CN105755301A - Preparation method of high-purity oxygen-free copper rod - Google Patents
Preparation method of high-purity oxygen-free copper rod Download PDFInfo
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- CN105755301A CN105755301A CN201610267271.2A CN201610267271A CN105755301A CN 105755301 A CN105755301 A CN 105755301A CN 201610267271 A CN201610267271 A CN 201610267271A CN 105755301 A CN105755301 A CN 105755301A
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- oxygen
- free copper
- negative electrode
- free
- ingot
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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
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
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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
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Continuous Casting (AREA)
Abstract
The invention relates to a preparation method of a high-purity oxygen-free copper rod and belongs to the technical field of oxygen-free copper rod preparation.The method comprises the steps that a cathode copper ingot subjected to surface treatment is firstly preheated and re-heat for temperature rise so that the copper ingot can be molten completely, heating melting continues after the surface of the molten copper ingot is covered with prepared dry graphite powder, then molten copper is poured into a mold containing zinc wires, standing and cooling are performed to reach room temperature, and a zinc-containing oxygen-free copper rod is obtained, then is mixed with a hydrochloric acid solution, is washed with deionized water and then is dried to obtain the high-purity oxygen-free copper rod.The prepared high-purity oxygen-free copper rod is low in oxygen content, and the oxygen content is 3-7 ppm.The surface of the high-purity oxygen-free copper rod is bright, and the phenomenon of surface scratching or wire breakage is not produced during machining.The preparation steps are simple, and the required costs are low.
Description
Technical field
The preparation method that the present invention relates to a kind of high-purity oxygen-free copper bar, belongs to oxygen-free copper bar preparing technical field.
Background technology
Oxygen-free copper (usually oxygen content is at the copper product of below 20ppm), owing to it has good conduction, heat conductivility, in being widely used in electronics, electrician, the production of electrical part and manufacturing.The vapotron of electron tube, cross the products such as conduit, magnetron, vacuum switch tube, oxygenless copper material will be used.
The low-oxygen copper pole oxygen content that the continuous casting and rolling supplied in the market produces, at 200～400ppm, utilizes the oxygen-free copper bar oxygen content of explained hereafter at 10～20ppm, and oxygen content is all higher.Too high oxygen level, has following impact to the quality of product: (1) can generate Cu with copper2O brittlement phase, forms Cu-Cu2O eutectic, is distributed on crystal boundary with reticular tissue, causes that the mechanical performance of copper bar declines, easily causes phenomenon of rupture in following process；(2) cause that oxygen-free copper bar conductivity declines；(3) copper material is made to crack when hydrogen annealing or needle-like bubble.
Summary of the invention
The technical problem to be solved: the copper bar oxygen content produced for continuous casting and rolling is high, the conductivity and the mechanical performance that cause copper bar decline, and crack or the problem of needle-like bubble when annealing, provide one and first surface treatment negative electrode copper ingot is carried out preheating reheating intensification, make copper ingot completely melted, and the dry graphite powder of preparation is covered to molten copper ingot surface, continue to add heat fusing, then molten copper slurry is built to the mould containing zinc silk, and standing is cooled to room temperature, must containing zinc oxygen-free copper bar, by zinc to the strength of affinity of oxygen more than the copper strength of affinity to oxygen, effectively prevent copper bar from aoxidizing, thus the method preparing high-purity oxygen-free copper bar, it is low that the present invention prepares oxygen-free copper bar oxygen content, oxygen content is 3～7ppm, and adding the problem not havinging injurious surface mark or broken string man-hour.
