WO2022044585A1 - Procédé de fabrication d'une microstructure remplie de métal - Google Patents

Procédé de fabrication d'une microstructure remplie de métal Download PDF

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Publication number
WO2022044585A1
WO2022044585A1 PCT/JP2021/026287 JP2021026287W WO2022044585A1 WO 2022044585 A1 WO2022044585 A1 WO 2022044585A1 JP 2021026287 W JP2021026287 W JP 2021026287W WO 2022044585 A1 WO2022044585 A1 WO 2022044585A1
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Prior art keywords
metal
resin layer
insulating film
filled microstructure
conductor
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PCT/JP2021/026287
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English (en)
Japanese (ja)
Inventor
順二 川口
吉則 堀田
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富士フイルム株式会社
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Priority to CN202180050316.XA priority Critical patent/CN115956144A/zh
Priority to JP2022545520A priority patent/JPWO2022044585A1/ja
Priority to KR1020237006062A priority patent/KR20230043153A/ko
Publication of WO2022044585A1 publication Critical patent/WO2022044585A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/20—Electrolytic after-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32

Definitions

  • the present invention relates to a method for manufacturing a metal-filled microstructure that removes the resin layer covering the surface of the oxide film after heating, and more particularly to a method for manufacturing a metal-filled microstructure in which the resin layer is heated in an atmosphere having an oxygen partial pressure of 10,000 Pa or less. ..
  • a structure in which a plurality of through holes provided in an insulating base material are filled with a conductive substance such as metal is one of the fields that have been attracting attention in nanotechnology in recent years, for example, as an anisotropic conductive member.
  • An anisotropic conductive member is inserted between an electronic component such as a semiconductor element and a circuit board, and an electrical connection can be obtained between the electronic component and the circuit board simply by applying pressure. Therefore, the electronic component such as a semiconductor element can be used. It is widely used as an electrical connection member, an inspection connector for performing a functional inspection, and the like.
  • electronic components such as semiconductor devices are significantly downsized. Electronic components such as conventional wire bonding methods that directly connect wiring boards, flip chip bonding, thermocompression bonding, etc. may not be able to sufficiently guarantee the stability of electrical connections of electronic components.
  • An anisotropic conductive member is attracting attention as a connecting member.
  • an anisotropic conductive member for example, in Patent Document 1, one surface of an aluminum substrate is anodized, and micropores and micropores existing on one surface of the aluminum substrate in the thickness direction are used.
  • an alkaline aqueous solution containing a metal M1 having a higher hydrogen overvoltage than aluminum is used to make a barrier of the anodic oxide film.
  • the metal filling step of performing electrolytic plating treatment to fill the inside of the micropore with the metal M2, and the metal filling step the aluminum substrate is removed.
  • Patent Document 1 has a resin layer forming step of providing a resin layer on the surface of the anodic oxide film on the side where the aluminum substrate is not provided, after the metal filling step and before the substrate removing step.
  • Patent Document 1 a resin layer is provided on the surface of the anodic oxide film on the side where the aluminum substrate is not provided.
  • the metal-filled microstructure is used, for example, for the electrical connection of two semiconductor chips. In this case, it is necessary to peel off the above-mentioned resin layer.
  • the metal-filled microstructure of Patent Document 1 is used for electrical connection between two semiconductor chips as described above, the electrical conductivity between the semiconductor chips may not be sufficient. A metal-filled microstructure with good electrical conductivity is desired.
  • An object of the present invention is to provide a method for manufacturing a metal-filled microstructure having good electrical conductivity.
  • one aspect of the present invention has a plurality of conductors provided in a state of penetrating the insulating film in the thickness direction and being electrically insulated from each other, and the conductor is an insulating film.
  • a method for producing a metal-filled microstructure which comprises a heating step of heating the layer and a removing step of removing the resin layer heated by the heating step from the insulating film, wherein the resin layer contains a heat-removable adhesive. Is to provide.
  • the oxygen partial pressure of the atmosphere is preferably 1.0 Pa or less.
  • the partial pressure of the inert gas in the atmosphere is preferably 85% or more of the total pressure in the atmosphere.
  • the partial pressure of the reducing gas in the atmosphere is preferably 85% or more of the total pressure in the atmosphere.
  • the total pressure of the atmosphere is preferably 5.0 Pa or less.
  • the conductor preferably contains a base metal.
