CN108213441A - A kind of preparation method of pure rhenium pipe - Google Patents

A kind of preparation method of pure rhenium pipe Download PDF

Info

Publication number
CN108213441A
CN108213441A CN201711424632.0A CN201711424632A CN108213441A CN 108213441 A CN108213441 A CN 108213441A CN 201711424632 A CN201711424632 A CN 201711424632A CN 108213441 A CN108213441 A CN 108213441A
Authority
CN
China
Prior art keywords
pipe
rhenium
processing
pure rhenium
jacket
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201711424632.0A
Other languages
Chinese (zh)
Other versions
CN108213441B (en
Inventor
王广达
刘国辉
熊宁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Aetna Tianlong Molybdenum Technology Co Ltd
Advanced Technology and Materials Co Ltd
Original Assignee
Aetna Tianlong Molybdenum Technology Co Ltd
Advanced Technology and Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aetna Tianlong Molybdenum Technology Co Ltd, Advanced Technology and Materials Co Ltd filed Critical Aetna Tianlong Molybdenum Technology Co Ltd
Priority to CN201711424632.0A priority Critical patent/CN108213441B/en
Publication of CN108213441A publication Critical patent/CN108213441A/en
Application granted granted Critical
Publication of CN108213441B publication Critical patent/CN108213441B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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]
    • 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
    • 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
    • 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
    • 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
    • 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

Abstract

The invention discloses a kind of preparation method of pure rhenium pipe, which includes the following steps：Prepared by raw material powder pretreatment, compression moulding processing, de- adhesive treatment, pre-sintering processing, jacket processing, hip treatment, go jacket processing, high temperature sintering processing.This method can prepare large scale, a variety of wall thickness pure rhenium pipe product, have the advantages that shape is regular, consistency is high and uniform small grains.

