CN112458329B - Method for preparing tungsten alloy with different components by sintering in same furnace - Google Patents
Method for preparing tungsten alloy with different components by sintering in same furnace Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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- C22C27/04—Alloys based on tungsten or molybdenum
Abstract
The invention discloses a method for preparing tungsten alloy with different components by sintering in the same furnace, which comprises the following steps: firstly, selecting fine tungsten powder and fine nickel powder, adding superfine iron powder, and mixing to obtain an activated high-tungsten mixture; secondly, selecting coarse tungsten powder and nickel powder, adding iron powder and mixing to obtain a passivated low-tungsten mixture; thirdly, respectively adopting cold isostatic pressing to perform pressing forming to obtain an activated high-tungsten green compact and a passivated low-tungsten green compact; and fourthly, sintering the activated high-tungsten compact and the passivated low-tungsten compact in the same furnace to respectively obtain the high-tungsten alloy and the low-tungsten alloy. According to the invention, through selection and design of raw material components and contents of the high-tungsten alloy and the low-tungsten alloy, the sintering temperature for activating the high-tungsten mixture is reduced, the sintering temperature for passivating the low-tungsten mixture is increased, the sintering temperature and the heat preservation time of the high-tungsten alloy and the low-tungsten alloy are converged, the purpose of sintering in the same furnace is realized, the sintering period of the tungsten alloys with different components is shortened, the production efficiency is improved, sintering conversion is not needed, and energy waste caused during sintering conversion is avoided.
Description
Technical Field
The invention belongs to the technical field of tungsten alloy material manufacturing, and particularly relates to a method for preparing tungsten alloys with different components by sintering in the same furnace.
Background
The tungsten alloy consists of a tungsten phase with a high melting point and a gamma phase (Ni-Cu and Ni-Fe) with a lower melting point, the melting points of the two phases are greatly different (the melting point of the tungsten phase is 3410 ℃, and the melting point of the gamma phase is lower), the tungsten alloy is usually sintered by adopting a liquid phase, and the sintering temperature and the heat preservation time must be strictly controlled in the sintering process. According to the equilibrium phase diagram of the W-Ni-Fe alloy, if the tungsten content in the alloy is higher, the sintering temperature is increased, and conversely, when the tungsten content is reduced, the sintering temperature is reduced, and when the conventional tungsten alloy is sintered and produced, the sintering temperature of 90WNiFe alloy is 1420 ℃, the heat preservation time is 35min, the sintering temperature of 93WNiFe alloy is 1465 ℃, the heat preservation time is 45min, the sintering temperature of 95WNiFe alloy is 1510 ℃, the heat preservation time is 60min, the sintering temperature of 97WNiFe alloy is 1580 ℃, and the heat preservation time is 70 min. Because the sintering temperature and the sintering heat preservation time of the tungsten alloy with different components are different, when the tungsten alloy with different components is sintered in a continuous molybdenum wire sintering furnace or a hydrogen introducing furnace, the sintering temperature and the heat preservation time (boat pushing speed) can be adjusted to sinter the tungsten alloy with the next component after the tungsten alloy with one component is discharged, the molybdenum wire sintering furnace needs at least 6 hours from feeding to discharging, the sintering time of each furnace of the hydrogen introducing furnace is 18-24 hours, the sintering conversion time is long, the tungsten alloy sintering production period is long, the sintering production efficiency is not high, the sintering capacity is restricted, and meanwhile, the energy waste is caused during the sintering conversion.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing tungsten alloy with different components by sintering in the same furnace aiming at the defects of the prior art. According to the method, through selection and design of raw material components and contents of the high-tungsten alloy and the low-tungsten alloy, the sintering temperature for activating the high-tungsten mixture is reduced, the sintering temperature for passivating the low-tungsten mixture is increased, the sintering temperature for preparing the tungsten alloys with different components is consistent with the heat preservation time, the purpose of sintering in the same furnace is achieved, the sintering period of the tungsten alloys with different components is shortened, the production efficiency is improved, sintering conversion is not needed, and energy waste caused by sintering conversion is avoided.
