CN101974701A - Double-annealing process treatment method for enhancing surface antioxidant capacity of copper element - Google Patents
Double-annealing process treatment method for enhancing surface antioxidant capacity of copper element Download PDFInfo
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Abstract
The invention relates to a double-annealing process treatment method for enhancing the surface antioxidant capacity of a copper element. The double-annealing process treatment method adds Al elements to the surface of Cu to segregate to form protective films on an integrated circuit copper lead and a copper radiator during Cu smelting and particularly generate a Cu-A2O3 composite protective film through double-annealing process treatment, thereby enhancing the surface antioxidant capacity of the copper element made of integrated circuit lead frame materials and the copper radiator. The double-annealing process treatment method comprises the following steps of: mixing a small amount of the Al with the Cu, and repeatedly smelting to prepare a copper-aluminium alloy in an electric arc furnace; sequentially carrying out the double-annealing process treatment at an H2 atmosphere and an Ar atmosphere, then preserving the temperature for certain time, and cooling to room temperature to prepare an antioxidant copper element. The invention has the advantage that after the Al elements are added, the Al contained in the copper-aluminium alloy is segregated to the surface of the Cu through segregation action during the annealing process and reacts with O remained at an annealing atmosphere to generate A2O3 on the surface of the copper-aluminium alloy and form a Cu-A2O3 composite adhesive film which has good mechanical property on the surface of the Cu.
Description
Technical field:
The present invention relates to a kind of method that improves the metallic surface resistance of oxidation, especially form the CuAl alloy by adding the Al element during melting Cu, successively at H
2With the Cu-Al that handles back Cu surface generation in the atmosphere of Ar through two annealing processs
2O
3The mixture protective membrane is and at H
2Once annealing under the atmosphere is compared, and the resistance of oxidation on circuit lead frame material copper components and parts and copper radiator surface is improved, and its Applicable temperature has risen to 973K by 673K.
Background technology:
Copper has physics-chem characteristics such as good electrical conductivity, thermal conductivity, erosion resistance and ductility, and its conductivity and heat conductivility are only second to silver, and fine copper can pull into very thin copper wire, makes very thin Copper Foil.Copper is owing to have an above-mentioned premium properties, so industrial purposes widely arranged, comprises aspects such as electric utility, machinofacture, traffic, building.At present, copper is mainly used in this field of Electrical and Electronic industry makes electric wire, communication cable and other finished products such as electric motor, generator amature and electronic machine, instrument etc., and this part consumption accounts for about half of industrial aggregate demand; In various household equipments and utensil, for conductive and heat-conductive, all to use copper, its intensity, ductility and solidity to corrosion make it become the excellence conductor of circuit, and it still makes the material of electric motor and transformer also as the power cable of high, medium and low voltage; In roof construction,, be worth with copper in order to resist extreme climate; Transportation equipment is mainly used copper, for example boats and ships, automobile and aircraft, and hull can prevent the formation of biofouling with cupronickel, lowers resistance.Copper material is that the history of making the optimal material of scatterer is of long duration, and can produce high quality, high-performance, life-span length, light weight, scatterer that price is low with lower energy consumption as the copper of primary metal.In the high temperature cooling system, and in the big electric current such as nuclear power generating equipment, powerful environment, the heat transfer tube of using on evaporator-condenser is all made of copper basically.
Oxidation unavoidably will take place in copper in Working environment, because the oxide compound of copper does not have self-protective, fine copper at high temperature oxidation-resistance is more weak; can make the further oxidation of copper; thereby influence the works better of components and parts, even components and parts are damaged, limited the further application of copper.
