CN109306420B - High-performance tungsten alloy bar and preparation method thereof - Google Patents
High-performance tungsten alloy bar and preparation method thereof Download PDFInfo
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- B22F3/10—Sintering only
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Abstract
The invention relates to a high-performance tungsten alloy bar and a preparation method thereof, wherein the bar comprises the following components in percentage by mass: 10-26% of rhenium, 0.3-3% of carbide and the balance of tungsten; the tungsten is partially replaced by Si, Al and K components. The preparation steps of the high-performance tungsten alloy bar sequentially comprise: preparing tungsten-rhenium pre-alloy powder, preparing tungsten alloy powder, forming, sintering, rolling deformation, heat treating, and finally machining to obtain the high-performance tungsten-rhenium alloy bar. The tungsten alloy provided by the invention has the excellent performances of fine grains, uniform structure, lower content of impurity elements, high compactness, high strength, high temperature creep resistance and the like; the tungsten alloy material prepared by the preparation method provided by the invention has fine and uniform crystal grains, the room-temperature tensile strength is more than or equal to 1500MPa, the elongation after fracture is more than or equal to 15%, the 2000 ℃ tensile strength is more than or equal to 200MPa, and the elongation after fracture is more than or equal to 15%.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a high-performance tungsten alloy bar and a preparation method thereof.
Background
With the continuous development of the aerospace high-temperature application field, the requirements on the high-temperature strength, the ablation resistance, the high-temperature creep resistance and the like of the material are higher and higher. The tungsten alloy has a series of excellent performances of high melting point, high strength, high hardness, high plasticity, high recrystallization temperature, high resistivity, low vapor pressure, low electron work function, low plastic brittle transition temperature and the like; particularly, the tungsten alloy has excellent high-temperature mechanical property, so that the tungsten alloy becomes the first choice of the ultrahigh-temperature structural material used at the temperature of 2000 ℃.
At present, research on tungsten-rhenium alloy is mainly focused on the research on wire materials, and domestic research on large-size tungsten-rhenium alloy structural materials is not reported. In order to make the tungsten-rhenium alloy have better performance under high temperature conditions, research is developed in the direction of refining, purifying and toughening, and the second-phase particle reinforced high-rhenium-content tungsten-rhenium alloy will become the focus of future research. In the text of research progress on tungsten-rhenium alloy preparation method and high-temperature mechanical properties (Wangfeng, Zhengxin, et al, China tungsten industry 2014, volume 2, 4, 29), authors mention that foreign W.D.Kloop and W.D.Witzke prepare W-25Re-0.27HfC alloy ingots by vacuum arc melting, and try to make W-25Re-0.27HfC alloy bars by hot extrusion cogging, but have not succeeded; todd Leonhardt prepares the blank through the powder metallurgy method, then go through hot isostatic pressing treatment, finally through rotary swaging and extrusion deformation processing method, get the round bar of W-24.5Re-2HfC about 30mm, room temperature tensile strength can reach 1400MPa, the elongation after fracture can reach more than 10%, 1900 deg.C tensile strength reaches more than 250MPa, but the elongation after fracture is less than 10%, and this kind of manufacturing approach craft is complicated, and the rotary swaging craft is not suitable for preparing the round bar of the bigger diameter, the hot extrusion craft material utilization rate is low, the cost is higher, is not suitable for producing the tungsten alloy on a large scale.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a high-performance tungsten alloy bar which can meet the use requirement of structural materials in the aerospace high-temperature application field at 2000 ℃.
The second purpose of the invention is to provide a preparation method of the high-performance tungsten alloy bar, which adopts a powder metallurgy process, and the prepared tungsten alloy material has fine and uniform crystal grains, the room-temperature tensile strength is more than or equal to 1500MPa, the elongation after fracture is more than or equal to 15%, the 2000 ℃ tensile strength is more than or equal to 200MPa, and the elongation after fracture is more than or equal to 15%.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-performance tungsten alloy bar comprises the following components in percentage by mass: 10-26% of rhenium, 0.3-3% of carbide and the balance of tungsten (namely the mass fraction of tungsten is 71-89.7%).
In the high-performance tungsten alloy bar, as a preferred embodiment, the tungsten is replaced by doped tungsten, and more preferably, the doped tungsten consists of the following components in percentage by mass: 0.015-0.035% of Si, 0.003-0.01% of Al, 0.006-0.016% of K and the balance of tungsten. Doping trace Si, Al and K is beneficial to further improving the processing performance of the material, especially for the tungsten-rhenium alloy with low rhenium content.
In the high-performance tungsten alloy bar, as a preferred embodiment, the carbide is one or more of HfC, TiC, ZrC and TaC; more preferably, the content of the carbide in the high-performance tungsten alloy bar is 0.3-1.5% by mass.
In the high-performance tungsten alloy bar, the principle of design of each component is as follows:
tungsten, a matrix for the alloy.
Rhenium, the purpose of introducing rhenium into tungsten is to utilize the "rhenium effect", the invention limits the rhenium content to 10-26 wt%, if the rhenium content is too high, W will be formed2Re3The second phase brings difficulty to the pressure processing, mechanical processing and heat treatment of the tungsten-rhenium alloy, and has obvious adverse effect on the material performance; if the rhenium alloy is too low, the rhenium effect is reduced.
