CN107790966A - A kind of 1030 DEG C of superhigh temperature vacuum weldings TU0 oxygen-free copper preparation methods - Google Patents
A kind of 1030 DEG C of superhigh temperature vacuum weldings TU0 oxygen-free copper preparation methods Download PDFInfo
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- CN107790966A CN107790966A CN201610837523.0A CN201610837523A CN107790966A CN 107790966 A CN107790966 A CN 107790966A CN 201610837523 A CN201610837523 A CN 201610837523A CN 107790966 A CN107790966 A CN 107790966A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
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Abstract
The present invention discloses a kind of 1030 DEG C of superhigh temperature vacuum welding TU0 oxygen-free copper preparation methods.The lossless pure anaerobic copper conductor material of the such superhigh temperature in China substantially relies on import at present.The present invention uses the technological process of " the continuously extruded drawing of Cu-CATH-1 melting continuous up-casting ", on the basis of " fine fodder sealing ", implement a kind of unidirectional high frequency adverse current of numerical control to melt to shake, protected during continuous up-casting using a kind of reducibility gas, continuous up-casting bar base is carried out cleaning processing with water using a kind of eccentric shaft round brush feed arrangement before continuously extruded, it is continuously extruded that microgap is carried out to the bar base through cleaning with water, during extruding nitrogen is passed through at even crowded cavity position, on-line cooling is carried out to drawing oil using a kind of concurrent flow cooler during drawing, drawing oil temperature fluctuation range is controlled at ± 2 DEG C.The present invention cleans protection to realize the production preparation of ultra-pure TU0 oxygen-free copper bars, scheduling product by above-mentioned overall process.The ultra-pure TU0 oxygen-free coppers prepared through the present invention, any surface finish such as minute surface, oxygen content reach below 3ppm, can meet the lossless vacuum welding of 1030 DEG C of superhigh temperature and high current vacuum ultra-high frequency use condition.
Description
Technical field
The invention belongs to nonferrous materials processing technique field, and in particular to a kind of 1030 DEG C of superhigh temperature vacuum weldings are used
TU0 oxygen-free copper preparation methods.
Technical background
Ultra-pure TU0 oxygen-free coppers are crucial materials needed for the manufacture of superhigh temperature vacuum and high current vacuum ultra-high frequency application field
Material, the lossless pure copper conductor material of the such superhigh temperature in China relies on import substantially at present.Partial vacuum equipment Manufacturing is given way
Using common oxygenless copper material, the problems such as causing downstream product quality and service life degradation.The production of oxygen-free copper is general
Its sublimate is realized using " fine fodder sealing " technology, this conventional art is the control that oxygen and impurity are carried out in fusion-casting process
System, is seldom strictly controlled the copper material oxygenation phenomenon in follow-up plastic working and heat treatment process, therefore, it is difficult to prepare
Go out oxygen and impurity content is less than 5ppm ultra-pure oxygen-free copper, it is impossible to meet the requirement of more than 1000 DEG C vacuum weldings.Because copper
Even if bubble and fracture defect may also be caused in high-temperature soldering containing the micro amount of oxygen and impurity less than 10ppm in material.China
The high-grade anaerobic copper products produced at present can only typically adapt to 800-900 DEG C of vacuum welding, more than 1000 DEG C vacuum welding institutes
Need anaerobic copper conductor be nearly all from external import, 1030 DEG C of superhigh temperature vacuum weldings with TU0 oxygen-free coppers more nobody can do.Cause
This, researchs and develops ultra-pure oxygen-free copper material, and solution makes it be provided simultaneously with ultralow oxygen content (≤3ppm) and metallurgical structure sublimate
Technical barrier, meet that domestic industries are badly in need of, have important practical significance.
The content of the invention
The present invention is for technical barrier existing for the production of China's high-purity oxygen-free copper, using " Cu-CATH-1-melting-above draw
The technological process of continuous casting-continuously extruded-drawing ", ultra-pure TU0 oxygen-free copper bars, scheduling product are realized by total process protective
Production.The invention provides a kind of 1030 DEG C of superhigh temperature vacuum weldings TU0 oxygen-free copper preparation methods, it is characterised in that by with
Lower step operation：
(1) raw material：It is raw material from Cu-CATH-1, content of impurities therein is not higher than 0.0065%.
