EP0756289A1 - Aluminiumleiter mit verbesserten elektrischen Kontakteigenschaften und Verfahren zur Herstellung desselben - Google Patents

Aluminiumleiter mit verbesserten elektrischen Kontakteigenschaften und Verfahren zur Herstellung desselben Download PDF

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Publication number
EP0756289A1
EP0756289A1 EP96420254A EP96420254A EP0756289A1 EP 0756289 A1 EP0756289 A1 EP 0756289A1 EP 96420254 A EP96420254 A EP 96420254A EP 96420254 A EP96420254 A EP 96420254A EP 0756289 A1 EP0756289 A1 EP 0756289A1
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EP
European Patent Office
Prior art keywords
conductor
treatment
bath
electrochemical treatment
iron
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP96420254A
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English (en)
French (fr)
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EP0756289B1 (de
Inventor
Richard Marsolais
Gabriel Colombier
Bernard Loreau
Didier Albert
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rio Tinto France SAS
Original Assignee
Aluminium Pechiney SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Aluminium Pechiney SA filed Critical Aluminium Pechiney SA
Publication of EP0756289A1 publication Critical patent/EP0756289A1/de
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/023—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon

Definitions

  • the invention relates to the field of electrical conductors in aluminum and more particularly electrical wires with a solid or wired core and the flats, and their aluminum connection devices.
  • the invention also relates to the surface treatments of these conductors.
  • the oxide layer whose electrical conductivity is low, prevents the passage of current at the place where the conductor is connected to the various devices or to the junctions of an electrical circuit.
  • the phenomenon is all the more annoying as the contact resistance can increase over time due to an evolution of the oxide layer under the effect of the passage of current, temperature or environmental conditions.
  • a commonly adopted solution consists in brushing the surfaces to be contacted and covering them with contact greases generally loaded with abrasive materials. This additional operation, most often manual and therefore expensive, hampers the development of aluminum as an electrical conductor.
  • the subject of the invention is an electrical conductor in aluminum alloy containing iron intermetallic phases, characterized in that its surface contains few particles of iron intermetallic phases with an equivalent diameter greater than 0.8 ⁇ m.
  • the electrical conductor in aluminum alloy according to the invention is characterized in that said alloy contains at least 98.5% of aluminum and between 0 and 1.5% of iron by weight, and in that less than 5% particles of intermetallic phases with iron at the surface of the conductor have an equivalent diameter greater than 0.8 ⁇ m. Preferably, less than 2% of said particles have an equivalent diameter greater than 0.8 ⁇ m.
  • the equivalent diameter corresponds to the diameter of a surface circle equivalent to the visible section of the particle.
  • the number and size of iron intermetallic phase particles can be measured by well known surface analysis techniques, such as low energy scanning electron microscopy (SEM) with atomic number contrast combined with a image analysis.
  • the particles of surface iron intermetallic phases include, as illustrated in FIG. 1, all the binary, ternary or other intermetallic particles, such as Al 3 Fe alone or in combination with Mn, Cu, Si, Ni, ..., which are not entirely immersed in the aluminum matrix or which, while being immersed in said matrix, approach within 0.2 ⁇ m of the surface of said matrix.
  • the proportion of iron by weight is between 0.05% and 1.0%.
  • An iron content of less than 0.05% leads to prohibitive manufacturing costs and generally reduces the mechanical characteristics of the conductor.
  • a proportion of iron greater than 1.0% leads to an electrical resistivity of the conductor which exceeds the tolerances normally allowed.
  • Said alloy optionally contains other elements in solid solution or precipitated in simple or intermetallic phase, such as Si, Cu, Mg, etc.
  • Said alloy is advantageously chosen from alloys of the AA1000 and AA6000 series, such as AA1110 (equivalent to AP 131050), AA1370, AA6101 and AA6201.
  • the conductor according to the invention can be obtained by spinning and / or drawing or molding according to known methods.
  • the conductors in the form of wires are preferably obtained by the CLC process (continuous casting and rolling) followed by wire drawing according to known methods.
  • the conductor can be in any metallurgical state compatible with the application.
  • the electrical resistivity of the conductor is preferably less than 3.5 ⁇ .cm, and more preferably less than 3.0 ⁇ .cm.
  • the conductor according to the invention is used in the form of a wire with a solid core, that is to say that it is formed of a single conductive strand possibly coated with an insulating sheath, or wired core, that is to say that it is formed by a set of elementary strands, generally twisted and possibly coated with an insulating sheath.
  • the conductor according to the invention is also advantageously used in electrical connection devices.