Description

A kind of preparation method of pure rhenium pipe
Technical field
The invention belongs to rare metal granite fields, and in particular to a kind of preparation method of pure rhenium pipe, method of the invention It is particularly suitable for preparing the pure rhenium pipe of large scale, is especially suitable for preparing the big pure rhenium pipe of draw ratio.
Background technology
Rhenium metal have high-melting-point, high density and good Toughness and high-temperature behavior, military project, aerospace, The sector applications such as semiconductor, microelectronics are extensive.The suppression performance of pure rhenium powder is poor, particularly with large-sized pure rhenium product It prepares, by conventional powder metallurgy process method, be easy to causeing blank can not be molded, be sintered problems of crack, seriously affect The production efficiency and quality of pure rhenium product, but since the resource content of rhenium is very rare, cost is very high, so pure for large scale The preparation of rhenium pipe needs to be developed according to actual needs.
Patent CN201610687814.6 discloses a kind of manufacturing method of the pure rhenium test tube of high density, and this method first has to pair Rhenium powder carries out spheroidising and ageing treatment, then carries out compression moulding, sintering and machining, produces pure rhenium test tube；This method Specially treated complex procedures, operation to rhenium powder are not easy to control, can seriously affect the qualification rate of becoming a useful person of rhenium pipe product.
Invention content
Present invention aims at a kind of preparation method of pure rhenium pipe is provided, by adding binding agent in pure rhenium powder, successively Through overvoltage, dewaxing, pre-sintering, jacket, hot isostatic pressing, remove jacket, high temperature sintering, prepare large scale, a variety of wall thickness it is pure Rhenium pipe product has the advantages that shape is regular, consistency is high and uniform small grains.
To achieve these goals, present invention employs following technical schemes：
A kind of preparation method of pure rhenium pipe, includes the following steps：
It is prepared by step 1, raw material powder pretreatment：Binding agent is added, and be uniformly mixed in pure rhenium powder, obtain pre- place Raw material powder after reason；
Step 2, compression moulding processing：Raw material powder after the pretreatment is put into mold, place is pressed Reason, obtains tubulose green compact；
Step 3 takes off adhesive treatment：The tubulose green compact is subjected to de- adhesive treatment；
Step 4, pre-sintering processing：Tubular blank obtained by step 3 is carried out in advance under reducing atmosphere or vacuum environment Sintering processes obtain being pre-sintered pipe；
Step 5, jacket processing：The pre-sintering pipe is subjected to jacket processing, and vacuumize；
Step 6, hip treatment：Blank after jacket is subjected to hip treatment；
Step 7 goes jacket to handle：Sheath material outside step 6 treated pipe is removed；
Step 8, high temperature sintering processing：High temperature sintering processing is carried out to step 7 treated pipe under vacuum, Obtain the pure rhenium tubing products.
In above-mentioned preparation method, as a kind of preferred embodiment, the preparation method further includes machining steps, to institute It states pure rhenium tubing products to be machined, obtains pure rhenium pipe finished product.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 1, the granularity of the pure rhenium powder is -200 ~-325 mesh (such as -230 mesh, -250 mesh, -230 mesh, -270 mesh, -300 mesh), the binding agent are paraffin, the paraffin Additive amount is 2%~5% (such as 2.5%, 3%, 3.5%, 4%, 4.5%) of the pure rhenium silty amount；
In above-mentioned preparation method, as a kind of preferred embodiment, in step 2, the compression moulding processing is using cold etc. Static pressure, it is preferable that the pressing pressure of the isostatic cool pressing for 100~250MPa (such as 110MPa, 120MPa, 130MPa, 140MPa, 150MPa, 155MPa, 165MPa, 180MPa, 200MPa, 220MPa, 240MPa, 245MPa), the dwell time for 0~ 50s (such as 2s, 5s, 10s, 15s, 20s, 30s, 40s, 45s)；
In above-mentioned preparation method, as a kind of preferred embodiment, in step 2, the relative density of the green compact for 55~ 75% (such as 56%, 58%, 60%, 65%, 68%, 70%, 72%, 74%).
In above-mentioned preparation method, as a kind of preferred embodiment, in step 3, the temperature of the de- adhesive treatment is 800 DEG C~1000 DEG C (such as 805 DEG C, 815 DEG C, 850 DEG C, 880 DEG C, 900 DEG C, 920 DEG C, 950 DEG C, 980 DEG C, 990 DEG C), heat preservation Time is 2h~6h (such as 2.2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 5.8h)；