(2) founding：Melting and casting are carried out using Contiuum type led-up continuous casting machine.During melting basis is covered in thick-layer charcoal
On, implement a kind of unidirectional high frequency adverse current of numerical control to melt and shake；During continuous up-casting, carried out using a kind of reproducibility mixed gas complete
Process is protected.
(3) it is continuously extruded：Using a kind of eccentric shaft round brush feed arrangement, carry out cleaning processing with water to above drawing bar base；To passing through
It is continuously extruded that the bar base cleaned with water carries out microgap, is passed through nitrogen even squeezing cavity position during extruding.
(4) drawing：Bar after continuously extruded, scheduling product are carried out with room temperature drawing, is cooled down using a kind of concurrent flow during drawing
Device carries out on-line cooling to drawing oil, and control drawing oil temperature fluctuation range is at ± 2 DEG C.
Technical principle
The production of oxygen-free copper typically realizes its sublimate using " fine fodder sealing " technology." fine fodder " is exactly to select impurity content
Low Cu-CATH-1 is raw material；" sealing " is exactly to carry out sealing protection in melting and casting overall process, prevents melt air-breathing.For
Realize melt sealant, general in industry use undercurrent type connected furnace, i.e. smelting furnace is linked as entirety, smelting furnace with being incubated foundry furnace
In copper melts enter holding furnace through undercurrent pipe, so metaideophone process is steadily without agitation, and avoid and air contact；It is general to use
Charcoal through calcining carries out thick-layer covering to copper water, and overburden cover reaches more than 150mm；Some Enterprises are molten insulation foundry furnace
Body surface face is also passed through inert gas and is protected by.Nevertheless, above-mentioned measure is still not up to wanting for ultra-pure oxygen-free copper production
Ask, the gas and impurity in copper melts cannot get composition and removes, and oxygen content is extremely difficult to below 5ppm.In addition, in industry mostly
Production of the number enterprises for oxygen-free copper, typically only focuses on fusion-casting process, to follow-up plastic working and heat treatment link generally not
Take corresponding safeguard measure.But in fact, oxygenation phenomenon may all occur in plastic working and heat treatment process for oxygen-free copper, especially
It is continuously extruded process, and the material on copper surface may be squeezed into interior tissue after intensive shear deforms, therefore more should be strict
Control oxidation and the pollution condition of blank surface.
The present invention takes a series of innovative technologies and overall process cleaning guarantor is carried out to material on the basis of " fine fodder sealing "
Shield, thus prepares ultra-pure TU0 oxygen-free coppers.The unidirectional high frequency adverse current vibrations method of smelting of a kind of numerical control as claimed in claim 1,
One annular magnetic stirrer of insertion in smelting furnace melt, by the agitator to melt apply it is a kind of slight controllable and with
The opposite inverse electromagnetic current of smelting furnace inductive electromagnetic.Usual oxygen-free copper uses commercial frequency cored induction furnace melting, is driven in induced field
The lower automatic gentle agitation of melt composition, but mixing direction is unidirectional, and locally lying in certain stirring dead band.What the present invention designed
Agitator can form the unidirectional adverse current magnetic field opposite with original magnetic field, and implement slight vibrations by control electric current frequency.It is this
Adverse current vibrations make Melt Stirring evenly, no dead band, effectively facilitate the gas in melt and float and discharge with minute impurities, because
This enhances the refining of anaerobic copper melts.
A kind of reproducibility mixed gas applied during continuous up-casting as claimed in claim 1 to bath surface, should
Protective gas is by N2、H2, tri- kinds of gas mixings of CO form, each component ratio is 50-70%N2+ 20-40%H2+ 10-30%
CO.The inert gas shielding such as generally use nitrogen or argon gas in industry, Some Enterprises use vacuum melting.Inert gas shielding is only
Contact of the cut-off air with melt is only played, prevents the effect of melt air-breathing and oxidation, and vacuum melting and Casting Equipment are complicated,
Cost is high, and technology controlling and process is difficult.The present invention under non-vacuum condition by bath surface apply reproducibility mixed gas, not only
Effectively contact of the cut-off melt with air, and the partial oxide of cover surface can be reduced, so as to promote in melt
Oxygen accelerates discharge of floating.Meanwhile the presence of reducing atmosphere also effectively increases the service life of graphite crystallizer.