  • the conductor according to the invention is advantageously obtained by a method comprising a surface treatment according to the second object of the invention.
  • Said method optionally includes drawing operations which are carried out before and / or after the surface treatment.
  • the aluminum conductor is treated on parade or, in particular in the case of unit parts, by immersion in a succession of tanks.
  • FIG. 2a the most advantageous configuration for parade treatment is that of FIG. 2a.
  • FIG. 2b the two successive treatments are clearly separated as shown in FIG. 2b.
  • These two configurations correspond to a liquid outlet: current is transmitted by an electrode to the electrolyte which in turn transmits it to the conductor to be treated.
  • a direct current outlet which allows good control of the voltage applied to the conductor but poses problems of deterioration of the conductor.
  • Figures 3a and 3b represent two configurations in direct connection: the current is transmitted directly to the conductor to be treated by a mechanical contact.
  • the first treatment is carried out in a very alkaline medium with a pH> 8.
  • a very alkaline medium with a pH> 8.
  • Different electrolytes meeting this criterion can be used but, because of their low cost and their great chemical stability, it is particularly advantageous to use sodium hydroxide (NaOH ) or caustic potash (KOH), concentration between 10 and 100 g / l.
  • NaOH sodium hydroxide
  • KOH caustic potash
  • concentration 10 and 100 g / l.
  • the treatment is carried out at a temperature between 40 ° C and 100 ° C, under an applied voltage between 2 and 10 V. Below 2 V the running speeds are too low ( ⁇ 10 m / min). Above 10 V the treatment leaves a significant residual oxide layer (> 100 ⁇ ) and leads to excessively high contact resistances.
  • the second treatment is carried out in a weakly acidic medium (pH between 4 and 7).
  • a weakly acidic medium pH between 4 and 7
  • Different electrolytes may be suitable such as boric acid, phosphoric acid, tartaric acid.
  • This treatment is carried out at an ambient temperature which depends on the electrolyte, but which is generally between ambient and 60 ° C.
  • Tartaric acid combined with ammonia to give ammonium tartrate proves to be a particularly suitable electrolyte because it gives good results at room temperature.
  • the applied voltage is between 1V and 5V. Below 1V, the treatment gives a too thin layer and leads to poor behavior over time of the contact resistances and the corrosion resistance. Above 5V the oxide layer formed is thick and leads to high contact resistances.
  • the immersion times or the running speed and the various treatment parameters, in particular the applied voltage are adjusted.
  • detergents or emulsifiers can be added to the electrolyte, according to a known technique, intended to limit pollution of the bath, electrodes and mechanisms by greases.
  • a nitric acid neutralization tank can be added between the two electrochemical treatments which substantially improves the results obtained.
  • Figure 1 shows a schematic cross section of an aluminum conductor according to the invention.
  • the conductor is formed of a matrix (1), particles of intermetallic phases with iron (2, 3, 4), possibly particles of intermetallic phases without iron (5) and possibly elements in solid solution.
  • the particles on the surface include particles brushing on the surface (2) and particles immersed in the aluminum matrix and approaching the surface from a distance P less than 0.2 ⁇ m, such as the particle (3).
  • FIG. 2a represents the preferred configuration of the invention with a liquid current socket.
  • the conductor (10) circulates continuously in the treatment tanks (13, 14 and 15) using, in the case of a wire, an unwinder (11) and a reel (12).
  • an alternating voltage (18) induces an alternating current in the conductor (10) using the electrodes (19 and 20).
  • a direct voltage (17) induces a direct current in the conductor (10) using the electrodes (20 and 21), the conductor (10) being in anodic polarization in the tank (15).
  • Figure 2b shows another configuration with a liquid outlet.
  • a tank (16) and an electrode additional (22) have been added to separate the two treatments, while maintaining the principle of taking liquid current.
  • Figures 3a and 3b show two other configurations with direct connection to the conductor (30 and 31).
  • Figure 4 is a diagram of the contact resistance measurement method.
  • FIG. 5 is a diagram of the test loop for the thermal cycling test.
  • Six junction fittings (50) are joined together by the conductors under test (51), one of which is used as a reference (52).
  • the temperature of the reference conductor (52) is measured in the middle using a thermocouple (53).
  • Voltage drop measurement points (54) are arranged at a distance (L) on either side of the center of each junction connection (50).
  • Two voltage drop measurement points (55) separated by a distance (Lo) are also arranged on the reference conductor (52).
  • the test loop is connected to a power supply (60) which delivers either an alternating current, for thermal cycling, or a direct current for resistance measurements of the fittings and the reference conductor.
