CN112609119B - Al-Re-Nb ternary alloy containing high-melting-point and low-boiling-point elements and preparation method thereof - Google Patents
Al-Re-Nb ternary alloy containing high-melting-point and low-boiling-point elements and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an Al-Re-Nb ternary alloy containing high-melting-point and low-boiling-point elements and a preparation method thereof, wherein the melting point of the Re element is 3180 ℃, the melting point of the Nb element is 2467 ℃, and the boiling point of the Al element is 2467 ℃. Three Al, Re and Nb elements with the purity of 99.99 percent are adopted to be smelted into the Al-Re-Nb ternary alloy. The preparation process of the alloy is simple and convenient, the cost is low, the melting loss of the alloy prepared by the method is greatly reduced, the actual density of the obtained alloy is close to the theoretical density, and the melting loss rate of the alloy is less than 1.9 percent.
Description
Technical Field
The invention relates to a high-temperature alloy preparation technology, in particular to an Al-Re-Nb ternary alloy containing high-melting-point and low-boiling-point elements and a preparation method thereof.
Background
The nickel-based superalloy has high temperature bearing capacity, good creep property and excellent structure stability, and has become a main material of various advanced aeroengine turbine blades. The addition of refractory elements Re, W, Co, Cr and Mo, especially Re, can cause the precipitation of TCP phase from the Ni-based superalloy and accelerate the formation and propagation of cracks. The metal Al has stronger high-temperature oxidation resistance, and the lasting strength and the tensile strength of the nickel-based high-temperature alloy are improved along with the increase of the aluminum content, but the cold-hot fatigue, the plasticity and the welding performance are correspondingly reduced. The metal Nb precipitates a gamma' strengthening phase through aging, and the gamma grains are refined, so that the strength and the hardness of the nickel-based high-temperature alloy can be improved, and the ductility and the toughness of the nickel-based high-temperature alloy can be improved, but when the Nb content is more than 2%, the strength is increased and slowed down, but the ductility and the toughness are sharply reduced. Therefore, basic data can be provided for the component optimization design of the novel nickel-based superalloy by researching the Al-Re-Nb ternary system phase system. The melting point of the metal Re is 3180 ℃, the boiling point of the metal Al is 2467 ℃, and the boiling point of the metal Al is far lower than that of the metal Re, so that the melting loss of Al element in the alloy is serious by the traditional preparation method, which is a key factor for restricting the preparation of Al-Re-Nb ternary system and even higher system alloys, and thus no report of an Al-Re-Nb multi-element system related system is seen so far. And the research of the system-related systems has important theoretical guiding significance and practical application value for revealing the forming mechanism and forming rule of the TCP phase under the interaction of refractory elements, designing the nickel-based high-temperature alloy with high temperature bearing capacity and capable of inhibiting the precipitation of the harmful TCP phase. Therefore, an effective way for reducing the alloy melting loss during the preparation process must be found.
Disclosure of Invention
The invention mainly aims to provide an Al-Re-Nb ternary alloy containing high-melting-point and low-boiling-point elements and a preparation method thereof, which can effectively reduce the melting loss of the Al element and prepare the Al-Re-Nb ternary alloy with uniform components.
The invention provides an Al-Re-Nb ternary alloy containing high-melting-point and low-boiling-point elements simultaneously, which comprises the following components in percentage by mass: 40-45% of Al, 25-35% of Re and the balance of Nb; or 25-30% of Al, 35-45% of Re and the balance of Nb; or 15-25% of Al, 45-55% of Re and the balance of Nb; the melting point of the high-melting-point metal Re is 3180 ℃, and the boiling point of the low-boiling-point metal Al is 2467 ℃.
Further, the melting point of Nb element is 2467 ℃.
Furthermore, the purities of the raw material components of the Re element, the Nb element and the Al element are all 99.99%.