In above-mentioned preparation method, as a kind of preferred embodiment, in step 4, it is described be pre-sintered processing temperature be 1000 DEG C~1350 DEG C (such as 1020 DEG C, 1050 DEG C, 1100 DEG C, 1150 DEG C, 1200 DEG C, 1250 DEG C, 1300 DEG C, 1335 DEG C), Soaking time is 1h~5h (such as 1.5h, 2h, 3h, 4h, 4.5h), it is highly preferred that the reducing atmosphere is hydrogen atmosphere, Or, the vacuum degree under the vacuum environment is 10-1Pa-10-4Pa；Pre-sintering handles the intensity that can cure blank, ensures blank The integrality of shape is convenient to being further processed for follow-up blank.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 5, jacket used in the jacket processing Material is titanium plate and molybdenum bar, to ensure the purity of rhenium pipe finally obtained.
In above-mentioned preparation method, as a kind of preferred embodiment, in step 6, the temperature of the hip treatment is 1350 DEG C~1700 DEG C (such as 1360 DEG C, 1380 DEG C, 1400 DEG C, 1450 DEG C, 1500 DEG C, 1520 DEG C, 1540 DEG C, 1600 DEG C, 1650 DEG C, 1690 DEG C), pressure for 120~180Mpa (such as 125MPa, 130MPa, 140MPa, 150MPa, 160MPa, 170MPa, 175MPa), the pressure-maintaining and heat-preservation time is 1~4h (such as 1.5h, 2h, 2.5h, 3h, 3.5h)；
In above-mentioned preparation method, as a kind of preferred embodiment, in step 6, the pipe after the hip treatment Consistency be 85%~92% (such as 86%, 88%, 90%, 91%).
In above-mentioned preparation method, as a kind of preferred embodiment, in step 7, further include using described in machining removal Pipe superficial layer after hip treatment, the thickness of the superficial layer for 0.1-0.5mm (such as 0.12mm, 0.2mm, 0.3mm、0.4mm、0.45mm)。
In above-mentioned preparation method, as a kind of preferred embodiment, in step 8, the sintering temperature of the high temperature sintering processing It spends for 2150 DEG C~2400 DEG C (such as 2160 DEG C, 2180 DEG C, 2200 DEG C, 2250 DEG C, 2350 DEG C, 2380 DEG C, 2390 DEG C), heat preservation Time is 2~6h (such as 2.2h, 2.5h, 3h, 4h, 5h, 5.5h)；
In above-mentioned preparation method, as a kind of preferred embodiment, in step 8, the consistency of the pure rhenium tubing products is 97% and above (such as 97.5%, 98%, 98.5%, 99%).
In above-mentioned preparation method, as a kind of preferred embodiment, the specification of the pure rhenium tubing products or pure rhenium pipe finished product For：250~700mm of length (such as 260mm, 300mm, 350mm, 400mm, 450mm, 500mm, 550mm, 600mm, 650mm, 690mm), 0.5~4mm of wall thickness (0.6mm, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 3.9mm).
Compared with prior art, the present invention have the advantages that for：
In preparation method provided by the invention, pre-processed by adding suitable paraffin to rhenium powder, facilitate big ruler The compression moulding of very little rhenium base；By being pre-sintered, the intensity of blank is enhanced, ensure that blank is complete in subsequent preparation process Property；With hot isostatic pressing, consistency and uniformity are effectively raised, and overcomes the pure rhenium pipe of large scale in sintering process The problems such as fracture, cracking；The purity and consistency of the pure rhenium pipe of large scale are further improved finally by vacuum high-temperature sintering, is reached To 97% and above relative density.The obtained pure rhenium pipe of large scale of preparation method of the present invention have size is big, wall thickness is adjustable, The advantages of consistency height, regular shape and uniform small grains, such as the method for the present invention can prepare 250~700mm of length, wall The rhenium tubing of 0.5~4mm of thickness；In addition, the method for the present invention technical thought is novel, technological operation relative ease.
Description of the drawings
Fig. 1 is the metallographic structure photo of the tubing prepared using preparation method provided by the invention.
Specific embodiment
The preparation method of the pure rhenium pipe of the present invention is illustrated with reference to the accompanying drawings and examples.It should be understood that these realities Example is applied to be only used for explaining the present invention rather than limit the scope of the invention.Externally it should be understood that reading present disclosure Later, those skilled in the art make various changes or modifications the present invention, and such equivalent forms equally fall within the appended power of the application Sharp claim limited range.
Rhenium powder raw material used is the high-purity rhenium powder that commercially available purity is 99.99% in following embodiment, other used are former Material can be bought from the market.
Embodiment 1
1) rhenium powder pre-processes：The pure rhenium powder of 5Kg is weighed, adds 3.5% paraffin (the i.e. addition of paraffin by mass percentage Measure 3.5% for rhenium silty amount) as binding agent, and be uniformly mixed, the granularity of the rhenium powder is -300 mesh；
2) die mould：Wax powder end will be mixed to be put into mold, carry out isostatic cool pressing compression moulding, pressing pressure 150MPa, pressurize Time is 40s, obtains the tubulose green compact that relative density is 66%；
