CN110000391A - A kind of preparation method of molybdenum tube - Google Patents
A kind of preparation method of molybdenum tube Download PDFInfo
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- CN110000391A CN110000391A CN201910152097.0A CN201910152097A CN110000391A CN 110000391 A CN110000391 A CN 110000391A CN 201910152097 A CN201910152097 A CN 201910152097A CN 110000391 A CN110000391 A CN 110000391A
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- molybdenum
- molybdenum tube
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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
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
-
- 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
- B22F5/106—Tube or ring forms
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, 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
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
-
- 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 methods of rotary target material molybdenum tube, comprising the following steps: S1. carries out dress powder and hip treatment to molybdenum powder, obtains molybdenum tube base；S2. the molybdenum tube base is squeezed and is made annealing treatment, the molybdenum tube is made.The present invention has many advantages, such as that process is few, with short production cycle, high, the grain structure fine uniform by the molybdenum tube density of this method preparation, density >=99% theoretical density, average grain size≤40 μ, maximum length can be more than 4 meters, can be good at meeting plane and show and the sputter coating requirement of the industries such as photovoltaic.
Description
Technical field
The present invention relates to a kind of preparation method of molybdenum tube more particularly to a kind of preparation methods of rotary target material molybdenum tube, and
The molybdenum tube prepared by this method, belongs to refractory metal pipe preparation technical field.
Background technique
Refractory metal molybdenum has that fusing point is high, intensity is high, thermal expansion coefficient is low, resistivity is low, good thermal stability etc. is excellent
Point, be widely used in plane show, the magnetron sputtering platings industry such as photovoltaic.Molybdenum titanium sputtering target is flat from that can be divided into shape
Face target and tubular target.Compared to planar targets, substantial advantage is shown using the design of tubular target structure.The service life of target
Sputtering power is defined as multiplied by sputtering time (kWh), or can on substrate deposition materials overall thickness.From flat target to
Variation of the rotary target on geometry and design increases the utilization rate of target, and utilization rate can from the 30%-50% of flat target
Increase to 80% or more of rotary target.In addition, if measure the service life of target material with kWh, then the service life of rotary target than
Flat target is 5 times long.Since rotary target ceaselessly rotates in sputtering process, so it is existing to generate resedimentation on its surface
As.Just because of tubular rotary target have the advantages that it is above-mentioned these, tubulose molybdenum target material just gradually replaces planar targets aobvious in plane
Show and is widely applied with industries such as thin-film solar cells.
Tubulose molybdenum target material is prepared, adoptable method includes extrusion, forging method and hot isostatic pressing method etc..
US20060042728A1 discloses a kind of production method of tubulose Mo target with uniform grain size and texture, and Mo powder exists
Compression moulding under the pressure of 200~250MPa sinters blank at a temperature of 1780~2175 DEG C, blank is machined to pipe
Base is most squeezed and is made annealing treatment afterwards, and the tubulose Mo target of even tissue is obtained.CN200680000272.5 discloses a kind of pipe
The production method of shape target, using 0.5~10 μm of Fisher particle size of Mo powder, in the flexible mold using sand core, to metal powder
Carry out cold isostatic compaction；Under temperature T (1600 DEG C of 2500 DEG C of < T <) reducing atmosphere or vacuum in, pass through sintering preparation
Mo pipe blank out；Pipe blank is heated to forming temperature TDBTT < T < (- 800 DEG C of T fusing point), and center roller squeezes and carries out target pipe
Production；Target pipe is attached with support tube finally, and is machined, Mo tubular target is finally prepared.The tubular target
It comprising a Mo pipe or a Mo compo pipe, while also including a support tube made of non-magnetic material, oxygen content is low
In 50 μ g/g, density is greater than the 99% of theoretical density, and lateral average grain diameter in the axial direction is less than 100 μm.
CN201710356089.9 discloses a kind of manufacturing method of sputter coating Mo rotary target material.High-purity Mo powder is equably filled out
It fills in tubular die, extrusion forming is prepared into tubulose silty Mo base；Tubulose silty Mo base is put into cold isostatic press compacting, etc.