In order to solve the technical problems, the invention adopts the technical scheme that: the method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized by comprising the following steps of:
selecting fine tungsten powder and fine nickel powder with the particle size of 2.5-3.0 microns, adding superfine iron powder with the particle size of 3.3-4.3 microns, and mixing to obtain an activated high-tungsten mixture; the mass ratio of the fine nickel powder to the superfine iron powder in the activated high-tungsten mixture is (3-4): 1;
selecting coarse tungsten powder and nickel powder with the particle size of 5.0-6.0 microns, adding iron powder with the particle size of 6.6-8.0 microns, and mixing to obtain a passivated low-tungsten mixture; the mass ratio of nickel powder to iron powder in the passivated low-tungsten mixture is (2.33-2): 1;
the mass content of tungsten in the activated high-tungsten mixture in the first step is larger than that of tungsten in the passivated low-tungsten mixture in the second step;
step three, respectively carrying out cold isostatic pressing forming on the activated high-tungsten mixture obtained in the step one and the passivated low-tungsten mixture obtained in the step two to obtain an activated high-tungsten green compact and a passivated low-tungsten green compact;
and step four, simultaneously sending the activated high-tungsten green compact and the passivated low-tungsten green compact obtained in the step three into a continuous molybdenum wire sintering furnace or a hydrogen furnace for same-furnace sintering to respectively obtain high-tungsten alloy and low-tungsten alloy.
The invention adopts a powder metallurgy liquid phase sintering method to prepare tungsten alloy, firstly carries out activation design on the tungsten alloy with high tungsten content: the method comprises the steps of selecting fine-particle raw material powder to prepare an activated high-tungsten mixture, reducing the sintering temperature of the activated high-tungsten mixture by utilizing the characteristics that the finer the powder particles are, the more irregular the surface of the powder particles is, the larger the surface energy is, the higher the stored energy is, the higher the tendency of the powder particles to be converted into a low-energy state is, and the sintering is easier to carry out, increasing the content of nickel elements by improving the mass ratio of nickel powder to superfine iron powder in the activated high-tungsten mixture, effectively reducing the sintering temperature of the activated high-tungsten mixture, further enhancing the sintering activation performance of the activated high-tungsten mixture, and finally obtaining the activated high-tungsten mixture with reduced sintering temperature; then carrying out passivation design on the low-tungsten-content tungsten alloy: the method selects raw material powder with coarse particles to prepare the passivated low-tungsten mixture, utilizes the characteristics that the surface energy is smaller, the stored energy is lower and the required sintering temperature is higher when the powder particles are coarser, improves the sintering temperature of the passivated low-tungsten mixture, plays a role in passivating and sintering, and simultaneously reduces the content of nickel element by reducing the mass ratio of nickel powder to iron powder in the passivated low-tungsten mixture, effectively improves the sintering temperature of the passivated low-tungsten mixture, further reduces the sintering activation performance of the passivated low-tungsten mixture, improves the burning resistance of the passivated low-tungsten mixture, and obtains the passivated low-tungsten mixture with the improved sintering temperature.
According to the method, through the design of the components and the raw material granularity of different tungsten alloys, the activated high-tungsten mixture with the reduced sintering temperature and the passivated low-tungsten mixture with the improved sintering temperature are respectively prepared, so that the sintering temperature and the heat preservation time for preparing the tungsten alloys with different components converge, the purpose of sintering in the same furnace is realized, the sintering period of the tungsten alloys with different components is shortened, the production efficiency is improved, sintering conversion is not needed, and the waste of energy is avoided during the sintering conversion.