3) it dewaxes：Dewaxing treatment, 950 DEG C of dewaxing temperature, soaking time 4h are carried out to tubulose green compact using dewaxing furnace；
4) it is pre-sintered：The blank that step 3) obtains is subjected to pre-sintering processing in vacuum condition, 1300 DEG C of pre-sintering temperature, Soaking time 3h, vacuum degree 10-2Pa obtains being pre-sintered pipe；
5) jacket：Pipe jacket being pre-sintered as sheath material using titanium plate and molybdenum bar and being vacuumized, wherein titanium plate is used In cladding outer surface of tube blank, molybdenum bar is inserted into the hollow cavity of pipe；
6) hot isostatic pressing：By after jacket blank carry out high temperature and pressure hip treatment, 1550 DEG C of hip temperature, Hot isostatic pressing pressure 150MPa, heat-insulation pressure keeping time 3h；Obtain the pure rhenium pipe that consistency is 90%；
7) jacket is removed：Using sheath material outside machining removal rhenium pipe and the molybdenum bar among rhenium pipe, and remove rhenium pipe surface Thickness is the metal layer of 0.2mm, to ensure the high-purity of rhenium product；
8) high temperature sintering：The pure rhenium pipe that step 7) obtains is subjected to high temperature sintering processing under vacuum, vacuum degree is 10-3Pa, 2300 DEG C, soaking time 5h of sintering temperature, the consistency of the pure rhenium tubing products of gained is 98.5%, and purity reaches 99.99%；Rhenium tubing products size is：Outer diameter 30mm, internal diameter 16mm, length 450mm.
Production practices prove that the rhenium pipe that the embodiment technique is prepared is not easy cracked.
Fig. 1 is the metallographic structure photo of rhenium tubing products manufactured in the present embodiment, from figure 1 it appears that the crystalline substance of tubing Grain is tiny, uniform, and average grain size is 30 μm.
Embodiment 2
1) rhenium powder pre-processes：The pure rhenium powder of 5Kg is weighed, adds 2.5% paraffin (the i.e. addition of paraffin by mass percentage Measure 2.5% for rhenium silty amount) as binding agent, and be uniformly mixed, the granularity of the rhenium powder is -200 mesh；
2) die mould：Wax powder end will be mixed to be put into mold, carry out isostatic cool pressing compression moulding, pressing pressure 250MPa, pressurize Time is 10s, obtains the tubulose green compact that relative density is 70%；
3) it dewaxes：Dewaxing treatment, 800 DEG C of dewaxing temperature, soaking time 6h are carried out to tubulose green compact using dewaxing furnace；
4) it is pre-sintered：The blank that step 3) obtains is subjected to pre-sintering processing, vacuum degree 10 in vacuum condition-2Pa, in advance 1000 DEG C, soaking time 5h of sintering temperature, vacuum degree 10-2Pa obtains being pre-sintered pipe；
5) jacket：Pipe jacket being pre-sintered as sheath material using titanium plate and molybdenum bar and being vacuumized, wherein titanium plate is used In cladding outer surface of tube blank, molybdenum bar is inserted into the hollow cavity of pipe；
6) hot isostatic pressing：By after jacket blank carry out high temperature and pressure hip treatment, 1350 DEG C of hip temperature, Hot isostatic pressing pressure 180MPa, heat-insulation pressure keeping time 1.5h；Obtain the pure rhenium pipe that consistency is 86%；
7) jacket is removed：Using sheath material outside machining removal rhenium pipe and the molybdenum bar among rhenium pipe, and remove rhenium pipe surface Thickness is the metal layer of 0.4mm, to ensure the high-purity of rhenium product；
8) high temperature sintering：The pure rhenium pipe that step 7) obtains is subjected to high temperature sintering processing, sintering temperature under vacuum 2150 DEG C, soaking time 6h, the consistency of the pure rhenium tubing products of gained is 97.5%, and purity reaches 99.99%；Rhenium tubing products size For：Outer diameter 25mm, internal diameter 21mm, length 550mmmm, the crystal grain of tubing is tiny, uniform, and average grain size is 25 μm.
Production practices prove that the rhenium pipe that the embodiment technique is prepared is not easy cracked.
Embodiment 3
1) rhenium powder pre-processes：The pure rhenium powder of 5Kg is weighed, adds 5% paraffin (the i.e. additive amount of paraffin by mass percentage 5% for rhenium silty amount) it as binding agent, and is uniformly mixed, the granularity of the rhenium powder is -325 mesh；
2) die mould：Wax powder end will be mixed to be put into mold, carry out isostatic cool pressing compression moulding, pressing pressure 100MPa, pressurize Time is 50s, obtains the tubulose green compact that relative density is 58%；
3) it dewaxes：Dewaxing treatment, 1000 DEG C of dewaxing temperature, soaking time 2.5h are carried out to tubulose green compact using dewaxing furnace；
4) it is pre-sintered：The blank that step 3) obtains is subjected to pre-sintering processing, vacuum degree 10 in vacuum condition-4Pa, in advance 1200 DEG C, soaking time 2h of sintering temperature obtains being pre-sintered pipe；