Add alloying elements in pure Cu, for example Ni, Cr, Ti etc. can improve the resistance of oxidation of pure Cu, but after having added above-mentioned alloying element, the resistance of copper alloy will improve, thereby influences its conductive capability.And after in fine copper, adding the relatively low alloying element Mg of resistivity, form copper-magnesium alloy, and after the annealed processing of alloy, the magnesium oxide films that the surface forms is discontinuous, and the surface is fine and close and relatively poor with matrix bond inadequately, so its resistance of oxidation is limited.In addition, the resistivity of Al is relatively low, and is cheap with respect to other metals, and Al
2O
3Has self-protective.In Cu, mix a spot of Al element, form copper aluminium light alloy, by single H
2Anneal forms oxidation barrier film on the surface.Though this method can improve its surface oxidation-resistant ability, because the thickness of surface oxidation-resistant film is less, resistance of oxidation improves limited, and the oxidation resistance temperature of alloy only limits to 673K.When use temperature was higher than 673K, the rate of oxidation of Cu was accelerated, and effect is not very desirable.
Summary of the invention
The objective of the invention is at above-mentioned the deficiencies in the prior art; a kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation are provided; this method is after copper lead of integrated circuit and copper radiator are adding a small amount of Al element, and increase surface protection film thickness is to improve its surface oxidation-resistant ability after two annealing processs are handled.Alloy is successively at H
2After carrying out anneal in the atmosphere of Ar, the Cu surface generate continuous, fine and close and with matrix bond Cu-Al preferably
2O
3The mixture protective membrane, its thickness can well solve the problem of oxidation of Cu, has strengthened the resistance of oxidation on Cu surface, has prolonged the work-ing life of copper coin device.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation may further comprise the steps:
A, be that the pure Cu of 99.99wt.% is that the pure Al of 99.99wt.% mixes with granular purity with blocky purity, pure Cu content is 99.8～98.0wt.% in the compound, and pure Al content is 0.2～2.0wt.%;
B, mixed material is placed electric arc furnace, then body of heater is evacuated to 0.5Pa～5.0Pa after, feed high-purity argon gas, the purity of argon gas is 99.999%～99.9999%, it is 3000～6000cm that high-purity argon gas feeds flow
3/ min, air pressure are a normal atmosphere, adopt water-cooled, and the infusible mode in bottom is smelted;
C, startup electric arc furnace make Cu and Al alloying element in 1423K～1473K fusing by glow discharge, melt back 6～8 times, and the X alloy ingot is made in each melting 5～8 minutes;
D, the X alloy ingot is cut into small pieces with line after, on roller mill, be rolled into the thin slice that thickness is 0.5mm, it is the X alloy disk of 5mm that the thin slice punching out is become diameter, and putting into then and being connected with purity is that the process furnace of 99.999%～99.9999% high-purity hydrogen is annealed in 673K～973K temperature;
E, in annealing temperature, be incubated 360min～1440min, in being connected with the environment that purity is 99.999%～99.9999% high-purity hydrogen, be cooled to room temperature;
F, feed high purity argon in stove, alloy is further annealed, annealing temperature is 473K～1273K, and soaking time is 360min～720min, is cooled to room temperature in being connected with the environment of high-purity argon gas, is prepared into anti-oxidant copper sample.
The described melt back of step c 6～8 times, each smelting temperature is 1423K～1473K, and smelting time is 5～8 minutes, stops melting afterwards, reduces to room temperature, opens stove and spins upside down material, and refuse is smelted once more, and so melt back is 6～8 times.
The described glow discharge power of step c is 2～10kW.
The gas feeding amount of the described feeding high-purity hydrogen of steps d is 50～200cm
3/ min.
The gas feeding amount of the described feeding high-purity argon gas of step f is 50～200cm
3/ min.
