US20190076927A1 - Porous copper body, porous copper composite member, method for producing porous copper body, and method for producing porous copper composite member - Google Patents

Porous copper body, porous copper composite member, method for producing porous copper body, and method for producing porous copper composite member Download PDF

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US20190076927A1
US20190076927A1 US16/081,527 US201716081527A US2019076927A1 US 20190076927 A1 US20190076927 A1 US 20190076927A1 US 201716081527 A US201716081527 A US 201716081527A US 2019076927 A1 US2019076927 A1 US 2019076927A1
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copper
fibers
porous
powders
porous copper
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Jun Kato
Koichi Kita
Toshihiko Saiwai
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Mitsubishi Materials Corp
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Mitsubishi Materials Corp
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Assigned to MITSUBISHI MATERIALS CORPORATION reassignment MITSUBISHI MATERIALS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: KATO, JUN, KITA, KOICHI, SAIWAI, Toshihiko
Publication of US20190076927A1 publication Critical patent/US20190076927A1/en
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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
    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1103—Making porous workpieces or articles with particular physical characteristics
    • B22F3/1112—Making porous workpieces or articles with particular physical characteristics comprising hollow spheres or hollow fibres
    • 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
    • B22F3/11—Making porous 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
    • 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
    • B22F3/11—Making porous workpieces or articles
    • B22F3/1143—Making porous workpieces or articles involving an oxidation, reduction or reaction step
    • 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
    • B22F3/23—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces involving a self-propagating high-temperature synthesis or reaction sintering step
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/002—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of porous nature
    • 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
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/062—Fibrous particles
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
    • 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
    • C22C1/08—Alloys with open or closed pores
    • 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

Definitions

  • the present disclosure relates to a porous copper body formed from copper or a copper alloy, a porous copper composite member in which the porous copper body is bonded to a main member body, a method of manufacturing the porous copper body, and a method of manufacturing the porous copper composite member.
  • the porous copper body and the porous copper composite member are used, for example, as electrodes and current collectors in various batteries, heat exchanger components, heat pipes, and the like.
  • PTL 1 discloses a method in which a pressure-sensitive adhesive is applied to a skeleton of a three-dimensional network structure (for example, synthetic resin foam having open cells such as urethane foam, polyethylene foam, natural fiber cloth, man-made fiber cloth, and the like) made of a material burned off by heating and a formed body on which a metal powdery material is adhered is used, or a method of using a sheet-like formed body which is made of a material burned off by heating and in which a metal powder material has been mixed to a material (for example, pulp or wool fiber) capable of forming a three-dimensional network structure, as a method of manufacturing a metal sintered body (porous copper sintered body) forming the three-dimensional network structure.
  • a three-dimensional network structure for example, synthetic resin foam having open cells such as urethane foam, polyethylene foam, natural fiber cloth, man-made fiber cloth, and the like
  • PTL 2 discloses a method of obtaining a porous material by electrically heating a copper fiber under pressure.
  • porous copper body in addition to having a high porosity and an open cell structure, in a case of being used as a conductive member such as an electrode and a current collector, excellent conductivity is required, and in a case of being used as a heat conduction member such as a heat exchanger component and heat pipe, excellent heat conductivity is required.
  • conductivity and heat conductivity are not considered, and in particular, in a case where the porosity is high, bonding between metal powders or the copper fibers is insufficient, resulting in a concern that conductivity and heat conductivity may be insufficient.
  • the disclosure has been made in consideration of the above-described circumstances, and an object thereof is to provide a porous copper body which has sufficient conductivity and heat conductivity, even in a case where a porosity is high, and is particularly suitable for a conductive member and a heat-transfer member, a porous copper composite member in which the porous copper body is bonded to a main member body, a method of manufacturing the porous copper body, and method of manufacturing the porous copper composite member.
  • a porous copper body is provided.
  • the porous copper body is a porous copper body, including: a skeleton having a three-dimensional network structure, in which a porosity is in a range of 50% to 90%, and a porosity-normalized electrical conductivity ⁇ N which is defined by dividing a electrical conductivity of the porous copper body, measured by a 4-terminal sensing, by an apparent density ratio of the porous copper body is 20% IACS or higher.
  • a porosity-normalized electrical conductivity ⁇ N which is defined by dividing a electrical conductivity of the porous copper body, measured by a 4-terminal sensing, by an apparent density ratio of the porous copper body is 20% IACS or higher. Accordingly, the porous copper body is excellent in conductivity and particularly suitable for a conductive member. In addition, free electrons are responsible for thermal conduction as well as electrical conduction. Accordingly, when conductivity is ensured, heat conductivity is also ensured. Therefore, the porous copper body of the disclosure is also excellent in heat conductivity and particularly suitable for a heat-transfer member.