The preparation method of the Al-Re-Nb ternary alloy simultaneously containing the high-melting-point and low-boiling-point elements comprises the following steps:
(1) after sample preparation according to the mass percentage, all Al particles are placed at the bottom of a molten pool of a water-cooled copper plate of a vacuum arc furnace, all Nb pieces are laid on the Al particles, and finally, Re particles are centrally placed on the center positions of the Nb pieces;
(2) during smelting, after the tungsten electrode head is ignited, placing an electric arc at a position 1.5-2 cm above pure titanium, slowly increasing the current to 55-60A, continuing for 2-5 min, and absorbing oxygen possibly remaining in the furnace; then adjusting the current to be minimum or turning off the current, moving a tungsten pole, placing an electric arc between 1.2 cm and 1.8cm above the Re particles, slowly increasing the current until the Re particles start to melt, enabling the flowing Re liquid to cover the lower Nb sheet, melting the Nb sheet, transferring heat to the Al particles, slowly melting the Al into the molten Re-Nb metal liquid, and simultaneously slowly reducing the current to prevent the Al from volatilizing; the circulating cooling water is always ensured to be filled at the bottom of the crucible in the whole smelting process;
(3) applying current of 35-100A according to the melting condition of the alloy, wherein the total melting time of each sample is 30-45S, repeating the melting after sample turning for more than 3 times to ensure that the alloy components are uniform, and obtaining the Al-Re-Nb ternary alloy; when current is applied for a plurality of times, different currents can generate an alternating magnetic field, so that the electromagnetic stirring effect is exerted on the sample in a molten state, and the homogenization of components is facilitated.
Further, the average particle size of the Al and Re particles is 1-3 mm; the thickness of the Nb sheet is 0.2-0.6 mm.
The obtained product is in the shape of button.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts a step-by-step dissolution method, Al particles with low boiling point are positioned at the bottom of a copper crucible, Nb pieces are paved on the Al particles, and smaller Re particles are intensively arranged at the central position above the Nb pieces, namely right below a tungsten electrode (electric arc). The melting of high-melting-point Re is facilitated, the liquid Re flows to coat Nb sheets, Nb is dissolved, the flowing Re-Nb metal liquid coats Al particles, Al is quickly dissolved in the molten Nb, the high-melting-point Re and Nb are fully melted by the stepwise dissolving method, the volatilization of the low-boiling-point Al is effectively reduced, the melting loss of the alloy is greatly reduced, the actual density of the obtained alloy is close to the theoretical density, the melting loss rate of the alloy is less than 1.9%, and the stability of chemical components is ensured.
(2) The Re element is a key element for improving the temperature bearing capacity of the aeroengine in the high-temperature alloy, and is an expensive alloy element. The preparation method of the Al-Re-Nb ternary alloy can accurately obtain the chemical components of the phase regions of alloys with different components, reduce the number of samples required in the research of the phase system of the Al-Re-Nb ternary system, obviously reduce the cost of raw materials and save the experimental time.
Drawings
FIG. 1 is a diagram of a method for placing metal elements in a water-cooled copper plate molten pool crucible during Al-Re-Nb ternary alloy smelting.
FIG. 2 is a diagram of theoretical density, actual density and melting loss of Al-Re-Nb ternary alloy.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples, but the present invention is not limited thereto.
Example 1
The Al-Re-Nb ternary alloy containing the elements with high melting points and low boiling points, which is prepared by the invention, comprises the following components in percentage by mass: 40% of Al, 35% of Re and the balance of Nb.
The preparation method of the Al-Re-Nb ternary alloy comprises the following steps:
selecting materials: selecting three pure metal raw materials of Al, Re and Nb with the purity of 99.99 percent; al and Re were grains having a grain size of about 2mm, and Nb was a flake having a thickness of about 0.5 mm.
Raw material treatment and batching: and respectively putting the metal raw materials into an acetone solution for ultrasonic cleaning for 15 minutes, taking out the metal raw materials, putting the metal raw materials into alcohol for ultrasonic cleaning for 15 minutes, and immediately drying the metal raw materials by using a blower after the cleaning is finished. And weighing the required raw materials according to the mass percent on an electronic balance with the precision of 0.0001.