The high-melting-point carbide is introduced, so that the high-melting-point carbide is used for dispersion strengthening, and the high-temperature strength of a tungsten matrix is improved, the content of the carbide is limited to 0.3-3 wt%, the dispersion strengthening effect is poor when the content of the carbide is too low, and a large amount of carbide in a crystal boundary can be caused when the content of the carbide is too high, so that the performance of the material is seriously influenced; the carbide content is preferably controlled to 0.3 to 1.5 wt%.
The preparation method of the high-performance tungsten alloy bar sequentially comprises the following steps:
step one, preparing tungsten-rhenium prealloying powder: respectively weighing a tungsten source and a rhenium source according to the component proportion of the high-performance tungsten alloy bar, and pretreating to obtain tungsten-rhenium pre-alloy powder;
step two, preparing tungsten alloy powder: respectively weighing high-melting-point carbide powder and the tungsten-rhenium pre-alloy powder according to the component proportion of the high-performance tungsten alloy bar, and mixing to obtain tungsten alloy powder;
step three, forming treatment: filling the tungsten alloy powder into a designed die cavity according to the designed weight for forming treatment to obtain a formed blank;
step four, sintering treatment: sintering the formed blank in a reducing atmosphere, inert gas or vacuum condition to obtain a sintered blank;
step five, rolling deformation treatment: carrying out rolling deformation treatment on the sintered blank obtained in the step four to obtain a rolled bar blank;
step six, heat treatment: and carrying out annealing heat treatment on the rolled bar billet obtained in the fifth step to obtain the high-performance tungsten-rhenium alloy bar.
The preparation method of the invention has the technical principle that: on one hand, tungsten powder or doped tungsten powder and ammonium rhenate powder are mixed, and proper reduction process is adopted to prepare tungsten-rhenium pre-alloy powder with special proportion; on the other hand, the high-temperature mechanical property of the alloy is further improved by introducing a high-melting-point carbide dispersion particle reinforced phase; and in the third aspect, the single-fire large-deformation densification treatment of the alloy is realized by a continuous rolling deformation processing process, and compared with a free forging process, the method has the advantages of fine grains, high density and high qualification rate.
In the above preparation method, as a preferred embodiment, the preparation method further includes a machining step of machining the heat-treated high-performance tungsten-rhenium alloy bar to obtain a finished high-performance tungsten-rhenium alloy bar.
In the above preparation method, as a preferred embodiment, the tungsten source is tungsten powder or doped tungsten powder, the rhenium source is ammonium rhenate powder or rhenium powder, the rhenium source is preferably ammonium rhenate, and the ammonium rhenate is used as a rhenium source, so that the prepared tungsten-rhenium pre-alloy powder is more uniform and consistent; the rhenium powder can also be directly used as a source for directly mixing materials, but the uniformity of the powder is not as good as that of the reduction process of the tungsten powder doped with ammonium rhenate, and the purity of the tungsten powder or the tungsten powder doped with the ammonium rhenate and the tungsten powder meets the national standard. Further preferably, the Fisher-Tropsch particle size of the tungsten source is 2.0-5.0 μm (such as 2.2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm, 4.8 μm). The doped tungsten powder is tungsten powder doped with Si, Al and K, and the purity of tungsten in the doped tungsten powder is more than or equal to 99.4%; preferably, by mass percent, Si: 0.015-0.035%, Al: 0.003-0.01%, K: 0.006-0.016%, and the balance of tungsten.
In the above production method, as a preferred embodiment, in the first step, when the rhenium source is ammonium rhenate powder, the pretreatment includes a mixing treatment and a reduction treatment in this order; more preferably, the mixing time of the mixing treatment is 0.5-3h (such as 0.6h, 0.8h, 1.2h, 1.5h, 2h, 2.5h, 2.8h), and the rotation speed is 10-25r/min (such as 12r/min, 15r/min, 18r/min, 20r/min, 23 r/min); further preferably, the reduction treatment sequentially comprises: carrying out primary hydrogen reduction treatment, mixing and secondary hydrogen reduction treatment; wherein the first hydrogen reduction treatment is carried out at 300-500 deg.C (such as 305 deg.C, 310 deg.C, 330 deg.C, 360 deg.C, 400 deg.C, 430 deg.C, 450 deg.C, 470 deg.C, 485 deg.C, 495 deg.C) for 20-60min (such as 22min, 25min, 30min, 40min, 50min, 55min, 58 min); the temperature of the second hydrogen reduction treatment is 700-900 ℃ (such as 705 ℃, 715 ℃, 730 ℃, 750 ℃, 780 ℃, 820 ℃, 850 ℃, 880 ℃, 890 ℃ and 895 ℃) and the time is 20-60min (such as 22min, 25min, 30min, 40min, 50min, 55min and 58 min); further preferably, in the first hydrogen reduction treatment and the second hydrogen reduction treatment, the hydrogen flow rate is 3-10L/min. The tungsten-rhenium pre-alloy powder prepared by adopting the multi-step reduction process is more beneficial to improving the uniformity of the powder.
