CN111763838A - Preparation process of tantalum-tungsten alloy wire - Google Patents

Preparation process of tantalum-tungsten alloy wire Download PDF

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Publication number
CN111763838A
CN111763838A CN202010658600.2A CN202010658600A CN111763838A CN 111763838 A CN111763838 A CN 111763838A CN 202010658600 A CN202010658600 A CN 202010658600A CN 111763838 A CN111763838 A CN 111763838A
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tantalum
tungsten alloy
powder
alloy wire
mixed
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CN202010658600.2A
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Chinese (zh)
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王建生
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Baoji Hengye Nonferrous Metal Technology Co ltd
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Baoji Hengye Nonferrous Metal Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/04Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02Alloys based on vanadium, niobium, or tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon

Abstract

The invention discloses a preparation process of a tantalum-tungsten alloy wire material, which comprises the following steps of mixing powder, weighing tantalum powder with the average particle size of 3-5 mu m and tungsten powder with the average particle size of 3 mu m serving as raw materials according to a required proportion, mixing, and placing the mixed powder in a drum mixer to be uniformly mixed to obtain mixed powder. According to the invention, the pressed compact is smelted for multiple times under a vacuum condition, is overturned in each smelting process, and is smelted for the next time, so that the smelting effect is better, the smelting is prevented from being uneven, the process is simplified, the raw material cost and the processing cost are effectively reduced, and the tantalum-tungsten alloy wire obtained through multiple vacuum annealing and wire drawing treatments has small average grain size and obviously improved mechanical properties such as Vickers hardness, tensile strength, yield strength, elongation and the like.