Charging: all the Al particles are placed at the bottom of the molten pool of the water-cooled copper plate of the vacuum arc furnace, then all the Nb pieces are laid on the Al particles, and finally the Re particles are concentrated on the center position above the Nb pieces, as shown in figure 1.
The smelting process comprises the following steps: the smelting is carried out by adopting a WK-II type non-consumable vacuum arc smelting furnace, and the smelting furnace consists of a vacuum pump, an arc welding machine and a furnace chamber. Vacuum pumping is carried out to 5 x 10-1Pa, closing the low vacuum valve, opening the molecular pump and the high vacuum valve, pumping high vacuum to 5 × 10-3Pa, and then purging with argon. Repeating the above operations for 2-3 times to obtain a final high vacuum of 5 × 10- 3Pa, filling argon to 0Pa, and starting smelting. During smelting, after a tungsten electrode head is ignited, placing an electric arc at a position 1.5-2 cm above pure titanium, slowly increasing the current to 60A, continuing for 3min, and absorbing oxygen possibly remaining in the furnace; then, the current is adjusted to the minimum, the tungsten pole rod is moved to the crucible containing the sample, and the melting of the sample is started. At the beginning of smelting, a tungsten pole is adjusted to place an electric arc above Re particles by about 1.5cm, the current is slowly increased to 90A, the Re particles begin to melt, and the flowing Re liquid is coatedMelting the Nb-layered sheet, transferring heat to Al particles, slowly melting Al into the molten Re-Nb metal liquid, slowly reducing the current to 80A after the Al particles are completely melted into the Re-Nb metal liquid, preventing the Al from volatilizing, melting for 30S according to the alloy melting condition, then slowly reducing the current to the minimum, preventing the sample from exploding, and finishing the melting of the sample; in order to ensure the uniformity of the alloy components, turning over the sample after closing the electric arc and cooling for 10 minutes and repeatedly smelting for 3 times, thus obtaining the Al-Re-Nb ternary alloy.
Example 2
The Al-Re-Nb ternary alloy containing the elements with high melting points and low boiling points, which is prepared by the invention, comprises the following components in percentage by mass: 28% of Al, 40% of Re and the balance of Nb.
The preparation method of the Al-Re-Nb ternary alloy comprises the following steps:
selecting materials: selecting three pure metal raw materials of Al, Re and Nb with the purity of 99.99 percent; al and Re were grains having a grain size of about 2mm, and Nb was a flake having a thickness of about 0.5 mm.
Raw material treatment and batching: and respectively putting the metal raw materials into an acetone solution for ultrasonic cleaning for 15 minutes, taking out the metal raw materials, putting the metal raw materials into alcohol for ultrasonic cleaning for 15 minutes, and immediately drying the metal raw materials by using a blower after the cleaning is finished. And weighing the required raw materials according to the mass percent on an electronic balance with the precision of 0.0001.
Charging: all the Al particles are placed at the bottom of the molten pool of the water-cooled copper plate of the vacuum arc furnace, then all the Nb pieces are laid on the Al particles, and finally the Re particles are concentrated on the center position above the Nb pieces, as shown in figure 1.
The smelting process comprises the following steps: the smelting is carried out by adopting a WK-II type non-consumable vacuum arc smelting furnace, and the smelting furnace consists of a vacuum pump, an arc welding machine and a furnace chamber. Vacuum pumping is carried out to 5 x 10-1Pa, closing the low vacuum valve, opening the molecular pump and the high vacuum valve, pumping high vacuum to 5 × 10-3Pa, and then purging with argon. Repeating the above operations for 2-3 times to obtain a final high vacuum of 5 × 10- 3Pa, filling argon to 0Pa, and starting smelting. During smelting, after the tungsten electrode head is arc-ignited,placing the electric arc at a position 1.5-2 cm above the pure titanium, slowly increasing the current to 60A, continuing for 3min, and absorbing oxygen possibly remaining in the furnace; then, the current is turned off, a tungsten pole is moved, an electric arc is placed above Re particles by about 1.5cm, the current is slowly increased to 95A, the Re particles start to melt, flowing Re liquid covers the lower Nb piece, the Nb piece is melted, heat is transferred to Al particles, Al is slowly melted into the melted Re-Nb metal liquid, after the Al particles are completely melted into the Re-Nb metal liquid, the current is slowly reduced to 80A, the Al is prevented from volatilizing, 35S is melted according to the alloy melting condition, then the current is slowly reduced to the minimum, the sample is prevented from being cracked, and the sample is melted completely; in order to ensure the uniformity of the alloy components, turning over the sample after closing the electric arc and cooling for 10 minutes and repeatedly smelting for 3 times, thus obtaining the Al-Re-Nb ternary alloy.
