EP2600996B1 - Procédé de fabrication selon la technique de la métallurgie des poudres d'un matériau cu-cr - Google Patents

Procédé de fabrication selon la technique de la métallurgie des poudres d'un matériau cu-cr Download PDF

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EP2600996B1
EP2600996B1 EP11751787.0A EP11751787A EP2600996B1 EP 2600996 B1 EP2600996 B1 EP 2600996B1 EP 11751787 A EP11751787 A EP 11751787A EP 2600996 B1 EP2600996 B1 EP 2600996B1
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powder
temperature limit
grains
size distribution
powder mixture
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EP2600996A2 (fr
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Claudia Kowanda
Frank Müller
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Plansee Powertech AG
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Plansee Powertech AG
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0425—Copper-based 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/06—Alloys based on chromium
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/0203—Contacts characterised by the material thereof specially adapted for vacuum switches
    • H01H1/0206—Contacts characterised by the material thereof specially adapted for vacuum switches containing as major components Cu and Cr
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/10—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/20—Refractory metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the present invention relates to a method for the powder metallurgical production of a Cu-Cr material for a switching contact, in particular for vacuum switches. It involves the production of a high-performance Cu-Cr material.
  • the switching contacts require a switching capacity that is as constant as possible over the service life, a high dielectric strength and the lowest possible burnup.
  • the aim is to achieve a high erosion resistance, a good electrical and thermal conductivity, the lowest possible tendency to weld during the switching operation and a high dielectric strength and a sufficient mechanical strength of the switching contact.
  • Copper-chrome contacts for vacuum switches are thereby produced by producing a thin copper-chromium sheet as the starting material for the contacts by means of a casting or spraying process with subsequent rapid cooling. In this case, concentration profiles set in a direction perpendicular to the belt direction. A state diagram of the Cu-Cr system is also shown and described.
  • the EP0469578 A2 describes a method for producing a Cu-Cr contact material according to which an alloy of copper and chromium is melted and atomized, and the recovered Cu-Cr alloy powder is sintered in a copper matrix.
  • the WO2010050352 A1 describes a method for producing a material for switch contacts, according to which atomized Cu-Cr alloy powder is mixed with Cr powder and Cu powder, compacted and sintered.
  • the method for powder metallurgy producing a Cu-Cr material for a switching contact comprises the following steps: pressing a Cu-Cr powder mixture formed from Cu powder and Cr powder, sintering the pressed Cu-Cr powder mixture to the material of the Cu-Cr switch contact.
  • the sintering and / or a subsequent thermal treatment process is carried out with an alternating temperature profile in which the Cu-Cr powder mixture or the Cu-Cr material is heated at least twice alternately above an upper temperature limit and cooled again below a lower temperature limit. All steps are performed at temperatures that do not form a molten phase.
  • the entire manufacturing process of the Cu-Cr material is thus carried out purely by powder metallurgy at temperatures below the temperature of the eutectic (1075 ° C) of the Cu-Cr system, so that no forms molten phase.
  • the term "pure powder metallurgy" in this case refers to a process in which there is no formation of a molten phase.
  • Either sintering or a subsequent thermal treatment process (or both) with an alternating temperature profile is performed.
  • An alternating temperature profile is understood here to mean that an increase in temperature and a decrease in temperature take place alternately, wherein a temperature increase and a temperature decrease occur in each case at least twice.
  • the temperature increase and the temperature reduction preferably take place at least three times.
  • the alternating temperature profile can be traversed, for example, during the sintering of the pressed Cu-Cr green body. However, it is also possible, for example, to expose the already (conventionally) sintered Cu-Cr material to the alternating temperature profile in a subsequent thermal treatment process.
  • the upper temperature limit can preferably be chosen so that the greatest possible solubility of Cr in Cu is given in solid solution.
  • the lower temperature limit may preferably be chosen to provide a significantly lower solubility of Cr in Cu in solid solution than at the upper temperature limit.
  • the production of the Cu-Cr material may be e.g. such that already the finished switching contact is provided in its final form, or e.g. also such that the switching contact is given its final shape only by suitable post-processing.
  • the Cu-Cr material By purely powder metallurgical production of the Cu-Cr material can be provided in a particularly economical manner. Due to the alternating temperature profile (pendulum annealing) it is achieved that many Cr grains with grain sizes with a cross section between 0.1 ⁇ m 2 and 50 ⁇ m 2 (measured in the micrograph) are formed in a Cu matrix.