  • an oxidation-reduction layer be formed on a surface of the skeleton.
  • the oxidation-reduction layer is formed on the surface of the skeleton, unevenness is formed on the surface to increase a specific surface area. For example, it is possible to greatly improve various characteristics such as heat-exchange efficiency through a porous skeleton surface and the like. In addition, by performing an oxidation-reduction treatment, it is possible to further improve the porosity-normalized electrical conductivity ⁇ N .
  • the skeleton may be a sintered body of: at least one of copper powders and copper fibers; or both of copper powders and copper fibers, both of copper powders and copper fibers being made of copper or a copper alloy.
  • the porous copper body in which the porosity is in the range of 50% to 90% by adjusting a filling rate of copper powders and copper fibers which are formed from copper or a copper alloy.
  • a diameter R be in a range of 0.02 mm to 1.0 mm and a ratio L/R between a length L and the diameter R be in a range of 4 to 2500.
  • the diameter R is set in a range of 0.02 mm to 1.0 mm, and the ratio L/R between the length L and the diameter R is set in a range of 4 to 2500, a sufficient void is secured between the copper fibers, and a shrinkage rate in the sintering can be suppressed. Accordingly, it is possible to raise the porosity, and it is possible to attain excellent dimensional accuracy.
  • the oxidation-reduction layers formed on surfaces of: at least one of copper powders and copper fibers; or both of copper powders and copper fibers be integrally bonded to each other.
  • the oxidation-reduction layers are integrally bonded to each other in the bonding portion of: at least one of copper powders and copper fibers; or both of copper powders and copper fibers, accordingly, the porous copper body is excellent in bonding strength.
  • the copper fibers and the copper powders are strongly bonded to each other, it is also possible to improve conductivity and heat conductivity.
  • a porous copper composite member including a bonded body of a main member body and the above-described porous copper body.
  • the porous copper composite member is formed from a bonded body of the porous copper body which is excellent in conductivity and heat conductivity and the main member body, accordingly, it is possible to exhibit excellent conductivity and heat conductivity as the porous copper composite member.
  • a bonding surface in the main member body with the porous copper body be formed from copper or a copper alloy and a bonding portion of the porous copper body and the main member body be a sintered layer.
  • the bonding portion of the porous copper body and the main member body is the sintered layer, the porous copper body and the main member body are strongly bonded to each other, and thus it is possible to obtain excellent strength, conductivity, and heat conductivity, as the porous copper composite member.
  • a method of manufacturing the above-described porous copper body including performing an oxidation treatment on a skeleton having a three-dimensional network structure under conditions of a holding temperature of 500° C. to 1050° C. in an oxidizing atmosphere; performing a reduction treatment on the skeleton having a three-dimensional network structure under conditions of a holding temperature of 500° C. to 1050° C. in a reducing atmosphere; and setting the porosity-normalized electrical conductivity ⁇ N to 20% 1ACS or higher by the oxidation treatment and the reduction treatment.
  • the conductivity is improved. Accordingly, it is possible to set the porosity-normalized electrical conductivity ⁇ N to 20% IACS or higher.
  • a method of manufacturing the above-described porous copper body including: performing an oxidation treatment on at least one of copper powders and copper fibers, or both of copper powders and copper fibers, under conditions of a holding temperature of 500° C. to 1050° C. in an oxidizing atmosphere; and performing a reduction treatment on at least one of copper powders and copper fibers, or both of copper powders and copper fibers, under conditions of a holding temperature of 500° C. to 1050° C.
  • the skeleton including a sintered body of: at least one of copper powders and copper fibers; or both of copper powders and copper fibers, are formed and the porosity-normalized electrical conductivity ⁇ N is set to 20% IACS or higher by the oxidation treatment and the reduction treatment.
  • the method of manufacturing the porous copper body as described above by performing the oxidation treatment and the reduction treatment on at least one of copper powders and copper fibers, or both of copper powders and copper fibers, under above-described conditions, it is possible to form the skeleton including a sintered body of: at least one of copper powders and copper fibers; or both of copper powders and copper fibers, and it is possible to obtain a porous copper body formed from the sintered body.
  • the conductivity is improved. Accordingly, it is possible to set the porosity-normalized electrical conductivity ⁇ N to 20% IACS or higher.
  • a method of manufacturing a porous copper composite member including a bonded body of a main member body and a porous copper body is provided, the method including a bonding process of bonding the porous copper body that is manufactured by the above-described method of manufacturing the porous copper body, and the main member body.