Example 3
The Al-Re-Nb ternary alloy containing the elements with high melting points and low boiling points, which is prepared by the invention, comprises the following components in percentage by mass: 20% of Al, 50% of Re and the balance of Nb.
The preparation method of the Al-Re-Nb ternary alloy comprises the following steps:
selecting materials: selecting three pure metal raw materials of Al, Re and Nb with the purity of 99.99 percent; al and Re were grains having a grain size of about 2mm, and Nb was a flake having a thickness of about 0.5 mm.
Raw material treatment and batching: and respectively putting the metal raw materials into an acetone solution for ultrasonic cleaning for 15 minutes, taking out the metal raw materials, putting the metal raw materials into alcohol for ultrasonic cleaning for 15 minutes, and immediately drying the metal raw materials by using a blower after the cleaning is finished. And weighing the required raw materials according to the mass percent on an electronic balance with the precision of 0.0001.
Charging: all the Al particles are placed at the bottom of the molten pool of the water-cooled copper plate of the vacuum arc furnace, then all the Nb pieces are laid on the Al particles, and finally the Re particles are concentrated on the center position above the Nb pieces, as shown in figure 1.
The smelting process comprises the following steps: the smelting is carried out by adopting a WK-II type non-consumable vacuum arc smelting furnace, and the smelting furnace consists of a vacuum pump, an arc welding machine and a furnace chamber. Vacuum pumping is carried out to 5 x 10-1Pa, closing the low vacuum valve, opening the molecular pump and the high vacuum valve, pumping high vacuum to 5 × 10-3Pa, and then purging with argon. Repeating the above operations for 2-3 times to obtain a final high vacuum of 5 × 10- 3Pa, filling argon to 0Pa, and starting smelting. During smelting, after the tungsten electrode is ignited, an electric arc is placed at a position 1.5-2 cm above pure titanium, the current is slowly increased to 60A, the duration is continued for 3min, and possible residual oxygen in the furnace is absorbed. Then, the current is regulated to be minimum, a tungsten pole is moved, an electric arc is placed about 1.6cm above Re particles, the current is slowly increased to 100A, the Re particles start to melt, flowing Re liquid covers a lower Nb sheet, the Nb sheet is melted, heat is transferred to Al particles, the Al is slowly melted into the melted Re-Nb molten metal, after the Al particles are completely melted into the Re-Nb molten metal, the current is slowly reduced to 80A, the Al is prevented from volatilizing, 35S is melted according to the alloy melting condition, then the current is slowly reduced to be minimum, the sample is prevented from exploding, and the sample is completely melted; in order to ensure the uniformity of the alloy components, turning over the sample after closing the electric arc and cooling for 10 minutes and repeatedly smelting for 4 times, thus obtaining the Al-Re-Nb ternary alloy.
And (3) subsequent treatment: after the smelting is finished, waiting for 10 minutes, opening the furnace door for sampling after the furnace temperature is reduced, putting the sample into alcohol for ultrasonic cleaning for 15 minutes, and then putting the sample into a drying oven for drying treatment. Weighing the mass of the sample on an electronic balance with the precision of 0.0001, and calculating the melting loss rate of the alloy according to the mass of the sample before and after melting, wherein the melting loss rate is shown in a formula (1); the density of the sample was measured by Archimedes' method as shown in equation (2).
The theoretical density, actual density and melting loss of examples 1 to 3 are shown in Table 1.