  • FIG. 6 shows the distribution of the sizes of particles of intermetallic phases with iron of a conductor of aluminum alloy AA 1370 according to the prior art (a, b) and according to the invention (c, d).
  • the ordinate gives the frequency of appearance of the particles.
  • the distributions a and c correspond to the equivalent diameter of the particles; the distributions b and d correspond to the maximum dimension.
  • FIG. 7 shows the distribution of the sizes of particles of intermetallic phases with iron of an aluminum alloy conductor AP 131050 according to the prior art (a, b) and according to the invention (c, d).
  • the ordinate gives the frequency of appearance of the particles.
  • the distributions a and c correspond to the diameter equivalent of particles; the distributions b and d correspond to the maximum dimension.
  • Examples 1 to 4 relate to conductors in the form of wires. In these examples, drivers have undergone the following tests:
  • the so-called crossed wire method was used, the principle of which is illustrated in FIG. 4.
  • Two wires were held and put under mechanical tension (T) by stirrups and then brought into contact gently .
  • a force F was applied to the contact which resulted in a deflection of the wires.
  • a current I was imposed on the circuit and the resulting voltage U was then measured.
  • the contact resistance was measured at a large number of points on the wire, namely about fifty points on three generators, i.e. 150 points in total and on three different samples.
  • the quality of the contact was expressed in terms of the mean value of the 10 best values, Rc.
  • the measurement was carried out under a force (F) of 5 newtons, for ⁇ 0.8 and 3 newtons for ⁇ 0.5, an intensity of 100 mA and a voltage in 20 mV open circuit.
  • the test loop was subjected to 200 thermal cycles by passing an overcurrent which brought the reference conductors to 120 ° C. Each cycle included a 15 minute warm up period and a 15 minute natural cool down period.
  • the evaluation of the contact resistance was carried out using the measurement of the junction resistance. For this we imposed an intensity (Io) in the loop and we measured the voltage drop (Uo) between two points each located at a distance (L) and on either side of the center of the fitting, the conductors being naked in these places.
  • the change in the junction resistance of all the fittings was given by the change in the ratio (K) between the start and the end of the test, which change was expressed as a percentage.
  • the distance (L) was 125 mm, the length (Lo) 254 mm and the intensity (Io) of 1A.
  • the wires treated according to the invention were exposed to a salt spray (5% NaCl) for 96 hours. At the end of this period, a new measurement of the contact resistance was carried out using the crossed wire method.
  • Lot A came from a spool of raw wire.
  • Lot B has undergone a surface treatment according to the invention, by scrolling in successive tanks: the AC treatment was carried out in a 60 ° C. bath containing 50 g / l of 98% pure NaOH and at a voltage of 5 V, the scrolling speed being 12 m / min ; the DC treatment was carried out in a bath containing 30 g / l of tartaric acid, the pH of which had been adjusted to 5 using ammonia, and at a voltage of 1 V.
  • Lot A came from a spool of raw wire.
  • Lot B underwent a surface treatment according to the invention, by scrolling through successive tanks, with an intermediate neutralization phase: the treatment with alternating current was carried out in a bath at 62 ° C.
  • the DC treatment was carried out in a bath containing 30 g / l of tartaric acid, the pH of which had been adjusted to 5 using ammonia, and at a voltage of 1 V; the intermediate neutralization treatment was carried out in a 69% nitric acid bath.
  • Lot A came from a coil of nickel-plated wire (obtained from the Tréfileries et Laminoirs de la M joserrateil (TLM), from the ALCATEL CABLE group).
  • Lot B came from a spool of raw, unshaven wire and was kept untreated.
  • Batches C, D and E come from a spool of wire having undergone a shaving phase during drawing. Lot C was kept without treatment.
  • Lot D underwent the anodization treatment of the prior art, in a bath containing 100 g / l of phosphoric acid, at an alternating voltage of 5 V, at a temperature of 75 ° C and at a running speed of 60 m / min.
  • Lot E underwent a surface treatment according to the invention, with an intermediate neutralization phase, by passing through successive tanks: the treatment with alternating current was carried out in a bath at 65 ° C. containing 50 g / l of NaOH 98% pure and at a voltage of 7.5 V, the running speed being 48 m / min; the DC treatment was carried out in a bath containing 30 g / l of tartaric acid, the pH of which had been adjusted to 5.5 with ammonia, and under a 1.5 V voltage; the intermediate neutralization treatment was carried out in a 69% nitric acid bath.
  • the corrosion pits observed on the wires of lot B are much less deep than those observed on the wires of lot A.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Conductive Materials (AREA)
EP19960420254 1995-07-27 1996-07-25 Aluminiumleiter mit verbesserten elektrischen Kontakteigenschaften und Verfahren zur Herstellung desselben Expired - Lifetime EP0756289B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9509382 1995-07-27
FR9509382A FR2737336B1 (fr) 1995-07-27 1995-07-27 Procede de traitement de surface de fils electriques en aluminium