For solving above-mentioned technical problem, the present invention adopts the technical scheme as described below to be:
(1) choose negative electrode copper ingot, clean its surface with dehydrated alcohol, be prepared into surface treatment negative electrode copper ingot, subsequently surface treatment negative electrode copper ingot is placed in crucible, crucible is placed in vaccum sensitive stove, it is evacuated to 10～20Pa, at 300～500 DEG C, negative electrode copper ingot is preheated 25～30min；
(2) graphite is placed in 120～200 DEG C of Muffle furnaces; when nitrogen protection; heat to graphite rubescent after; standing cools down and mill sieves, and is prepared into the dry graphite powder of 50～70 orders, after above-mentioned negative electrode copper ingot has preheated; vaccum sensitive stove is warming up to 1120～1180 DEG C; treating that copper ingot is completely melted, cover the dry graphite powder of above-mentioned preparation to molten copper ingot surface, control cladding thickness is 150～200mm；
(3) continue to add heat fusing 1～2h, again under 10～20Pa vacuum, molten copper slurry is built to semi-high speed steel mould, mould is contained within a spring-like zinc silk, and length is identical with die length, and spring outer diameter is die width, diameter is 0.1～0.2mm, after having built, stand and be cooled to room temperature, be prepared into containing zinc oxygen-free copper bar；
(4) 1:10 in mass ratio, mixing above-mentioned preparation with the stirring of 1mol/L hydrochloric acid solution containing zinc oxygen-free copper bar, after bubble-free produces, oxygen-free copper bar is taken out and with deionized water wash to pH to 7.0, it is subsequently placed in 65～80 DEG C of vacuum resistance furnaces and dries 6～8h, control vacuum is 10～20Pa, to be dried complete after, a kind of high-purity oxygen-free copper bar can be prepared into.
High-purity oxygen-free copper bar resistivity prepared by the present invention is 0.01785～0.01798 Ω (mm)2/ m, oxygen content is 3～7ppm, and percentage elongation is 42.6～45.3%.
The present invention is compared with additive method, and Advantageous Effects is:
(1) to prepare oxygen-free copper bar oxygen content low for the present invention, and oxygen content is 3～7ppm；
(2) surface-brightening, and adding the phenomenon not havinging injurious surface mark or broken string man-hour；
(3) preparation process of the present invention is simple, and required cost is low.
Detailed description of the invention
First choose negative electrode copper ingot, clean its surface with dehydrated alcohol, be prepared into surface treatment negative electrode copper ingot, subsequently surface treatment negative electrode copper ingot is placed in crucible, crucible is placed in vaccum sensitive stove, it is evacuated to 10～20Pa, at 300～500 DEG C, negative electrode copper ingot is preheated 25～30min；Again graphite is placed in 120～200 DEG C of Muffle furnaces; when nitrogen protection; heat to graphite rubescent after; standing cools down and mill sieves, and is prepared into the dry graphite powder of 50～70 orders, after above-mentioned negative electrode copper ingot has preheated; vaccum sensitive stove is warming up to 1120～1180 DEG C; treating that copper ingot is completely melted, cover the dry graphite powder of above-mentioned preparation to molten copper ingot surface, control cladding thickness is 150～200mm；Continue to add heat fusing 1～2h, again under 10～20Pa vacuum, molten copper slurry is built to semi-high speed steel mould, mould is contained within a spring-like zinc silk, and length is identical with die length, and spring outer diameter is die width, diameter is 0.1～0.2mm, after having built, stand and be cooled to room temperature, be prepared into containing zinc oxygen-free copper bar；Last 1:10 in mass ratio, mixing above-mentioned preparation with the stirring of 1mol/L hydrochloric acid solution containing zinc oxygen-free copper bar, after bubble-free produces, oxygen-free copper bar is taken out and with deionized water wash to pH to 7.0, it is subsequently placed in 65～80 DEG C of vacuum resistance furnaces and dries 6～8h, control vacuum is 10～20Pa, to be dried complete after, a kind of high-purity oxygen-free copper bar can be prepared into.