Beneficial effect: the rate of oxidation of fine copper lead-in wire is very fast in the unicircuit, add the Al alloying element and formed X alloy, in two annealing process treating processess, Al segregates to the Cu surface in the alloy, Al because and the strong affinity interaction between the O generated Al by the oxidation of residual in hydrogen oxygen institute
2O
3, form Cu-Al on the surface of Cu
2O
3The mixture coherent film has improved the oxidation resistant ability of copper wire surface, suppresses the further oxidation of copper lead-in wire.With single H
2Annealing treating process is compared, and this pair annealing process has increased the thickness of surface complex, has improved the oxidation resistant temperature of copper coin device, thereby has greatly improved the use temperature and the work-ing life that has prolonged scatterer of copper lead-in wire and scatterer.Specifically, with at H
2The single annealing process is handled the Cu-Al that forms under the atmosphere
2O
3Film compares, and the complexes membrane thickness that forms after two annealing processs are handled increases, the resistance of oxidation enhancing, and the oxidation resistance temperature of copper lead of integrated circuit and copper radiator has risen to 973K by 673K.
Description of drawings:
X alloy surface C u, Al, the O concentration depth profiling of Fig. 1 after hydrogen and the two annealing processs processing of argon gas.
Wherein: (a) Al content is X alloy surface C u, Al, the O concentration depth profiling of 0.2%wt.;
(b) Al content is X alloy surface C u, Al, the O concentration depth profiling of 1.0%wt.;
(c) Al content is X alloy surface C u, Al, the O concentration depth profiling of 2.0%wt..
Fig. 2 Al content is the transmission electron microscope morphology observation of the X alloy of 0.2%wt..
Wherein: (a) X alloy surface C u/Al under two annealing process treatment condition
2O
3Mixture forms the cross section close-up view;
(b) Cu/Al
2O
3Mixture cross section enlarged view;
(c) Cu/Al
2O
3Mixture Cu nanoparticle enlarged view, illustration are copper particle transmission electron microscope diffractogram.
Fig. 3 fine copper and through two annealed X alloys respectively at the oxidation kinetics curve of 673K and 973K.
Embodiment:
Further specify particular content of the present invention and embodiment thereof below in conjunction with the accompanying drawing illustrated embodiment.
A kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation comprise following order and step:
A, be that the pure Cu of 99.99wt.% is that the pure Al of 99.99wt.% mixes with granular purity with blocky purity, pure Cu content is 99.8～98.0wt.% in the compound, and pure Al content is 0.2～2.0wt.%;
B, mixed material is placed electric arc furnace, then body of heater is evacuated to 0.5Pa～5.0Pa after, feeding purity is 99.999%～99.9999% high-purity argon gas, it is 3000～6000cm that high-purity argon gas feeds flow
3/ min, air pressure are a normal atmosphere;
C, startup electric arc furnace, by glow discharge, discharge power is 2～10kW, make Cu and Al alloying element be warming up to 1423K～1473K fusing, melt back 6～8 times, each smelting temperature is 1423K～1473K, melting 5～8 minutes, stop melting afterwards, reduce to room temperature, open stove, spin upside down material, refuse is smelted once more, and so melt back is made the X alloy ingot 6～8 times;
D, the X alloy ingot is rolled into the thin slice that thickness is 0.5mm with the line back that is cut into small pieces on roller mill, it is the X alloy disk of 5mm that the thin slice punching out is become diameter, and putting into then and being connected with purity is that the process furnace of 99.999%～99.9999% high-purity hydrogen is annealed in 673K～973K temperature;
E, in annealing temperature, be incubated 360min～1440min, in being connected with the environment that purity is 99.999%～99.9999% high-purity hydrogen, be cooled to room temperature;
F, feed high purity argon in stove, alloy is further annealed, annealing temperature is 473K～1273K, and soaking time is 360min～720min, is cooled to room temperature in being connected with the environment of high-purity argon gas, is prepared into anti-oxidant copper sample.
