CN108213441B - Preparation method of pure rhenium tube - Google Patents
Preparation method of pure rhenium tube Download PDFInfo
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- CN108213441B CN108213441B CN201711424632.0A CN201711424632A CN108213441B CN 108213441 B CN108213441 B CN 108213441B CN 201711424632 A CN201711424632 A CN 201711424632A CN 108213441 B CN108213441 B CN 108213441B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The invention discloses a preparation method of a pure rhenium tube, which comprises the following steps: the method comprises the steps of raw material powder pretreatment preparation, compression molding treatment, binder removal treatment, pre-sintering treatment, canning treatment, hot isostatic pressing treatment, canning removal treatment and high-temperature sintering treatment. The method can prepare the pure rhenium tube product with large size and various wall thicknesses, and has the advantages of regular shape, high density and fine and uniform crystal grains.
Description
Technical Field
The invention belongs to the field of rare refractory metals, and particularly relates to a preparation method of a pure rhenium tube.
Background
The metal rhenium has high melting point, high density, good room temperature toughness and high temperature performance, and is widely applied to the industries of war industry, aerospace, semiconductors, microelectronics and the like. The pressing performance of the pure rhenium powder is poor, particularly for the preparation of large-size pure rhenium products, the problems that blanks cannot be formed, sintered and cracked and the like are easily caused by a conventional powder metallurgy process method, the production efficiency and the quality of pure rhenium products are seriously influenced, and the preparation of the large-size pure rhenium pipes needs to be developed according to actual needs because the rhenium resource content is very rare and the cost is very high.
Patent CN201610687814.6 discloses a method for manufacturing a high-density pure rhenium test tube, which comprises spheroidizing rhenium powder, aging, press forming, sintering, and machining to obtain a pure rhenium test tube; the method has complex special treatment process of rhenium powder, is difficult to control operation, and can seriously influence the yield of rhenium tube products.
Disclosure of Invention
The invention aims to provide a preparation method of a pure rhenium tube, which is characterized in that a binder is added into pure rhenium powder, and the pure rhenium tube product with large size and various wall thicknesses is prepared through compression, dewaxing, pre-sintering, sheathing, hot isostatic pressing, sheathing removal and high-temperature sintering in sequence, and has the advantages of regular shape, high density and fine and uniform crystal grains.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a pure rhenium tube comprises the following steps:
step one, pretreatment preparation of raw material powder: adding a binder into the pure rhenium powder, and uniformly mixing to obtain pretreated raw material powder;
step two, compression molding treatment: putting the pretreated raw material powder into a die, and performing compression molding treatment to obtain a tubular pressed blank;
step three, binder removal treatment: performing binder removal treatment on the tubular pressed compact;
step four, pre-sintering treatment: performing pre-sintering treatment on the tubular blank obtained in the step three in a reducing atmosphere or a vacuum environment to obtain a pre-sintered tube blank;
step five, canning treatment: sheathing the presintered tube blank, and vacuumizing;
step six, hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sheathed blank;
seventhly, removing the sheath: removing the sheath material outside the tube blank treated in the step six;
step eight, high-temperature sintering treatment: and (4) carrying out high-temperature sintering treatment on the tube blank treated in the step seven under a vacuum condition to obtain the pure rhenium tube product.
In the above preparation method, as a preferred embodiment, the preparation method further includes a machining step of machining the pure rhenium pipe product to obtain a finished pure rhenium pipe product.
In the above preparation method, as a preferred embodiment, in the first step, the pure rhenium powder is sieved pure rhenium powder, a specification of a sieved mesh of the pure rhenium powder is selected from 200 to 325 meshes (e.g., 230 meshes, 250 meshes, 270 meshes, and 300 meshes), the binder is paraffin, and an addition amount of the paraffin is 2% to 5% (e.g., 2.5%, 3%, 3.5%, 4%, and 4.5%) of the mass of the pure rhenium powder;
in the above production method, as a preferred embodiment, in the second step, a cold isostatic pressing is used for the press forming, and preferably, the cold isostatic pressing has a pressing pressure of 100 to 250MPa (e.g., 110MPa, 120MPa, 130MPa, 140MPa, 150MPa, 155MPa, 165MPa, 180MPa, 200MPa, 220MPa, 240MPa, 245MPa) and a dwell time of 0 to 50s (e.g., 2s, 5s, 10s, 15s, 20s, 30s, 40s, 45 s).