Mo base is obtained after static pressure is fine and close；Molding Mo base is put into vacuum sintering furnace and is sintered, sintered Mo base is put into burning
In freezing of a furnace, it is passed through hydrogen shield, is taken out after heating, heat preservation and carries out hammering repeatedly；Mo base after forging is put into vacuum annealing furnace
It inside anneals, then Mo base cools to room temperature with the furnace；Mo rotary target material is obtained after processing to the Mo base after annealing.
CN201410469381.8 discloses a kind of manufacturing method of low cost Mo pipe target.This method is successively wrapped using Mo powder as raw material
Include dress powder step, isostatic cool pressing step, sintering step and hot isostatic pressing step.It is with simple process, and technique distance is short, matter
Measure easily controllable, production cost is low, and target purity is high, gas content is low, the tiny advantage of even tissue, crystal grain.But the patent
Method prepares molybdenum tube using the technique of isostatic cool pressing hot isostatic pressing again, also needs preparation isostatic cool pressing soft mode and outer steel sleeve, dress
The processes such as powder, isostatic cool pressing, Median frequency sintering, jacket, hot isostatic pressing, production technology is increasingly complex and the production cycle is longer.
As plane is shown and the continuous development of the industries sputter coating technologies such as photovoltaic, to the skill of rotation molybdenum target material
Art requires higher and higher.On the one hand, it is desirable that target has the grain structure of more fine uniform, it is desirable that average grain size≤40
Micron, using molybdenum tube target average grain size≤100 micron of prior art preparation, it is difficult to fully meet use demand；It is another
Aspect, it is desirable that molybdenum tube size is increasingly longer, as G11 for TFT-LCD display molybdenum tube target length more than 4 meters, using existing
Isostatic cool pressing+extruding, isostatic cool pressing+forging, isostatic cool pressing+hot isostatic pressing technique be difficult to produce.Such as using cold
The molybdenum tube base consistency of the technique of equal static pressure+extruding, isostatic cool pressing preparation is lower, and Yao Shixian high densification needs to be more than 70%
Extrusion deformation degree is very high to the tonnage demand of extrusion equipment；Isostatic cool pressing+forging technology production molybdenum tube target grain structure and cause
Density inhomogeneity, it is difficult to meet the sputter coating requirement of plane display industry；It is such as straight using isostatic cool pressing+hot isostatic pressing technique
It delivers a child and produces the molybdenum tube target long more than 4 meters, required isostatic cool pressing and hot isostatic apparatus are more than 5 meters, and current appointed condition is difficult
To meet the requirements.
Summary of the invention
The purpose of the present invention is provide a kind of preparation side of rotary target material molybdenum tube according to defect existing in the prior art
Method, the present invention have many advantages, such as that process is few, with short production cycle, by this method preparation molybdenum tube grain structure fine uniform,
Density is high, and maximum length can be more than 4 meters, can be good at meeting plane and shows and want with the sputter coating of the industries such as photovoltaic
It asks.
According to an aspect of the invention, there is provided a kind of preparation method of molybdenum tube, comprising the following steps:
S1. dress powder and hip treatment are carried out to molybdenum powder, obtains molybdenum tube base；
S2. the molybdenum tube base is squeezed and is made annealing treatment, the molybdenum tube is made.
According to certain embodiments of the present invention, the dress powder processing includes the following steps:
Molybdenum powder is fitted into jacket by 1A.；
1B. carries out vacuum outgas to the jacket that step 1A is obtained and soldering and sealing is handled.
According to the preferred embodiment of the present invention, the jacket is the tubular jacket of metal material, preferably stainless steel
The tubular jacket of matter.
The present invention selects the advantages of stainless steel capsule material to be in used hip temperature section, stainless steel
With good deformability, and stainless steel capsule is easily worked, and is easy welding.
In some specific embodiments, the step 1A can be carried out as follows: molybdenum powder is packed into metal material
In tubular jacket, abundant jolt ramming.