Consult Fig. 1, in the sputter starting stage, the strength of signal of Al and O is stronger, and the strength of signal of Cu is more weak, and illustrating at alloy surface has a large amount of Al
2O
3Exist.Along with the increase of sputtering time, the degree of depth is deepened, and the strength of signal of Al and O weakens gradually, and the strength of signal of Cu begins grow, surpass the strength of signal of Al and O and almost remain unchanged, illustrate in alloy inside near the fine copper composition, these all show at alloy surface and exist Cu-Al
2O
3Mixture.Wherein, Al content is that the protective membrane thickness that the alloy surface of 0.2%wt., 1.0%wt. and 2.0%wt. forms is respectively 360nm, 380nm and 210nm.
Consult Fig. 2, (a) scheme the coherent film Al of alloy, surface generation as can be seen
2O
3And the linking of their middle transitional layers is tightr, and Al
2O
3Oxide thickness is thicker; (b) Al that generates as can be seen among the figure
2O
3Matrix is evenly distributed on the Cu particle surface; (c) figure is the transmission electron microscope diffraction pattern of X alloy, has been covered with Al around the Cu particle
2O
3Matrix.
Consult Fig. 3, its surface oxidation-resistant ability of X alloy after two annealing processs are handled is higher than fine copper far away, and still has goodish resistance of oxidation when 973K.
Embodiment 1
A, be that the pure Cu of 99.99wt.% is that the pure Al of 99.99wt.% mixes with granular purity with blocky purity, pure Cu content is 99.8wt.% in the compound, and pure Al content is 0.2wt.%;
B, mixed material is placed electric arc furnace, close fire door, then body of heater is vacuumized, after vacuum reaches 0.5Pa, stop to vacuumize, feeding purity in electric arc furnace is 99.9999% high-purity argon gas, and the feeding flow is 3000cm
3/ min, air pressure are a normal atmosphere;
C, startup electric arc furnace, by glow discharge, discharge power is made as 2kW, make Cu and Al alloying element be warming up to the 1473K fusing, stop melting in melting under the 1473K temperature after 5 minutes, reduce to room temperature, open stove, spin upside down material, overturn and closed upper furnace door, and then body of heater vacuumized, when vacuum reaches 0.5Pa, stop to vacuumize, feeding purity is 99.9999% high-purity argon gas, alloy is warming up to the 1473K fusing, and fusing was smelted 5 minutes under the 1473K temperature, and so melt back is made the X alloy ingot 6 times;
D, the X alloy ingot is cut into small pieces with line after, on roller mill, be rolled into the thin slice that thickness is 0.5mm, it is the X alloy disk of 5mm that the thin slice punching out is become diameter, put into process furnace then, close fire door, and carry out encapsulation process, avoid the air admission body of heater.Feeding purity in process furnace is 99.9999% high-purity hydrogen, and the feeding amount is 50cm
3/ min after the air emptying in the stove to be heated, is heated to body of heater and stops heating behind the 873K, and alloy is annealed under this temperature;
E, stopping anneal alloy is incubated 1440min in the annealing temperature of 873K after, is 50cm in the feeding amount
3The purity of/min is to be cooled to room temperature in the environment of 99.9999% high-purity hydrogen;
F, in stove, feed 50cm
3/ min high purity argon is further annealed alloy, and annealing temperature is 873K, and soaking time is 480min, is cooled to room temperature in being connected with the environment of high-purity argon gas, is prepared into anti-oxidant copper sample.