In the above production method, as a preferred embodiment, in the second step, the relative density of the green compact is 55 to 75% (for example, 56%, 58%, 60%, 65%, 68%, 70%, 72%, 74%).
In the above preparation method, as a preferred embodiment, in the third step, the temperature of the binder removal treatment is 800 ℃ to 1000 ℃ (such as 805 ℃, 815 ℃, 850 ℃, 880 ℃, 900 ℃, 920 ℃, 950 ℃, 980 ℃ and 990 ℃), and the heat preservation time is 2h to 6h (such as 2.2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h and 5.8 h).
In the above-mentioned preparation method, as a preferred embodiment, in the fourth step, the temperature of the pre-sintering treatment is 1000 ℃ to 1350 ℃ (such as 1020 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃, 1250 ℃, 1300 ℃, 1335 ℃), the holding time is 1h to 5h (such as 1.5h, 2h, 3h, 4h, 4.5h), more preferably, the reducing atmosphere is a hydrogen atmosphere, or the vacuum degree in the vacuum environment is 10-1Pa-10-4Pa; the pre-sintering treatment can solidify the strength of the blank, ensure the integrity of the shape of the blank and facilitate the further treatment of the subsequent blank.
In the above preparation method, as a preferred embodiment, in step five, the sheathing materials used in the sheathing treatment are titanium plates and molybdenum rods, so as to ensure the purity of the finally obtained rhenium tube.
In the sixth preferred embodiment of the above preparation method, in the sixth step, the hot isostatic pressing treatment is performed at 1350 ℃ to 1700 ℃ (such as 1360 ℃, 1380 ℃, 1400 ℃, 1450 ℃, 1500 ℃, 1520 ℃, 1540 ℃, 1600 ℃, 1650 ℃ and 1690 ℃), at a pressure of 120Mpa to 180Mpa (such as 125Mpa, 130Mpa, 140Mpa, 150Mpa, 160Mpa, 170Mpa and 175Mpa), and at a pressure-holding and heat-preserving time of 1h to 4h (such as 1.5h, 2h, 2.5h, 3h and 3.5 h).
In the sixth preferred embodiment of the above manufacturing method, the density of the hot isostatic pressed tube blank is 85% to 92% (e.g., 86%, 88%, 90%, 91%).
In the above manufacturing method, as a preferred embodiment, in the seventh step, the surface layer of the tube blank after the hot isostatic pressing treatment is removed by machining, and the thickness of the surface layer is 0.1-0.5mm (e.g. 0.12mm, 0.2mm, 0.3mm, 0.4mm, 0.45 mm).
In the above preparation method, as a preferred embodiment, in the eighth step, the sintering temperature of the high-temperature sintering treatment is 2150 ℃ to 2400 ℃ (such as 2160 ℃, 2180 ℃, 2200 ℃, 2250 ℃, 2350 ℃, 2380 ℃ and 2390 ℃), and the holding time is 2 to 6 hours (such as 2.2 hours, 2.5 hours, 3 hours, 4 hours, 5 hours and 5.5 hours).
In the above-mentioned preparation method, as a preferred embodiment, in step eight, the density of the pure rhenium tube product is 97% or more (e.g., 97.5%, 98%, 98.5%, 99%).
In the above preparation method, as a preferred embodiment, the specification of the pure rhenium pipe product or the pure rhenium pipe finished product is as follows: the length is 250-700 mm (such as 260mm, 300mm, 350mm, 400mm, 450mm, 500mm, 550mm, 600mm, 650mm, 690mm), and the wall thickness is 0.5-4 mm (0.6mm, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 3.9 mm).