  • the Cu-Cr material formed thus has a particle size distribution of the Cr grains measured in the micrograph, which has a first maximum in the range of grain sizes with a cross section between 0.1 ⁇ m 2 and 50 ⁇ m 2 .
  • the determination of the particle size distribution is carried out microscopically in a grinding by measuring the surfaces of the respective Cr grains. Microscopic is understood here by light microscopy and electron microscopy.
  • a Cu-Cr material is provided for a switching contact, which is produced in a very economical manner while high erosion resistance, good electrical and thermal conductivity, a low tendency to weld in the switching process and a high dielectric strength and sufficient mechanical Strength of the switch contact achieved.
  • the advantageous particle size distribution described is also achieved without difficulty if relatively coarse Cr powder (for example having particle diameters between 20 ⁇ m and 200 ⁇ m) is used as the starting material.
  • the resulting Cu-Cr material has a microstructure in which in the micrograph in a Cu Matrix are present in addition to some smaller Cr grains relatively large Cr grains with a grain diameter in the range between 100 microns and 150 microns. This then typically results in a unimodal grain size distribution with a maximum, for example, with grain sizes in the range between 100 ⁇ m 2 and 25000 ⁇ m 2 . This suggests that the particle sizes of the Cr powder as the starting material in the resulting Cu-Cr material are substantially maintained unless the alternating temperature profile is traversed.
  • the method for producing the Cu-Cr material With the method for producing the Cu-Cr material, a low porosity, a high density, an extremely low degree of impurities, finely and homogeneously isotropically distributed Cr grains in a Cu matrix and a uniform homogeneous chemical composition of the Cu-Cr Material reached.
  • the resulting Cu-Cr material is ideal for switching contacts for use in vacuum switching technology, both as a circuit breaker in the high and medium voltage range and as a vacuum contactor switch in the low voltage range.
  • the upper temperature limit is in a range between 1065 ° C and 1025 ° C and the lower temperature limit is at least 50 ° C below the upper temperature limit.
  • the lower temperature limit is preferably at least 100 ° C below the upper temperature limit.
  • the upper temperature limit is in a temperature range just below the temperature of the eutectic (1075 ° C), that is, a range in which up to about 0.7 at% Cr can be dissolved in the Cu matrix in solid solution. This corresponds to the range in which the maximum solubility of Cr in Cu is given in solid solution.
  • the upper temperature limit is far enough below the temperature of the eutectic that the formation of a molten phase is reliably prevented even with slight temperature fluctuations.
  • the lower temperature limit is well below the upper temperature limit, ie in a range in which (in thermal equilibrium) a significantly smaller amount of Cr in the Cu matrix can be dissolved in solid solution.
  • Cr in the case of heating above the upper temperature limit Cr, it is enriched in the material of the Cu matrix (up to a maximum of approximately 0.7 at%).
  • the amount of Cr dissolved in solid solution exceeds the solubility corresponding to this lower temperature value, which is significantly less than 0.7 at%. Consequently, Cr is precipitated from the Cu matrix and Cr grains with small grain sizes are formed. In a repeated passing through the alternating temperature profile, the number of Cr grains formed with small grain sizes increases first.
  • the method further comprises the step of: mixing Cu powder and Cr powder into a Cu-Cr powder mixture.
  • the Cu-Cr powder mixture can be easily provided by using conventional Cr powder and Cu powder.
  • the Cu particles in the Cu-Cr powder mixture have a particle size distribution with a maximum particle diameter ⁇ 80 ⁇ m, preferably ⁇ 50 ⁇ m, on.
  • a maximum particle diameter is determined by means of a sieve analysis. In this case, a sieve with a corresponding mesh size (eg 80 microns or 50 microns) is used and only particles that fall through the sieve are used.
  • the Cr particles in the Cu-Cr powder mixture have a particle size distribution with a maximum particle diameter ⁇ 200 ⁇ m, preferably ⁇ 160 ⁇ m, on.
  • the maximum particle diameter is again determined with a sieve analysis with a corresponding mesh size of the sieve.
  • the value for the maximum particle diameter is small enough so as not to form excessively large Cr grains in the Cu-Cr material.