In the preparation method, for feasibility of subsequent processes, as a preferred embodiment, the particle size of the ammonium rhenate powder is-150 to-400 meshes; the Fisher particle size of the rhenium powder is-150 to-400 meshes. When the raw material powder is too fine, the moldability is poor, and when it is too coarse, the sintered density is low.
In the above preparation method, as a preferred embodiment, when the rhenium source is rhenium powder, the pretreatment is a mixing treatment; more preferably, the mixing time of the mixing treatment is 0.5-3h (such as 0.6h, 0.8h, 1.2h, 1.5h, 2h, 2.5h, 2.8h), and the rotation speed is 10-25r/min (such as 12r/min, 15r/min, 18r/min, 20r/min, 23 r/min).
In the above production method, as a preferred embodiment, when the rhenium source is rhenium powder, the first and second steps are replaced by a mixing step including: mixing the tungsten source, the rhenium powder and the high-melting-point carbide powder together for 1-4h (such as 1.2h, 1.5h, 2h, 2.5h, 3h, 3.5h and 3.8h) at a rotation speed of 10-25r/min (such as 12r/min, 15r/min, 18r/min, 20r/min and 23 r/min).
In the above production method, as a preferred embodiment, in the second step, the carbide may be one or more of HfC, TiC, ZrC, TaC, and the like; in the second step, the mass fraction of the high-melting-point carbide is 0.3-3%, namely the addition amount of the high-melting-point carbide is 0.3-3% of the mass of the tungsten alloy powder (namely the mass sum of the high-melting-point carbide powder and the tungsten-rhenium pre-alloy powder); further preferably, the carbide powder has a grain size of-150 to-400 meshes and a purity of more than 99.5%.
In the above preparation method, as a preferred embodiment, in the second step, the mixing treatment may be performed to a degree that the mixture is uniform; more preferably, the mixing process is carried out by a double motion mixer with a mixing time of 4-8h (e.g. 4.2h, 4.5h, 5h, 6h, 7h, 7.5h, 7.8h) and a rotation speed of 10-30r/min (e.g. 12r/min, 14r/min, 16r/min, 18r/min, 20r/min, 23r/min, 26r/min, 28 r/min).
In the above manufacturing method, as a preferred embodiment, in the third step, the forming process is a cold isostatic pressing process; more preferably, the cold isostatic pressing treatment has a pressing pressure of 150 to 250MPa (e.g., 155MPa, 165MPa, 180MPa, 200MPa, 220MPa, 240MPa), a dwell time of 0 to 30s (e.g., 2s, 5s, 10s, 15s, 20s, 25s, 28s), and when the pressure is too low, the forming cannot be performed, and when the pressure is too high, cracks are likely to occur; preferably, the relative density of the molded blank is 55-65% (such as 56%, 58%, 60%, 62%, 64%), and the relative density of the molded blank is not too high, otherwise, the subsequent sintering process is not favorable for exhausting and removing impurities.
In the above production method, as a preferred embodiment, in the fourth step, the sintering treatment is performed in a reducing atmosphere, and the sintering treatment may be performed under an inert gas or vacuum condition, but the exhaust gas impurity removal effect is not as good as that in the reducing atmosphere; more preferably, the sintering treatment is carried out in a hydrogen atmosphere, wherein the hydrogen has the functions of reduction, degassing and impurity removal, and moreover, the sintering hydrogen also has the functions of protection and workpiece oxidation prevention, and the hydrogen is cheap and widely used; further preferably, the flow rate of the hydrogen is 20-60L/min (such as 22L/min, 25L/min, 30L/min, 35L/min, 40L/min, 45L/min, 50L/min, 55L/min, 58L/min).
In the above preparation method, as a preferred embodiment, in step four, in the sintering treatment, the sintering temperature is 2000-2350 ℃ (such as 2020 ℃, 2050 ℃, 2100 ℃, 2150 ℃, 2200 ℃, 2250 ℃, 2300 ℃, 2330 ℃), and the holding time is 3-6 h (such as 3.2h, 3.5h, 4h, 4.5h, 5h, 5.5h, 5.8 h); preferably, the relative density of the sintered blank is more than or equal to 90 percent, namely the density of the sintered blank reaches more than 90 percent of the theoretical density. In the step, if the sintering temperature is too low, the density of the sintered blank is insufficient, deformation processing is not facilitated, crystal grains are easy to grow up and the cost of the product is increased greatly.