Compared with the prior art, the invention has the following beneficial effects:
in the preparation method provided by the invention, the rhenium powder is added with a proper amount of paraffin for pretreatment, so that the large-size rhenium blank is convenient to be pressed and formed; the strength of the blank is enhanced through pre-sintering, and the integrity of the blank in the subsequent preparation process is ensured; by applying hot isostatic pressing, the density and the uniformity are effectively improved, and the problems of fracture, cracking and the like of a large-size pure rhenium tube blank in the sintering process are solved; finally, the purity and the density of the large-size pure rhenium tube are further improved through vacuum high-temperature sintering, and the relative density of 97 percent or more is achieved. The large-size pure rhenium pipe obtained by the preparation method has the advantages of large size, adjustable wall thickness, high compactness, regular shape and fine and uniform crystal grains, for example, the method can be used for preparing a rhenium pipe with the length of 250-700 mm and the wall thickness of 0.5-4 mm; in addition, the method has novel technical thought and relatively simple and convenient process operation.
Drawings
FIG. 1 is a metallographic structure photograph of a pipe prepared by the preparation method provided by the present invention.
Detailed Description
The following describes the preparation method of pure rhenium tube according to the present invention 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 rhenium powder raw material used in the following examples was commercially available high purity rhenium powder with a purity of 99.99%, and other raw materials used were commercially available.
Example 1
1) And (3) rhenium powder pretreatment: weighing 5Kg of pure rhenium powder (the rhenium powder is sieved by a 300-mesh sieve), adding 3.5% of paraffin wax (namely, the addition of the paraffin wax is 3.5% of the mass of the rhenium powder) serving as a binder according to mass percent, and uniformly mixing;
2) profiling: putting the wax-doped powder into a mould, and carrying out cold isostatic pressing forming under the pressing pressure of 150MPa for 40s to obtain a tubular green compact with the relative density of 66%;
3) dewaxing: dewaxing the tubular pressed blank by using a dewaxing furnace at the dewaxing temperature of 950 ℃ for 4 hours;
4) pre-sintering: pre-sintering the blank obtained in the step 3) under a vacuum condition, wherein the pre-sintering temperature is 1300 ℃, the heat preservation time is 3 hours, and the vacuum degree is 10-2Pa, obtaining a presintered pipe blank;
5) and (3) canning: wrapping and vacuumizing the pre-sintered tube blank by using a titanium plate and a molybdenum rod as wrapping materials, wherein the titanium plate is used for wrapping the outer surface of the tube blank, and the molybdenum rod is inserted into a hollow cavity of the tube blank;
6) hot isostatic pressing: performing high-temperature and high-pressure hot isostatic pressing treatment on the wrapped blank, wherein the hot isostatic pressing temperature is 1550 ℃, the hot isostatic pressing pressure is 150MPa, and the heat preservation and pressure maintaining time is 3 h; obtaining a pure rhenium tube blank with the density of 90 percent;
7) removing the sheath: removing a sheath material outside the rhenium pipe and a molybdenum rod between the rhenium pipe by machining, and removing a metal layer with the thickness of 0.2mm on the surface of the rhenium pipe to ensure the high purity of a rhenium product;
8) and (3) high-temperature sintering: carrying out high-temperature sintering treatment on the pure rhenium tube obtained in the step 7) under a vacuum condition with the vacuum degree of 10-3Pa, the sintering temperature is 2300 ℃, and the heat preservation time is 5 hours, so that the density of the obtained pure rhenium pipe product is 98.5 percent, and the purity reaches 99.99 percent; the rhenium tube product has the following dimensions: 30mm outside diameter, 16mm inside diameter, 450mm length.
Production practices prove that the rhenium pipe prepared by the process of the embodiment is not easy to crack.
FIG. 1 is a photograph of the metallographic structure of the rhenium tube product prepared in this example, and it can be seen from FIG. 1 that the grains of the tube material are fine and uniform, and the average grain size is 30 μm.