  • the porous copper body which is manufactured by the above-described method of manufacturing the porous copper body, is provided, and thus it is possible to manufacture a porous copper composite member excellent in heat conductivity and conductivity.
  • a shape of the main member body include a plate, a rod, a pipe, and the like.
  • a bonding surface to which the porous copper body is bonded may be constituted by copper or a copper alloy, and the porous copper body and the main member body may be bonded to each other through sintering.
  • the main member body and the porous copper body can be integrated with each other through sintering, and thus it is possible to manufacture a porous copper composite member excellent in stability of characteristics.
  • a porous copper body which has sufficient conductivity and heat conductivity, even in a case where a porosity is high, and is particularly suitable for a conductive member and a heat-transfer member, a porous copper composite member in which the porous copper body is bonded to a main member body, a method of manufacturing the porous copper body, and method of manufacturing the porous copper composite member.
  • FIG. 1 is an enlarged schematic view of a porous copper body according to a first embodiment of the disclosure.
  • FIG. 2 is a flowchart illustrating an example of a method of manufacturing the porous copper body illustrated in FIG. 1 .
  • FIG. 3 is a view illustrating a manufacturing process of manufacturing the porous copper body illustrated in FIG. 1 .
  • FIG. 4 is a view illustrating an external appearance of a porous copper composite member according to a second embodiment of the disclosure.
  • FIG. 5 is a flowchart illustrating an example of a method of manufacturing the porous copper composite member illustrated in FIG. 4 .
  • FIG. 7 is an external view of a porous copper composite member according to still another embodiment of the disclosure.
  • FIG. 8 is an external view of a porous copper composite member according to still another embodiment of the disclosure.
  • FIG. 9 is an external view of a porous copper composite member according to still another embodiment of the disclosure.
  • FIG. 10 is an external view of a porous copper composite member according to still another embodiment of the disclosure.
  • FIG. 11 is an external view of a porous copper composite member according to still another embodiment of the disclosure.
  • the porous copper body 10 includes a skeleton 12 in which a plurality of copper fibers 11 are sintered.
  • the copper fibers 11 are formed from copper or a copper alloy, a diameter R is set in a range of 0.02 mm to 1.0 mm, and a ratio L/R between a length L and the diameter R is set in a range of 4 to 2500.
  • the copper fibers 11 are formed from, for example, C1020 (oxygen-free copper).
  • the copper fiber 11 is subjected to shape imparting such as twisting and bending.
  • an apparent density ratio D A is set to 51% or less of a true density D T of the copper fiber 11 .
  • a shape of the copper fiber 11 is an arbitrary shape such as a linear shape and a curved shape as long as the apparent density ratio D A is 51% or less of the true density D T of the copper fiber 11 .
  • predetermined shape-imparting processing such as twisting processing and bending processing
  • isotropy in various characteristics such as heat-transfer characteristics and conductivity of the porous copper body 10 .
  • the copper fiber 11 is manufactured through adjustment into a predetermined circle-converted diameter R by a drawing method, a coil cutting method, a wire cutting method, a melting spraying method, and the like, length adjustment for satisfying predetermined L/R, and cutting.
  • the circle-converted diameter R is a value that is calculated on the basis of a cross-sectional area A of each fiber, and is defined by the following expression on the assumption of a perfect circle regardless of a cross-sectional shape.
  • an oxidation-reduction layer is formed on a surface of the skeleton 12 (copper fiber 11 ).
  • oxidation-reduction layers formed on surfaces of the plurality of copper fibers 11 are integrally bonded to each other.
  • each of the oxidation-reduction layers has a porous structure, which causes minute unevenness on the surface of skeleton 12 (copper fiber 11 ).
  • a specific surface area of the entirety of the porous copper body 10 is set to 0.01 m 2 /g or greater.
  • the specific surface area of the entirety of the porous copper body 10 is preferably 0.03 m 2 /g or greater.
  • a porosity P is in a range of 50% to 90% and a porosity-normalized electrical conductivity ⁇ N IACS) which is defined by dividing a electrical conductivity ⁇ P of the porous copper body 10 , measured by a 4-terminal sensing, by an apparent density ratio D A of the porous copper body 10 is 20% IACS or higher.
  • the porosity-normalized electrical conductivity ⁇ N , the apparent density ratio D A , and the porosity P are respectively calculated by the following expressions.
  • ⁇ N ⁇ P ⁇ (1/ D A )
  • m is the mass (g) of the porous copper body 10 .
  • V is the volume (cm 3 ) of the porous copper body 10 .
  • D T is the true density (g/cm 3 ) of the copper fibers 11 constituting the porous copper body 10 .
  • the porosity P is preferably in a range of 70% to 90%. However, there is no limitation thereto.