A kind of eccentric shaft round brush feed arrangement as claimed in claim 1, it is to drive one by individually a set of electric system
To eccentric shaft, axle surface is fixed with steel brush；The system is arranged on continuous extruder arrival end, before bar base enters extruding race,
Steel brush on the eccentric shaft of rotation is cleaned with water to round bar base surface, and its eccentric rotary is advantageous to uniformly clear to the progress of bar base surface
Brush.During extruding as claimed in claim 1 the guard method of nitrogen, and the weight of the present invention are passed through at even crowded cavity position
Innovate.Although blank need not heat when continuously extruded, blank produces very high under extruding wheel power friction and extruding
Temperature rise, thermal deformation is actually become, so if being not added with protecting, surface is easy to aoxidize.Have been reported for continuously extruded mistake
The protection against oxidation of blank in journey, nitrogen usually is passed through in extruding race, but actually blank is squeezed into cavity and mould
When it may also happen that oxidation.Present invention adjustment extruding race gap, microgap extruding condition is reached, air, which is difficult to enter, to be squeezed
Pinch roller groove, then using nitrogen protection is passed through in cavity, can effectively prevent blank and product surface from aoxidizing.
A kind of concurrent flow cooler as claimed in claim 1 is by a hydraulic pump, a cooler and is attached thereto
More plastic tubes composition.The oxygen-free copper bar of continuously extruded acquisition, follow-up generally require of row carry out room temperature finishing drawing, during drawing
Need to be cooled down and lubricated using drawing oil.But during the production of continuous batch metaplasia, drawing oil temperature, which has, to be raised, especially
It is under conditions of improper ventilation.Oil temperature rise can not only reduce its cooling effect to drawing mould and workpiece surface, and
Make the viscosity of oil reduce, greasy property is deteriorated, in some instances it may even be possible to workpiece surface is produced oxidation and is bonded.And the fluctuation of drawing oil temperature
Necessarily cause the fluctuation of workpiece surface finish, and then reduce product surface quality.The present invention is directed to the problem, specially devises
A kind of drawing oil cooler, the drawing oil that fuel tank is flowed back into from mould enters cooler through hydraulic pump, in the parallel of cooler
When being flowed repeatedly in stream aluminum pipe, heat is scattered and disappeared in the environment, is achieved in the stability contorting of oil temperature, improves workpiece surface matter
Amount.
Comparative advantages
China's oxygen-free copper typically uses traditional smelting technology melting of " fine fodder sealing " at present, and oxygen content is typically in 5-
Within 20ppm, 800-900 DEG C of vacuum welding requirement can only be typically adapted to, oxygen-free copper needed for more than 1000 DEG C vacuum weldings is led
Body is nearly all from external import.Compared with traditional handicraft, present invention employs overall process to clean protection technique：In smelting furnace
Implement a kind of unidirectional high frequency adverse current of numerical control to melt to shake, overall process is carried out using a kind of reproducibility mixed gas during continuous up-casting
Protection, using a kind of eccentric shaft round brush feed arrangement processing clean with water to above drawing bar base before continuously extruded, even crowded during extruding
Cavity position is passed through nitrogen protection, carries out on-line cooling to drawing oil using a kind of concurrent flow cooler during drawing, controls drawing
Oil temperature fluctuation range thus form the lossless pure copper conductor material of a whole set of TU0 superhigh temperature and continuously manufacture new work at ± 2 DEG C
Skill.The ultra-pure TU0 anaerobics copper conductor material prepared using new technology of the present invention, oxygen content stability contorting is within 3ppm, table
Face is bright and clean close to minute surface, can fully meet the lossless vacuum welding of 1030 DEG C of superhigh temperature and high current vacuum ultra-high frequency uses bar
Part.
