CN106893882B - A kind of preparation method of copper gadolinium intermediate alloy - Google Patents
A kind of preparation method of copper gadolinium intermediate alloy Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of copper gadolinium intermediate alloy, belong to Cu alloy material melting and casting technical field.The present invention takes vacuum melting mode, according to the quality of copper gadolinium intermediate alloy than sorting, ingredient, shove charge；It vacuumizes, heats up, applying argon gas stirs after metal is completely melt, heat preservation refining, degasification；It at the uniform velocity casts, prepares the copper gadolinium intermediate alloy that gadolinium concentrations are 3%~9% (mass percent).The present invention improves smelting efficiency using special loading method, the melt quality in fusing, reaction and refining process is adjusted by the temperature in each stage in control smelting technology, use water cooled mo(u)ld casting to reduce segregation, the copper gadolinium intermediate alloy ingot casting ingredient prepared through the method is uniform and deviation is small, impurity content is low, fusing point is low, internal no significant defect, is very suitable for the preparation for the modified copper alloy of gadolinium.
Description
Technical field
The present invention relates to a kind of preparation methods of copper gadolinium intermediate alloy, belong to Cu alloy material melting and casting technical field.
Background technique
Rare earth element mainly plays purification, removal impurity and refinement crystal grain in copper, is significantly improving the strength of materials
With it is smaller to Conductivity while heat resistance, moreover it is possible to significantly improve the casting character of alloy.Utilize China's rare earth characteristic
Advantage researches and develops the rare earth modified copper with Good All-around Property and copper alloy and the efficient of developing rare earth is answered using with high-end
With, support and develop China's Copper fabrication industry have great importance.
Research can significantly change certain characteristics in copper or copper alloy it is known that adding minimal amount of rare earth element, this
A additive amount is generally no greater than 1wt.%, by taking a kind of rail traffic contact line copper-tin alloy as an example, only it need to add 0.01~
The cerium-rich mischmetal of 0.04wt.%.Therefore, generally use copper-rare earth intermediate alloy mode added into copper or copper alloy it is dilute
Earth elements.Research about copper-light rare earth binary intermediate alloy or multicomponent alloy refining agent is existing very much, preparation process and skill
Art tends to be mature, and relatively fewer for the research in terms of copper and heavy rare earth element alloying.
Gadolinium is that one kind has magnetic yttrium group heavy rare earth element at room temperature, is existed using its physical property and oxide characteristics
The functional characteristic of copper product can also be extended while improving copper and copper alloy matrix degree of purity, and there is very high research and application
Value.For the service efficiency for improving gadolinium element, also need to add using intermediate alloy mode.But gadolinium element chemistry activity is high, heated
Shi Jiyi reacts with media such as water and airs, high melt when scaling loss it is serious, preparation significant loss is small, the uniform copper-gadolinium of ingredient
Binary intermediate alloy is sufficiently complex.It is currently extremely limited about the research of copper-gadolinium binary intermediate alloy, it is molten in intermediate alloy
It is still necessary to further perfect in terms of refining and foundry engieering.
Summary of the invention
Main mesh of the invention is to propose a kind of preparation method suitable for copper gadolinium intermediate alloy.Through the method preparation
Copper gadolinium intermediate alloy ingredient is uniform, impurity content is low, fusing point is low, the preparation of the highly beneficial subsequent element modified copper alloy of gadolinium.
Preparation method proposed by the present invention suitable for copper gadolinium intermediate alloy takes vacuum melting mode, including walks as follows
It is rapid:
(1) according to the quality of copper gadolinium intermediate alloy than sorting, ingredient, shove charge；
(2) it vacuumizes, heats up, applying argon gas stirs after metal is completely melt, heat preservation refining, degasification；
(3) it at the uniform velocity casts.
In step (1), the mass percent of gadolinium element is 3%~9% in copper gadolinium intermediate alloy, and surplus is copper；With metal
Copper, gadolinium are raw material, and copper raw material selects A grades of catholyte copper, and purity is not less than 99.9965% (mass percent), gadolinium raw material
Purity is selected to be not less than 99.0% (mass percent) gadolinium element.
In step (1), copper raw material is weighed by design weight when ingredient；It should be on the basis of design weight when weighing gadolinium raw material
3~6% (mass percents) of upper increase, i.e. gadolinium raw material are 103~106% (mass percents) of design weight.
In step (1), melting is carried out using graphite crucible；Charging method are as follows: be laid with 2-5 layers of cutting in graphite crucible bottom
At the electrolytic copper plate (size of electrolytic copper plate fritter is 140mm × 80mm or less) of fritter, gadolinium raw material is broken into average grain diameter
Particle less than 15mm be uniformly laid on electrolysis layers of copper above, then on it cover 1~2 layer of electrolytic copper plate, repeatedly until
All filling finishes raw material.