5) jacket：Base jacket being pre-sintered as sheath material using titanium plate and molybdenum bar and being vacuumized, wherein titanium plate is used for Outer surface of tube blank is coated, molybdenum bar is inserted into the hollow cavity of pipe；
6) hot isostatic pressing：By after jacket blank carry out high temperature and pressure hip treatment, 1450 DEG C of hip temperature, Hot isostatic pressing pressure 125MPa, dwell time 2.5h；Obtain the pure rhenium pipe that consistency is 88%；
7) jacket is removed：Using sheath material outside machining removal rhenium pipe and the molybdenum bar among rhenium pipe, and remove rhenium pipe surface Thickness is the metal layer of 0.2mm, to ensure the high-purity of rhenium product；
8) high temperature sintering：The pure rhenium pipe that step 7) obtains is subjected to high temperature sintering processing, sintering temperature under vacuum 2400 DEG C, soaking time 3h, the consistency of the pure rhenium tubing products of gained is 97%, and purity reaches 99.99%；Rhenium tubing products size For：Outer diameter 20mm, internal diameter 18mm, length 650mm, the crystal grain of tubing is tiny, uniform, and average grain size is 40 μm.
Production practices prove that the rhenium pipe that the embodiment technique is prepared is not easy cracked.
Comparative example 1
1) rhenium powder pre-processes：The pure rhenium powder of 5Kg is weighed, adds 3.5% paraffin (the i.e. addition of paraffin by mass percentage Measure 3.5% for rhenium silty amount) as binding agent, and be uniformly mixed, the granularity of the rhenium powder is -300 mesh；
2) die mould：Wax powder end will be mixed to be put into mold, carry out isostatic cool pressing compression moulding, pressing pressure 150MPa, pressurize Time is 40s, obtains the tubulose green compact that relative density is 66%, tubulose green compact size：Outer diameter 30mm, internal diameter 16mm, length 450mm；
3) it dewaxes：Dewaxing treatment, 950 DEG C of dewaxing temperature, soaking time 4h are carried out to tubulose green compact using dewaxing furnace；
4) high temperature sintering：The rhenium pipe that step 3) obtains is subjected to high temperature sintering processing under vacuum, vacuum degree is 10-3Pa, 2300 DEG C of sintering temperature, soaking time 5h.
In high-temperature sintering process, most of pipes crack, and yield rate is extremely low.
Embodiment 4-7
In addition to the parameter of hip treatment step is different from embodiment 1, other operating procedures and the same embodiment of parameter 1.Hip treatment parameter such as the following table 1 of embodiment 4-7, rhenium tubing products size obtained is the same as embodiment 1, the cause of rhenium tubing products Density is referring to table 1.
1 embodiment 4-7 hip treatments parameter of table and rhenium tubing products consistency
Production practices prove, the rhenium pipe that 4 and 6 technique of embodiment is prepared is not easy cracked, and product qualification rate is high, The rhenium pipe that the technique of embodiment 5 and 7 is prepared is easily cracked, and product qualification rate is relatively low.
Comparative example 2
1) rhenium powder pre-processes：The pure rhenium powder of 5Kg is weighed, adds 3.5% paraffin (the i.e. addition of paraffin by mass percentage Measure 3.5% for rhenium silty amount) as binding agent, and be uniformly mixed, the granularity of the rhenium powder is -300 mesh；
2) die mould：Wax powder end will be mixed to be put into mold, carry out isostatic cool pressing compression moulding, pressing pressure 150MPa, pressurize Time is 40s, obtains the tubulose green compact that relative density is 66%；
3) it dewaxes：Dewaxing treatment, 950 DEG C of dewaxing temperature, soaking time 4h are carried out to tubulose green compact using dewaxing furnace；
4) jacket：It by the pipe jacket after dewaxing and is vacuumized as sheath material using titanium plate and molybdenum bar, wherein titanium plate For coating outer surface of tube blank, molybdenum bar is inserted into the hollow cavity of pipe；
5) hot isostatic pressing：By after jacket blank carry out high temperature and pressure hip treatment, 1550 DEG C of hip temperature, Hot isostatic pressing pressure 150MPa, heat-insulation pressure keeping time 3h；
6) jacket is removed：Using sheath material outside machining removal rhenium pipe and the molybdenum bar among rhenium pipe, and remove rhenium pipe surface Thickness is the metal layer of 0.3mm, to ensure the high-purity of rhenium product；
7) high temperature sintering：The pure rhenium pipe that step 6) obtains is subjected to high temperature sintering processing under vacuum, vacuum degree is 10-3Pa, 2300 DEG C, soaking time 5h of sintering temperature, the consistency of the pure rhenium tubing products of gained is 93%；Rhenium tubing products size is： Outer diameter 30mm, internal diameter 16mm, length 450mm.
The average grain size that the present embodiment obtains tubing is 60 μm.
Production practices prove that for the comparative example after pre-treatment step is omitted, the rhenium pipe prepared is easily cracking, production Product qualification rate is very low.