  • the copper fiber 11 is distributed from a distributor 31 toward the inside of a stainless steel container 32 to volumetrically fill the stainless steel container 32 . According to this, lamination of the copper fibers 11 is performed (copper fiber lamination process S 01 ).
  • the copper fibers 11 which volumetrically fill the stainless steel container 32 , are subjected to an oxidation-reduction treatment (oxidation-reduction treatment process S 02 ).
  • the oxidation-reduction treatment process S 02 includes an oxidation treatment process S 21 of performing an oxidation treatment of the copper fibers 11 , and a reduction treatment process S 22 of reducing and sintering the copper fibers 11 which are subjected to the oxidation treatment.
  • the stainless steel container 32 which is filled with the copper fibers 11 , is put in a heating furnace 33 and is heated in an oxidizing atmosphere to perform an oxidation treatment of the copper fiber 11 (oxidation treatment process S 21 ).
  • oxidation treatment process S 21 an oxide layer having a thickness of 1 ⁇ m to 100 ⁇ m is formed on a surface of each of the copper fibers 11 through the oxidation treatment process S 21 .
  • Conditions of the oxidation treatment process S 21 in this embodiment are as follows. Specifically, an atmosphere is set to an atmospheric atmosphere (atmospheric atmosphere (a)), a holding temperature is set to 500° C. to 1050° C., and a holding time is set in a range of 5 minutes to 300 minutes.
  • atmospheric atmosphere atmospheric atmosphere (atmospheric atmosphere (a)
  • a holding temperature is set to 500° C. to 1050° C.
  • a holding time is set in a range of 5 minutes to 300 minutes.
  • the holding temperature in the oxidation treatment process S 21 is lower than 500° C.
  • the oxide layer is not sufficiently formed on the surface of the copper fiber 11 .
  • the holding temperature in the oxidation treatment process S 21 is higher than 1050° C.
  • oxidation may progress to the inside of the copper fiber 11 .
  • the holding temperature in the oxidation treatment process S 21 is set to 500° C. to 1050° C. Furthermore, in the oxidation treatment process S 21 , it is preferable that the lower limit of the holding temperature be set to 600° C. or higher, and the upper limit of the holding temperature be set to 1000° C. or lower so as to reliably form the oxide layer on the surface of the copper fiber 11 .
  • the holding time in the oxidation treatment process S 21 is shorter than 5 minutes, there is a concern that the oxide layer may not be sufficiently formed on the surface of the copper fiber 11 .
  • the holding time in the oxidation treatment process S 21 is longer than 300 minutes, there is a concern that oxidation may progress to the inside of the copper fiber 11 .
  • the holding time in the oxidation treatment process S 21 is set in a range of 5 minutes to 300 minutes. Furthermore, it is preferable that the lower limit of the holding time in the oxidation treatment process S 21 be set to 10 minutes or longer so as to reliably form the oxide layer on the surface of the copper fiber 11 . In addition, it is preferable that the upper limit of the holding time in the oxidation treatment process S 21 be set to 100 minutes or shorter so as to reliably suppress oxidation to the inside of the copper fiber 11 .
  • the stainless steel container 32 which is filled with the copper fiber 11 , is put in the heating furnace 34 and is heated in a reduction atmosphere. According to this, the oxidized copper fiber 11 is subjected to a reduction treatment to form an oxidation-reduction layer, and the copper fibers 11 are bonded to each other to form the skeleton 12 (reduction treatment process S 22 ).
  • Conditions of the reduction treatment process S 22 in this embodiment are as follows. Specifically, an atmosphere is set to a mixed gas atmosphere of argon and hydrogen (Ar+H2 atmosphere (b)), a holding temperature is set to 500° C. to 1050° C., and a holding time is set in a range of 5 minutes to 300 minutes.
  • the holding temperature in the reduction treatment process S 22 is lower than 500° C.
  • the oxide layer formed on the surface of the copper fiber 11 may not be sufficiently reduced.
  • the holding temperature in the reduction treatment process S 22 is higher than 1050° C.
  • heating may be performed to near the melting point of copper, and thus a decrease in strength and porosity may occur.
  • the holding temperature in the reduction treatment process S 22 is set to 500° C. to 1050° C. Furthermore, it is preferable that the lower limit of the holding temperature in the reduction treatment process S 22 be set to 600° C. or higher so as to reliably reduce the oxide layer formed on the surface of the copper fiber 11 . In addition, it is preferable that the upper limit of the holding temperature in the reduction treatment process S 22 be set to 1000° C. or lower so as to reliably suppress the decrease in strength and the porosity.