According to the preferred embodiment of the present invention, the temperature of Fruit storage is 700-900 DEG C in the step 1B, excellent
It is selected as 800-850 DEG C；Vacuum degree is greater than 1 × 10-2Pa, processing time are 60-180 minutes.
According to the preferred embodiment of the present invention, the step 1B can be carried out as follows: by the set after dress powder jolt ramming
Pipe is heated to 700-900 DEG C, preferably 800-850 DEG C, is then being greater than 1 × 10-260-180 is de-gassed under the vacuum degree of Pa
Minute.
The effect of vacuum outgas is to remove the elemental gas such as the oxygen adsorbed in molybdenum powder, is conducive to the densification of green body.Institute
There is preferable degasifying effect in the process parameters range of selection.
According to certain embodiments of the present invention, the Fisher particle size of the molybdenum powder is 2.0-3.5 μm, preferably 3.0-3.2 μ
M, purity >=99.95%.Selecting the molybdenum powder of the range has preferable powder suppression performance, and the blank density of preparation is higher.
According to the preferred embodiment of the present invention, the temperature of the hip treatment is 1300-1400 DEG C, preferably
1350℃；Pressure is 150-250MPa, preferably 160-200MPa, more preferably 180MPa；Time is 1-5h, preferably 2-
3h。
Molybdenum tube base is prepared compared to traditional isostatic cool pressing+Median frequency sintering technique, the present invention is quiet using direct heat etc.
It presses the molybdenum tube base consistency of technique preparation higher and crystallite dimension more fine uniform, can be prepared by subsequent thermal extrusion process
More excellent performance of long size molybdenum tube material out.
According to the preferred embodiment of the present invention, in the hip treatment step, one is placed inside jacket
Support core stick, supporting the material of plug is tungsten alloy or molybdenum alloy.The effect of support plug is to guarantee what hot isostatic pressing was prepared out
Molybdenum tube base has preferable straightness and dimensional accuracy.
According to certain embodiments of the present invention, the step S2 includes:
2A. carries out extrusion process to the molybdenum tube base；
2B. makes annealing treatment the molybdenum tube base after extrusion process.
According to the preferred embodiment of the present invention, the temperature of the extrusion process is 1250-1350 DEG C, and extrusion ratio is greater than 2.
In some specific embodiments, the step 2A can be carried out as follows: molybdenum tube base is heated to 1250-
1350 DEG C, 30-60 minutes are kept the temperature, and carry out extrusion process processing.
According to the preferred embodiment of the present invention, the temperature of the annealing is 1150-1250 DEG C, time 60-120
Minute.
According to certain embodiments of the present invention, the method also includes following steps:
S3. machining processes, finished product molybdenum tube are carried out to the molybdenum tube after the annealing.
Machining processes are carried out to the molybdenum tube after extrusion forming, coating metal, therefore molybdenum and sheath material can be removed
Between occur diffusion into the surface reaction the molybdenum tube performance produced will not be had an impact.
According to another aspect of the present invention, the molybdenum tube prepared according to the above method, the density of the molybdenum tube are additionally provided
>=99% theoretical density, average grain size≤40 μm.Molybdenum tube maximum length of the invention can be more than 4 meters, can be good at full
Sufficient plane is shown and the requirement of the sputter coating of the industries such as photovoltaic.
Compared with prior art, technical solution of the present invention has the advantage that
(1) there is more tiny, uniform grain structure using the molybdenum tube blank of hot isostatic pressing preparation, through same process
After hot extrusion denaturation, it can prepare with more uniform small grains tissue, the longer rotary target material molybdenum tube of size.
(2) simultaneously, the molybdenum tube base consistency prepared using traditional isostatic cool pressing+Median frequency sintering technique is lower, relatively
For density generally 96% or so, this just needs subsequent be squeezed and deformed to have biggish extrusion ratio, usually to reach 3.5 or more,
This has very high requirement to the extruding tonnage of extrusion equipment；And use hot isostatic pressing preparation molybdenum tube blank can get close to
The consistency of theoretical density, it is therefore desirable to subsequent extrusion deflection it is smaller, the tonnage of extrusion equipment is wanted to substantially reduce
It asks, reduces production difficulty.