The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized in that in the step one, the activated high-tungsten mixture also contains cobalt powder, the granularity of the cobalt powder is 0.9-1.5 mu m, and the granularity of the fine nickel powder is 2.2-2.8 mu m. Preferably, the metal element cobalt is added, the characteristic that the metal cobalt, nickel and iron belong to the same transition group elements and have close properties is utilized, the wettability of the nickel-based solid solution to tungsten powder particles is effectively improved, and WNi is inhibited4The generation of intermetallic compounds further reduces the sintering temperature of the activated high-tungsten mixture; meanwhile, the cobalt element and ferronickel in the alloy are bonded and simultaneously act, so that the effect of synergistically strengthening sintering is achieved, and the strength and ductility of the high-tungsten alloy are greatly improved at a lower sintering temperature.
The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized in that the mass content of the fine tungsten powder in the activated high-tungsten mixture is 93-97%, and the mass content of the cobalt powder is 0.25-2%.
The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized in that the mass ratio of the fine nickel powder to the superfine iron powder is 4: 1. The activation high-tungsten mixture has higher nickel content under the mass ratio of the optimized nickel powder to the superfine iron powder, and effectively reduces the sintering temperature of the activation high-tungsten mixture.
The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized in that the particle size of the nickel powder in the second step is 3.0-3.6 mu m. The nickel powder with the optimal granularity has thicker particles, the activation sintering performance of the nickel is weakened, and the passivation sintering effect is achieved, so that the sintering temperature of the passivation low-tungsten mixture is increased.
The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized in that the mass content of the coarse tungsten powder in the passivated low-tungsten mixture in the step two is 90-95%.
The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized in that the mass ratio of the nickel powder to the iron powder in the passivated low-tungsten mixture in the step two is 2.33: 1. The nickel content in the passivated low-tungsten mixture is lower under the mass ratio of the optimized nickel powder to the iron powder, the activation sintering characteristic of nickel is weakened, and the sintering temperature of the passivated low-tungsten mixture is effectively reduced.
The method for preparing the tungsten alloy with different components by co-furnace sintering is characterized in that the co-furnace sintering temperature in the fourth step is 1440-1530 ℃, and the heat preservation time is 21-50 min. Compared with the conventional tungsten alloy liquid phase sintering, the optimized co-furnace sintering process parameter reduces the heat preservation time, avoids the excessive growth of tungsten crystal grains caused by the excessively fast growth rate of the crystal grains of fine particle raw materials of the high tungsten alloy, and simultaneously avoids the collapse and deformation caused by the excessively high sintering temperature of the low tungsten alloy, thereby not only ensuring that the higher tungsten alloy is not under-sintered, but also ensuring that the low tungsten alloy is not over-sintered, and ensuring that the performance of the high tungsten alloy and the performance of the low tungsten alloy can both meet the requirement of the standard of the tungsten-based high-density alloy B777-15.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the fine-particle raw material powder is selected and combined to improve the mass ratio of the nickel element to the iron element, so that the sintering temperature for activating the high-tungsten mixture is reduced, the coarse-particle raw material powder is selected and combined to reduce the mass ratio of the nickel element to the iron element, so that the sintering temperature for passivating the low-tungsten mixture is improved, the sintering temperature for preparing tungsten alloys with different components is consistent with the heat preservation time, the purpose of sintering in the same furnace is realized, the sintering period of the tungsten alloys with different components is shortened, the production efficiency is improved, sintering conversion is not needed, and the waste of energy sources during sintering conversion is avoided.
2. The invention adopts the same-furnace sintering, reduces the sintering heat preservation time of the high-tungsten alloy, effectively refines the crystal grains of the high-tungsten alloy, promotes the tissue homogenization, avoids the collapse deformation of the low-tungsten alloy during sintering and further effectively ensures the performances of the high-tungsten alloy and the low-tungsten alloy through the design of the components and the content of the alloy.
3. The method is simple, is suitable for the tungsten-nickel-iron alloy with different components, has strong practicability, can be carried out on a conventional continuous molybdenum wire sintering furnace and a hydrogen introducing furnace, and has lower requirements on sintering equipment.