A, be that the pure Cu of 99.99wt.% is that the pure Al of 99.99wt.% mixes with granular purity with blocky purity, pure Cu content is 99.0wt.% in the compound, and pure Al content is 1.0wt.%;
B, mixed material is placed electric arc furnace, close fire door, then body of heater is vacuumized, after vacuum reaches 0.5Pa, stop to vacuumize, feeding purity in electric arc furnace is 99.9999% high-purity argon gas, and the feeding flow is 3000cm
3/ min, air pressure are a normal atmosphere;
C, startup electric arc furnace, by glow discharge, discharge power is made as 2kW, make Cu and Al alloying element be warming up to the 1473K fusing, stop melting in melting under the 1473K temperature after 5 minutes, reduce to room temperature, open stove, spin upside down material, overturn and closed upper furnace door, and then body of heater vacuumized, when vacuum reaches 0.5Pa, stop to vacuumize, feeding purity is 99.9999% high-purity argon gas, alloy is warming up to the 1473K fusing, and fusing was smelted 5 minutes under the 1473K temperature, and so melt back is made the X alloy ingot 6 times;
D, the X alloy ingot is cut into small pieces with line after, on roller mill, be rolled into the thin slice that thickness is 0.5mm, it is the X alloy disk of 5mm that the thin slice punching out is become diameter, put into process furnace then, close fire door, and carry out encapsulation process, avoid the air admission body of heater.Feeding purity in process furnace is 99.9999% high-purity hydrogen, and the feeding amount is 50cm
3/ min after the air emptying in the stove to be heated, is heated to body of heater and stops heating behind the 873K, and alloy is annealed under this temperature;
E, stopping anneal alloy is incubated 1440min in the annealing temperature of 873K after, is 50cm in the feeding amount
3The purity of/min is to be cooled to room temperature in the environment of 99.9999% high-purity hydrogen;
F, in stove, feed 50cm
3/ min high purity argon is further annealed alloy, and annealing temperature is 873K, and soaking time is 480min, is cooled to room temperature in being connected with the environment of high-purity argon gas, is prepared into anti-oxidant copper sample.
Embodiment 3
A, be that the pure Cu of 99.99wt.% is that the pure Al of 99.99wt.% mixes with granular purity with blocky purity, pure Cu content is 98.0wt.% in the compound, and pure Al content is 2.0wt.%;
B, mixed material is placed electric arc furnace, close fire door, then body of heater is vacuumized, after vacuum reaches 0.5Pa, stop to vacuumize, feeding purity in electric arc furnace is 99.9999% high-purity argon gas, and the feeding flow is 3000cm
3/ min, air pressure are a normal atmosphere;
C, startup electric arc furnace, by glow discharge, discharge power is made as 2kW, make Cu and Al alloying element be warming up to the 1473K fusing, stop melting in melting under the 1473K temperature after 5 minutes, reduce to room temperature, open stove, spin upside down material, overturn and closed upper furnace door, and then body of heater vacuumized, when vacuum reaches 0.5Pa, stop to vacuumize, feeding purity is 99.9999% high-purity argon gas, alloy is warming up to the 1473K fusing, and fusing was smelted 5 minutes under the 1473K temperature, and so melt back is made the X alloy ingot 6 times;
D, the X alloy ingot is rolled into the thin slice that thickness is 0.5mm with the line back that is cut into small pieces on roller mill, it is the X alloy disk of 5mm that the thin slice punching out is become diameter, puts into process furnace then, closes fire door, and carry out encapsulation process, avoid the air admission body of heater.Feeding purity in process furnace is 99.9999% high-purity hydrogen, and the feeding amount is 50cm
3/ min after the air emptying in the stove to be heated, is heated to body of heater and stops heating behind the 873K, and alloy is annealed under this temperature;
E, stopping anneal alloy is incubated 1440min in the annealing temperature of 873K after, is 50cm in the feeding amount
3The purity of/min is to be cooled to room temperature in the environment of 99.9999% high-purity hydrogen;
F, feed high purity argon in stove, alloy is further annealed, annealing temperature is 873K, and soaking time is 480min, is cooled to room temperature in being connected with the environment of high-purity argon gas, is prepared into anti-oxidant copper sample.
