value is 8.3 to 12 MPa.m1/2。
CN201911005065.4A 2019-10-22 2019-10-22 Nb-Si base multi-component alloy material for improving oxidation resistance in wide temperature range Pending CN110643874A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4865644A (en) * 1987-07-23 1989-09-12 Westinghouse Electric Corporation Superconducting niobium alloys
EP1215296A1 (en) * 2000-12-13 2002-06-19 General Electric Company Niobium-silicide based composites resistant to high temperature oxidation
CN106048356A (en) * 2016-01-28 2016-10-26 西北工业大学 Multi-element Nb-Si-based super-high-temperature alloy material and preparing method thereof
CN106048355B (en) * 2016-01-28 2017-10-13 西北工业大学 The preparation method of Nb Si based ultra-high temperature alloy pigs

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4865644A (en) * 1987-07-23 1989-09-12 Westinghouse Electric Corporation Superconducting niobium alloys
EP1215296A1 (en) * 2000-12-13 2002-06-19 General Electric Company Niobium-silicide based composites resistant to high temperature oxidation
CN106048356A (en) * 2016-01-28 2016-10-26 西北工业大学 Multi-element Nb-Si-based super-high-temperature alloy material and preparing method thereof
CN106048355B (en) * 2016-01-28 2017-10-13 西北工业大学 The preparation method of Nb Si based ultra-high temperature alloy pigs

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