CN112496327A - Preparation method of seamless iridium tube with high length-diameter ratio - Google Patents
Preparation method of seamless iridium tube with high length-diameter ratio Download PDFInfo
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- CN112496327A CN112496327A CN202011276640.7A CN202011276640A CN112496327A CN 112496327 A CN112496327 A CN 112496327A CN 202011276640 A CN202011276640 A CN 202011276640A CN 112496327 A CN112496327 A CN 112496327A
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- iridium
- sintering
- seamless
- tube
- rotary swaging
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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
- B22F5/106—Tube or ring forms
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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
-
- 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
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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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
- B22F3/24—After-treatment of workpieces or articles
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Forging (AREA)
Abstract
The invention relates to the technical field of metal material processing, in particular to a preparation method of a seamless iridium tube with a high length-diameter ratio, which aims to solve the problem that the slit iridium tube in the prior art limits the exertion of excellent performance of iridium metal, and has the technical key points that: comprises the following steps: s1: filling iridium powder with the purity of not less than 99.95% into a tubular plastic mould, and compacting the iridium powder by adopting high-frequency vibration without loosening; s2: after the charging is finished, cold isostatic pressing is adopted, the pressurizing speed is stable, the pressure is maintained for 5-10min after the pressure is increased to the maximum pressure value, and then the pressure is slowly released; s3: sintering the pressed tubular green body at high temperature; s4: turning the sintered tube blank until the outer diameter of the head is the same as that of the waist; preheating the turned pipe blank in a pipe furnace; s5: and (3) performing successive rotary swaging on a hot rotary swaging machine, after the rotary swaging of each pass is finished, putting the pipe furnace for heat compensation until the rotary swaging reaches the required size, and performing stress relief annealing to obtain the seamless iridium pipe with high length-diameter ratio.
Description
Technical Field
The invention relates to the technical field of metal material processing, in particular to a preparation method of a seamless iridium tube with a high length-diameter ratio.
Background
Iridium is a silvery white metal, and has high melting point, high hardness, corrosion resistance, high-temperature mechanical properties and surface emissivity. The iridium tube is made of pure iridium, and in the field of high-temperature crystal growth, when a Czochralski single crystal manufacturing method is adopted to pull the single crystal, the iridium tube is required to be used as a seed crystal pull rod; in the field of aerospace, the iridium tube is used as a blackbody cavity for measuring a high-temperature airflow temperature field.
Because the iridium has high work hardening rate, large deformation resistance and extremely poor normal-temperature plasticity, the iridium is difficult to be processed into the pipe by a common method, and the processing difficulty is higher especially when the ratio of the diameter to the wall thickness of the pipe is less than 6 and the ratio of the length to the diameter is more than 10. The method of plate roll welding is mostly adopted at home and abroad, the roundness is poor, obvious welding seams exist, and due to the difference of the welding seams and the plates in structure and performance, the exertion of the excellent performance of iridium metal is limited, and the service life of iridium metal is influenced.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of poor roundness and obvious weld formation of the iridium tube in the prior art, so that the preparation method of the seamless iridium tube with high length-diameter ratio is provided.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of a seamless iridium tube with high length-diameter ratio comprises the following steps:
s1: filling iridium powder with the purity of not less than 99.95% into a tubular plastic mould, and compacting the iridium powder by adopting high-frequency vibration without loosening;
s2: after the charging is finished, cold isostatic pressing is adopted, the pressurizing speed is stable, the pressure is maintained for 5-10min after the pressure is increased to the maximum pressure value, and then the pressure is slowly released;
s3: sintering the pressed tubular green body at high temperature;
s4: turning the sintered tube blank until the outer diameter of the head is the same as that of the waist; preheating the turned pipe blank in a pipe furnace;
s5: and (3) performing successive rotary swaging on a hot rotary swaging machine, after the rotary swaging of each pass is finished, putting the tube furnace for heat compensation until the rotary swaging reaches the required size, and performing stress relief annealing to obtain the high-length-diameter ratio seamless iridium tube with good roundness, smooth inner and outer walls and uniform and compact tissue.
Preferably, in S1, the iridium powder has a particle size of 0.5 to 10 μm. The plastic mold is one of a polyurethane mold, a rubber mold or a polyvinyl chloride mold.
Preferably, the outer diameter of the plastic mold is not more than 50mm, the length of the plastic mold is not more than 300mm, and a smooth steel bar is inserted into the center of the plastic mold to serve as a core mold.