Example 2
1) And (3) rhenium powder pretreatment: weighing 5Kg of pure rhenium powder (the rhenium powder is sieved by a 200-mesh sieve), adding 2.5% of paraffin wax (namely, the addition of the paraffin wax is 2.5% of the mass of the rhenium powder) serving as a binder according to mass percent, and uniformly mixing;
2) profiling: putting the wax-doped powder into a mould, and carrying out cold isostatic pressing forming under the pressing pressure of 250MPa for 10s to obtain a tubular green compact with the relative density of 70%;
3) dewaxing: dewaxing the tubular pressed blank by using a dewaxing furnace, wherein the dewaxing temperature is 800 ℃, and the heat preservation time is 6 hours;
4) pre-sintering: pre-sintering the blank obtained in the step 3) under a vacuum condition with a vacuum degree of 10-2Pa, presintering temperature 1000 ℃, heat preservation time 5h and vacuum degree 10-2Pa, obtaining a presintered pipe blank;
5) and (3) canning: wrapping and vacuumizing the pre-sintered tube blank by using a titanium plate and a molybdenum rod as wrapping materials, wherein the titanium plate is used for wrapping the outer surface of the tube blank, and the molybdenum rod is inserted into a hollow cavity of the tube blank;
6) hot isostatic pressing: performing high-temperature and high-pressure hot isostatic pressing treatment on the wrapped blank, wherein the hot isostatic pressing temperature is 1350 ℃, the hot isostatic pressing pressure is 180MPa, and the heat preservation and pressure maintaining time is 1.5 h; obtaining a pure rhenium tube blank with the density of 86%;
7) removing the sheath: removing a sheath material outside the rhenium pipe and a molybdenum rod between the rhenium pipe by machining, and removing a metal layer with the thickness of 0.4mm on the surface of the rhenium pipe to ensure the high purity of a rhenium product;
8) and (3) high-temperature sintering: carrying out high-temperature sintering treatment on the pure rhenium tube obtained in the step 7) under a vacuum condition, wherein the sintering temperature is 2150 ℃, the heat preservation time is 6 hours, the density of the obtained pure rhenium tube product is 97.5%, and the purity reaches 99.99%; the rhenium tube product has the following dimensions: the external diameter is 25mm, the internal diameter is 21mm, the length is 550mmmm, the crystal grains of the pipe are fine and uniform, and the average crystal grain size is 25 mu m.
Production practices prove that the rhenium pipe prepared by the process of the embodiment is not easy to crack.
Example 3
1) And (3) rhenium powder pretreatment: weighing 5Kg of pure rhenium powder (the rhenium powder is sieved by a 325-mesh sieve), adding 5% of paraffin wax (namely, the addition of the paraffin wax is 5% of the mass of the rhenium powder) serving as a binder according to mass percent, and uniformly mixing;
2) profiling: putting the wax-doped powder into a mould, and carrying out cold isostatic pressing forming under the pressing pressure of 100MPa for 50s to obtain a tubular green compact with the relative density of 58%;
3) dewaxing: dewaxing the tubular pressed blank by using a dewaxing furnace, wherein the dewaxing temperature is 1000 ℃, and the heat preservation time is 2.5 h;
4) pre-sintering: pre-sintering the blank obtained in the step 3) under a vacuum condition with a vacuum degree of 10-4Pa, the presintering temperature is 1200 ℃, and the heat preservation time is 2 hours, so that a presintering pipe blank is obtained;
5) and (3) canning: sheathing and vacuumizing the pre-sintered blank by using a titanium plate and a molybdenum rod as sheathing materials, wherein the titanium plate is used for coating the outer surface of the tube blank, and the molybdenum rod is inserted into a hollow cavity of the tube blank;
6) hot isostatic pressing: carrying out high-temperature and high-pressure hot isostatic pressing treatment on the sheathed blank, wherein the hot isostatic pressing temperature is 1450 ℃, the hot isostatic pressing pressure is 125MPa, and the pressure maintaining time is 2.5 h; obtaining a pure rhenium tube blank with the density of 88%;
7) removing the sheath: removing a sheath material outside the rhenium pipe and a molybdenum rod between the rhenium pipe by machining, and removing a metal layer with the thickness of 0.2mm on the surface of the rhenium pipe to ensure the high purity of a rhenium product;
8) and (3) high-temperature sintering: carrying out high-temperature sintering treatment on the pure rhenium tube obtained in the step 7) under a vacuum condition, wherein the sintering temperature is 2400 ℃, the heat preservation time is 3 hours, the density of the obtained pure rhenium tube product is 97%, and the purity reaches 99.99%; the rhenium tube product has the following dimensions: the external diameter is 20mm, the internal diameter is 18mm, the length is 650mm, the crystal grains of the pipe are fine and uniform, and the average crystal grain size is 40 mu m.