Example 1
First choose negative electrode copper ingot, clean its surface with dehydrated alcohol, be prepared into surface treatment negative electrode copper ingot, subsequently surface treatment negative electrode copper ingot is placed in crucible, crucible is placed in vaccum sensitive stove, it is evacuated to 20Pa, at 500 DEG C, negative electrode copper ingot is preheated 30min；Again graphite is placed in 200 DEG C of Muffle furnaces; when nitrogen protection; heat to graphite rubescent after; standing cools down and mill sieves, and is prepared into the dry graphite powder of 70 orders, after above-mentioned negative electrode copper ingot has preheated; vaccum sensitive stove is warming up to 1180 DEG C; treating that copper ingot is completely melted, cover the dry graphite powder of above-mentioned preparation to molten copper ingot surface, control cladding thickness is 200mm；Continue to add heat fusing 2h, again under 20Pa vacuum, molten copper slurry is built to semi-high speed steel mould, mould is contained within a spring-like zinc silk, and length is identical with die length, and spring outer diameter is die width, diameter is 0.2mm, after having built, stand and be cooled to room temperature, be prepared into containing zinc oxygen-free copper bar；Last 1:10 in mass ratio, mixing above-mentioned preparation with the stirring of 1mol/L hydrochloric acid solution containing zinc oxygen-free copper bar, after bubble-free produces, oxygen-free copper bar is taken out and with deionized water wash to pH to 7.0, it is subsequently placed in 80 DEG C of vacuum resistance furnaces and dries 8h, control vacuum is 20Pa, to be dried complete after, a kind of high-purity oxygen-free copper bar can be prepared into.After testing, it is low that the present invention prepares oxygen-free copper bar oxygen content, and oxygen content is 7ppm；Surface-brightening, and adding the phenomenon not havinging injurious surface mark or broken string man-hour.
Example 2
First choose negative electrode copper ingot, clean its surface with dehydrated alcohol, be prepared into surface treatment negative electrode copper ingot, subsequently surface treatment negative electrode copper ingot is placed in crucible, crucible is placed in vaccum sensitive stove, it is evacuated to 10Pa, at 300 DEG C, negative electrode copper ingot is preheated 25min；Again graphite is placed in 120 DEG C of Muffle furnaces; when nitrogen protection; heat to graphite rubescent after; standing cools down and mill sieves, and is prepared into the dry graphite powder of 50 orders, after above-mentioned negative electrode copper ingot has preheated; vaccum sensitive stove is warming up to 1120 DEG C; treating that copper ingot is completely melted, cover the dry graphite powder of above-mentioned preparation to molten copper ingot surface, control cladding thickness is 150mm；Continue to add heat fusing 1h, again under 10Pa vacuum, molten copper slurry is built to semi-high speed steel mould, mould is contained within a spring-like zinc silk, and length is identical with die length, and spring outer diameter is die width, diameter is 0.1mm, after having built, stand and be cooled to room temperature, be prepared into containing zinc oxygen-free copper bar；Last 1:10 in mass ratio, mixing above-mentioned preparation with the stirring of 1mol/L hydrochloric acid solution containing zinc oxygen-free copper bar, after bubble-free produces, oxygen-free copper bar is taken out and with deionized water wash to pH to 7.0, it is subsequently placed in 65 DEG C of vacuum resistance furnaces and dries 6h, control vacuum is 10Pa, to be dried complete after, a kind of high-purity oxygen-free copper bar can be prepared into.After testing, it is low that the present invention prepares oxygen-free copper bar oxygen content, and oxygen content is 3ppm；Surface-brightening, and adding the phenomenon not havinging injurious surface mark or broken string man-hour.