Preferably, in the step S2, the pressurization speed is not higher than 5MPa/S, the maximum pressure value is 100-400MPa, and the pressure release speed is not higher than 10 MPa/S.
Preferably, in S3, the sintering temperature is 2300-2400 ℃, the sintering time is 8-12 hours, the density of the sintered pipe blank reaches 95-99.5%, and the high-temperature sintering is one of pressureless vertical melting sintering, pressureless induction sintering, hot-pressing sintering, hot isostatic pressing sintering and spark plasma sintering.
Preferably, in the S4, the preheating temperature is 1300-1600 ℃, and the preheating time is 20-40 min.
Preferably, the heat supplementing time is 5-10min, and the heat supplementing process is repeated until the swaging is performed to the required size.
The preparation method of the seamless iridium tube with the high length-diameter ratio can prepare the seamless iridium tube with the high length-diameter ratio, which has good roundness, smooth inner and outer walls and uniform and compact tissue, and is applied to seed crystal iridium rods and iridium blackbody cavities for temperature measurement of a high-temperature airflow field in a Czochralski single crystal manufacturing method. Because no welding seam exists, the good performance of the iridium is better exerted, and the service life is longer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A preparation method of a seamless iridium tube with high length-diameter ratio comprises the following steps:
s1: and (3) filling iridium powder with the purity of not less than 99.95% into a tubular plastic mould.
Specifically, in one embodiment, the iridium powder particle size is 0.5 μm to 10 μm. The plastic mold is a polyurethane mold, and in other embodiments, the plastic mold may also be a rubber mold, a polyvinyl chloride mold, or other existing plastic molds.
In one embodiment, the plastic mold has an outer diameter not greater than 50mm and a length not greater than 300 mm. A smooth steel bar is inserted into the center of the plastic mold to be used as a core mold, and the iridium powder is compacted by adopting high-frequency vibration without loosening.
S2: after the charging is finished, cold isostatic pressing is adopted, the pressurizing speed is stable, the pressure is maintained for 5-10min after the pressure is increased to the maximum pressure value, and then the pressure is slowly released;
specifically, in one embodiment, the pressing speed is not higher than 5MPa/s,
the maximum pressure value is 100-400MPa, and the pressure relief speed is not higher than 10 MPa/s.
S3: and sintering the pressed tubular green body at high temperature.
Specifically, in one embodiment, the sintering temperature is 2300-2400 ℃, the sintering time is 8-12h, and the density of the sintered pipe blank reaches 95-99.5%. In one embodiment, the high-temperature sintering is pressureless sintering, and in other embodiments, the high-temperature sintering may also be pressureless induction sintering, hot-pressing sintering, hot isostatic pressing sintering, and spark plasma sintering, or any other known high-temperature sintering method.
S4: turning the sintered tube blank until the outer diameter of the head is the same as that of the waist; and preheating the turned pipe blank in a tube furnace.
Specifically, the preheating temperature is 1300-1600 ℃, and the preheating time is 20-40 min.
S5: and (3) performing successive rotary swaging on a hot rotary swaging machine, after the rotary swaging of each pass is finished, putting the tube furnace for heat compensation until the rotary swaging reaches the required size, and performing stress relief annealing to obtain the high-length-diameter ratio seamless iridium tube with good roundness, smooth inner and outer walls and uniform and compact tissue.
Specifically, the heat supplementing time is 5-10min, and the heat supplementing process is repeated until the rotary swaging is carried out to the required size. The hot rotary swaging machine comprises two hammers, three hammers and four hammers, and the hammers are made of hard alloy hammers without limitation.
The preparation method of the high-length-diameter-ratio seamless iridium tube can prepare the high-length-ratio seamless iridium tube which is good in roundness, smooth in inner and outer walls and uniform and compact in tissue, and is applied to a seed crystal iridium rod in a Czochralski single crystal manufacturing method and an iridium blackbody cavity for measuring temperature in a high-temperature airflow field. Because no welding seam exists, the good performance of the iridium is better exerted, and the service life is longer.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications can be made without departing from the scope of the invention.