Embodiment
It is specifically described below in conjunction with the principle and feature of the present invention, illustrated embodiment is served only for explaining the present invention, makes
Above-mentioned and other purpose, feature and other advantages of the present invention become apparent from, and are not intended to limit the application of the present invention.
Embodiment 1
(1) prepared by continuous up-casting bar base：It is raw material from Cu-CATH-1, content of impurities therein is not higher than
0.0065%；Melting and casting are carried out using Contiuum type led-up continuous casting machine.During melting on the basis of the covering of thick-layer charcoal, to molten
The unidirectional high frequency adverse current of a kind of numerical control that body implements the present invention shakes；During continuous up-casting, using one kind of the present invention by N2、H2, CO tri-
The reducibility gas of kind gas mixing composition carries out total process protective.
(2) continuously extruded and drawing：Using a kind of eccentric shaft round brush feed arrangement, continuous up-casting bar base is carried out cleaning place with water
Reason；It is continuously extruded that microgap is carried out to the bar base through cleaning with water, is passed through nitrogen even squeezing cavity position during extruding；After continuously extruded
Bar, scheduling product carry out room temperature drawing, on-line cooling is carried out to drawing oil using a kind of concurrent flow cooler during drawing, control is drawn
Oil temperature fluctuation range is pulled out at ± 2 DEG C.
Experiment shows, through the ultra-pure TU0 oxygen-free coppers of the invention prepared, any surface finish such as minute surface, non-oxidation vestige；Through burning
Hydrogen method is tested, oxygen content 3ppm.
Comparative example 1
(1) prepared by continuous up-casting bar base：It is raw material from Cu-CATH-1, content of impurities therein is not higher than
0.0065%；Melting and casting are carried out using Contiuum type led-up continuous casting machine.It is not right during melting on the basis of the covering of thick-layer charcoal
The unidirectional high frequency adverse current of a kind of numerical control that melt implements the present invention shakes；During continuous up-casting, using a kind of pure N2Protection.To above drawing bar
Base carries out annealing in hydrogen atmosphere method test, oxygen content 10-15ppm.
(2) continuously extruded and drawing：Bar base oxygen content is below standard, and subsequent extrusion and drawing are not carried out.
Comparative example 2
(1) prepared by continuous up-casting bar base：It is raw material from Cu-CATH-1, content of impurities therein is not higher than
0.0065%；Melting and casting are carried out using Contiuum type led-up continuous casting machine.During melting on the basis of the covering of thick-layer charcoal, to molten
The unidirectional high frequency adverse current of a kind of numerical control that body implements the present invention shakes；During continuous up-casting, using one kind of the present invention by N2、H2, CO tri-
The reducibility gas of kind gas mixing composition carries out total process protective.Annealing in hydrogen atmosphere method test is carried out to above drawing bar base, oxygen content is
3ppm。
(2) continuously extruded and drawing：Using a kind of eccentric shaft round brush feed arrangement, continuous up-casting bar base is carried out cleaning place with water
Reason；Bar base through cleaning with water is carried out continuously extruded, be not passed through nitrogen protection during extruding；Bar after continuously extruded, scheduling product are entered
Row room temperature drawing, on-line cooling is not carried out to drawing oil during drawing.
Experiment shows, uneven using the TU0 oxygen-free coppers of the preparation of comparative example 2, surface smoothness；Test, contain through annealing in hydrogen atmosphere method
Oxygen amount is 8-10ppm.
Above-described embodiment shows that embodiment 1 prepares ultra-pure TU0 oxygen-free coppers, oxygen content control using the technique of the present invention
In 3ppm, the requirement of high-temperature vacuum welding can be met；For comparative example 1 not using the casting method of the present invention, oxygen content is substantially higher,
Reach 10-15ppm, it is impossible to meet the requirement of high-temperature vacuum welding；Comparative example 2 employs the founding of the present invention, but continuously
Do not cause surface smoothness uneven, and material oxygenation, oxygen content reach using the method for the present invention in extruding and drawing process
8-10ppm, it is impossible to meet the requirement of more than 1000 DEG C of high-temperature vacuum welding.