Example 3
First choose negative electrode copper ingot, clean its surface with dehydrated alcohol, be prepared into surface treatment negative electrode copper ingot, subsequently surface treatment negative electrode copper ingot is placed in crucible, crucible is placed in vaccum sensitive stove, it is evacuated to 15Pa, at 400 DEG C, negative electrode copper ingot is preheated 27min；Again graphite is placed in 180 DEG C of Muffle furnaces; when nitrogen protection; heat to graphite rubescent after; standing cools down and mill sieves, and is prepared into the dry graphite powder of 60 orders, after above-mentioned negative electrode copper ingot has preheated; vaccum sensitive stove is warming up to 1170 DEG C; treating that copper ingot is completely melted, cover the dry graphite powder of above-mentioned preparation to molten copper ingot surface, control cladding thickness is 170mm；Continue to add heat fusing 1h, again under 15Pa vacuum, molten copper slurry is built to semi-high speed steel mould, mould is contained within a spring-like zinc silk, and length is identical with die length, and spring outer diameter is die width, diameter is 0.15mm, after having built, stand and be cooled to room temperature, be prepared into containing zinc oxygen-free copper bar；Last 1:10 in mass ratio, mixing above-mentioned preparation with the stirring of 1mol/L hydrochloric acid solution containing zinc oxygen-free copper bar, after bubble-free produces, oxygen-free copper bar is taken out and with deionized water wash to pH to 7.0, it is subsequently placed in 70 DEG C of vacuum resistance furnaces and dries 7h, control vacuum is 15Pa, to be dried complete after, a kind of high-purity oxygen-free copper bar can be prepared into.After testing, it is low that the present invention prepares oxygen-free copper bar oxygen content, and oxygen content is 5ppm；Surface-brightening, and adding the phenomenon not havinging injurious surface mark or broken string man-hour.
Claims (1)
1. the preparation method of a high-purity oxygen-free copper bar, it is characterised in that concrete preparation process is:
(1) choose negative electrode copper ingot, clean its surface with dehydrated alcohol, be prepared into surface treatment negative electrode copper ingot, subsequently surface treatment negative electrode copper ingot is placed in crucible, crucible is placed in vaccum sensitive stove, it is evacuated to 10～20Pa, at 300～500 DEG C, negative electrode copper ingot is preheated 25～30min；
(2) graphite is placed in 120～200 DEG C of Muffle furnaces; when nitrogen protection; heat to graphite rubescent after; standing cools down and mill sieves, and is prepared into the dry graphite powder of 50～70 orders, after above-mentioned negative electrode copper ingot has preheated; vaccum sensitive stove is warming up to 1120～1180 DEG C; treating that copper ingot is completely melted, cover the dry graphite powder of above-mentioned preparation to molten copper ingot surface, control cladding thickness is 150～200mm；
(3) continue to add heat fusing 1～2h, again under 10～20Pa vacuum, molten copper slurry is built to semi-high speed steel mould, mould is contained within a spring-like zinc silk, and length is identical with die length, and spring outer diameter is die width, diameter is 0.1～0.2mm, after having built, stand and be cooled to room temperature, be prepared into containing zinc oxygen-free copper bar；
(4) 1:10 in mass ratio, mixing above-mentioned preparation with the stirring of 1mol/L hydrochloric acid solution containing zinc oxygen-free copper bar, after bubble-free produces, oxygen-free copper bar is taken out and with deionized water wash to pH to 7.0, it is subsequently placed in 65～80 DEG C of vacuum resistance furnaces and dries 6～8h, control vacuum is 10～20Pa, to be dried complete after, a kind of high-purity oxygen-free copper bar can be prepared into.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610267271.2A CN105755301A (en) | 2016-04-27 | 2016-04-27 | Preparation method of high-purity oxygen-free copper rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610267271.2A CN105755301A (en) | 2016-04-27 | 2016-04-27 | Preparation method of high-purity oxygen-free copper rod |
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| Publication Number | Publication Date |
|---|---|
| CN105755301A true CN105755301A (en) | 2016-07-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610267271.2A Withdrawn CN105755301A (en) | 2016-04-27 | 2016-04-27 | Preparation method of high-purity oxygen-free copper rod |
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| Country | Link |
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| CN (1) | CN105755301A (en) |
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2016
- 2016-04-27 CN CN201610267271.2A patent/CN105755301A/en not_active Withdrawn
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Application publication date: 20160713 |