In the above preparation method, as a preferred embodiment, the rolling deformation treatment in the fifth step sequentially includes a heating treatment and a rolling treatment, the heating temperature of the heating treatment is 1400 to 1650 ℃ (such as 1420 ℃, 1450 ℃, 1500 ℃, 1550 ℃, 1600 ℃, 1630 ℃), and the holding time is 20 to 60min (such as 25min, 30min, 40min, 50min, 55 min); during rolling treatment, the initial rolling temperature is the heating temperature of the heating treatment, the rolling speed is 1-2.5 m/s (such as 1.2m/s, 1.5m/s, 1.8m/s, 2m/s and 2.3m/s), the rolling pass is 5-12 passes (such as 6 passes, 7 passes, 8 passes, 9 passes, 10 passes and 11 passes), and the total rolling deformation is not less than 60%. The pass deformation is moderate, and if the pass deformation is too large, the deformation resistance is increased, so that the bar material is clamped in the roller, the smooth rolling cannot be realized, or the blank is torn; preferably, the first pass deformation is 30-40% (e.g., 32%, 34%, 36%, 38%), the last pass deformation is 8-12% (e.g., 9%, 10%, 11%), and the intermediate pass deformation is gradually reduced; more preferably, the first pass deformation is 34-36%, the last pass deformation is 10%, and the intermediate pass deformation is gradually reduced. The deformation in the application refers to the deformation of the cross section area of the bar, namely: the deformation amount is (cross-sectional area before rolling-sectional area after rolling)/cross-sectional area before rolling. The main purpose of continuous rolling is to refine the grains, reduce the number of thermal cycles in deformation processing and avoid the occurrence of recrystallization behavior in processing.
In the above preparation method, as a preferred embodiment, in the annealing heat treatment in the sixth step, the annealing temperature is 900 to 1300 ℃ (such as 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1280 ℃), and the heat preservation time is 30 to 120min (such as 35min, 50min, 60min, 80min, 90min, 100min, 110min, 115 min). The annealing heat treatment mainly aims at removing internal stress caused by rolling deformation, the stress can not be eliminated when the temperature is too low, and crystal grain growth is easy to occur when the temperature is too high.
Compared with the prior art, the invention has the following beneficial effects:
1) the tungsten alloy provided by the invention has the excellent performances of fine grains, uniform structure, lower content of impurity elements, high compactness, high strength, high temperature creep resistance and the like;
2) on one hand, the preparation method of the invention further improves the high-temperature mechanical property of the alloy by introducing the high-melting-point carbide dispersion particle reinforced phase; on the other hand, the tungsten powder and the rhenium ammonium acid powder are preferably mixed and reduced to prepare the tungsten-rhenium pre-alloy powder, so that the uniform mixing of the powder is realized; and in the third aspect, the single-fire large-deformation densification treatment of the alloy is realized through a continuous rolling deformation processing technology, and the effects of fine grains, high density and uniform and consistent tissue are realized. The tungsten alloy material prepared by the preparation method provided by the invention has fine and uniform crystal grains, the room-temperature tensile strength is more than or equal to 1500MPa, the elongation after fracture is more than or equal to 15%, the 2000 ℃ tensile strength is more than or equal to 200MPa, and the elongation after fracture is more than or equal to 15%.
Drawings
FIG. 1 is a cross-sectional metallographic structure photograph of a high-performance tungsten alloy bar prepared by the preparation method provided by the invention;
FIG. 2 is a longitudinal section metallographic structure photograph of a high-performance tungsten alloy bar prepared by the preparation method provided by the invention.
Detailed Description
The tungsten alloy rods and the preparation method thereof according to the present invention will be described with reference to the accompanying drawings and examples. It should be understood that these examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. It should be understood that various changes and modifications can be made by those skilled in the art after reading the disclosure of the present invention, and equivalents fall within the scope of the appended claims.
The starting materials used in the following examples are all commercially available.
Example 1
(1) Preparation of tungsten-rhenium prealloyed powder: weighing 39000g of tungsten powder with the Fisher particle size of 3.0 mu m and the purity of 99.95 percent and 14400g of ammonium rhenate powder with the purity of 99.99 percent and sieved by a 200-mesh sieve after grinding respectively, and then adding the ammonium rhenate powder into a mixer filled with the tungsten powder for mixing at the rotating speed of 20r/min for 1 hour; after being mixed evenly, the mixture is subjected to first hydrogen reduction treatment, namely, the mixture reacts for 40min at the temperature of 420 ℃; then carrying out second hydrogen reduction treatment, namely reacting for 35min at 850 ℃; in the hydrogen reduction treatment process, the hydrogen flow is 7L/min. After the reduction reaction was complete, 49000g of rhenium-tungsten prealloy powder was obtained.
(2) Preparing tungsten alloy powder: weighing 1000g of HfC powder with the granularity of-200 meshes and the purity of 99.6 percent; the powder and tungsten-rhenium pre-alloy powder are uniformly mixed in a double-motion mixer for 8 hours at the rotating speed of 30r/min to obtain 50000g of tungsten alloy powder (namely W-20 Re-2 HfC).
(3) Cold isostatic pressing: firstly, 50000g of the tungsten alloy powder prepared in the step (2) is placed into a die, and then the pressure is maintained for 20s under the pressure of 200MPa to obtain a formed blank with the relative density of 60%.
(4) And (3) high-temperature sintering: and (4) placing the formed blank obtained in the step (3) into a medium-frequency high-temperature hydrogen sintering furnace for sintering, wherein the sintering maximum temperature is 2350 ℃, and the heat preservation is carried out for 6 hours at the maximum temperature, so as to obtain a sintered blank with the relative density of 93% and the diameter of 85 mm.