  • the individual particles can also be formed large enough so that no excessive risk of contamination by oxides occurs and in conventional production plants, a high density and a low degree of porosity can be achieved.
  • the Cr particles in the Cu-Cr powder mixture have a particle size distribution with a minimum particle diameter ⁇ 20 ⁇ m, preferably ⁇ 32 ⁇ m.
  • the minimum particle diameter is also determined with a sieve analysis (with a mesh size of, for example, 20 ⁇ m or 32 ⁇ m), but in this case only the particles which do not fall through the sieve are used. In this case, the minimum particle diameter is large enough so that there is no excessive risk of oxide contamination, and high density and a low degree of porosity can be achieved in conventional production equipment.
  • the Cu-Cr powder mixture has a Cu content between 30% by weight and 80% by weight and a Cr content between 70% by weight and 20% by weight. In this case, it is achieved that both a high erosion resistance and a low tendency to weld as well as good electrical and thermal conductivity and sufficient mechanical strength can be provided. If the Cr content exceeds 70% by weight, this leads to a marked deterioration of the thermal and electrical conductivity. If the Cr content is less than 20% by weight, no satisfactory burn-off resistance and welding tendency can be obtained.
  • the powder-metallurgically produced Cu-Cr switch contact has a Cu content between 30 wt .-% and 80 wt .-% and a Cr content between 70 wt .-% and 20 wt .-%.
  • the Cu-Cr switch contact has Cr grains in a Cu matrix.
  • a particle size distribution of the Cr grains measured in the micrograph has a first maximum in the range of particle sizes with a cross-sectional area between 0.1 ⁇ m 2 and 50 ⁇ m 2 .
  • the switching contact is made by a powder metallurgy process of Cu powder and Cr powder without formation of a molten phase. It is thus a purely powder metallurgically produced Cu-Cr switching contact.
  • the Cu-Cr switch contact may be designed for vacuum switch.
  • a Cu matrix is understood to mean a material which mainly consists of Cu but may also have a small proportion of Cr in solid solution. There may also be traces of impurities.
  • Cr grains are formed.
  • the grain size distribution of the Cr grains is determined as follows: A micrograph of the Cu-Cr material of the switch contact is made and analyzed microscopically. In the micrograph, the Cr grains are identified and the cross-sectional areas of the Cr grains are measured. The evaluation is carried out over a sufficiently large surface area or different surface areas, which form a sufficiently large total area, so that a representative, statistical statement is possible. The evaluation can be done eg by hand or supported by a suitable software.
  • the particle size distribution is seen.
  • the particle size distribution has a maximum in a range of particle sizes with a measured cross-sectional area between 0.1 ⁇ m 2 and 50 ⁇ m 2 .
  • the powder-metallurgically produced Cu-Cr switch contact achieves the advantages described above with respect to the method of powder metallurgy producing a Cu-Cr material for a switch contact. Due to the pure powder metallurgical production a particularly economical production is possible. Because of the grain size distribution with the maximum in the range of grain sizes with a cross-sectional area between 0.1 ⁇ m 2 and 50 ⁇ m 2 , the Cu-Cr switch contact has a large number of fine Cr grains. The fine Cr grains are largely homogeneously distributed. In this way, a very good erosion resistance is achieved.
  • the Cu-Cr switch contact is obtainable by a purely powder metallurgical process in which sintering or a subsequent thermal treatment process is carried out with an alternating temperature profile in which a Cu-Cr powder mixture or the material of the Cu-Cr switch contact alternates at least twice is heated above an upper temperature limit and cooled again below a lower temperature limit, and wherein all steps are carried out at temperatures, where no molten phase is formed.
  • the production in a purely powder metallurgical process can be seen on the Cu-Cr switch contact.
  • the grain size distribution of the Cr grains has a second maximum in the range of grain sizes with a cross-sectional area between 100 ⁇ m 2 and 10000 ⁇ m 2 .
  • a bimodal Cr phase distribution which has two maxima, a first maximum for grain sizes with a measured cross-sectional area between 0.1 ⁇ m 2 and 50 ⁇ m 2 and a second maximum for grain sizes with a measured cross-sectional area between 100 ⁇ m 2 and 10000 ⁇ m 2 .
  • This particle size distribution results from the purely powder metallurgical production process using coarse Cr powder, for example with particle diameters between 20 .mu.m and 200 .mu.m.