  • the holding time in the reduction treatment process S 22 is shorter than 5 minutes, there is a concern that the oxide layer formed on the surface of the copper fiber 11 may not be sufficiently reduced, and sintering may become insufficient.
  • the holding time in the reduction treatment process S 22 is longer than 300 minutes, there is a concern that thermal shrinkage may increase and strength may decrease due to the sintering.
  • the holding time in the reduction treatment process S 22 is set in a range of 5 minutes to 300 minutes. Furthermore, it is preferable that the lower limit of the holding time in the reduction treatment process S 22 be set to 10 minutes or longer so as to reliably reduce the oxide layer formed on the surface of the copper fiber 11 and to allow sintering to sufficiently progress. In addition, it is preferable that the upper limit of the holding time in the reduction treatment process S 22 be set to 100 minutes or shorter so as to reliably suppress the thermal shrinkage or the decrease in strength due to the sintering.
  • An oxidation-reduction layer is formed on the surface of the copper fiber 11 (skeleton 12 ) by the oxidation treatment process S 21 and the reduction treatment process S 22 , and thus minute unevenness having a unique microporous structure occurs. That is, the oxidation-reduction layers has a porous structure, which causes minute unevenness on the surface of the copper fiber 11 . According to this, a specific surface area of the entirety of the porous copper body 20 is set to 0.01 m 2 /g or greater.
  • the oxide layer is formed on the surface of the copper fiber 11 by the oxidation treatment process S 21 , and a plurality of the copper fibers 11 are cross-linked by the oxide layer. Then, when the reduction treatment process S 22 is performed, the oxide layer formed on the surface of the copper fiber 11 is reduced, and thus the above-described oxidation-reduction layer is formed. In addition, a plurality of the oxidation-reduction layers are bonded to each other, and the copper fibers 11 are sintered, and thus the skeleton 12 is formed.
  • the copper fibers 11 are sintered, and thus the skeleton 12 is formed, and the oxidation-reduction layer is formed on the surface of the skeleton 12 (copper fiber 11 ). Further, the above-described porosity-normalized electrical conductivity ⁇ N is set to 20% IACS or higher. Accordingly, the porous copper body 10 according to this embodiment is manufactured.
  • the porosity P is as high as in a range of 50% to 90% and the porosity-normalized electrical conductivity ⁇ N is 20% IACS or higher. Accordingly, the porous copper body is excellent in conductivity and heat conductivity, and has excellent characteristics as a conductive member and a heat-transfer member.
  • the oxidation-reduction layer is formed on the surface of the skeleton 12 , unevenness having a unique microporous structure is formed on the surface to increase a specific surface area. For example, it is possible to greatly improve various characteristics such as heat-exchange efficiency through a porous skeleton surface and the like. In addition, by performing an oxidation-reduction treatment, it is possible to further improve the porosity-normalized electrical conductivity ⁇ N .
  • the porous copper body 10 is excellent in bonding strength.
  • the copper fibers 11 in which the diameter R is set in a range of 0.02 mm to 1.0 mm and the ratio L/R between the length L and the diameter R is set in a range of 4 to 2500, are sintered to form the skeleton 12 , a sufficient void is secured between the copper fibers 11 , and a shrinkage rate in the sintering can be suppressed. Accordingly, it is possible to raise the porosity, and it is possible to attain excellent dimensional accuracy.
  • this embodiment includes the copper fiber lamination process S 01 in which the copper fibers 11 of which the diameter R is set in a range of 0.02 mm to 1.0 mm and the ratio L/R between the length L and the diameter R is set in a range of 4 to 2500 are laminated so that the volume density D P becomes 50% or less of the true density D T of the copper fibers 11 . Accordingly, it is possible to secure a void between the copper fibers 11 , and thus it is possible to suppress shrinkage. According to this, it is possible to manufacture the porous copper body 10 in which the porosity is high and the dimensional accuracy is excellent.
  • the diameter R of the copper fibers 11 is less than 0.02 mm, a bonding area between the copper fibers 11 is small, and thus there is a concern that sintering strength may be deficient.
  • the diameter R of the copper fibers 11 is greater than 1.0 mm, the number of contact points at which the copper fibers 11 come into contact with each other is deficient, and thus there is a concern that the sintering strength also becomes deficient.
  • the diameter R of the copper fibers 11 is set in a range of 0.02 mm to 1.0 mm. Furthermore, it is preferable that the lower limit of the diameter R of the copper fibers 11 be set to 0.05 mm or greater, and the upper limit of the diameter R of the copper fibers 11 be set to 0.5 mm or less so as to attain an additional improvement in strength.
  • the ratio L/R between the length L and the diameter R of the copper fibers 11 is less than 4, when laminating the copper fibers 11 , it is difficult for the volume density D P to be 50% or less of the true density D T of the copper fibers 11 , and thus there is a concern that it is difficult to obtain the porous copper body 10 having a high porosity P.