Detailed description of the invention
Fig. 1 is the grain structure photo of the rotary target material molybdenum tube prepared according to the embodiment of the present invention 1, resection (GB/T
Average grain size 6394-2002) measured is 37 μm.
Fig. 2 is the grain structure photo of the rotary target material molybdenum tube prepared according to the embodiment of the present invention 2, resection (GB/T
Average grain size 6394-2002) measured is 28 μm.
Fig. 3 is the grain structure photo of the rotary target material molybdenum tube prepared according to the embodiment of the present invention 3, resection (GB/T
Average grain size 6394-2002) measured is 22 μm.
Fig. 4 is the grain structure photo of the rotary target material molybdenum tube prepared according to the embodiment of the present invention 4, resection (GB/T
Average grain size 6394-2002) measured is 23 μm.
Specific embodiment
Illustrate the present invention, but the range that these embodiments are not intended to limit the invention below in conjunction with specific embodiment, it should
The technical staff in field can make some nonessential modifications and adaptations according to the content of aforementioned present invention.
Embodiment 1
Choose the molybdenum powder 124Kg that Fisher particle size is 2.8 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 750 DEG C, is evacuated to vacuum degree higher than 1 × 10-2Pa, heat preservation 2 hours after with
Furnace is cooling, carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, supports plug for molybdenum conjunction
Golden bar, the hip moulding 2 hours under conditions of temperature is 1300 DEG C, pressure is 160MPa, and furnace cooling, are prepared
Internal diameter 130mm, outer diameter 185mm, the molybdenum tube base that length is 900mm, being detected its consistency is 10.12g/cm3；Molybdenum tube base is put
Be placed in intermediate frequency furnace, 1250 DEG C at a temperature of heat 30 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 2, be made
Extruding molybdenum tube having a size of internal diameter 128mm, outer diameter 158mm, length 1800mm；Molybdenum tube will be squeezed to be placed in vacuum furnace
It is made annealing treatment, annealing temperature is 1150 DEG C, annealing time 1h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 132mm, outer diameter 151mm, length 1500mm.Through detecting, the molybdenum tube density of preparation reaches 10.18g/
cm3(99.5% theoretical density), 37 μm of average grain size, grain structure photo is as shown in Figure 1.
Embodiment 2
Choose the molybdenum powder 331Kg that Fisher particle size is 3.2 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 850 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 1.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1350 DEG C, pressure is 180MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 227mm, the molybdenum tube base that length is 1250mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1300 DEG C at a temperature of heat 50 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 2.4,
Extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 3000mm；Molybdenum tube will be squeezed and be placed in heating in vacuum
It is made annealing treatment in furnace, annealing temperature is 1200 DEG C, annealing time 1.5h；It carries out machining and prepares final size to be interior
The rotary target material molybdenum tube of diameter 135mm, outer diameter 167mm, length 2692mm.Through detecting, the molybdenum tube density of preparation reaches 10.20g/
cm3(99.7% theoretical density), 28 μm of average grain size, grain structure photo is as shown in Figure 2.
Embodiment 3
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1200 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), 22 μm of average grain size, grain structure photo is as shown in Figure 3.
Embodiment 4
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1350 DEG C, pressure is 180MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 245mm, the molybdenum tube base that length is 1491mm, being detected its consistency is 10.08g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 131mm, outer diameter 176mm, length 4470mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1200 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.19g/
cm3(99.6% theoretical density), 23 μm of average grain size, grain structure photo is as shown in Figure 4.