Publications (2)

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EP0756289A1 true EP0756289A1 (de) 1997-01-29
EP0756289B1 EP0756289B1 (de) 1999-03-24

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EP19960420254 Expired - Lifetime EP0756289B1 (de) 1995-07-27 1996-07-25 Aluminiumleiter mit verbesserten elektrischen Kontakteigenschaften und Verfahren zur Herstellung desselben

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EP (1) EP0756289B1 (de)
DE (1) DE69601837T2 (de)
FR (1) FR2737336B1 (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9859038B2 (en) 2012-08-10 2018-01-02 General Cable Technologies Corporation Surface modified overhead conductor
US10726975B2 (en) 2015-07-21 2020-07-28 General Cable Technologies Corporation Electrical accessories for power transmission systems and methods for preparing such electrical accessories
US10957468B2 (en) 2013-02-26 2021-03-23 General Cable Technologies Corporation Coated overhead conductors and methods

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2179515A1 (en) * 1972-04-11 1973-11-23 Pechiney Aluminium Aluminium-based electrical conductor - by drawing and heat treating alloy contg magnesium, silicon and iron
US3827917A (en) * 1969-06-18 1974-08-06 Kaiser Aluminium Chem Corp Aluminum electrical conductor and process for making the same
FR2298619A1 (fr) * 1975-01-22 1976-08-20 Pechiney Aluminium Procede et traitement superficiel d'un fil en aluminium a usage electrique
GB2099017A (en) * 1981-05-18 1982-12-01 Pirelli Brasil Aluminium alloy, and production of electrical conductors therefrom

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3827917A (en) * 1969-06-18 1974-08-06 Kaiser Aluminium Chem Corp Aluminum electrical conductor and process for making the same
FR2179515A1 (en) * 1972-04-11 1973-11-23 Pechiney Aluminium Aluminium-based electrical conductor - by drawing and heat treating alloy contg magnesium, silicon and iron
FR2298619A1 (fr) * 1975-01-22 1976-08-20 Pechiney Aluminium Procede et traitement superficiel d'un fil en aluminium a usage electrique
GB2099017A (en) * 1981-05-18 1982-12-01 Pirelli Brasil Aluminium alloy, and production of electrical conductors therefrom

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9859038B2 (en) 2012-08-10 2018-01-02 General Cable Technologies Corporation Surface modified overhead conductor
US10586633B2 (en) 2012-08-10 2020-03-10 General Cable Technologies Corporation Surface modified overhead conductor
US10957468B2 (en) 2013-02-26 2021-03-23 General Cable Technologies Corporation Coated overhead conductors and methods
US10726975B2 (en) 2015-07-21 2020-07-28 General Cable Technologies Corporation Electrical accessories for power transmission systems and methods for preparing such electrical accessories

Also Published As

Publication number Publication date
FR2737336B1 (fr) 1997-09-05
FR2737336A1 (fr) 1997-01-31
DE69601837T2 (de) 1999-08-12
DE69601837D1 (de) 1999-04-29
EP0756289B1 (de) 1999-03-24

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