  • the ratio L/R between the length L and the diameter R of the copper fibers 11 is greater than 2500, it is difficult to uniformly disperse the copper fibers 11 , and thus there is a concern that it is difficult to obtain the porous copper body 10 having a uniform porosity P.
  • the ratio L/R between the length L and the diameter R of the copper fibers 11 is set in a range of 4 to 2500. Furthermore, it is preferable that the lower limit of the ratio L/R between the length L and the diameter R of the copper fibers 11 be set to 10 or greater so as to attain an additional improvement in porosity. In addition, it is preferable that the upper limit of the ratio L/R between the length L and the diameter R of the copper fibers 11 be set to 500 or less so as to reliably obtain the porous copper body 10 having a uniform porosity P.
  • the oxidation treatment process S 21 of oxidizing the copper fibers 11 and the reduction treatment process S 22 of reducing the oxidized copper fibers 11 are provided, and thus it is possible to form the oxidation-reduction layer on the surface of the copper fibers 11 (skeleton 12 ).
  • FIG. 4 illustrates the porous copper composite member 100 according to this embodiment.
  • the porous copper composite member 100 includes a copper plate 120 (main member body) formed from copper or a copper alloy, and a porous copper body 110 that is bonded to a surface of the copper plate 120 .
  • the porous copper body 110 a plurality of copper fibers are sintered and a skeleton is formed in the same manner as in the first embodiment.
  • the copper fibers are formed from copper or a copper alloy, and a diameter R is set in a range of 0.02 mm to 1.0 mm, and a ratio L/R between a length L and the diameter R is set in a range of 4 to 2500.
  • the copper fibers are formed from, for example, C1020 (oxygen-free copper).
  • the copper fibers are subjected to shape imparting such as twisting and bending.
  • an apparent density ratio D A is set to 51% or less of a true density D T of the copper fiber.
  • an oxidation-reduction treatment (an oxidation treatment and a reduction treatment) is performed as described later.
  • an oxidation-reduction layer is formed on the surface of the copper fibers (skeleton) which constitute the porous copper body 110 and the copper plate 120 , and minute unevenness occurs on the surface of copper fibers (skeleton) and the copper plate 120 .
  • a specific surface area of the entirety of the porous copper body 110 is set to 0.01 m 2 /g or greater.
  • the specific surface area of the entirety of the porous copper body 110 is preferably 0.03 m 2 /g or greater.
  • an oxidation-reduction layer formed on the surface of the copper fibers and an oxidation-reduction layer formed on the surface of the copper plate are integrally bonded to each other at a bonding portion between the copper fibers which constitute the porous copper body 110 and the surface of the copper plate 120 .
  • a porosity P is in a range of 50% to 90% and a porosity-normalized electrical conductivity ⁇ N which is defined by dividing a electrical conductivity ⁇ P of the porous copper body 110 , measured by a 4-terminal sensing, by an apparent density ratio D A of the porous copper body 110 is 20% IACS or higher.
  • the porosity P is preferably in a range of 70% to 90%. However, there is no limitation thereto.
  • the copper plate 120 that is a main member body is prepared (copper plate-disposing process S 100 ).
  • copper fibers are dispersed and laminated on a surface of the copper plate 120 (copper fiber lamination process S 101 ).
  • a plurality of the copper fibers are laminated so that a volume density D Y becomes 50% or less of the true density D T of the copper fibers.
  • the copper fibers laminated on the surface of the copper plate 120 are sintered to shape the porous copper body 110 , and the porous copper body 110 and the copper plate 120 are bonded to each other (a sintering process S 102 and a bonding process S 103 ).
  • the sintering process S 102 and the bonding process S 103 include an oxidation treatment process S 121 of performing an oxidation treatment of the copper fibers and the copper plate 120 , and a reduction treatment process S 122 of reducing and sintering the copper fibers and the copper plate 120 which are subjected to the oxidation treatment.
  • the copper plate 120 on which the copper fibers are laminated is put in a heating furnace, and is heated in an oxidizing atmosphere to perform an oxidation treatment of the copper fibers (oxidation treatment process S 121 ).
  • oxidation treatment process S 121 for example, an oxide layer having a thickness of 1 ⁇ m to 100 ⁇ m is formed on the surface of the copper fibers and the copper plate 120 .
  • conditions of the oxidation treatment process S 121 in this embodiment are as follows. Specifically, a holding temperature is set to 500° C. to 1050° C. and preferably 600° C. to 1000° C., and a holding time is set in a range of 5 minutes to 300 minutes and preferably in a range of 10 minutes to 100 minutes.