Description

Preparation process of tantalum-tungsten alloy wire
Technical Field
The invention relates to the technical field of metal material preparation, in particular to a preparation process of a tantalum-tungsten alloy wire.
Background
The tantalum-tungsten binary system alloy formed by adding a certain amount of tungsten element into tantalum has the corrosion resistance of tantalum and the good high-temperature strength of tungsten. The alloy has the advantages of high temperature resistance, high strength, good fracture toughness, corrosion resistance and the like, and is applied to the fields of aviation, aerospace, chemical engineering, nuclear industry, high temperature technology and the like. Because the tantalum-tungsten ingot has large deformation resistance, in order to prevent cracking in the forging process, the existing process for producing the tantalum-tungsten alloy is to perform warm forging on a tantalum-tungsten ingot blank, even to perform hot forging or extrusion cogging at the temperature of more than 1200 ℃, and then perform heat treatment and rolling. By using the method, a heating furnace needs to be configured, the surface of the tantalum-tungsten alloy ingot is oxidized after being heated, and the oxide layer needs to be removed after the tantalum-tungsten alloy ingot is processed, so that the production cost is increased, the process is complicated, the produced tantalum-tungsten alloy plate has uneven structure, larger alloy crystal grains and poorer mechanical property.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation process of a tantalum-tungsten alloy wire.
The invention provides a preparation process of a tantalum-tungsten alloy wire, which comprises the following steps:
s1, mixing powder, namely weighing and mixing tantalum powder with the average particle size of 3-5 microns and tungsten powder with the average particle size of 3 microns serving as raw materials according to a required proportion, and placing the mixed powder into a drum mixer to be uniformly mixed to obtain mixed powder;
s2, screening the mixed materials, and sieving the mixed powder with a 120-mesh sieve to obtain fine powder;
s3: pressing the blank, namely placing the screened mixed powder on an oil press to press the blank, wherein the pressing pressure is 300-400 MPa, so as to obtain the blank;
s4: arc melting, namely putting the billet block into a crucible of an arc melting furnace, closing a furnace door, vacuumizing until the pressure in a hearth is lower than 0.003Pa, stopping vacuumizing, filling high-purity argon to 0.05MPa, vacuumizing, and repeating the vacuumizing step for three times to melt to obtain a tantalum-tungsten alloy billet;
s5: forging and profile rolling, namely forging and profile rolling the tantalum-tungsten alloy blank obtained in the step S4 in sequence to obtain a plate-shaped rolled strip;
s6: and drawing, namely drawing the rolled bar obtained in the step S5 at high temperature until the total deformation of the rolled bar is more than 70% to obtain a tantalum-tungsten alloy wire, and continuously annealing the tantalum-tungsten alloy wire to obtain the required tantalum-tungsten alloy wire.
Preferably, the powder mixing conditions of S1 are as follows: tantalum powder and tungsten powder are mixed according to the ratio of 9:1 and then are put into a drum mixer to rotate at 400 r/min-600 r/min, and the mixing time is 6h-12 h.
Preferably, the compaction in S3 is performed by unidirectional compaction or bidirectional compaction.
Preferably, the step of arc melting in S4 is to put the compact formed by pressing into a crucible of an arc melting furnace, close the furnace door, evacuate the interior of the crucible to a vacuum state, make the internal pressure lower than 0.003Pa, fill high purity argon gas to 0.05MPa, evacuate, heat to 2000 ℃ -2400 ℃, control the melting current to 400A-500A, continue for 3-5 minutes, turn over and melt for the next time, continue for 3-4 times.
Preferably, the rolled bar obtained in the step S5 is drawn at the temperature of 700-850 ℃ until the total deformation of the rolled bar is more than 70%, so as to obtain the tantalum-tungsten alloy wire with the diameter of phi 2-phi 5 mm.
Preferably, in the step S6, after the tantalum-tungsten alloy wire is subjected to drawing treatment at high temperature, the temperature of vacuum annealing is controlled to be 1200-1400 ℃, the annealing duration is 90-150min, and before the annealing treatment, the tungsten alloy wire is subjected to alkali washing, wherein the alkali washing solution is a mixed solution of commercial washing powder and hot water, and after the alkali washing is finished, the tungsten alloy wire is washed with clean water.
The invention has the beneficial effects that:
in the process of electric arc melting, the pressed compact is melted for multiple times under the vacuum condition, is overturned in each melting process and is melted for the next time, so that the melting effect is better, the non-uniform melting is prevented, the tantalum-tungsten alloy wire manufactured in the way is simplified in process, the raw material cost and the processing cost are effectively reduced, and the obtained tantalum-tungsten alloy wire has small average grain size, Vickers hardness, tensile strength, yield strength, elongation and other mechanical properties after multiple times of vacuum annealing and wire drawing treatment.