The technical solution of the present invention is further described in detail by examples below.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, adding fine tungsten powder with the granularity of 3.0 mu m, superfine iron powder with the granularity of 4.3 mu m, fine nickel powder with the granularity of 2.8 mu m and cobalt powder with the granularity of 1.5 mu m into a mixer to be mixed to obtain an activated high-tungsten mixture; the mass content of the fine tungsten powder in the activated high-tungsten mixture is 93%, the mass content of the nickel powder is 4%, the mass content of the superfine iron powder is 1%, and the mass content of the cobalt powder is 2%;
step two, adding coarse tungsten powder with the granularity of 6.0 mu m, iron powder with the granularity of 8.0 mu m and nickel powder with the granularity of 3.6 mu m into a mixer to be mixed to obtain a passivated low-tungsten mixture; the mass content of the coarse tungsten powder in the passivated low-tungsten mixture is 90%, the mass content of the nickel powder is 7%, and the mass content of the iron powder is 3%;
step three, respectively filling the activated high-tungsten mixture obtained in the step one and the passivated low-tungsten mixture obtained in the step two into a latex sleeve, and performing cold isostatic pressing forming to obtain a 93WNiFe green compact and a 90WNiFe green compact;
step four, simultaneously feeding the 93WNiFe green compacts and the 90WNiFe green compacts obtained in the step three into a continuous molybdenum wire sintering furnace for sintering in the same furnace to respectively obtain 93WNiFe alloy and 90WNiFe alloy; the sintering temperature in the same furnace is 1440 ℃, the heat preservation time is 21min, and the boat pushing speed is 19 mm/min.
Example 2
The embodiment comprises the following steps:
step one, adding fine tungsten powder with the particle size of 2.8 microns, fine nickel powder with the particle size of 2.5 microns, superfine iron powder with the particle size of 4.0 microns and cobalt powder with the particle size of 1.2 microns into a mixer, and mixing to obtain an activated high-tungsten mixture; the mass content of the fine tungsten powder in the activated high-tungsten mixture is 95%, the mass content of the fine nickel powder is 3.56%, the mass content of the superfine iron powder is 1.19%, and the mass content of the cobalt powder is 0.25%;
step two, adding coarse tungsten powder with the particle size of 5.5 mu m, nickel powder with the particle size of 3.2 mu m and iron powder with the particle size of 7.0 mu m into a mixer, and mixing to obtain a passivated low-tungsten mixture; the mass content of the coarse tungsten powder in the passivated low-tungsten mixture is 93%, the mass content of the nickel powder is 4.67%, and the mass content of the iron powder is 2.33%;
step three, respectively filling the activated high-tungsten mixture obtained in the step one and the passivated low-tungsten mixture obtained in the step two into a latex sleeve, and performing cold isostatic pressing forming to obtain a 95WNiFe green compact and a 93WNiFe green compact;
step four, simultaneously feeding the 95WNiFe pressed blank and the 93WNiFe pressed blank obtained in the step three into a hydrogen furnace to be sintered in the same furnace, and respectively obtaining a 95WNiFe alloy and a 93WNiFe alloy; the sintering temperature in the same furnace is 1480 ℃, and the heat preservation time is 33 min.
Example 3
The embodiment comprises the following steps:
step one, adding fine tungsten powder with the particle size of 2.5 microns, fine nickel powder with the particle size of 2.2 microns, superfine iron powder with the particle size of 3.3 microns and cobalt powder with the particle size of 0.9 microns into a mixer to be mixed to obtain an activated high-tungsten mixture; the mass content of the fine tungsten powder in the activated high-tungsten mixture is 97%, the mass content of the fine nickel powder is 2.16%, the mass content of the superfine iron powder is 0.54%, and the mass content of the cobalt powder is 0.3%;
step two, adding coarse tungsten powder with the particle size of 5.0 mu m, nickel powder with the particle size of 3.0 mu m and iron powder with the particle size of 6.6 mu m into a mixer, and mixing to obtain a passivated low-tungsten mixture; the mass content of the coarse tungsten powder in the passivated low-tungsten mixture is 95%, the mass content of the nickel powder is 3.5%, and the mass content of the iron powder is 1.5%;
step three, respectively carrying out cold isostatic pressing forming on the activated high-tungsten mixture obtained in the step one and the passivated low-tungsten mixture obtained in the step two to obtain a 97WNiFe green compact and a 95WNiFe green compact;
step four, simultaneously feeding the 97WNiFe pressed compact and the 95WNiFe pressed compact obtained in the step three into a continuous molybdenum wire sintering furnace for sintering in the same furnace to respectively obtain a 97WNiFe alloy and a 95WNiFe alloy; the temperature of the same furnace sintering is 1530 ℃, the heat preservation time is 50min, and the boat pushing speed is 8 mm/min.