The alloy melting loss rate calculation formula is as follows:
in the formula: x represents the alloy melting loss (%); w1Representing the total weight (g) of alloy raw materials before sample melting; w2Represents the total weight (g) of the sample after melting.
The actual density calculation formula of the sample is as follows:
in the formula: ρ represents the actual density (g/cm) of the sample3)；G1Representing the total weight (g) of alloy raw materials before sample melting; g2Represents the total weight (g) of the sample after smelting; rhoWater (W)＝1g/cm3。
TABLE 1 theoretical density, actual density and melting loss for examples 1-3
As can be seen from Table 1, the Al-Re-Nb ternary alloy prepared by the invention can fully melt high-melting-point Re and Nb, effectively reduce volatilization of low-boiling-point Al, greatly reduce the melting loss of the alloy, ensure that the actual density of the obtained alloy is close to the theoretical density, ensure that the melting loss of the alloy is less than 1.9 percent and ensure the stability of chemical components.
Claims (5)
1. The Al-Re-Nb ternary alloy simultaneously containing high-melting-point and low-boiling-point elements is characterized by comprising the following components in percentage by mass: 40-45% of Al, 25-35% of Re and the balance of Nb; or 25-30% of Al, 35-45% of Re and the balance of Nb; or 15-25% of Al, 45-55% of Re and the balance of Nb; the melting point of the high-melting-point metal Re element is 3180 ℃, and the boiling point of the low-boiling-point metal Al element is 2467 ℃.
2. The Al-Re-Nb ternary alloy containing both high-melting point and low-boiling point elements according to claim 1, wherein: the purities of the Re element, the Nb element and the Al element which are raw material components are all 99.99 percent.
3. The Al-Re-Nb ternary alloy containing both high-melting point and low-boiling point elements according to claim 1, wherein: the melting point of the Nb element is 2467 ℃.
4. A method for preparing an Al-Re-Nb ternary alloy containing both high-melting point and low-boiling point elements as claimed in any one of claims 1 to 3, characterized in that: the alloy is prepared by vacuum melting Al and Re particles and Nb sheets, and specifically comprises the following steps:
(1) placing all Al particles at the bottom of a molten pool of a water-cooled copper plate of a vacuum arc furnace, then flatly paving all Nb slices on the Al particles, and finally intensively placing Re particles at the central position above the Nb slices, wherein the raw materials meet the following mass percentages:
40-45% of Al, 25-35% of Re and the balance of Nb;
or 25-30% of Al, 35-45% of Re and the balance of Nb;
or 15-25% of Al, 45-55% of Re and the balance of Nb;
(2) during smelting, after the tungsten electrode head is ignited, placing an electric arc at a position 1.5-2 cm above pure titanium, slowly increasing the current to 55-60A, continuing for 2-5 min, and absorbing oxygen possibly remaining in the furnace; then adjusting the current to be minimum or turning off the current, moving a tungsten pole, placing an electric arc between 1.2 cm and 1.8cm above the Re particles, slowly increasing the current until the Re particles start to melt, enabling the flowing Re liquid to cover the lower Nb sheet, melting the Nb sheet, transferring heat to the Al particles, slowly melting the Al into the molten Re-Nb metal liquid, and simultaneously slowly reducing the current to prevent the Al from volatilizing; the circulating cooling water is always ensured to be filled at the bottom of the crucible in the whole smelting process;
(3) applying 35-100A of current according to the melting condition of the alloy, wherein the total melting time of each sample is 30-45S, turning over the sample to repeatedly melt again in order to ensure that the alloy components are uniform, and repeatedly melting for more than 3 times in the way to obtain the Al-Re-Nb ternary alloy; when current is applied for a plurality of times, different currents can generate an alternating magnetic field, so that the electromagnetic stirring effect is exerted on the sample in a molten state, and the homogenization of components is facilitated.
5. The method for preparing the Al-Re-Nb ternary alloy containing the elements with high melting point and low boiling point simultaneously as claimed in claim 4, wherein the method comprises the following steps: the average particle size of the Al and Re particles is 1-3 mm; the thickness of the Nb sheet is 0.2-0.6 mm.
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