(5) Rolling deformation processing: and (3) carrying out rolling deformation processing on the sintered blank obtained in the step (4), wherein the heating temperature is 1600 ℃, the heat preservation time is 60min, then carrying out 6-pass continuous rolling to obtain a rolled blank with the diameter of 40mm, the rolling speed is 2m/s, the first-pass deformation is 35%, the last-pass deformation is 10%, and the intermediate-pass deformation is gradually reduced.
(6) Annealing heat treatment: and (4) placing the rolled blank obtained in the step (5) in a hydrogen protection heating furnace for annealing heat treatment, wherein the annealing temperature is 1100 ℃, and the temperature is kept for 60 min.
(7) And (3) machining: and (4) machining the bar blank obtained in the step (6), and turning off oxide skin on the surface to obtain the required high-performance tungsten alloy bar.
Fig. 1 is a cross-sectional metallographic structure photograph of the high-performance tungsten alloy bar prepared in this example, and fig. 2 is a longitudinal-sectional metallographic structure photograph of the high-performance tungsten alloy bar prepared in this example, and it can be seen from the photographs that the tungsten-rhenium layer has fine and uniform grains and forms an obvious fibrous structure in the longitudinal direction. After a tensile test (the room temperature tensile test is carried out according to GB/T228.1-2010 part 1 room temperature test method of the metal material tensile test), and the high temperature tensile test is carried out according to GB/T4338-2006 part 1 high temperature tensile test method), the room temperature tensile strength reaches 1620MPa, and the elongation after fracture is 16%; the high-temperature strength at 2000 ℃ reaches 220MPa, and the elongation after fracture is 20%.
Example 2
(1) Preparation of tungsten-rhenium prealloyed powder: respectively weighing 16900g of doped tungsten powder (0.035 wt% of Si, 0.008 wt% of Al, 0.007 wt% of K and the balance of tungsten) with a Fisher particle size of 4.0 μm and a purity of 99.95% and 4320g of ammonium rhenate powder with a purity of 99.99% and sieved by a 200-mesh sieve after grinding, adding the ammonium rhenate powder into a mixer filled with the tungsten powder for mixing at a rotation speed of 15r/min for 1 hour; after being uniformly mixed, the mixture is subjected to first hydrogen reduction treatment, namely reaction at 400 ℃ for 35min, and then subjected to second hydrogen reduction treatment, namely reaction at 800 ℃ for 45 min; in the hydrogen reduction treatment process, the hydrogen flow is 6L/min. After the reduction was complete, 19900g of rhenium tungsten prealloy powder were obtained.
(2) Preparing tungsten alloy powder: weighing 100g of ZrC powder with the granularity of-300 meshes and the purity of 99.6 percent; the powder and the tungsten-rhenium pre-alloy powder are evenly mixed in a double-motion mixer for 4 hours at the rotating speed of 20r/min to obtain 20000g of tungsten alloy powder (namely W-15 Re-0.5 ZrC).
(3) Cold isostatic pressing: 20000g of the tungsten alloy powder prepared in the step (2) is placed in a die, and then the pressure is maintained for 10s under the pressure of 250MPa to obtain a formed blank with the relative density of 65%.
(4) And (3) high-temperature sintering: and (4) placing the formed blank obtained in the step (3) into a medium-frequency high-temperature hydrogen sintering furnace for sintering, wherein the sintering maximum temperature is 2200 ℃, and the heat preservation is carried out for 5 hours at the maximum temperature, so that a sintered blank with the relative density of 92% and the diameter of 40mm is obtained.
(5) Rolling deformation processing: and (3) carrying out rolling deformation processing on the sintered blank obtained in the step (4), wherein the heating temperature is 1500 ℃, the heat preservation time is 30min, and then carrying out 6-pass continuous rolling to obtain a rolled blank with the diameter of 20mm, wherein the rolling speed is 1.8m/s, the deformation of the first pass is 32%, the deformation of the last pass is 12%, and the deformation of the middle pass is gradually reduced.
(6) Annealing heat treatment: and (4) placing the rolled blank obtained in the step (5) in a hydrogen protection heating furnace for annealing heat treatment, wherein the annealing temperature is 1300 ℃, and the heat preservation time is 40 min.
(7) And (3) machining: and (4) machining the bar blank obtained in the step (6), and turning off oxide skin on the surface to obtain the required high-performance tungsten alloy bar.
The metallographic structure of the tungsten alloy rods prepared in this example was similar to that of the rods prepared in example 1. Through a tensile test, the room-temperature tensile strength reaches 1520MPa, and the elongation after fracture is 19 percent; the high-temperature strength at 2000 ℃ reaches 225MPa, and the elongation after fracture is 20%.
Example 3
(1) Preparation of tungsten-rhenium prealloyed powder: 22200g of tungsten powder with the Fisher particle size of 3.3 mu m and the purity of 99.95 percent and 10800g of ammonium rhenate powder with the purity of 99.99 percent, which is ground and sieved by a 200-mesh sieve, are respectively weighed, and then the ammonium rhenate powder is added into a mixer filled with the tungsten powder to be mixed, the rotating speed is 25r/min, and the mixing time is 2 hours; after being uniformly mixed, the mixture is subjected to first hydrogen reduction treatment, namely reaction at 450 ℃ for 45min, and then subjected to second hydrogen reduction treatment, namely reaction at 750 ℃ for 35 min; in the hydrogen reduction treatment process, the hydrogen flow is 10L/min. After the reduction reaction was completed, 29700g of rhenium-tungsten prealloy powder was obtained.