The tungsten alloys obtained in examples 1 to 3 of the present invention were subjected to performance testing, and the results are shown in table 1 below.
TABLE 1
As can be seen from table 1, the tungsten alloys obtained in embodiments 1 to 3 of the present invention all satisfy the requirements of the standard of tungsten-based high-density alloy B777-15 in terms of yield strength, tensile strength, elongation, hardness, and density, and are suitable for the production of conventional tungsten alloy products.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (6)
1. The method for preparing the tungsten alloy with different components by sintering in the same furnace is characterized by comprising the following steps of:
selecting fine tungsten powder and fine nickel powder with the particle size of 2.5-3.0 microns, adding superfine iron powder with the particle size of 3.3-4.3 microns, and mixing to obtain an activated high-tungsten mixture; the mass ratio of the fine nickel powder to the superfine iron powder in the activated high-tungsten mixture is (3-4): 1; the activated high-tungsten mixture also contains cobalt powder, the granularity of the cobalt powder is 0.9-1.5 mu m, and the granularity of the fine nickel powder is 2.2-2.8 mu m;
selecting coarse tungsten powder and nickel powder with the particle size of 5.0-6.0 microns, adding iron powder with the particle size of 6.6-8.0 microns, and mixing to obtain a passivated low-tungsten mixture; the mass ratio of nickel powder to iron powder in the passivated low-tungsten mixture is (2.33-2): 1;
the mass content of tungsten in the activated high-tungsten mixture in the first step is larger than that of tungsten in the passivated low-tungsten mixture in the second step; the particle size of the nickel powder is 3.0-3.6 mu m;
step three, respectively carrying out cold isostatic pressing forming on the activated high-tungsten mixture obtained in the step one and the passivated low-tungsten mixture obtained in the step two to obtain an activated high-tungsten green compact and a passivated low-tungsten green compact;
and step four, simultaneously sending the activated high-tungsten green compact and the passivated low-tungsten green compact obtained in the step three into a continuous molybdenum wire sintering furnace or a hydrogen furnace for same-furnace sintering to respectively obtain high-tungsten alloy and low-tungsten alloy.
2. The method for preparing the tungsten alloy with different components by sintering in the same furnace according to claim 1, wherein the mass content of the fine tungsten powder in the activated high-tungsten mixture is 93-97%, and the mass content of the cobalt powder is 0.25-2%.
3. The method for preparing the tungsten alloy with different components by sintering in the same furnace according to claim 1, wherein the mass ratio of the fine nickel powder to the superfine iron powder is 4: 1.
4. The method for preparing the tungsten alloy with different components by sintering in the same furnace as claimed in claim 1, wherein the mass content of the coarse tungsten powder in the passivated low tungsten mixture in the second step is 90-95%.
5. The method for preparing the tungsten alloy with different components by sintering in the same furnace according to claim 1, wherein the mass ratio of the nickel powder to the iron powder in the passivated low tungsten mixture in the second step is 2.33: 1.
6. The method for preparing the tungsten alloy with different components by co-furnace sintering as claimed in claim 1, wherein the co-furnace sintering temperature in the fourth step is 1440 ℃ to 1530 ℃, and the holding time is 21min to 50 min.
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