Comparative example 1
Choose the molybdenum powder 331Kg that Fisher particle size is 3.2 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 850 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 1.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1200 DEG C, pressure is 180MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 228mm, the molybdenum tube base that length is 1250mm, being detected its consistency is 10.00g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1300 DEG C at a temperature of heat 50 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 2.4,
Extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175.5mm, length 3000mm；Extruding molybdenum tube is placed in vacuum to add
It is made annealing treatment in hot stove, annealing temperature is 1200 DEG C, annealing time 1.5h；Machining is carried out to prepare final size and be
The rotary target material molybdenum tube of internal diameter 135mm, outer diameter 167mm, length 2692mm.Through detecting, the molybdenum tube density of preparation reaches
10.12g/cm3(98.9% theoretical density), 30 μm of average grain size.
Comparative example 2
Choose the molybdenum powder 331Kg that Fisher particle size is 3.2 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 850 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 1.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1600 DEG C, pressure is 180MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 226.5mm, the molybdenum tube base that length is 1257mm, being detected its consistency is 10.14g/cm3；By molybdenum tube
Base is placed in intermediate frequency furnace, 1300 DEG C at a temperature of heat 50 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio is
2.4, extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 3000mm；Molybdenum tube will be squeezed and be placed in vacuum
It is made annealing treatment in heating furnace, annealing temperature is 1200 DEG C, annealing time 1.5h；It carries out machining and prepares final size
For the rotary target material molybdenum tube of internal diameter 135mm, outer diameter 167mm, length 2692mm.Through detecting, the molybdenum tube density of preparation reaches
10.21g/cm3(99.8% theoretical density), 42 μm of average grain size.
Embodiment 5
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1300 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1200 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), 20 μm of average grain size.
Embodiment 6
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1250 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1200 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), 19 μm of average grain size.
Comparative example 3
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1150 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, knot
Fruit molybdenum tube has 1/4 not squeeze out completely.
Comparative example 4
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1450 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, knot
Fruit molybdenum tube radially cracks in extrusion process, squeezes failure.
Embodiment 7
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 2, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 193.5mm, length 3000mm；Molybdenum tube will be squeezed and be placed in heating in vacuum
It is made annealing treatment in furnace, annealing temperature is 1200 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 189mm, length 2700mm.Through detecting, the molybdenum tube density of preparation reaches 10.19g/
cm3(99.8% theoretical density), 35 μm of average grain size.
Comparative example 5
Choose the molybdenum powder 124Kg that Fisher particle size is 2.8 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 750 DEG C, is evacuated to vacuum degree higher than 1 × 10-2Pa, heat preservation 2 hours after with
Furnace is cooling, carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, supports plug for molybdenum conjunction
Golden bar, the hip moulding 2 hours under conditions of temperature is 1300 DEG C, pressure is 160MPa, and furnace cooling, are prepared
Internal diameter 130mm, outer diameter 185mm, the molybdenum tube base that length is 905mm, being detected its consistency is 10.08g/cm3；Molybdenum tube base is put
Be placed in intermediate frequency furnace, 1250 DEG C at a temperature of heat 30 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 1.5, system
The extruding molybdenum tube obtained is having a size of internal diameter 128mm, outer diameter 167mm, length 1358mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1150 DEG C, annealing time 1h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 132mm, outer diameter 160mm, length 1100mm.Through detecting, the molybdenum tube density of preparation reaches 10.11g/
cm3(98.8% theoretical density), 45 μm of average grain size.
Embodiment 8
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1150 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), 21 μm of average grain size.
Embodiment 9
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1250 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), 23 μm of average grain size.
Comparative example 6
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1050 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), perfect recrystallization does not occur for grain structure.