In step (2), starting to heat up with mid power when being evacuated to pressure less than 0.1Pa, (heating rate is 18~22
DEG C/min), until when cathode copper starts fusing and splashes with trace meter liquid, applying argon gas to 20~30Pa increases power heating
(heating rate is 28~32 DEG C/min) persistently stirs 2~3 minutes to reaction to 1220~1250 DEG C after raw material all fusing
Completely, it is cooled to 1150~1170 DEG C of heat preservations to refine for 8~12 minutes, degasification to pressure is less than 0.8Pa.
In step (3), cast temperature is 1210~1230 DEG C.
In step (3), casting die is the water cooled copper mould with graphite funnel.
The present invention improves smelting efficiency using special loading method, is adjusted by the temperature in each stage in control smelting technology
Melt quality in fusing, reaction and refining process uses water cooled mo(u)ld casting to reduce segregation.The advantages of this method is that can have
Effect reduces the scaling loss of gadolinium, uniform, the internal no significant defect of intermediate alloy ingot chemistry (metallographic structure such as Fig. 1 institute of preparation
Show), ingredient and design composition tolerances are small, are very suitable for the preparation for the modified copper alloy of gadolinium.
Detailed description of the invention
Fig. 1 is Cu-5wt.%Gd intermediate alloy as-cast metallographic structure.
Specific embodiment
Below by way of specific example, the technical scheme of the present invention will be further described, but is not meant to protect the present invention
Protect the limitation of range.
The preparation method of copper gadolinium intermediate alloy of the invention, takes vacuum melting mode, includes the following steps:
(1) shove charge: sorting, ingredient choose the A grade catholyte copper that purity is not less than 99.9965% (mass percent)
Gadolinium with purity not less than 99.0% (mass percent) as raw material, by gadolinium element accounting 3%~9% (mass percent),
Surplus is that copper prepares intermediate alloy and weighs gadolinium and cathode copper, should be increased on the basis of design weight when wherein weighing gadolinium raw material
3~6% (mass percents).The 2-5 layers of electrolytic copper plate for being cut into fritter first are laid in graphite crucible bottom when charging, will be crushed
It is uniformly laid on above electrolysis layers of copper at gadolinium raw material of the average grain diameter less than 15mm, then covers 1~2 layer of electrolytic copper plate on it,
Repeatedly until raw material whole filling finishes.
(2) start heat up with mid power (heating rate is 18~22 DEG C/min) when being evacuated to pressure less than 0.1Pa,
When starting fusing to cathode copper and splash with trace meter liquid, applying argon gas to 20~30Pa increases power heating (heating rate
It is 28~32 DEG C/min) to 1220~1250 DEG C, 2~3 minutes is persistently stirred after raw material all fusing to fully reacting, cooling
It keeps the temperature 8~12 minutes to 1150~1170 DEG C to refine, degasification to pressure is less than 0.8Pa.
(3) temperature is promoted to 1210~1230 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
Embodiment 1:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=97:3.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
97kg is cut into the fritter of about (120mm ± 20mm) × (70mm ± 10mm)；The gadolinium 3.15kg that purity is greater than 99.0wt.% is chosen,
The fritter of average grain diameter 12mm is broken into as raw material.5 layers of electrolytic copper plate are laid in 200kg graphite crucible bottom, by gadolinium particle
It is uniformly laid on above electrolysis layers of copper, then covers 2 layers of electrolytic copper plate on it, be laid with repeatedly up to all filling finishes raw material.
(2) it is evacuated to pressure 8.0 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 30Pa increases power and is warming up to 1250 DEG C, persistently stirs 3 after raw material all fusing
Minute to fully reacting, is cooled to 1170 DEG C of heat preservations and refines for 12 minutes, degasification to pressure is 0.6Pa.
(3) temperature is promoted to 1230 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:96.9wt.%, Gd:
3.1wt.%, and chemical component is uniform, inside no significant defect, impurity content is low, fusing point is low.
Embodiment 2:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=96:4.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
96kg is cut into the fritter of about (120mm ± 20mm) × (70mm ± 10mm)；The gadolinium 4.24kg that purity is greater than 99.0wt.% is chosen,
The fritter of average grain diameter 12mm is broken into as raw material.5 layers of electrolytic copper plate are laid in 200kg graphite crucible bottom, by gadolinium particle
It is uniformly laid on above electrolysis layers of copper, then covers 2 layers of electrolytic copper plate on it, be laid with repeatedly up to all filling finishes raw material.
(2) it is evacuated to pressure 9.0 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 30Pa increases power and is warming up to 1250 DEG C, persistently stirs 3 after raw material all fusing
Minute to fully reacting, is cooled to 1170 DEG C of heat preservations and refines for 12 minutes, degasification to pressure is 0.6Pa.
(3) temperature is promoted to 1230 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:95.9wt.%, Gd:
4.1wt.%, and chemical component is uniform, inside no significant defect, impurity content is low, fusing point is low.
Embodiment 3:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=95:5.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
47.5kg is cut into the fritter of about (100mm ± 20mm) × (50mm ± 10mm)；Choose the gadolinium that purity is greater than 99.0wt.%
2.625kg is broken into the fritter of average grain diameter 10mm as raw material.4 layers of electrolytic copper plate are laid in 100kg graphite crucible bottom,
Gadolinium particle is uniformly laid on above electrolysis layers of copper, then covers 2 layers of electrolytic copper plate on it, is laid with repeatedly until raw material all fills
It completes complete.
(2) it is evacuated to pressure 8.0 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 25Pa increases power and is warming up to 1240 DEG C, persistently stirs 3 after raw material all fusing
Minute to fully reacting, is cooled to 1160 DEG C of heat preservations and refines for 11 minutes, degasification to pressure is 0.5Pa.
(3) temperature is promoted to 1220 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:95.0wt.%, Gd:
5.0wt.%, impurity content is low, fusing point is low.As shown in Figure 1, being Cu-5wt.%Gd intermediate alloy as-cast metallographic structure, by figure
It can be seen that in alloy chemical constituents analysis uniformly, internal no significant defect.
Embodiment 4:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=94:6.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
47kg is cut into the fritter of about (100mm ± 20mm) × (50mm ± 10mm)；The gadolinium 3.12kg that purity is greater than 99.0wt.% is chosen,
The fritter of average grain diameter 10mm is broken into as raw material.4 layers of electrolytic copper plate are laid in 100kg graphite crucible bottom, by gadolinium particle
It is uniformly laid on above electrolysis layers of copper, then covers 2 layers of electrolytic copper plate on it, be laid with repeatedly up to all filling finishes raw material.
(2) it is evacuated to pressure 8.5 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 25Pa increases power and is warming up to 1240 DEG C, persistently stirs 3 after raw material all fusing
Minute to fully reacting, is cooled to 1160 DEG C of heat preservations and refines for 11 minutes, degasification to pressure is 0.5Pa.
(3) temperature is promoted to 1220 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:94.0wt.%, Gd:
6.0wt.%, and chemical component is uniform, inside no significant defect, impurity content is low, fusing point is low.
Embodiment 5:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=93:7.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
37.2kg is cut into the fritter of about (80mm ± 20mm) × (30mm ± 10mm)；Choose the gadolinium that purity is greater than 99.0wt.%
2.912kg is broken into the fritter of average grain diameter 8mm as raw material.3 layers of electrolytic copper plate are laid in 70kg graphite crucible bottom, it will
Gadolinium particle is uniformly laid on above electrolysis layers of copper, then covers 1 layer of electrolytic copper plate on it, is laid with repeatedly until raw material all loads
It finishes.
(2) it is evacuated to pressure 6.0 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 25Pa increases power and is warming up to 1240 DEG C, persistently stirs 2 after raw material all fusing
Minute to fully reacting, is cooled to 1160 DEG C of heat preservations and refines for 10 minutes, degasification to pressure is 0.5Pa.
(3) temperature is promoted to 1220 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:93.1wt.%, Gd:
6.9wt.%, and chemical component is uniform, inside no significant defect, impurity content is low, fusing point is low.
Embodiment 6:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=92:8.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
18.4kg is cut into the fritter of about (50mm ± 10mm) × (30mm ± 10mm)；Choose the gadolinium that purity is greater than 99.0wt.%
1.648kg is broken into the fritter of average grain diameter 5mm as raw material.2 layers of electrolytic copper plate are laid in 50kg graphite crucible bottom, it will
Gadolinium particle is uniformly laid on above electrolysis layers of copper, then covers 1 layer of electrolytic copper plate on it, is laid with repeatedly until raw material all loads
It finishes.
(2) it is evacuated to pressure 5.0 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 20Pa increases power and is warming up to 1230 DEG C, persistently stirs 2 after raw material all fusing
Minute to fully reacting, is cooled to 1150 DEG C of heat preservations and refines for 9 minutes, degasification to pressure is 0.4Pa.
(3) temperature is promoted to 1210 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:92.1wt.%, Gd:
7.9wt.%, and chemical component is uniform, inside no significant defect, impurity content is low, fusing point is low.
Embodiment 7:
A kind of preparation method of copper gadolinium intermediate alloy, takes vacuum melting mode, includes the following steps:
(1) design intermediate alloy mass ratio is Cu:Gd=91:9.It chooses purity and is greater than 99.9965wt.% electrolytic copper plate
9.1kg is cut into the fritter of about (30mm ± 10mm) × (30mm ± 10mm)；Choose the gadolinium that purity is greater than 99.0wt.%
0.927kg is broken into the fritter of average grain diameter 5mm as raw material.2 layers of electrolytic copper plate are laid in 20kg graphite crucible bottom, it will
Gadolinium particle is uniformly laid on above electrolysis layers of copper, then covers 1 layer of electrolytic copper plate on it, is laid with repeatedly until raw material all loads
It finishes.
(2) it is evacuated to pressure 3.0 × 10-2Start to heat up with mid power when Pa, until cathode copper start fusing and with
When trace meter liquid splashes, applying argon gas to 20Pa increases power and is warming up to 1220 DEG C, persistently stirs 2 after raw material all fusing
Minute to fully reacting, is cooled to 1150 DEG C of heat preservations and refines for 8 minutes, degasification to pressure is 0.4Pa.
(3) temperature is promoted to 1210 DEG C, and reactant is at the uniform velocity poured into the water cooled copper mould with graphite funnel.
According to copper gadolinium intermediate alloy prepared by said ratio and technique, chemical component Cu:91.2wt.%, Gd:
8.8wt.%, and chemical component is uniform, inside no significant defect, impurity content is low, fusing point is low.
The present invention takes vacuum melting mode to prepare the copper gadolinium intermediate alloy that gadolinium concentrations are 3%~9% (mass percent),
The copper gadolinium intermediate alloy ingot casting ingredient prepared through the method is uniform and deviation is small, impurity content is low, fusing point is low, internal nothing obviously lacks
It falls into, is very suitable for the preparation for the modified copper alloy of gadolinium.
Claims (7)
1. a kind of preparation method of copper gadolinium intermediate alloy, includes the following steps:
(1) according to the quality of copper gadolinium intermediate alloy than sorting, ingredient, shove charge；The matter of gadolinium element in the copper gadolinium intermediate alloy
Measuring percentage is 3%~9%, and surplus is copper；The charging method of use are as follows: graphite crucible bottom be laid with 2-5 layers be cut into it is small
Gadolinium raw material is broken into particle of the average grain diameter less than 15mm and is uniformly laid on above electrolysis layers of copper by the electrolytic copper plate of block, then
1~2 layer of electrolytic copper plate is covered thereon, repeatedly until raw material whole filling finishes；
(2) it vacuumizes, heats up, applying argon gas stirs after metal is completely melt, heat preservation refining, degasification；
(3) it at the uniform velocity casts, casting die is the water cooled copper mould with graphite funnel.
2. the preparation method of copper gadolinium intermediate alloy as described in claim 1, it is characterised in that: using metallic copper, gadolinium as raw material, copper
Raw material is catholyte copper, and purity is not less than 99.9965w%；Gadolinium raw material is the gadolinium that purity is not less than 99.0w%.
3. the preparation method of copper gadolinium intermediate alloy as claimed in claim 2, it is characterised in that: when ingredient, gadolinium is in design weight
On the basis of increase by 3~6w%.
4. the preparation method of copper gadolinium intermediate alloy as described in claim 1, it is characterised in that: the size of the electrolytic copper plate of fritter
For 140mm × 80mm or less.
5. the preparation method of copper gadolinium intermediate alloy as described in claim 1, it is characterised in that: be evacuated to pressure and be less than
Start to heat up with mid power when 0.1Pa, until when cathode copper starts fusing and splashes with trace meter liquid, applying argon gas to 20~
30Pa increases power and is warming up to 1220~1250 DEG C, and 2~3 minutes are persistently stirred after raw material all fusing to fully reacting, drop
Temperature keeps the temperature 8~12 minutes to 1150~1170 DEG C and refines, and degasification to pressure is less than 0.8Pa.
6. the preparation method of copper gadolinium intermediate alloy as claimed in claim 5, it is characterised in that: the mid power heating
Rate is 18~22 DEG C/min, and the rate for increasing power heating is 28~32 DEG C/min.
7. the preparation method of copper gadolinium intermediate alloy as described in claim 1, it is characterised in that: the cast temperature is 1210
~1230 DEG C.
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