Production practices prove that the rhenium pipe prepared by the process of the embodiment is not easy to crack.
Comparative example 1
1) And (3) rhenium powder pretreatment: weighing 5Kg of pure rhenium powder (the rhenium powder is sieved by a 300-mesh sieve), adding 3.5% of paraffin wax (namely, the addition of the paraffin wax is 3.5% of the mass of the rhenium powder) serving as a binder according to mass percent, and uniformly mixing;
2) profiling: putting the wax-doped powder into a mould, and carrying out cold isostatic pressing forming, wherein the pressing pressure is 150MPa, the pressure maintaining time is 40s, so as to obtain a tubular pressed blank with the relative density of 66%, and the size of the tubular pressed blank is as follows: the outer diameter is 30mm, the inner diameter is 16mm, and the length is 450 mm;
3) dewaxing: dewaxing the tubular pressed blank by using a dewaxing furnace at the dewaxing temperature of 950 ℃ for 4 hours;
4) high temperatureAnd (3) sintering: carrying out high-temperature sintering treatment on the rhenium tube blank obtained in the step 3) under a vacuum condition, wherein the vacuum degree is 10-3Pa, the sintering temperature is 2300 ℃, and the holding time is 5 h.
In the high-temperature sintering process, most of the tube blanks crack, and the yield is extremely low.
Examples 4 to 7
The procedure and parameters were the same as in example 1, except that the parameters of the hot isostatic pressing step were different from those of example 1. The parameters of hot isostatic pressing treatment for examples 4-7 are shown in table 1 below, and the rhenium tube product prepared has the same dimensions as example 1, and the density of the rhenium tube product is shown in table 1.
Table 1 examples 4-7 hipping parameters and rhenium tube article densification
Production practices prove that the rhenium pipes prepared by the processes of the embodiments 4 and 6 are not easy to crack, the product percent of pass is extremely high, the rhenium pipes prepared by the processes of the embodiments 5 and 7 are easy to crack, and the product percent of pass is low.
Comparative example 2
1) And (3) rhenium powder pretreatment: weighing 5Kg of pure rhenium powder (the rhenium powder is sieved by a 300-mesh sieve), adding 3.5% of paraffin wax (namely, the addition of the paraffin wax is 3.5% of the mass of the rhenium powder) serving as a binder according to mass percent, and uniformly mixing;
2) profiling: putting the wax-doped powder into a mould, and carrying out cold isostatic pressing forming under the pressing pressure of 150MPa for 40s to obtain a tubular green compact with the relative density of 66%;
3) dewaxing: dewaxing the tubular pressed blank by using a dewaxing furnace at the dewaxing temperature of 950 ℃ for 4 hours;
4) and (3) canning: wrapping and vacuumizing the dewaxed tube blank by using a titanium plate and a molybdenum rod as wrapping materials, wherein the titanium plate is used for wrapping the outer surface of the tube blank, and the molybdenum rod is inserted into a hollow cavity of the tube blank;
5) hot isostatic pressing: performing high-temperature and high-pressure hot isostatic pressing treatment on the wrapped blank, wherein the hot isostatic pressing temperature is 1550 ℃, the hot isostatic pressing pressure is 150MPa, and the heat preservation and pressure maintaining time is 3 h;
6) removing the sheath: removing a sheath material outside the rhenium pipe and a molybdenum rod between the rhenium pipe by machining, and removing a metal layer with the thickness of 0.3mm on the surface of the rhenium pipe to ensure the high purity of a rhenium product;
7) and (3) high-temperature sintering: carrying out high-temperature sintering treatment on the pure rhenium tube obtained in the step 6) under a vacuum condition with the vacuum degree of 10-3Pa, the sintering temperature is 2300 ℃, the heat preservation time is 5h, and the density of the obtained pure rhenium pipe product is 93 percent; the rhenium tube product has the following dimensions: 30mm outside diameter, 16mm inside diameter, 450mm length.