Comparative example 7
Choose the molybdenum powder 493Kg that Fisher particle size is 3.0 μm；Molybdenum powder is fitted into stainless steel capsule, is filled on shaking platform
Divide jolt ramming；The stainless steel capsule of jolt ramming is heated to 800 DEG C, is evacuated to vacuum degree higher than 5 × 10-3Pa, after heat preservation 2.5 hours
Furnace cooling carries out soldering and sealing using argon arc welding；The stainless steel capsule of soldering and sealing is placed in hot isostatic pressing furnace, support plug is tungsten
Alloy bar material, hip moulding 3h under conditions of temperature is 1400 DEG C, pressure is 200MPa, and furnace cooling, are prepared
Internal diameter 135mm, outer diameter 244mm, the molybdenum tube base that length is 1500mm, being detected its consistency is 10.13g/cm3；By molybdenum tube base
Be placed in intermediate frequency furnace, 1350 DEG C at a temperature of heat 60 minutes, then come out of the stove and carry out hot extrusion, extrusion ratio 3, system
The extruding molybdenum tube obtained is having a size of internal diameter 130mm, outer diameter 175mm, length 4500mm；Molybdenum tube will be squeezed and be placed in vacuum furnace
In made annealing treatment, annealing temperature be 1450 DEG C, annealing time 2h；It carries out machining and prepares final size to be internal diameter
The rotary target material molybdenum tube of 135mm, outer diameter 167mm, length 4100mm.Through detecting, the molybdenum tube density of preparation reaches 10.21g/
cm3(99.8% theoretical density), 42 μm of average grain size.
Any numerical value mentioned in the present invention, if between any minimum and any highest value be there are two
The interval of unit then includes each all values for increasing a unit from minimum to peak.For example, if stating one kind
The value of the state-variables such as the amount of component, or temperature, pressure, time is 50-90, in the present specification it means that specific
List 51-89,52-88 ... and the numerical value such as 69-71 and 70-71.For the value of non-integer, can with due regard to
0.1,0.01,0.001 or 0.0001 is a unit.This is only some special examples indicated.In this application, with similar side
The all possible combinations of formula, the numerical value between cited minimum and peak are considered to have disclosed.
It should be noted that embodiment described above for explaining only the invention, is not constituted to of the invention any
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word used in it is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to particular case disclosed in it, on the contrary, this hair
It is bright to can be extended to other all methods and applications with the same function.
Claims (10)
1. a kind of preparation method of molybdenum tube, comprising the following steps:
S1. dress powder and hip treatment are carried out to molybdenum powder, obtains molybdenum tube base；
S2. the molybdenum tube base is squeezed and is made annealing treatment, the molybdenum tube is made.
2. preparation method according to claim 1, which is characterized in that the dress powder processing includes the following steps:
Molybdenum powder is fitted into jacket by 1A.；
1B. carries out vacuum outgas to the jacket that step 1A is obtained and soldering and sealing is handled.
3. preparation method according to claim 1 or 2, which is characterized in that the jacket is the tubular jacket of metal material,
The preferably tubular jacket of stainless steel material.
4. preparation method according to any one of claim 1-3, which is characterized in that in the step 1B at vacuum outgas
The temperature of reason is 700-900 DEG C, preferably 800-850 DEG C；Vacuum degree is greater than 1 × 10-2Pa, processing time are 60-180 minutes.
5. preparation method described in any one of -4 according to claim 1, which is characterized in that the Fisher particle size of the molybdenum powder is
2.0-3.5 μm, preferably 3.0-3.2 μm, purity >=99.95%.
6. preparation method according to any one of claims 1-5, which is characterized in that the temperature of the hip treatment
It is 1300-1400 DEG C, pressure 150-250MPa, preferably 160-200MPa, time 1-5h, preferably 2-3h.
7. preparation method according to claim 1 to 6, which is characterized in that the temperature of the extrusion process is
1250-1350 DEG C, extrusion ratio is greater than 2；The temperature of the annealing is 1150-1250 DEG C.
8. preparation method described in any one of -7 according to claim 1, which is characterized in that in the hip treatment step
In, a support plug is placed inside jacket, supporting the material of plug is tungsten alloy or molybdenum alloy.
9. preparation method according to claim 1 to 8, which is characterized in that the method also includes walking as follows
It is rapid:
S3. machining processes, finished product molybdenum tube are carried out to the molybdenum tube after the annealing.
10. the molybdenum tube of method preparation according to claim 1 to 9, density >=99% of the molybdenum tube are theoretical close
Degree, average grain size≤40 μm.
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