Claims (5)
1. the two annealing process treatment processs that improve copper coin device surface resistance of oxidation is characterized in that, may further comprise the steps:
A, be that the pure Cu of 99.99wt.% is that the pure Al of 99.99wt.% mixes with granular purity with blocky purity, pure Cu content is 99.8～98.0wt.% in the compound, and pure Al content is 0.2～2.0wt.%;
B, mixed material is placed electric arc furnace, then body of heater is evacuated to 0.5Pa～5.0Pa after, feed high-purity argon gas, the purity of argon gas is 99.999%～99.9999%, it is 3000～6000cm that high-purity argon gas feeds flow
3/ min, air pressure are a normal atmosphere, adopt water-cooled, and the infusible mode in bottom is smelted;
C, startup electric arc furnace make Cu and Al alloying element in 1423K～1473K fusing by glow discharge, melt back 6～8 times, and the X alloy ingot is made in each melting 5～8 minutes;
D, the X alloy ingot is cut into small pieces with line after, on roller mill, be rolled into the thin slice that thickness is 0.5mm, it is the X alloy disk of 5mm that the thin slice punching out is become diameter, and putting into then and being connected with purity is that the process furnace of 99.999%～99.9999% high-purity hydrogen is annealed in 673K～973K temperature;
E, in annealing temperature, be incubated 360min～1440min, in being connected with the environment that purity is 99.999%～99.9999% high-purity hydrogen, be cooled to room temperature;
F, feed high purity argon in stove, alloy is further annealed, annealing temperature is 473K～1273K, and soaking time is 360min～720min, is cooled to room temperature in being connected with the environment of high-purity argon gas, is prepared into anti-oxidant copper sample.
2. according to the described a kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation of claim 1, it is characterized in that, the described melt back of step c 6～8 times, each smelting temperature is 1423K～1473K, and smelting time is 5～8 minutes, stops melting afterwards, reduce to room temperature, open stove and spin upside down material, refuse is smelted once more, and so melt back is 6～8 times.
3. according to the described a kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation of claim 1, it is characterized in that the described glow discharge power of step c is 2～10kW.
4. according to the described a kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation of claim 1, it is characterized in that the gas feeding amount of the described feeding high-purity hydrogen of steps d is 50～200cm
3/ min.
5. according to the described a kind of two annealing process treatment processs that improve copper coin device surface resistance of oxidation of claim 1, it is characterized in that the gas feeding amount of the described feeding high-purity argon gas of step f is 50～200cm
3/ min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110863121A (en) * | 2019-11-18 | 2020-03-06 | 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 | Oxidation-resistant copper-aluminum alloy, preparation method thereof and electrical contact prepared from alloy |
| CN113862506A (en) * | 2021-10-15 | 2021-12-31 | 吉林大学 | Method for improving oxidation resistance of metal copper |
| CN117305741A (en) * | 2023-12-01 | 2023-12-29 | 中铝科学技术研究院有限公司 | High-conductivity low-surface-profile copper foil and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101831566A (en) * | 2010-06-10 | 2010-09-15 | 吉林大学 | Method for preparing composite membrane for improving oxidation resistance of copper lead of integrated circuit |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101831566A (en) * | 2010-06-10 | 2010-09-15 | 吉林大学 | Method for preparing composite membrane for improving oxidation resistance of copper lead of integrated circuit |
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| 《吉林大学硕士学位论文》 20090915 董婧文 退火工艺对铜铝合金高温抗氧化性的影响 第42页第7行-倒数第1行，第60页的第5章 结论部分 1-5 , 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110863121A (en) * | 2019-11-18 | 2020-03-06 | 内蒙古电力(集团)有限责任公司内蒙古电力科学研究院分公司 | Oxidation-resistant copper-aluminum alloy, preparation method thereof and electrical contact prepared from alloy |
| CN113862506A (en) * | 2021-10-15 | 2021-12-31 | 吉林大学 | Method for improving oxidation resistance of metal copper |
| CN117305741A (en) * | 2023-12-01 | 2023-12-29 | 中铝科学技术研究院有限公司 | High-conductivity low-surface-profile copper foil and preparation method and application thereof |
| CN117305741B (en) * | 2023-12-01 | 2024-04-12 | 中铝科学技术研究院有限公司 | High-conductivity low-surface-profile copper foil and preparation method and application thereof |
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Open date: 20110216 |