(2) Preparing tungsten alloy powder: weighing 300g of TaC powder with the granularity of-200 meshes and the purity of 99.6 percent; the powder and tungsten-rhenium pre-alloy powder are uniformly mixed in a double-motion mixer for 6 hours at a rotating speed of 15r/min to obtain 30000g of tungsten alloy powder (namely W-25 Re-1 TaC).
(3) Cold isostatic pressing: 30000g of the tungsten alloy powder prepared in the step (2) is placed into a die, and then the pressure is maintained for 20 seconds under the pressure of 180MPa, so that a formed blank with the relative density of 62% is obtained.
(4) And (3) high-temperature sintering: and (4) placing the formed blank obtained in the step (3) into a medium-frequency high-temperature hydrogen sintering furnace for sintering, wherein the sintering highest temperature is 2300 ℃, and the heat preservation is carried out for 6 hours at the highest temperature, so as to obtain a sintered blank with the relative density of 95% and the diameter of 65 mm.
(5) Rolling deformation processing: and (4) carrying out rolling deformation processing on the sintered blank obtained in the step (4), wherein the heating temperature is 1550 ℃, the heat preservation time is 60min, then carrying out 8-pass continuous rolling to obtain a rolled blank with the diameter of 30mm, the rolling speed is 1.5m/s, the first-pass deformation is 38%, the last-pass deformation is 8%, and the intermediate-pass deformation is gradually reduced.
(6) Annealing heat treatment: and (4) placing the rolled blank obtained in the step (5) in a hydrogen protection heating furnace for annealing heat treatment, wherein the annealing temperature is 1200 ℃, and the heat preservation time is 60 min.
(7) And (3) machining: and (4) machining the bar blank obtained in the step (6), and turning off oxide skin on the surface to obtain the required high-performance tungsten alloy bar.
The metallographic structure of the tungsten alloy rods prepared in this example was similar to that of the rods prepared in example 1. Through a tensile test, the tensile strength at room temperature reaches 1650MPa, and the elongation after fracture reaches 21 percent; the strength at 2000 ℃ reaches 235MPa, and the elongation after fracture is 18%.
Example 4
(1) Preparation of tungsten-rhenium prealloyed powder: 13125g of doped tungsten powder (namely 0.025 wt% of Si, 0.015 wt% of Al, 0.015 wt% of K and the balance of W) with the Fisher particle size of 4.5 mu m and the purity of 99.95% and 2160g of ammonium rhenate powder with the purity of 99.99% and sieved by a 200-mesh sieve after grinding are respectively weighed, and then the ammonium rhenate powder is added into a mixer filled with the tungsten powder for mixing at the rotation speed of 25r/min for 1 hour; after being uniformly mixed, the mixture is subjected to first hydrogen reduction treatment, namely reaction at 400 ℃ for 50min, and then subjected to second hydrogen reduction treatment, namely reaction at 850 ℃ for 40 min; in the hydrogen reduction treatment process, the hydrogen flow is 3L/min. After the reduction was complete, 14625g of rhenium tungsten prealloy powder were obtained.
(2) Preparing tungsten alloy powder: weighing 375g of TiC powder with the granularity of-200 meshes and the purity of 99.6 percent; the powder and tungsten-rhenium pre-alloy powder are mixed evenly in a double-motion mixer for 5 hours at a rotating speed of 20r/min, and 15000g of tungsten alloy powder (namely W-10 Re-2.5 TiC) is obtained.
(3) Cold isostatic pressing: firstly, 15000g of the tungsten alloy powder prepared in the step (2) is put into a die, and then the pressure is maintained for 10s under the pressure of 200MPa, so that a formed blank with the relative density of 65 percent is obtained.
(4) And (3) high-temperature sintering: and (4) placing the formed blank obtained in the step (3) into a medium-frequency high-temperature hydrogen sintering furnace for sintering, wherein the highest sintering temperature is 2320 ℃, and the temperature is kept at the highest temperature for 6 hours to obtain a sintered blank with the relative density of 95% and the diameter of 35 mm.
(5) Rolling deformation processing: and (4) carrying out rolling deformation processing on the sintered blank obtained in the step (4), wherein the heating temperature is 1500 ℃, the heat preservation time is 40min, then carrying out 8-pass continuous rolling to obtain a rolled blank with the diameter of 15mm, the rolling speed is 2.2m/s, the deformation of the first pass is 30%, the deformation of the last pass is 8%, and the deformation of the middle pass is gradually reduced.
(6) Annealing heat treatment: and (4) placing the rolled blank obtained in the step (5) in a hydrogen protection heating furnace for annealing heat treatment, wherein the annealing temperature is 1100 ℃, and the temperature is kept for 50 min.
(7) And (3) machining: and (4) machining the bar blank obtained in the step (6), and turning off oxide skin on the surface to obtain the required high-performance tungsten alloy bar.