Above-described embodiment is used for explaining the present invention, rather than limits the invention, and is not departing from the principle of the invention
Under the premise of, some improvements and modifications can also be made, these improvements and modifications are also considered as protection scope of the present invention.
Claims (5)
- A kind of 1. 1030 DEG C of superhigh temperature vacuum weldings TUO oxygen-free copper preparation methods, it is characterised in that：Operate according to the following steps：(1) raw material：It is raw material from Cu-CATH-1, content of impurities therein is not higher than 0.0065%.(2) founding：Melting and casting are carried out using Contiuum type led-up continuous casting machine.During melting on the basis of the covering of thick-layer charcoal, Implement a kind of unidirectional high frequency adverse current of numerical control to melt to shake；During continuous up-casting, full mistake is carried out using a kind of reproducibility mixed gas Journey is protected.(3) it is continuously extruded：Using a kind of eccentric shaft round brush feed arrangement, continuous up-casting bar base is carried out cleaning processing with water；To through clear It is continuously extruded that the bar base of brush carries out microgap, is passed through nitrogen even squeezing cavity position during extruding.(4) drawing：Bar after continuously extruded, scheduling product are carried out with room temperature drawing, uses a kind of concurrent flow cooler pair during drawing Drawing oil carries out on-line cooling, and control drawing oil temperature fluctuation range is at ± 2 DEG C.
- A kind of 2. unidirectional high frequency adverse current vibrations method of smelting of numerical control as claimed in claim 1, it is characterised in that：Melted in smelting furnace One magnetic stirrer of insertion in vivo, by the agitator to melt apply it is a kind of slight controllable and with smelting furnace inductive electromagnetic phase Anti- inverse electromagnetic current.
- 3. a kind of reproducibility mixed gas method applied during continuous up-casting as claimed in claim 1 to bath surface, It is characterized in that：The protective gas is by N2、H2, tri- kinds of gas mixings of CO form, each component ratio is 50-70%N2+20- 40%H2+ 10-30%CO.
- A kind of 4. eccentric shaft round brush feed arrangement as claimed in claim 1, it is characterised in that：By single a set of electric system A pair of eccentric shafts are driven, axle surface is fixed with steel brush；The system is arranged on continuous extruder arrival end, enters extruding wheel in bar base Before groove, the steel brush on the eccentric shaft of rotation is cleaned with water to round bar base surface.
- A kind of 5. concurrent flow cooler as claimed in claim 1, it is characterised in that：By a hydraulic pump, a cooler and The more plastic tubes composition being attached thereto.Drawing oil enters cooler through hydraulic pump, in the concurrent flow aluminum pipe of cooler repeatedly During flowing, heat is scattered and disappeared in the environment, is achieved in Oil-temperature control.
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Cited By (4)
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| CN109290534A (en) * | 2018-11-21 | 2019-02-01 | 邹志琼 | Crystallizer is used in a kind of manufacture of copper rod |
| CN112974561A (en) * | 2021-03-25 | 2021-06-18 | 宁波金田电材有限公司 | Extrusion forming die and preparation method of special-shaped copper bar |
| CN113290217A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Vacuum continuous casting process of high-purity oxygen-free copper rod |
| CN116020988A (en) * | 2023-02-07 | 2023-04-28 | 虹华科技股份有限公司 | Processing technology of 6N or above high-purity oxygen-free copper rod |
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| CN109290534B (en) * | 2018-11-21 | 2020-08-04 | 徐州诚凯知识产权服务有限公司 | Crystallizer for manufacturing copper bars |
| CN112974561A (en) * | 2021-03-25 | 2021-06-18 | 宁波金田电材有限公司 | Extrusion forming die and preparation method of special-shaped copper bar |
| CN113290217A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Vacuum continuous casting process of high-purity oxygen-free copper rod |
| CN113290217B (en) * | 2021-05-28 | 2022-09-23 | 金川集团股份有限公司 | Vacuum continuous casting process of high-purity oxygen-free copper rod |
| CN116020988A (en) * | 2023-02-07 | 2023-04-28 | 虹华科技股份有限公司 | Processing technology of 6N or above high-purity oxygen-free copper rod |
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