  • the number of Cr grains corresponding to the first maximum is greater than the number of Cr grains corresponding to the second maximum, ie, there are more grains having a grain size corresponding to the first maximum than grains having a grain size corresponding to the first maximum have second maximum corresponding grain size.
  • the Cu-Cr switch contact has a relative density> 90%.
  • good electrical and thermal conductivity and high mechanical strength are reliably provided.
  • Such a high specific gravity can be reliably achieved by using relatively coarse Cr powder and Cu powder in conventional production equipment.
  • relative density is meant the ratio between the density achieved and the theoretically achievable density for the composition.
  • the Combination of this high density and the high proportion of fine Cr grains in the Cu matrix can be achieved by combining a use of coarse Cr powder (with particle diameters between 20 ⁇ m and 200 ⁇ m) and using an alternating temperature profile alternating at least twice a warming above an upper temperature limit and again a cooling below a lower temperature limit, reach.
  • a first step -S1- Cu powder having a maximum particle diameter of preferably at most 50 ⁇ m with Cr powder having a maximum particle diameter of at most 200 ⁇ m (preferably at most 160 ⁇ m) and a minimum particle diameter of at least 20 ⁇ m (preferably at least 32 microns) mixed into a Cu-Cr powder mixture.
  • Cr powder having a maximum particle diameter of at most 200 ⁇ m (preferably at most 160 ⁇ m) and a minimum particle diameter of at least 20 ⁇ m (preferably at least 32 microns) mixed into a Cu-Cr powder mixture As an example, a first Cu-Cr powder mixture having a Cr content of 25% by weight and a Cu content of 75% by weight and a second Cu-Cr powder mixture having a Cr content of 43% by weight have been exemplified .-% and a Cu content of 57 wt .-% produced.
  • a second step -S2- the Cu-Cr powder mixture is pressed.
  • the Cu-Cr powder mixture is compacted by cold pressing at a compression pressure in a range between 400 MPa and 850 MPa.
  • the green compact formed in this way is sintered in a sintering process at temperatures in a temperature range well below the temperature of the eutectic (ie, significantly below 1075 ° C.).
  • the sintering process can be carried out, for example, at temperatures in a temperature range between 850 ° C and 1070 ° C. The temperatures must be high enough so that the sintering process proceeds sufficiently and with sufficient speed, and low enough that no molten phase forms even with unavoidable temperature gradients.
  • FIG. 2 An exemplary light microscopic micrograph of a powder-metallurgically produced Cu-Cr material after step -S3- is in Fig. 2 shown.
  • Fig. 2 It can be seen that Cr grains with different grain sizes are incorporated in a Cu matrix.
  • FIG. 1 An evaluation of the grain size distribution of the Cr grains in the thus prepared Cu-Cr material is shown in FIG Fig. 1 represented by a solid line.
  • a micrograph of the Cu-Cr material was prepared and the size of the Cr grains was examined microscopically and measured. 10 different regions of the Cu-Cr material were analyzed to obtain a statistically meaningful distribution.
  • Fig. 1 is the measured on the horizontal axis Cross-sectional area of Cr grains in ⁇ m 2 plotted on a logarithmic scale. On the vertical axis, the corresponding number of grains normalized to a unit area of 1 mm 2 is also shown in a logarithmic representation. As in Fig.
  • the Cu-Cr material in this stage of the process has a monomodal particle size distribution with particle sizes in a range between about 10 microns 2 and 25000 microns 2 .
  • the particle size distribution has a maximum, which is at a particle size> 100 microns 2 .
  • the Cu-Cr material is then subjected to a thermal treatment process with an alternating temperature profile, as will be described below.
  • the Cu-Cr material is alternately heated to a temperature above an upper temperature limit and cooled to a temperature below a lower temperature limit.
  • the alternating heating and cooling take place at least twice. In these process steps, too, care is taken that no molten phase is formed, i. the Cu-Cr material is kept at temperatures below the temperature of the eutectic (1075 ° C) of the Cu-Cr system. This will be described in more detail below.
  • the Cu-Cr material is heated to a temperature above the upper temperature limit.
  • the upper temperature limit is preferably relatively close below the temperature of the eutectic of the Cu-Cr system, so that the Cu-Cr material is brought to a temperature just below the temperature of the eutectic, but far enough away from the temperature of the eutectic that forming a liquid phase is reliably prevented.