The metallographic structure of the tungsten alloy rods prepared in this example was similar to that of the rods prepared in example 1. Through a tensile test, the tensile strength at room temperature reaches 1510MPa, and the elongation after fracture is 17 percent; the high-temperature strength at 2000 ℃ reaches 225MPa, and the elongation after fracture is 16%.
Example 5
(1) Preparation of tungsten-rhenium prealloyed powder: 7850g of tungsten powder with the Fisher particle size of 2.6 mu m and the purity of 99.95 percent and 2880g of ammonium rhenate powder with the purity of 99.99 percent, which is ground and sieved by a 200-mesh sieve, are respectively weighed, and then the ammonium rhenate powder is added into a mixer filled with the tungsten powder to be mixed at the rotating speed of 20r/min for 2 hours; after being uniformly mixed, the mixture is subjected to first hydrogen reduction treatment, namely reaction at 450 ℃ for 60min, and then subjected to second hydrogen reduction treatment, namely reaction at 800 ℃ for 40 min; in the hydrogen reduction treatment process, the hydrogen flow is 5L/min. After the reduction reaction was completed, 9850g of rhenium-tungsten prealloy powder was obtained.
(2) Preparing tungsten alloy powder: weighing 150g of HfC powder with the granularity of-300 meshes and the purity of 99.6 percent; the powder and tungsten-rhenium pre-alloy powder are uniformly mixed in a double-motion mixer for 6 hours at the rotating speed of 25r/min to obtain 10000g of tungsten alloy powder (namely W-20 Re-1.5 HfC).
(3) Cold isostatic pressing: firstly, 10000g of tungsten alloy powder prepared in the step (2) is put into a die, and then the pressure is maintained for 15s under the pressure of 200MPa to obtain a formed blank with the relative density of 65 percent.
(4) And (3) high-temperature sintering: and (4) placing the formed blank obtained in the step (3) into a medium-frequency high-temperature hydrogen sintering furnace for sintering, wherein the sintering highest temperature is 2300 ℃, and the heat preservation is carried out for 4 hours at the highest temperature, so as to obtain a sintered blank with the relative density of 95% and the diameter of 30 mm.
(5) Rolling deformation processing: and (3) carrying out rolling deformation processing on the sintered blank obtained in the step (4), wherein the heating temperature is 1450 ℃, the heat preservation time is 40min, then carrying out 8-pass continuous rolling to obtain a rolled blank with the diameter of 15mm, the rolling speed is 2m/s, the deformation of the first pass is 35%, the deformation of the last pass is 10%, and the deformation of the middle pass is gradually reduced.
(6) Annealing heat treatment: and (4) placing the rolled blank obtained in the step (5) in a hydrogen protection heating furnace for annealing heat treatment, wherein the annealing temperature is 1000 ℃, and the heat preservation time is 90 min.
(7) And (3) machining: and (4) machining the bar blank obtained in the step (6), and turning off oxide skin on the surface to obtain the required high-performance tungsten alloy bar.
The metallographic structure of the tungsten alloy rods prepared in this example was similar to that of the rods prepared in example 1. Through a tensile test, the tensile strength at room temperature reaches 1650MPa, and the elongation after fracture reaches 21 percent; the high-temperature strength at 2000 ℃ reaches 230MPa, and the elongation after fracture is 18 percent.
Examples 6 to 13
The processes and parameters of examples 6 to 13 were the same as those of example 5, except that the rolling deformation process was different from that of example 5. The rolling deformation process of examples 6-13 is shown in Table 1, and the properties of the bars prepared in examples 6-13 are shown in Table 2.
TABLE 1 Rolling deformation Process conditions for examples 6-13
Table 2 properties of bars prepared in examples 6-13
Claims (25)
1. The high-performance tungsten alloy bar is characterized by comprising the following components in percentage by mass: 10-26% of rhenium, 0.3-3% of carbide and the balance of tungsten;
the preparation method of the high-performance tungsten alloy bar sequentially comprises the following steps:
step one, preparing tungsten-rhenium prealloying powder: respectively weighing a tungsten source and a rhenium source according to the component ratio of the tungsten alloy bar, and pretreating to obtain tungsten-rhenium pre-alloy powder;
step two, preparing tungsten alloy powder: respectively weighing high-melting-point carbide powder and the tungsten-rhenium pre-alloy powder according to the component proportion of the tungsten alloy bar, and mixing to obtain tungsten alloy powder;
step three, forming treatment: filling the tungsten alloy powder obtained in the step two into a designed die cavity according to the designed weight for forming treatment to obtain a formed blank;
step four, sintering treatment: sintering the formed blank obtained in the step three in a reducing atmosphere, inert gas or vacuum condition to obtain a sintered blank;
step five, rolling deformation treatment: carrying out rolling deformation treatment on the sintered blank obtained in the step four to obtain a rolled bar blank; the rolling deformation treatment sequentially comprises heating treatment and rolling treatment, wherein the heating temperature of the heating treatment is 1400-1650 ℃, and the heat preservation time is 20-60 min; during the rolling treatment, the total rolling deformation is not less than 60%; the first pass deformation is 30-40%, the last pass deformation is 8-12%, the intermediate pass deformation is gradually reduced, and the rolling speed is 1-2.5 m/s;
step six, heat treatment: annealing heat treatment is carried out on the rolled bar billet obtained in the fifth step, so that the high-performance tungsten-rhenium alloy bar is obtained; the annealing temperature of the annealing heat treatment is 900-1300 ℃, and the heat preservation time is 30-120 min.