The average grain size of the pipe obtained in this example was 60 μm.
Production practice proves that after the pretreatment step is omitted, the prepared rhenium tube is easy to crack, and the product percent of pass is very low.
Claims (12)
1. The preparation method of the pure rhenium tube is characterized by comprising the following steps:
step one, pretreatment preparation of raw material powder: adding a binder into the pure rhenium powder, and uniformly mixing to obtain pretreated raw material powder;
step two, compression molding treatment: putting the pretreated raw material powder into a die, and performing compression molding treatment to obtain a tubular pressed blank;
step three, binder removal treatment: performing binder removal treatment on the tubular pressed compact;
step four, pre-sintering treatment: performing pre-sintering treatment on the tubular blank obtained in the step three in a reducing atmosphere or a vacuum environment to obtain a pre-sintered tube blank; the temperature of the pre-sintering treatment is 1000-1350 ℃, and the heat preservation time is 1-5 h;
step five, canning treatment: sheathing the presintered tube blank, and vacuumizing;
step six, hot isostatic pressing treatment: carrying out hot isostatic pressing treatment on the sheathed blank; the hot isostatic pressing treatment temperature is 1350-1700 ℃, the pressure is 120-180 Mpa, and the pressure maintaining and heat preserving time is 1-4 h;
seventhly, removing the sheath: removing the sheath material outside the tube blank treated in the step six;
step eight, high-temperature sintering treatment: carrying out high-temperature sintering treatment on the tube blank treated in the step seven under a vacuum condition to obtain the pure rhenium tube product; the sintering temperature of the high-temperature sintering treatment is 2150-2400 ℃, and the heat preservation time is 2-6 hours.
2. The method of claim 1, further comprising a machining step of machining the pure rhenium tube product to obtain a finished pure rhenium tube product.
3. The preparation method of claim 1 or 2, characterized in that in the first step, the pure rhenium powder is sieved pure rhenium powder, the specification of a sieved screen of the pure rhenium powder is selected from 200-325 meshes, the binder is paraffin, and the addition amount of the paraffin is 2-5% of the mass of the pure rhenium powder.
4. The production method according to claim 1 or 2, wherein in the second step, the press forming process uses a cold isostatic press, the cold isostatic press has a press pressure of 100 to 250MPa, and a dwell time of 0 to 50 s.
5. The method according to claim 4, wherein in the second step, the relative density of the green compact is 55 to 75%.
6. The preparation method according to claim 1 or 2, characterized in that, in the third step, the temperature of the binder removal treatment is 800-1000 ℃, and the holding time is 2-6 h.
7. The method according to claim 1 or 2, wherein in the fourth step, the reducing atmosphere is a hydrogen atmosphere, or the vacuum degree in the vacuum environment is 10-1Pa-10-4Pa。
8. The method according to claim 1 or 2, wherein in the fifth step, the sheathing materials used for the sheathing treatment are titanium plates and molybdenum rods.
9. The production method according to claim 1 or 2, wherein in the sixth step, the density of the hot isostatic pressed tube blank is 85% to 92%.
10. The production method according to claim 1 or 2, characterized in that step seven, the method further comprises removing a surface layer of the hot isostatic pressed tube blank by machining, wherein the thickness of the surface layer is 0.1-0.5 mm.
11. The production method according to claim 1 or 2, wherein in step eight, the density of the pure rhenium tube product is 97% or more.
12. The production method according to claim 1 or 2, wherein the specifications of the pure rhenium pipe product or the pure rhenium pipe finished product are: the length is 250-700 mm, and the wall thickness is 0.5-4 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711424632.0A CN108213441B (en) | 2017-12-25 | 2017-12-25 | Preparation method of pure rhenium tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711424632.0A CN108213441B (en) | 2017-12-25 | 2017-12-25 | Preparation method of pure rhenium tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108213441A CN108213441A (en) | 2018-06-29 |
| CN108213441B true CN108213441B (en) | 2019-12-31 |
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| CN113333771B (en) * | 2021-06-11 | 2022-07-01 | 安泰科技股份有限公司 | Rhenium powder and rhenium product with purity of 6N or above and preparation method thereof |
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