Claims (7)
1. A preparation method of a seamless iridium tube with high length-diameter ratio is characterized by comprising the following steps: comprises the following steps:
s1: filling iridium powder with the purity of not less than 99.95% into a tubular plastic mould, and compacting the iridium powder by adopting high-frequency vibration without loosening;
s2: after the charging is finished, cold isostatic pressing is adopted, the pressurizing speed is stable, the pressure is maintained for 5-10min after the pressure is increased to the maximum pressure value, and then the pressure is slowly released;
s3: sintering the pressed tubular green body at high temperature;
s4: turning the sintered tube blank until the outer diameter of the head is the same as that of the waist; preheating the turned pipe blank in a pipe furnace;
s5: and (3) performing successive rotary swaging on a hot rotary swaging machine, after the rotary swaging of each pass is finished, putting the tube furnace for heat compensation until the rotary swaging reaches the required size, and performing stress relief annealing to obtain the high-length-diameter ratio seamless iridium tube with good roundness, smooth inner and outer walls and uniform and compact tissue.
2. The method of claim 1, wherein the step of forming the high aspect ratio seamless iridium tube comprises: in the S1, the iridium powder has a particle size of 0.5 to 10 μm. The plastic mold is one of a polyurethane mold, a rubber mold or a polyvinyl chloride mold.
3. The method of claim 1, wherein the step of forming the high aspect ratio seamless iridium tube comprises: the outer diameter of the plastic mold is not more than 50mm, the length of the plastic mold is not more than 300mm, and a smooth steel bar is inserted into the center of the plastic mold to serve as a core mold.
4. The method of claim 1, wherein the step of forming the high aspect ratio seamless iridium tube comprises: in the step S2, the pressurization speed is not higher than 5MPa/S, the maximum pressure value is 100-400MPa, and the pressure relief speed is not higher than 10 MPa/S.
5. The method of claim 1, wherein the step of forming the high aspect ratio seamless iridium tube comprises: in the S3, the sintering temperature is 2300-2400 ℃, the sintering time is 8-12h, the density of the sintered tube blank reaches 95-99.5%, and the high-temperature sintering is one of pressureless vertical melting sintering, pressureless induction sintering, hot-pressing sintering, hot isostatic pressing sintering and spark plasma sintering.
6. The method of claim 1, wherein the step of forming the high aspect ratio seamless iridium tube comprises: in the S4, the preheating temperature is 1300-1600 ℃, and the preheating time is 20-40 min.
7. The method of claim 1, wherein the step of forming the high aspect ratio seamless iridium tube comprises: the heat supplementing time is 5-10min, and the heat supplementing process is repeated until the rotary swaging is carried out to the required size.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011276640.7A CN112496327A (en) | 2020-11-16 | 2020-11-16 | Preparation method of seamless iridium tube with high length-diameter ratio |
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| CN202011276640.7A CN112496327A (en) | 2020-11-16 | 2020-11-16 | Preparation method of seamless iridium tube with high length-diameter ratio |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002198158A (en) * | 2000-12-27 | 2002-07-12 | Ngk Spark Plug Co Ltd | Manufacturing method of spark plug, and the spark plug |
| CN101831568A (en) * | 2010-05-21 | 2010-09-15 | 西北有色金属研究院 | Method for preparing superhigh temperature resistant iridium alloy by using powder metallurgy method |
| CN111411251A (en) * | 2020-05-07 | 2020-07-14 | 贵研铂业股份有限公司 | Anti-oxidation coating for rhenium spray pipe, preparation method of anti-oxidation coating and rhenium-anti-oxidation coating spray pipe |
-
2020
- 2020-11-16 CN CN202011276640.7A patent/CN112496327A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002198158A (en) * | 2000-12-27 | 2002-07-12 | Ngk Spark Plug Co Ltd | Manufacturing method of spark plug, and the spark plug |
| CN101831568A (en) * | 2010-05-21 | 2010-09-15 | 西北有色金属研究院 | Method for preparing superhigh temperature resistant iridium alloy by using powder metallurgy method |
| CN111411251A (en) * | 2020-05-07 | 2020-07-14 | 贵研铂业股份有限公司 | Anti-oxidation coating for rhenium spray pipe, preparation method of anti-oxidation coating and rhenium-anti-oxidation coating spray pipe |
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Address after: 214000 Xinba village, Xibei Town, Xishan District, Wuxi City, Jiangsu Province Applicant after: Intel platinum Co.,Ltd. Address before: 214000 Xinba village, Xibei Town, Xishan District, Wuxi City, Jiangsu Province Applicant before: WUXI INTERNATIONAL PLATINUM Co.,Ltd. |
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