  • the upper temperature limit value is thus preferably in a range between 1025 ° C and 1065 ° C.
  • the Cu-Cr material is cooled to a temperature below a lower temperature limit.
  • the lower temperature limit is preferably in a range which is at least 50 ° C below the upper temperature limit, more preferably in an area more than 100 ° C below the upper temperature limit.
  • the lower temperature limit is preferably at most 250 ° C below the upper temperature limit, more preferably at most 180 ° C below the upper temperature limit.
  • the lower temperature limit should be chosen so that there is a much lower solubility of Cr in solid solution in Cu than at the upper temperature limit. The reason for this choice will be explained in more detail.
  • the Cu-Cr material can be cooled to temperatures in the range of about 850 ° C. It is recommended not to set the lower temperature limit too low to ensure a sufficient degree of diffusion processes in the Cu-Cr material. At the upper temperature level and the lower temperature level, the Cu-Cr material is held for some time each.
  • the step -S4- is repeated, i. the Cu-Cr material is again raised to a temperature above the upper temperature limit.
  • the step -S5- is repeated, i. the Cu-Cr material is again cooled to a temperature below the lower temperature limit.
  • the steps -S4- and -S5- are repeated a total of n times, but a total of at least twice, preferably at least three times. It has been found that when the steps -S4- and -S5- are passed through from 2 times to about 6 times (2 ⁇ n ⁇ 6), an improvement of the Cu-Cr material is achieved and with a larger number of repetitions no further improvement is expected.
  • the Cu-Cr material is thus exposed to a pendulum annealing. At least steps -S4- and -S5- are carried out in a protective gas oven under reducing atmosphere and / or in a vacuum oven to avoid unwanted oxidation with oxygen. Subsequently, the manufacturing process is terminated.
  • Fig. 3 shows a light microscopic micrograph of powder metallurgically produced Cu-Cr material after passing through the described alternating temperature profile.
  • Fig. 3 It can be seen that, after performing the pendulum annealing, the content of Cr grains having a small cross-sectional area compared with the state before the pendulum annealing (cf. Fig. 2 ), clear has increased.
  • a closer analysis of the grain size of the Cr grains reveals that a bimodal grain size distribution has been established which has two maxima.
  • Fig. 1 is shown as a dashed line, the determined particle size distribution after passing through the alternating temperature profile.
  • the grain size distribution was determined in the same manner as above with respect to the solid line of Fig. 1 has been described. It can be seen that, after the pendulum annealing, instead of the previously existing monomodal particle size distribution (solid line), there is a bimodal particle size distribution.
  • the particle size distribution has a first maximum in a range of grain sizes with a cross-sectional area between 0.1 ⁇ m 2 and 50 ⁇ m 2 . Furthermore, the particle size distribution has a second maximum in the range of grain sizes with a cross-sectional area between 100 ⁇ m 2 and 10,000 ⁇ m 2 .
  • the number of Cr grains corresponding to the first maximum is greater than the number of Cr grains corresponding to the second maximum.
  • the number of Cr grains corresponding to the first maximum is larger than the number of Cr grains corresponding to the second maximum by a factor> 5.
  • there is a very homogeneous distribution of the Cr grains in the Cu matrix The proportion of Cr grains with a cross-sectional area ⁇ 10 ⁇ m 2 measured in the micrograph is thus very high.
  • the thermal treatment with the alternating temperature profile thus achieves a shift to a high proportion of very small finely divided Cr grain precipitates in the Cu matrix.
  • the described starting materials having a relatively coarse particle size of the Cr powder, it is possible to produce very dense Cu-Cr materials with low porosity in a purely powder metallurgical process with conventional production plants, which also have a low level of impurities.
  • the pure powder metallurgy production is recognizable on the Cu-Cr material. Due to the very finely distributed Cr grains, the purely powder-metallurgically produced Cu-Cr material has a high erosion resistance, a high dielectric strength and a sufficient mechanical strength of the switching contact.