Claims (10)

1. a kind of preparation method of pure rhenium pipe, which is characterized in that include the following steps：
It is prepared by step 1, raw material powder pretreatment：Binding agent is added, and be uniformly mixed in pure rhenium powder, after obtaining pretreatment Raw material powder；
Step 2, compression moulding processing：Raw material powder after the pretreatment is put into mold, processing is pressed, obtains To tubulose green compact；
Step 3 takes off adhesive treatment：The tubulose green compact is subjected to de- adhesive treatment；
Step 4, pre-sintering processing：Tubular blank obtained by step 3 is pre-sintered under reducing atmosphere or vacuum environment Processing obtains being pre-sintered pipe；
Step 5, jacket processing：The pre-sintering pipe is subjected to jacket processing, and vacuumize；
Step 6, hip treatment：Blank after jacket is subjected to hip treatment；
Step 7 goes jacket to handle：Sheath material outside step 6 treated pipe is removed；
Step 8, high temperature sintering processing：High temperature sintering processing is carried out to step 7 treated pipe under vacuum, is obtained The pure rhenium tubing products.
2. preparation method according to claim 1, which is characterized in that the preparation method further includes machining steps, right The pure rhenium tubing products are machined, and obtain pure rhenium pipe finished product；
Preferably, in step 1, the granularity of the pure rhenium powder is -200~-325 mesh, and the binding agent is paraffin, the paraffin Additive amount be the pure rhenium silty amount 2%~5%.
3. according to claim 1-3 any one of them preparation methods, which is characterized in that in step 2, at the compression moulding Reason is using isostatic cool pressing, it is preferable that the pressing pressure of the isostatic cool pressing is 100~250MPa, and the dwell time is 0~50s；More Preferably, the relative density of the green compact is 55~75%.
4. according to claim 1-4 any one of them preparation methods, which is characterized in that in step 3, at the de- binding agent The temperature of reason is 800 DEG C~1000 DEG C, and soaking time is 2h~6h.
5. according to claim 1-4 any one of them preparation methods, which is characterized in that in step 4, the pre-sintering processing Temperature for 1000 DEG C~1350 DEG C, soaking time is 1h~5h, it is preferable that the reducing atmosphere is hydrogen atmosphere or institute It is 10 to state the vacuum degree under vacuum environment-1Pa-10-4Pa。
6. according to claim 1-5 any one of them preparation methods, which is characterized in that in step 5, the jacket handles institute The sheath material used is titanium plate and molybdenum bar.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that in step 6, at the hot isostatic pressing The temperature of reason is 1350 DEG C~1700 DEG C, and pressure is 120~180Mpa, and the pressure-maintaining and heat-preservation time is 1~4h；Preferably, step 6 In, the consistency of the pipe after the hip treatment is 85%~92%.
8. according to claim 1-7 any one of them preparation methods, which is characterized in that in step 7, further include and added using machine Work removes the pipe superficial layer after the hip treatment, and the thickness of the superficial layer is 0.1-0.5mm.
9. according to claim 1-8 any one of them preparation methods, which is characterized in that in step 8, at the high temperature sintering The sintering temperature of reason is 2150 DEG C~2400 DEG C, and soaking time is 2~6h；Preferably, the consistency of the pure rhenium tubing products is 97% and more than.
10. according to claim 1-9 any one of them preparation methods, which is characterized in that the pure rhenium tubing products or pure rhenium pipe The specification of finished product is：250~700mm of length, 0.5~4mm of wall thickness.
CN201711424632.0A 2017-12-25 2017-12-25 Preparation method of pure rhenium tube Active CN108213441B (en)