  • the copper plate 120 on which the copper fibers are laminated is put in a sintering furnace, and is heated in a reduction atmosphere to perform a reduction treatment of the copper fibers and the copper plate 120 which are oxidized. According to this, the copper fibers are bonded to each other, and the copper fibers and the copper plate 120 are bonded to each other (reduction treatment process S 122 ).
  • conditions of the reduction treatment process S 122 in this embodiment are as follows.
  • An atmosphere is set to a mixed gas atmosphere of nitrogen and hydrogen
  • a holding temperature is set to 500° C. to 1050° C. and preferably 600° C. to 1000° C.
  • a holding time is set in a range of 5 minutes to 300 minutes and preferably in a range of 10 minutes to 100 minutes.
  • An oxidation-reduction layer is formed on the surface of the copper fibers (skeleton) and the copper plate 120 by the oxidation treatment process S 121 and the reduction treatment process S 122 , and minute unevenness occurs.
  • the oxide layer is formed on the copper fibers (skeleton) and the surface of the copper plate 120 by the oxidation treatment process S 121 . Due to the oxide layer, a plurality of the copper fibers are cross-linked to each other, and the copper fibers and the copper plate 120 are cross-linked to each other. Then, when the reduction treatment process S 122 is performed, the oxide layer formed on the surface of the copper fibers (skeleton) and the copper plate 120 is reduced, and the copper fibers are sintered through the oxidation-reduction layer. According to this, the skeleton is formed, and the porous copper body 110 and the copper plate 120 are bonded to each other. Further, the above-described porosity-normalized electrical conductivity ⁇ N of the porous copper body 110 is set to 20% IACS or higher.
  • the porous copper composite member 100 according to this embodiment is manufactured.
  • the porosity-normalized electrical conductivity ⁇ N of the porous copper body 110 is set to 20% IACS or higher. Accordingly, the porous copper composite member 100 is excellent in conductivity and heat conductivity, and it is possible to improve conductivity and heat conductivity of the entirety of the porous copper composite member 100 .
  • the oxidation-reduction layer is formed on the surface of the copper fibers which constitute the porous copper body 110 and the copper plate 120 , the specific surface area of the entirety of the porous copper body 110 is set to 0.01 m 2 /g or greater, and the porosity P is set in a range of 50% to 90%. Accordingly, it is possible to greatly improve heat-exchange efficiency, water retention and the like.
  • an oxidation-reduction layer formed on the surface of the copper fibers and an oxidation-reduction layer formed on the surface of the copper plate 120 are integrally bonded to each other at a bonding portion between the copper fibers which constitute the porous copper body 110 and the surface of the copper plate 120 . Accordingly, the porous copper body 110 and the copper plate 120 are strongly bonded to each other, and thus strength of a bonding interface, conductivity, and heat conductivity are excellent.
  • the copper fibers are laminated on the surface of the copper plate 120 formed from copper or a copper alloy, and the sintering process S 102 and the bonding process S 103 are simultaneously performed, and thus it is possible to simplify a manufacturing process.
  • porous copper body For example, description has been given of manufacturing of the porous copper body by using a manufacturing facility illustrated in FIG. 3 .
  • the porous copper body can be manufactured by using another manufacturing facility.
  • an oxidation atmosphere in which copper or a copper alloy is oxidized at a predetermined temperature may be used.
  • the atmosphere is not limited to the atmospheric atmosphere, and may be an atmosphere in which 0.5 vol % or greater of oxygen is contained in an inert gas (for example, nitrogen).
  • an inert gas for example, nitrogen
  • a nitrogen-hydrogen mixed gas containing several vol % or greater of hydrogen an argon-hydrogen mixed gas, a pure hydrogen gas, an ammonia decomposed gas which is industrially used in many cases, and the like and a propane decomposed gas which is industrially used in many cases, and the like.
  • the skeleton of the porous copper body is formed by sintering the copper fibers.
  • a porous copper body such as a fiber nonwoven fabric or a metal filter is prepared, and by performing the oxidation treatment on the porous copper body under conditions of a holding temperature of 500° C. to 1050° C. in an oxidizing atmosphere and performing the reduction treatment on the porous copper body under conditions of a holding temperature of 500° C. to 1050° C. in a reducing atmosphere, the porosity-normalized electrical conductivity ⁇ N may be set to 20% IACS or higher.
  • oxidation-reduction layer is formed on the surface of the skeleton.
  • the oxidation-reduction layer may not be sufficiently formed as long as the porosity-normalized electrical conductivity ⁇ N is 20% IACS or higher.