  • the formation of the finely divided Cr grains in the Cu matrix can be with regard to the example in the aforementioned DE 10 2006 021 772 A1 illustrated Explain the state diagram as follows: At temperatures above the upper limit of the temperature in a region near below the temperature of the eutectic, up to about 0.7 at% of Cr can be dissolved in solid solution in the material of the Cu matrix (in thermodynamic equilibrium). Upon cooling of the Cu-Cr material to a temperature below the lower temperature limit, the material is brought to a temperature at which only a much smaller proportion of Cr in solid solution in the material of the Cu matrix can be dissolved in the thermodynamic equilibrium. Upon cooling, Cr is thus precipitated out of the material of the Cu matrix and this precipitation takes place in the form of small grains.
  • the temperature change between the high and the low temperature level in the pendulum annealing should be chosen to be sufficiently slow that Cr is reliably precipitated from the Cu matrix on cooling, but not too slow so that larger Cr grains are not produced again by grain coarsening.
  • the treatment with the alternating Temperature profile only after the step -S3- of the sintering in the Cu-Cr material
  • the pressed Cu-Cr green compact is already repeatedly subjected to steps -S4- and -S5 during the sintering process.
  • the separate step -S3- is omitted and the sintering takes place during the steps -S4- and -S5-.

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Claims (7)

  1. Procédé de fabrication selon la technique de la métallurgie des poudres d'un matériau Cu-Cr pour un contact de commutation, notamment pour un commutateur sous vide, comprenant les étapes suivantes :
    (S2) la compression d'un mélange de poudre Cu-Cr formé à partir d'une poudre de Cu et d'une poudre de Cr,
    (S3) le frittage du mélange de poudre Cu-Cr comprimé pour former le matériau du contact de commutation Cu-Cr,
    caractérisé en ce que
    le frittage et/ou un procédé de traitement thermique ultérieur sont réalisés avec un profil de température alternant, selon lequel le mélange de poudre Cu-Cr ou le matériau Cu-Cr est au moins à deux reprises alternativement chauffé au-dessus d'une valeur limite de température supérieure (S4) et de nouveau refroidi en dessous d'une valeur limite de température inférieure (S5), toutes les étapes étant réalisées à des températures auxquelles aucune phase fondue ne se forme.
  2. Procédé selon la revendication 1, caractérisé en ce que la valeur limite de température supérieure se situe dans une plage comprise entre 1 065 °C et 1 025 °C et la valeur limite de température inférieure se situe au moins 50 °C en dessous de la valeur limite de température supérieure, de préférence au moins 100 °C en dessous de la valeur limite de température supérieure.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que le procédé comprend en outre l'étape suivante : (S1) le mélange d'une poudre de Cu et d'une poudre de Cr pour former un mélange de poudre Cu-Cr.
  4. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les particules de Cu dans le mélange de poudre Cu-Cr présentent une distribution des tailles de particules ayant un diamètre de particule maximal ≤ 80 µm, de préférence ≤ 50 µm.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les particules de Cr dans le mélange de poudre Cu-Cr présentent une distribution des tailles de particules ayant un diamètre de particule maximal ≤ 200 µm, de préférence ≤ 160 µm.
  6. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les particules de Cr dans le mélange de poudre Cu-Cr présentent une distribution des tailles de particules ayant un diamètre de particule minimal ≥ 20 µm, de préférence ≥ 32 µm.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le mélange de poudre Cu-Cr présente une teneur en Cu comprise entre 30 % en poids et 80 % en poids et une teneur en Cr comprise entre 70 % en poids et 20 % en poids.
EP11751787.0A 2010-08-03 2011-08-01 Procédé de fabrication selon la technique de la métallurgie des poudres d'un matériau cu-cr Active EP2600996B1 (fr)

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AT0048410U AT11814U1 (de) 2010-08-03 2010-08-03 Verfahren zum pulvermetallurgischen herstellen eines cu-cr-werkstoffs
PCT/AT2011/000319 WO2012016257A2 (fr) 2010-08-03 2011-08-01 Procédé de fabrication selon la technique de la métallurgie des poudres d'un matériau cu-cr

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US20160107237A1 (en) 2016-04-21
WO2012016257A3 (fr) 2012-11-01
AT11814U1 (de) 2011-05-15
WO2012016257A2 (fr) 2012-02-09
CN103201059A (zh) 2013-07-10
CN103201059B (zh) 2016-06-29
EP2600996A2 (fr) 2013-06-12
ES2686421T3 (es) 2018-10-17
US20130140159A1 (en) 2013-06-06

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