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 true CN108213441A (en) 2018-06-29
CN108213441B CN108213441B (en) 2019-12-31

Family

ID=62647935

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711424632.0A Active CN108213441B (en) 2017-12-25 2017-12-25 Preparation method of pure rhenium tube

Country Status (1)

Country Link
CN (1) CN108213441B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108907211A (en) * 2018-08-16 2018-11-30 北京科技大学 A method of preparing large scale molybdenum plate blank
CN109807338A (en) * 2019-01-25 2019-05-28 航天材料及工艺研究所 A kind of segmented preparation method of rhenium niobium Composite Nozzle
CN110216277A (en) * 2019-06-13 2019-09-10 金堆城钼业股份有限公司 A kind of preparation method of refractory metal composite pipe
CN111020330A (en) * 2019-12-13 2020-04-17 安泰天龙钨钼科技有限公司 Preparation method of molybdenum-rhenium alloy section bar
CN113333771A (en) * 2021-06-11 2021-09-03 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
CN113909490A (en) * 2021-09-10 2022-01-11 华中科技大学 Metal part and near-net forming method thereof
CN114131026A (en) * 2021-12-08 2022-03-04 西安瑞福莱钨钼有限公司 Process for producing molybdenum tube blank by using mould pressing method

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6102979A (en) * 1998-08-28 2000-08-15 The United States Of America As Represented By The United States Department Of Energy Oxide strengthened molybdenum-rhenium alloy
CN101177748A (en) * 2007-12-12 2008-05-14 安泰科技股份有限公司 Method for manufacturing difficult-to-form pure rhenium sheet
CN101230426A (en) * 2007-01-08 2008-07-30 贺利氏有限公司 High density, low oxygen Re and Re-based consolidated powder materials for use as deposition sources & methods of making the same
CN103740979A (en) * 2013-12-30 2014-04-23 安泰科技股份有限公司 Preparation method of molybdenum titanium alloy material with high density, large size and high homogeneity
CN106270530A (en) * 2016-08-18 2017-01-04 中铼新材料有限公司 A kind of manufacture method of high density pure rhenium test tube
CN106319463A (en) * 2016-09-22 2017-01-11 安泰天龙钨钼科技有限公司 Preparation method for rolling processing of tungsten-titanium alloy target material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6102979A (en) * 1998-08-28 2000-08-15 The United States Of America As Represented By The United States Department Of Energy Oxide strengthened molybdenum-rhenium alloy
CN101230426A (en) * 2007-01-08 2008-07-30 贺利氏有限公司 High density, low oxygen Re and Re-based consolidated powder materials for use as deposition sources & methods of making the same
CN101177748A (en) * 2007-12-12 2008-05-14 安泰科技股份有限公司 Method for manufacturing difficult-to-form pure rhenium sheet
CN103740979A (en) * 2013-12-30 2014-04-23 安泰科技股份有限公司 Preparation method of molybdenum titanium alloy material with high density, large size and high homogeneity
CN106270530A (en) * 2016-08-18 2017-01-04 中铼新材料有限公司 A kind of manufacture method of high density pure rhenium test tube
CN106319463A (en) * 2016-09-22 2017-01-11 安泰天龙钨钼科技有限公司 Preparation method for rolling processing of tungsten-titanium alloy target material