Drawings
FIG. 1 is a schematic view of a flow structure of a process for preparing tantalum-tungsten alloy wire according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, the preparation process of the tantalum-tungsten alloy wire comprises the following steps:
s1, powder mixing, namely, weighing and mixing tantalum powder with the average particle size of 3-5 microns and tungsten powder with the average particle size of 3 microns according to a required proportion, putting the mixed powder into a drum mixer for uniform mixing, preparing the tantalum powder and the tungsten powder according to the proportion of 9:1, putting the prepared powder into the drum mixer, rotating at 400-600 r/min, and mixing for 6-12 h to obtain mixed powder;
s2, screening the mixed materials, and sieving the mixed powder with a 120-mesh sieve to obtain fine powder;
s3: compacting, namely placing the mixed powder obtained by screening on an oil press to compact the mixed powder, wherein the compacting pressure is 300-400 MPa, so that a compact is obtained, and the compacting mode in S3 is one-way compacting or two-way compacting;
s4: arc melting, namely putting the briquette into a crucible of an arc melting furnace, closing the furnace door, vacuumizing until the pressure in a hearth is lower than 0.003Pa, stopping vacuumizing, filling high-purity argon gas to 0.05MPa, vacuumizing, repeating the vacuumizing steps for three times, and then melting to obtain a tantalum-tungsten alloy billet, wherein the arc melting step in S4 comprises the steps of putting the pressed briquette into the crucible of the arc melting furnace, closing the furnace door, vacuumizing the interior of the briquette into a vacuum state, ensuring that the internal pressure is lower than 0.003Pa, filling the high-purity argon gas to 0.05MPa, vacuumizing, heating to 2000-2400 ℃, controlling the melting current to 400-500A, turning over and melting for the next time after 3-5 minutes, and continuing for 3-4 times;
s5: forging and profile rolling, namely forging and profile rolling the tantalum-tungsten alloy blank obtained in the step S4 in sequence to obtain a plate-shaped rolled strip;
s6: drawing, namely drawing the rolled bar obtained in S5 at high temperature until the total deformation of the rolled bar is more than 70% to obtain a tantalum-tungsten alloy wire, continuously annealing the tantalum-tungsten alloy wire to obtain a required tantalum-tungsten alloy wire, drawing the rolled bar obtained in S5 at 700-850 ℃ until the total deformation of the rolled bar is more than 70% to obtain a tantalum-tungsten alloy wire with phi 2-phi 5mm, controlling the vacuum annealing temperature at 1200-1400 ℃ after the tantalum-tungsten alloy wire is drawn at high temperature in S6, and controlling the annealing duration time to be 90-150min, and before the annealing, performing alkali washing on the tungsten alloy wire, wherein the alkali washing solution is a mixed solution of commercial washing powder and hot water, and washing the tungsten alloy wire with clear water after the alkali washing is finished.
Example 1 tantalum powder with an average particle size of 3 to 5 μm and tungsten powder with an average particle size of 3 μm are used as raw materials and are mixed according to a ratio of 9:1 and then are put into a drum mixer to rotate at 400r/min for 6 hours, mixed uniformly at the present stage to obtain mixed powder, the mixed powder is sieved through a 120-mesh sieve to obtain fine powder, the sieved mixed powder is placed on an oil press to be pressed into briquettes in a one-way pressing mode or a two-way pressing mode, the pressing pressure is 300MPa to obtain briquettes, then the briquettes are placed into a crucible of an electric arc melting furnace, a furnace door is closed, vacuumizing is stopped until the pressure in a furnace hearth is lower than 0.003Pa, high-purity argon gas is filled to 0.05MPa, vacuumizing is carried out, heating is carried out to 2000, the smelting current is controlled to 400A, after 3 minutes, the briquettes are turned over and smelted for the next time, 3 times are continued, the method comprises the steps of repeating the vacuumizing step for three times, smelting to obtain a tantalum-tungsten alloy blank, sequentially forging and forming the obtained tantalum-tungsten alloy blank to obtain a plate-shaped rolled strip, drawing the rolled strip at 700 ℃ until the total deformation of the rolled strip is greater than 70% to obtain a tantalum-tungsten alloy wire with the diameter of phi 2mm, continuously annealing the tantalum-tungsten alloy wire, controlling the temperature of vacuum annealing at 1200 ℃ and the annealing duration time to be 90min, carrying out alkali washing on the tungsten alloy wire before the annealing treatment, wherein the alkali washing solution is a mixed solution of commercial washing powder and hot water, and washing with clean water after the alkali washing is finished to obtain the required tantalum-tungsten alloy wire.
The metallographic and mechanical property test of the tantalum-tungsten alloy wire material obtained in the embodiment shows that: the diameter of the tantalum-tungsten alloy wire is 2mm, the grain size is 22um, the Vickers hardness is 127HV1, the tensile strength is 370Mpa, the yield strength is 280Mpa, and the elongation is 43%.
Example 2, tantalum powder with an average particle size of 3 μm to 5 μm and tungsten powder with an average particle size of 3 μm are used as raw materials and are mixed according to a ratio of 9:1, then the raw materials are put into a drum mixer, the raw materials are rotated at 450r/min for 9 hours and are mixed uniformly at the present stage to obtain mixed powder, the mixed powder is sieved through a 120-mesh sieve to obtain fine powder, the sieved mixed powder is placed on an oil press to be pressed into briquettes in a unidirectional pressing mode or a bidirectional pressing mode, the pressing pressure is 350MPa to obtain briquettes, then the briquettes are put into a crucible of an electric arc melting furnace, a furnace door is closed, the furnace is vacuumized until the pressure is lower than 0.003Pa, the furnace is stopped to be vacuumized after high-purity argon is filled to 0.05MPa, the furnace is vacuumized, the furnace is heated to 2200 ℃, the melting current is controlled at 450A, the furnace is turned over and is melted for the next time after 4 minutes, the next time is continued, the method comprises the steps of repeating the vacuumizing step for three times, smelting to obtain a tantalum-tungsten alloy blank, sequentially forging and forming the obtained tantalum-tungsten alloy blank to obtain a plate-shaped rolled strip, drawing the rolled strip at 800 ℃ until the total deformation of the rolled strip is greater than 70% to obtain a tantalum-tungsten alloy wire with the diameter of 4mm, continuously annealing the tantalum-tungsten alloy wire, controlling the temperature of vacuum annealing at 1300 ℃ and the annealing duration time to be 120min, carrying out alkali washing on the tungsten alloy wire before the annealing treatment, wherein the alkali washing solution is a mixed solution of commercial washing powder and hot water, and washing with clean water after the alkali washing is finished to obtain the required tantalum-tungsten alloy wire.
The metallographic and mechanical property test of the tantalum-tungsten alloy wire material obtained in the embodiment shows that: the diameter of the tantalum-tungsten alloy wire is 4mm, the grain size is 22um, the Vickers hardness is 135HV1, the tensile strength is 395MPa, the yield strength is 314MPa, and the elongation is 47%.
Example 3 tantalum powder with an average particle size of 3 to 5 μm and tungsten powder with an average particle size of 3 μm were used as raw materials and mixed in a ratio of 9:1 and then loaded into a drum mixer, rotated at 600r/min and mixed for 12 hours, mixed uniformly at the present stage to obtain mixed powder, the mixed powder was sieved through a 120 mesh sieve to obtain fine powder, the sieved mixed powder was placed on an oil press to perform briquette pressing in a one-way pressing or two-way pressing manner at a pressing pressure of 400MPa to obtain briquettes, the briquettes were placed into a crucible of an arc melting furnace, the furnace door was closed, the furnace was evacuated until the pressure in the furnace was below 0.003Pa, evacuation was stopped after charging high purity argon gas to 0.05MPa, evacuation was performed to heat to 2400 MPa, and the melting current was controlled at 500A, after continuing for 5 minutes, the briquettes were turned over and melted for the next time, and continued for 4 times, the method comprises the steps of repeating the vacuumizing step for three times, smelting to obtain a tantalum-tungsten alloy blank, sequentially forging and forming the obtained tantalum-tungsten alloy blank to obtain a plate-shaped rolled strip, drawing the rolled strip at 850 ℃ until the total deformation of the rolled strip is greater than 70% to obtain a tantalum-tungsten alloy wire with the diameter of 5mm, continuously annealing the tantalum-tungsten alloy wire, controlling the temperature of vacuum annealing at 1400 ℃ and the annealing duration time at 150min, carrying out alkali washing on the tungsten alloy wire before the annealing treatment, wherein the alkali washing solution is a mixed solution of commercial washing powder and hot water, and washing with clean water after the alkali washing is finished to obtain the required tantalum-tungsten alloy wire.
The metallographic and mechanical property test of the tantalum-tungsten alloy wire material obtained in the embodiment shows that: the diameter of the tantalum-tungsten alloy wire is 5mm, the grain size is 22um, the Vickers hardness is 139HV1, the tensile strength is 403MPa, the yield strength is 319MPa, and the elongation is 50%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (6)

1. A preparation process of tantalum-tungsten alloy wire is characterized by comprising the following steps:
s1, mixing powder, namely weighing and mixing tantalum powder with the average particle size of 3-5 microns and tungsten powder with the average particle size of 3 microns serving as raw materials according to a required proportion, and placing the mixed powder into a drum mixer to be uniformly mixed to obtain mixed powder;
s2, screening the mixed materials, and sieving the mixed powder with a 120-mesh sieve to obtain fine powder;
s3: pressing the blank, namely placing the screened mixed powder on an oil press to press the blank, wherein the pressing pressure is 300-400 MPa, so as to obtain the blank;
s4: arc melting, namely putting the billet block into a crucible of an arc melting furnace, closing a furnace door, vacuumizing until the pressure in a hearth is lower than 0.003Pa, stopping vacuumizing, filling high-purity argon to 0.05MPa, vacuumizing, and repeating the vacuumizing step for three times to melt to obtain a tantalum-tungsten alloy billet;
s5: forging and profile rolling, namely forging and profile rolling the tantalum-tungsten alloy blank obtained in the step S4 in sequence to obtain a plate-shaped rolled strip;
s6: and drawing, namely drawing the rolled bar obtained in the step S5 at high temperature until the total deformation of the rolled bar is more than 70% to obtain a tantalum-tungsten alloy wire, and continuously annealing the tantalum-tungsten alloy wire to obtain the required tantalum-tungsten alloy wire.
2. The process for preparing a tantalum-tungsten alloy wire according to claim 1, wherein the powder mixing conditions of S1 are as follows: tantalum powder and tungsten powder are mixed according to the ratio of 9:1 and then are put into a drum mixer to rotate at 400 r/min-600 r/min, and the mixing time is 6h-12 h.
3. The process for preparing tantalum-tungsten alloy wire according to claim 1, wherein the compaction in S3 is performed by one-way compaction or two-way compaction.
4. The process for preparing a tantalum-tungsten alloy wire according to claim 1, wherein the step of arc melting in S4 is that the compact formed by pressing is placed in a crucible of an arc melting furnace, a furnace door is closed, the interior of the compact is evacuated to a vacuum state, the internal pressure is lower than 0.003Pa, high-purity argon is charged to 0.05MPa, then the compact is evacuated, the compact is heated to 2000 ℃ -2400 ℃, the melting current is controlled to 400A-500A, and after 3-5 minutes, the compact is turned over and the next melting is performed for 3-4 times.
5. The process of claim 1, wherein the rolled bar obtained in the step S5 is drawn at a temperature of 700 ℃ to 850 ℃ until the total deformation of the rolled bar is greater than 70%, so as to obtain a tantalum-tungsten alloy wire of Φ 2mm to Φ 5 mm.
6. The process for preparing tantalum-tungsten alloy wire according to claim 1, wherein in S6, after the tantalum-tungsten alloy wire is subjected to drawing treatment at high temperature, the temperature of vacuum annealing is controlled to be 1200-1400 ℃, the annealing duration is 90-150min, and before the annealing treatment, the tungsten alloy wire is subjected to alkali washing, wherein the alkali washing solution is a mixed solution of commercial washing powder and hot water, and the mixed solution is washed with clear water after the alkali washing is finished.
CN202010658600.2A 2020-07-09 2020-07-09 Preparation process of tantalum-tungsten alloy wire Pending CN111763838A (en)

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CN114807554A (en) * 2022-04-11 2022-07-29 合肥工业大学 Thermomechanical treatment method for improving hardness of Ta-2.5W alloy and application thereof
CN116607056A (en) * 2023-05-30 2023-08-18 宝鸡恒业有色金属科技有限公司 High-strength stretch-proof tantalum-tungsten alloy wire and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN114273676A (en) * 2021-12-30 2022-04-05 西安交通大学 Refractory tungsten-tantalum alloy complex structural component and additive manufacturing and forming method thereof
CN114807554A (en) * 2022-04-11 2022-07-29 合肥工业大学 Thermomechanical treatment method for improving hardness of Ta-2.5W alloy and application thereof
CN114807554B (en) * 2022-04-11 2024-04-16 合肥工业大学 Thermomechanical treatment method for improving hardness of Ta-2.5W alloy and application thereof
CN116607056A (en) * 2023-05-30 2023-08-18 宝鸡恒业有色金属科技有限公司 High-strength stretch-proof tantalum-tungsten alloy wire and preparation method thereof

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