  • copper fibers formed from oxygen-free copper (JIS C1020), phosphorous-deoxidized copper (JIS C1201 and C1220), or tough pitch copper (JIS C1100) are used.
  • other high conductivity copper alloys such as Cr-copper (C18200) or Cr—Zr copper (C18150) may be used.
  • the copper fibers are used, however, copper powders may be used and both the copper powders and the copper fibers may also be used.
  • An average particle diameter of the copper powders is preferably 0.005 mm to 0.3 mm and more preferably 0.01 mm to 0.1 mm.
  • the copper powder content is preferably 5% to 20% based on the copper fiber content.
  • porous copper composite member having a structure illustrated in FIG. 4 as an example.
  • a porous copper composite member having a structure as illustrated in FIG. 6 to FIG. 11 is also possible.
  • the bonding method in which the sintered layer including oxidation-reduction layer is formed on the bonding portion of the porous copper body and the main member body is exemplified as a desirable method, but there is no limitation thereto.
  • Various welding methods laser welding method and resistance welding process
  • a bonding method by a brazing method using brazing material melting at low temperature may also be used as long as the porosity-normalized electrical conductivity ⁇ N of the porous copper body is 20% IACS or higher.
  • it may be a porous copper composite member 200 having a structure in which, as a main member body, a plurality of copper tubes 220 are inserted into a porous copper body 210 .
  • FIG. 7 it may be a porous copper composite member 300 having a structure in which, as a main member body, a copper tube 320 curved in a U-shape is inserted into a porous copper body 310 .
  • FIG. 8 it may be a porous copper composite member 400 having a structure in which a porous copper body 410 is bonded to an inner peripheral surface of a copper tube 420 that is a main member body.
  • it may be a porous copper composite member 500 having a structure in which a porous copper body 510 is bonded to an outer peripheral surface of a copper tube 520 that is a main member body.
  • FIG. 10 it may be a porous copper composite member 600 having a structure in which a porous copper body 610 is bonded to an inner peripheral surface and an outer peripheral surface of a copper tube 620 that is a main member body.
  • it may be a porous copper composite member 700 having a structure in which a porous copper body 710 is bonded to both surfaces of a copper plate 720 that is a main member body.
  • the true density D T (g/cm 3 ) was measured by a precision balance to calculate the porosity P by the following expression.
  • the mass of the porous copper body was represented as m(g), and a volume of the porous copper body was V (cm 3 ).
  • the electrical conductivity ⁇ P (% IACS) was measured by the 4-terminal sensing under conditions of a voltage terminal interval of 150 mm and measuring current of 0.5 A with a microohm high tester 3227 manufactured by HIOKI E.E. CORPORATION, in accordance with JIS C 2525.
  • the porosity-normalized electrical conductivity ⁇ N was calculated by the following expression.
  • the apparent density ratio D A (%) was calculated according to the following expression.
  • m is the mass (g) of the porous copper body.
  • V is the volume (cm 3 ) of the porous copper body.
  • D T is the true density (g/cm 3 ) of copper or copper alloy constituting the porous copper body.
  • the porosity P was in a range of 50% to 90% and all the porosity-normalized electrical conductivity was higher than 20% IACS.
  • an oxidation-reduction treatment was performed using copper powders illustrated in Table 2 under conditions illustrated in Table 2 to manufacture a porous copper body.
  • the porosity and the porosity-normalized electrical conductivity were measured with respect to the porous copper body that was obtained.
  • the porosity and the porosity-normalized electrical conductivity were measured by the same method as in Example 1, except that, in Example 2, D T at the time of calculating the porosity-normalized electrical conductivity was set to a true density (g/cm 3 ) of the copper powders constituting the porous copper body. Evaluation results are illustrated in Table 2.
  • the porosity P was in a range of 50% to 90% and all the porosity-normalized electrical conductivity was higher than 20% IACS.
  • the porosity and the porosity-normalized electrical conductivity were measured.
  • the porosity and the porosity-normalized electrical conductivity were measured by the same method as in Example 1, except that, in Example 3, D T at the time of calculating the porosity-normalized electrical conductivity was set to a true density (g/cm 3 ) of the copper fibers constituting the porous copper body. Evaluation results are illustrated in Table 3.
  • the porosity P was in a range of 50% to 90% and all the porosity-normalized electrical conductivity was higher than 20% IACS.
  • porous copper body a porous copper composite member in which the porous copper body is bonded to a main member body, a method of manufacturing the porous copper body, and method of manufacturing the porous copper composite member of the disclosure, it is possible to obtain a porous copper body which has sufficient conductivity and heat conductivity, even in a case where a porosity is high.
  • the porous copper body is suitable for a conductive member and a heat-transfer member.

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