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108907211A (en) * 2018-08-16 2018-11-30 北京科技大学 A method of preparing large scale molybdenum plate blank
CN108907211B (en) * 2018-08-16 2021-10-08 北京科技大学 Method for preparing large-size molybdenum plate blank
CN109807338A (en) * 2019-01-25 2019-05-28 航天材料及工艺研究所 A kind of segmented preparation method of rhenium niobium Composite Nozzle
CN110216277A (en) * 2019-06-13 2019-09-10 金堆城钼业股份有限公司 A kind of preparation method of refractory metal composite pipe
CN110216277B (en) * 2019-06-13 2021-08-24 金堆城钼业股份有限公司 Preparation method of refractory metal composite pipe
CN111020330A (en) * 2019-12-13 2020-04-17 安泰天龙钨钼科技有限公司 Preparation method of molybdenum-rhenium alloy section bar
CN111020330B (en) * 2019-12-13 2021-06-01 安泰天龙钨钼科技有限公司 Preparation method of molybdenum-rhenium alloy section bar
CN113333771A (en) * 2021-06-11 2021-09-03 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
CN113909490A (en) * 2021-09-10 2022-01-11 华中科技大学 Metal part and near-net forming method thereof
CN114131026A (en) * 2021-12-08 2022-03-04 西安瑞福莱钨钼有限公司 Process for producing molybdenum tube blank by using mould pressing method

Also Published As

Publication number Publication date
CN108213441B (en) 2019-12-31

Similar Documents

Publication Publication Date Title
CN108213441A (en) A kind of preparation method of pure rhenium pipe
CN108160995A (en) The preparation method of pure rhenium product
CN103071793B (en) Molybdenum sputtering target material hot isostatic pressure production method
CN108070832A (en) The manufacturing method of molybdenum niobium target blankss
JP5684821B2 (en) Method for manufacturing tungsten target
JP2012251234A (en) Titanium alloy member and method for producing the same
CN102337419B (en) Method for preparing pore structure parameter controlled porous TiNi shape memory alloy
CN102041404A (en) Method for preparing low-oxygen titanium-zirconium-molybdenum (TZM) alloy and application
CN105441881A (en) Making method of chromium target and making method of combination of chromium target
CN109811177A (en) A kind of preparation method of highly conductive high-intensitive silver-graphene composite material
CN109576546A (en) A kind of preparation method of the high-strength tenacity without magnetic Ti (C, N) based ceramic metal
CN103938005A (en) Method for preparing ultra-fine grained titanium and titanium alloy from jet-milled titanium hydride powder
CN114990499B (en) Preparation method of molybdenum alloy target
CN112899624A (en) Aluminum-silicon alloy sputtering target material and preparation method and application thereof
CN103981398B (en) A kind of high-performance metal cramic coat material and preparation method thereof
CN106498314B (en) A kind of WC-TaC-CsfObdurability material and preparation method thereof
CN114921682A (en) High-thermal-conductivity isotropic graphite nodule-copper-based composite material and preparation method thereof
CN115106527A (en) Multistage sintering method of high-strength titanium alloy part based on spark plasma sintering
CN106119788A (en) A kind of modified tungsten nickel target prepares work method
CN113444949A (en) High-density W-Ta-Nb series refractory solid solution alloy and preparation method thereof
RU2521009C1 (en) METHOD OF OBTAINING COMPOSITE MATERIAL Al-Al2O3
CN105772711A (en) Surface treatment method of titanium powder and titanium alloy powder for sintering
CN111360247A (en) Low-cost titanium-aluminum intermetallic compound indirect 3D printing method
CN105603227A (en) Preparation method of Al-Co-Ni quasicrystal
KR20150074269A (en) Method of manufacturing high-toughness wc-cnt sintered body

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant