CN106521281A - Modifier and modifying method for low-melting-point impurity element lead in copper and copper alloy - Google Patents
Modifier and modifying method for low-melting-point impurity element lead in copper and copper alloy Download PDFInfo
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- CN106521281A CN106521281A CN201611038728.9A CN201611038728A CN106521281A CN 106521281 A CN106521281 A CN 106521281A CN 201611038728 A CN201611038728 A CN 201611038728A CN 106521281 A CN106521281 A CN 106521281A
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- copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/006—Pyrometallurgy working up of molten copper, e.g. refining
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
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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
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
Abstract
The invention provides a modifier for low-melting-point impurity element lead in copper and copper alloy materials and a modifying method for low-melting-point impurity element lead in copper and copper alloy materials. The copper and copper alloy materials to which the modifier and the modifying method are applicable are copper materials comprising, by weight, 0.001-3% of low-melting-point impurity element lead. According to the copper bar, copper pipe and copper wire modified by the modifying method, the room-temperature mechanical property is improved by 1-10 times than before, the high-temperature mechanical property is improved by 1-40 times than before, the electricity conducting and heat conducting property is improved by 1-2 times than before, and the corrosion resistance property is improved by 20-60% than before.
Description
Technical field
The present invention relates to a kind of process is modified by low melting point element in nonferrous materials, more particularly to one
Plant the modifying agent and method of modifying of low melting point element lead in copper and copper alloy.
Background technology
Low melting point element lead in copper and its alloy during casting blank solidification can finally on crystal boundary segregation separate out,
Make that the chemical composition of copper and Cu alloy material becomes is uneven, makes crystal boundary and intra-die bad student's potential difference, easily makes copper and copper
Alloy part produces micro- galvanic corrosion, therefore the presence of grain boundaries low melting point element can deteriorate the physical mechanics property of copper material
Can, shorten copper material service life, and lead in use can solution modeling, irreversible damage is caused to health
Evil.
The fusing point of lead is 327 DEG C, lead not solid solution substantially in copper, and micro lead forms low melting point with copper in the grain boundaries of copper
Copper-lead eutectic structure, 326 DEG C of eutectic temperature., when hot-working is carried out, copper-lead eutectic first melts, greatly for copper and its alloy
The adhesion between copper and its crystal grain of alloy is reduced, causes copper to produce " hot-short ".As lead can neither form solid solution with copper
Body, can not form compound with copper again, when the atomic hour of content of the lead in copper, meltable thin layer just occur, processed
Crackle is formed along thin layer in journey, the yield rate of Copper fabrication material is reduced.Increase with lead content, the high temperature of copper and Cu alloy material is crisp
Property area can also significantly increase, and increase the hot cracking tendency of copper.Therefore, in copper, the presence of micro lead becomes not only can the hot-working of copper
Difficulty, and room temperature and mechanical behavior under high temperature, electric conductivity and decay resistance of copper material etc. can be reduced.
At present, impurity-removing method conventional in copper processing industry is only for the removal of oxygen, mainly adopts phosphorus deoxidation and Linesless charcoal
Deoxidation, is not also specifically designed for removal and the method for modifying of low melting point element lead.In order to improve the lumber recovery of Copper fabrication material,
Product defects is reduced, the minimizing technology of low melting point element lead and modified Modification Treatment Technique in necessary conducting copper are most
The harm of low melting point element lead in copper may be reduced, the combination property of copper material is improved.
The content of the invention
Defect and danger that the present invention causes for low melting point element lead in copper in solution prior art and Cu alloy material
A kind of evil, there is provided the modifying agent of low melting point element lead in copper and Cu alloy material, and in copper and Cu alloy material
The method of modifying of low melting point element lead.
The copper and Cu alloy material that the present invention is suitable for refers to the copper product comprising low melting point element lead, wherein by weight
Percent meter, copper product of the lead content for 0.001-3%.
The modifying agent of low melting point element lead in a kind of copper and Cu alloy material, the modifying agent is by lanthanum, cerium, yttrium, neodymium
And inevitably impurity element is constituted, percentage,
Lanthanum 10-30%,
Cerium 50-70%,
Yttrium 10-20%,
Neodymium 1-10%,
Balance of inevitable impurity element and impurity content are 0-1%.
A kind of method for removing low melting point element lead in copper removal and copper alloy, comprises the following steps,
Step 1 melts copper material
Copper material containing low melting point element lead is inserted into smelting furnace, using graphite crucible, temperature control is at 1100-1250 DEG C
Copper material is all fused into copper liquid；
Step 2 pre-deoxidation
The copper liquid surface melted in smelting furnace is covered into the charcoal layer that a layer thickness is 4-10 centimetre, adds phosphorus content to exist afterwards
The copper phosphorus intermediate alloy of 10-14%, percentage, the addition of copper phosphorus intermediate alloy account for the copper liquid gross weight of fusing
0.1 ~ 0.3%, then react 0.5-1 hours, it is therefore an objective to make the abundant deoxidation of phosphorus；
Stokehold sample analysis are carried out in course of reaction, phosphorus content and oxygen content in copper liquid is determined by direct-reading spectrometer, in wood
In the presence of charcoal and the common deoxidation of copper phosphorus intermediate alloy, until most phosphorus content is controlled in 50-200ppm, oxygen content in copper liquid at last
Control is in 0-10ppm；
Step 3 copper material is modified
Copper liquid after pre-deoxidation is warming up to after 1250-1280 DEG C, above-mentioned modifying agent, and electromagnetic agitation 20-30 minute is added, so
After remove scum silica frost；
By the percent by weight of copper liquid, when in copper liquid, lead content is 0.001-3%, the addition of the modifying agent is 0.01-
10%；
The purpose of the step is modifying agent is fully melted and is had an effect with lead impurity element completely, generates REPb3、REPb、
RE3Pb、RE5Pb3Deng compound, RE represents lanthanum, cerium, yttrium, neodymium.These melting point compounds are high, and density is little, in copper liquid with compared with
Big surface tension, can be present in copper liquid with the likeness in form of spheroidal particle, can be deposited after final solidification in the form of Second Phase Particle
It is intra-die, plays a part of second-phase strength in copper material, the mechanical property of copper material can be improved.The addition of modifying agent
Make lead be changed into more uniform in crystal boundary from integrated distribution and be distributed in intra-die, improve the uniformity of chemical composition, can be with
Improve the electrical and thermal conductivity performance and decay resistance of copper material.
Step 4 casting copper material
Modified copper liquid is stood into 30-40 minutes, is then cast in the mould through preheating, is obtained to low melting point after cooling
The modified as cast condition copper material of lead impurity element.
Through the modified copper bar material of said method, copper pipe and copper wires, its room-temperature mechanical property is improved more before modified
1-10 times, mechanical behavior under high temperature improve more before modified 1-40 times, electrical and thermal conductivity performance improve 1-2 times, corrosion resistance more before modified
20-60% is improved more before modified can.
As shown in Fig. 1 Fig. 2, Fig. 1 is the non-modified microstructure morphology containing low melting point element copper in the present invention.
In figure, the main integrated distribution of impurity element is on crystal boundary.This is, as the fusing point of low melting point element is less than the fusing point of copper, to coagulate
Gu during be gathered in the liquid phase in solid-liquid interface forward position, and final solidify in grain boundaries.Therefore, the low-melting impurities in copper
Element can typically be gathered in grain boundaries.
Fig. 2 is the modified microstructure morphology containing low melting point element copper in the present invention.It is miscellaneous on crystal boundary in figure
Prime element is significantly reduced, and be the substitute is and is occurred in that equally distributed spheroidal particle in intra-die, and this is low-melting impurities
The compound that element and modifying agent are generated.
Further, based on the percentage by weight of copper material, when in copper material lead content be 0.001-0.01%, the modifying agent
Reasonable addition be 0.01-0.05%；When in copper material, lead content is 0.01-0.1%, the reasonable addition of the modifying agent is
0.05-1%；When in copper material, lead content is 0.1-1%, the reasonable addition of the modifying agent is 0.05-6%；When lead content in copper material
For 1-3%, the reasonable addition of the modifying agent is 6-10%.
The effect of Linesless charcoal and phosphor-copper pre-deoxidation in the present invention has in terms of two：On the one hand, Linesless charcoal can completely cut off air, prevent copper
Melt oxygen uptake；On the other hand, Linesless charcoal and phosphor-copper can pre-deoxidations.Add the low melting point element modifying agent can be with after pre-deoxidation
Modifying agent is acted on low melting point element, effectively prevent the autoxidation of modifying agent, play to modifying agent effect
Protective effect.In modified dose of modified Copper fabrication material, low melting point element is changed into ball from integrated distribution in crystal boundary
The form of shape particle is more uniform to be distributed in intra-die, and in deformation process, these particles can play obstruction dislocation motion
Effect, play a part of second-phase strength.The addition of modifying agent can also refine the microstructure of copper material so as to which crystal grain is obtained
Refinement, chemical composition become evenly, moreover it is possible to reduce the stress concentration in the course of processing, reduce impurity defect and there is the electricity for causing
Sub- scattering process, hence it is evident that improve the combination property of copper material.
Description of the drawings
Fig. 1 is the microstructure morphology of the non-modified copper containing low melting point element lead in the present invention.
Fig. 2 is the microstructure morphology of the modified copper containing low melting point element lead in the present invention.
Specific embodiment
With reference to embodiment, the present invention is described in detail, but protection domain is not limited by this.
A kind of process being modified to low melting point element lead in copper of embodiment 1, which concretely comprises the following steps, 1190
DEG C fusing containing 0.1% lead 9.91 kilograms of composition brass（Percentage）, it is 5 centimetres to cover a layer thickness on copper liquid surface
Charcoal layer, adds 21 grams of the copper phosphorus intermediate alloy of phosphorus content 13%, reacts 0.5 hour, then stokehold sample analysis, by direct-reading
Phosphorus content and oxygen content in spectrophotometer copper liquid, wherein, in copper liquid, phosphorus content is controlled in 70-80ppm, and Control for Oxygen Content exists
0-3ppm；After carrying out pre-deoxidation, copper liquid temperature is risen to into 1250 DEG C, add 33 grams of low melting point element modifying agent, wherein, lanthanum
7.1 grams, 18.3 grams of cerium, 4.7 grams of yttrium, 2.9 grams of neodymium, electromagnetic agitation 22 minutes, after copper liquid stands 30 minutes, are cast to 300 DEG C of Jing
In the preheating swage of 0.5 hour, the modified casting in bronze ingot of low melting point element lead is obtained.Its as-cast characteristic index is shown in Table 1.
A kind of process being modified to low melting point element lead in copper of embodiment 2, which concretely comprises the following steps, 1200
DEG C fusing containing 0.01% lead 9.99 kilograms of composition brass（Percentage）, a layer thickness is covered for 5.5 centimetres on copper liquid surface
Charcoal layer, add 20 grams of the copper phosphorus intermediate alloy of phosphorus content 14%, react 0.7 hour, then stokehold sample analysis, by straight
Read the phosphorus content and oxygen content in spectrophotometer copper liquid, wherein, in copper liquid, phosphorus content is controlled in 80-100ppm, oxygen content control
System is in 0-5ppm；After carrying out pre-deoxidation, copper liquid temperature is risen to into 1260 DEG C, add 3.1 grams of low melting point element modifying agent, its
In, 0.7 gram of lanthanum, 1.8 grams of cerium, 0.5 gram of yttrium, 0.1 gram of neodymium, electromagnetic agitation 25 minutes, after copper liquid stands 35 minutes, are cast to Jing
In 350 DEG C of preheatings swage of 0.4 hour, the modified casting in bronze ingot of low melting point element lead is obtained.Its as-cast characteristic index is shown in
Table 1.
A kind of process being modified to low melting point element lead in copper of embodiment 3, which concretely comprises the following steps, 1180
DEG C fusing containing 0.5% lead 10.27 kilograms of composition brass（Percentage）, a layer thickness is covered for 5.8 centimetres on copper liquid surface
Charcoal layer, add 18 grams of the copper phosphorus intermediate alloy of phosphorus content 12%, react 0.6 hour, then stokehold sample analysis, by straight
Read the phosphorus content and oxygen content in spectrophotometer copper liquid, wherein, in copper liquid, phosphorus content is controlled in 75-85ppm, Control for Oxygen Content
In 0-8ppm；After carrying out pre-deoxidation, copper liquid temperature is risen to into 1255 DEG C, add 98 grams of low melting point element modifying agent, wherein,
19.6 grams of lanthanum, 58..8 gram of cerium, 9.8 grams of yttrium, 9.8 grams of neodymium, electromagnetic agitation 23 minutes, after copper liquid stands 36 minutes, are cast to Jing
In 330 DEG C of preheatings swage of 0.6 hour, the modified casting in bronze ingot of low melting point element lead is obtained.Its as-cast characteristic index is shown in
Table 1.
A kind of process being modified to low melting point element lead in copper of embodiment 4, which concretely comprises the following steps, 1230
DEG C fusing containing 1.2% lead 10.02 kilograms of composition brass（Percentage）, a layer thickness is covered for 5.6 centimetres on copper liquid surface
Charcoal layer, add 23 grams of the copper phosphorus intermediate alloy of phosphorus content 10%, react 0.8 hour, then stokehold sample analysis, by straight
Read the phosphorus content and oxygen content in spectrophotometer copper liquid, wherein, in copper liquid, phosphorus content is controlled in 110-130ppm, oxygen content control
System is in 0-4ppm；After carrying out pre-deoxidation, copper liquid temperature is risen to into 1275 DEG C, add 410 grams of low melting point element modifying agent, its
In, 123 grams of lanthanum, 205 grams of cerium, 41 grams of yttrium, 41 grams of neodymium, electromagnetic agitation 30 minutes, after copper liquid stands 38 minutes, are cast to Jing 370
In DEG C preheating swage of 0.3 hour, the modified casting in bronze ingot of low melting point element lead is obtained.Its as-cast characteristic index is shown in Table 1.
Table 1
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to the tool in above-mentioned embodiment
Body details, in the range of the technology design of the present invention, can carry out various equivalents to technical scheme, these etc.
Protection scope of the present invention is belonged to conversion.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means.In order to avoid unnecessary repetition, the present invention to it is various can
The compound mode of energy is no longer separately illustrated.Additionally, any group can also be carried out between a variety of embodiments of the present invention
Close, as long as which is without prejudice to the thought of the present invention, which should equally be considered as content disclosed in this invention.
Claims (3)
1. in a kind of copper and Cu alloy material low melting point element lead modifying agent, it is characterised in that the modifying agent by lanthanum,
Cerium, yttrium, neodymium and inevitable impurity element composition, percentage,
Lanthanum is 10-30%,
Cerium is 50-70%,
Yttrium is 10-20%,
Neodymium is 1-10%,
Balance of inevitable impurity element and impurity content are 0-1%.
2. a kind of method for removing low melting point element lead in copper removal and copper alloy, comprises the following steps,
Step 1 melts copper material
Copper material containing low melting point element lead is inserted into smelting furnace, using graphite crucible, temperature control is at 1100-1250 DEG C
Copper material is all fused into copper liquid；
Characterized in that,
Step 2 pre-deoxidation
The copper liquid surface melted in smelting furnace is covered into the charcoal layer that a layer thickness is 4-10 centimetre, phosphorus content is added in 10-14%
Copper phosphorus intermediate alloy, percentage, the addition of copper phosphorus intermediate alloy account for the 0.1- of the copper liquid gross weight of fusing
0.3%, 0.5-1 hours are then reacted,
Stokehold sample analysis are carried out in course of reaction, phosphorus content and oxygen content in copper liquid is determined by direct-reading spectrometer, in wood
In the presence of charcoal and the common deoxidation of copper phosphorus intermediate alloy, until most phosphorus content is controlled in 50-200ppm, oxygen content in copper liquid at last
Control is in 0-10ppm；
Step 3 copper material is modified
Copper liquid after pre-deoxidation is warming up to after 1250-1280 DEG C, modifying agent described in claim 1, and electromagnetic agitation 20- is added
30 minutes, then remove scum silica frost；
By the percent by weight of copper liquid, when in copper liquid, lead content is 0.001-3%, the addition of the modifying agent is 0.01-
10%；
Step 4 casting copper material
Modified copper liquid is stood into 30-40 minutes, is then cast in the mould through preheating, is obtained to low melting point after cooling
The modified as cast condition copper material of lead impurity element.
3. a kind of method for removing low melting point element lead in copper removal and copper alloy according to claim 2, its feature exist
In based on the percentage by weight of copper material, when in copper material, lead content is 0.001-0.01%, the addition of modifying agent described in claim 1
Measure as 0.01-0.05%；When in copper material, lead content is 0.01-0.1%, the addition of modifying agent described in claim 1 is 0.05-
1%；When in copper material, lead content is 0.1-1%, the addition of modifying agent described in claim 1 is 0.05-6%；When lead content in copper material
For 1-3%, the addition of modifying agent described in claim 1 is 6-10%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108034837A (en) * | 2017-11-28 | 2018-05-15 | 上海龙阳精密复合铜管有限公司 | A kind of quick production method for removing red copper stove liquid impurity |
| CN111187917A (en) * | 2020-02-26 | 2020-05-22 | 烟台大学 | Removing agent and removing method for low-content impurity element tin in copper melt |
| CN111751298A (en) * | 2020-07-21 | 2020-10-09 | 襄阳金湛技术开发有限公司 | Method for measuring content of non-metal elements in crude lead |
| CN112008051A (en) * | 2020-09-04 | 2020-12-01 | 江苏亨通电力智网科技有限公司 | Production method of rare earth refined copper liquid reduction transition rod |
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| CN102925733A (en) * | 2012-11-13 | 2013-02-13 | 宁波兴业鑫泰新型电子材料有限公司 | Multifunctional covering agents of copper alloy suitable for lead frame |
| CN105603201A (en) * | 2016-03-21 | 2016-05-25 | 江西保太有色金属集团有限公司 | Impure red copper refining method through dumping, transferring, melting and casting |
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| CN101768680A (en) * | 2008-12-26 | 2010-07-07 | 北京有色金属研究总院 | Composite modifier for copper alloy of lead frame |
| CN102925733A (en) * | 2012-11-13 | 2013-02-13 | 宁波兴业鑫泰新型电子材料有限公司 | Multifunctional covering agents of copper alloy suitable for lead frame |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108034837A (en) * | 2017-11-28 | 2018-05-15 | 上海龙阳精密复合铜管有限公司 | A kind of quick production method for removing red copper stove liquid impurity |
| CN111187917A (en) * | 2020-02-26 | 2020-05-22 | 烟台大学 | Removing agent and removing method for low-content impurity element tin in copper melt |
| CN111187917B (en) * | 2020-02-26 | 2021-09-14 | 烟台大学 | Removing agent and removing method for low-content impurity element tin in copper melt |
| CN111751298A (en) * | 2020-07-21 | 2020-10-09 | 襄阳金湛技术开发有限公司 | Method for measuring content of non-metal elements in crude lead |
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| CN112008051A (en) * | 2020-09-04 | 2020-12-01 | 江苏亨通电力智网科技有限公司 | Production method of rare earth refined copper liquid reduction transition rod |
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