2. The high performance tungsten alloy rod according to claim 1, wherein the tungsten is replaced by doped tungsten.
3. The high performance tungsten alloy rod according to claim 2, wherein the doped tungsten consists of the following components in mass percent: 0.015-0.035% of Si, 0.003-0.01% of Al, 0.006-0.016% of K and the balance of tungsten.
4. The high performance tungsten alloy rod according to any one of claims 1 to 3, wherein the carbide is one or more of HfC, TiC, ZrC, TaC.
5. The high-performance tungsten alloy rod according to any one of claims 1 to 3, wherein the carbide is contained in the high-performance tungsten alloy rod in an amount of 0.3 to 1.5% by mass.
6. The high-performance tungsten alloy bar according to claim 1, wherein the tungsten source is tungsten powder or doped tungsten powder, and the rhenium source is ammonium rhenate powder or rhenium powder; the doped tungsten powder is tungsten powder doped with Si, Al and K, and the purity of tungsten in the doped tungsten powder is more than or equal to 99.4%.
7. The high performance tungsten alloy rod according to claim 6, wherein the Si: 0.015-0.035%, Al: 0.003-0.01%, K: 0.006-0.016%, and the balance of tungsten.
8. The high performance tungsten alloy rod of claim 6, wherein the rhenium source is ammonium rhenate.
9. The high performance tungsten alloy rod according to claim 8, wherein the tungsten source has a Fisher size of 2.0 to 5.0 μm; the particle size of the ammonium rhenate powder is-150 to-400 meshes; the Fisher particle size of the rhenium powder is-150 to-400 meshes.
10. The high performance tungsten alloy rod according to claim 1 or 6,
when the rhenium source is ammonium rhenate powder, the pretreatment sequentially comprises mixing treatment and reduction treatment.
11. The high performance tungsten alloy rod according to claim 10, wherein the mixing time of the mixing process in the pre-treatment is 0.5 to 3 hours and the rotation speed is 10 to 25 r/min.
12. The high performance tungsten alloy rod according to claim 10, wherein the reduction treatment comprises in sequence: carrying out primary hydrogen reduction treatment, mixing and secondary hydrogen reduction treatment; wherein the temperature of the first hydrogen reduction treatment is 300-500 ℃, and the time is 20-60 min; the temperature of the second hydrogen reduction treatment is 700-900 ℃, and the time is 20-60 min.
13. The high-performance tungsten alloy bar according to claim 12, wherein the hydrogen flow rate in the first hydrogen reduction treatment and the second hydrogen reduction treatment is 3-10L/min.
14. The high-performance tungsten alloy bar according to claim 1 or 6, wherein when the rhenium source is rhenium powder, the pretreatment is a mixing treatment, the mixing time of the mixing treatment is 0.5-3h, and the rotating speed is 10-25 r/min; alternatively, the first and second electrodes may be,
and when the rhenium source is rhenium powder, combining the first step and the second step into a mixing step, directly mixing the tungsten source, the rhenium powder and the high-melting-point carbide powder together, wherein the mixing time is 1-4h, and the rotating speed is 10-25 r/min.
15. The high performance tungsten alloy rod according to claim 1 or 6, wherein the carbide powder has a particle size of-150 to-400 mesh and a purity of greater than 99.5%.
16. The high-performance tungsten alloy bar according to claim 1 or 6, wherein in the second step, the mixing treatment is performed by a double-motion mixer, the mixing time is 4-8h, and the rotating speed is 10-30 r/min.
17. The high performance tungsten alloy rod according to claim 1 or 6, wherein the forming process is a cold isostatic pressing process in step three.
18. The high-performance tungsten alloy rod according to claim 17, wherein the cold isostatic pressing treatment has a pressing pressure of 150 to 250MPa and a dwell time of 0 to 30 s.
19. The high performance tungsten alloy rod according to claim 17, wherein the shaped billet has a relative density of 55 to 65%.
20. The high-performance tungsten alloy rod according to claim 1 or 6, wherein in step four, the sintering treatment is performed in a hydrogen atmosphere.
21. The high-performance tungsten alloy rod according to claim 20, wherein the flow rate of the hydrogen gas is 20 to 60L/min.
22. The high-performance tungsten alloy bar according to claim 1 or 6, wherein in the fourth step, the sintering temperature is 2000-2350 ℃, and the holding time is 3-6 h.
23. The high performance tungsten alloy rod according to claim 22, wherein the relative density of the sintered compact is 90% or more.
24. The high-performance tungsten alloy bar according to claim 1 or 6, wherein in the fifth step, the initial rolling temperature is the heating temperature of the heating treatment, and the rolling passes are 5-12.
25. The high performance tungsten alloy rod of claim 1, wherein the first pass deformation is 34-36%, the last pass deformation is 10%, and the intermediate pass deformation is gradually reduced.
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