  • the plurality of conductors preferably have a conductor having a cross-sectional area of 20 ⁇ m 2 or less in a cross section perpendicular to the longitudinal direction of the conductor. It is preferable that the temperature reached by the resin layer in the heating step is 150 ° C. or lower. It is preferable that the conductor protrudes from both sides in the thickness direction of the insulating film, and the resin layer is provided on both sides in the thickness direction of the insulating film.
  • the insulating film is preferably an anodic oxide film.
  • Metal-filled microstructure] 1 to 8 are schematic cross-sectional views showing an example of a method for manufacturing a metal-filled microstructure according to an embodiment of the present invention in order of steps.
  • the metal-filled microstructure 10 is provided with an insulating film 12 having electrical insulating properties and an insulating film 12 penetrating the insulating film 12 in the thickness direction Dt and being electrically insulated from each other. It has a plurality of conductors 14 and the like. The conductor 14 projects from at least one surface of the insulating film 12 in the thickness direction Dt.
  • the conductor 14 projects from at least one surface in the thickness direction Dt of the insulating film 12, it is preferable that the conductor 14 projects from the front surface 12a or the back surface 12b in a configuration that projects from one surface.
  • the insulating film 12 is composed of, for example, an anodic oxide film 15.
  • the plurality of conductors 14 are arranged on the insulating film 12 in a state of being electrically insulated from each other.
  • the insulating film 12 has a plurality of pores 13 penetrating in the thickness direction Dt.
  • Conductors 14 are provided in the plurality of pores 13.
  • the conductor 14 projects from the surface 12a of the insulating film 12 in the thickness direction Dt.
  • the metal-filled microstructure 10 has anisotropic conductivity in which conductors 14 are arranged in a state of being electrically insulated from each other.
  • the metal-filled microstructure 10 has conductivity in the thickness direction Dt, but the conductivity in the direction parallel to the surface 12a of the insulating film 12 is sufficiently low.
  • the outer shape of the metal-filled microstructure 10 is not particularly limited, and is, for example, a quadrangle or a circle.
  • the outer shape of the metal-filled microstructure 10 can be shaped according to the application, ease of manufacture, and the like.
  • a method for manufacturing a metal-filled microstructure an example in which the insulating film is composed of an anodic oxide film of aluminum will be described.
  • An aluminum substrate is used to form an anodic oxide film of aluminum. Therefore, in an example of the method for manufacturing a structure, first, as shown in FIG. 1, an aluminum substrate 30 is prepared. The size and thickness of the aluminum substrate 30 are appropriately determined according to the thickness of the insulating film 12 of the finally obtained metal-filled microstructure 10 (see FIG. 8), the apparatus to be processed, and the like.
  • the aluminum substrate 30 is, for example, a rectangular plate material.
  • the metal substrate is not limited to the aluminum substrate, and a metal substrate capable of forming the electrically insulating insulating film 12 can be used.
  • the surface 30a (see FIG. 1) on one side of the aluminum substrate 30 is anodized.
  • the surface 30a (see FIG. 1) on one side of the aluminum substrate 30 is anodized, and as shown in FIG. 2, the insulating film 12 having a plurality of pores 13 extending in the thickness direction Dt of the aluminum substrate 30. That is, the anodic oxide film 15 is formed.
  • a barrier layer 31 is present at the bottom of each pore 13.
  • the above-mentioned anodizing step is called an anodizing treatment step.
  • the insulating film 12 having the plurality of pores 13 has the barrier layer 31 at the bottom of the pores 13, but the barrier layer 31 shown in FIG. 2 is removed.
  • an insulating film 12 (see FIG. 3) having a plurality of pores 13 without the barrier layer 31 is obtained.
  • the step of removing the barrier layer 31 is referred to as a barrier layer removing step.
  • the barrier layer removing step the barrier layer 31 of the insulating film 12 is removed by using an alkaline aqueous solution containing ions of the metal M1 having a higher hydrogen overvoltage than aluminum, and at the same time, the bottom 32c of the pores 13 (see FIG. 3).
  • a metal layer 35a (see FIG. 3) made of a metal (metal M1) is formed on the surface 32d (see FIG. 3). As a result, the aluminum substrate 30 exposed to the pores 13 is covered with the metal layer 35a.
  • the alkaline aqueous solution containing the ion of the metal M1 may further contain an aluminum ion-containing compound (sodium aluminate, aluminum hydroxide, aluminum oxide, etc.).
  • the content of the aluminum ion-containing compound is preferably 0.1 to 20 g / L, more preferably 0.3 to 12 g / L, and even more preferably 0.5 to 6 g / L in terms of the amount of aluminum ions.
  • the metal layer 35a can be used as an electrode for electrolytic plating.
  • a metal 35b is used for plating, and the plating proceeds starting from the metal layer 35a formed on the surface 32d (see FIG. 3) of the bottom 32c (see FIG. 3) of the pore 13.
  • the metal 35b constituting the conductor 14 is filled inside the pores 13 of the insulating film 12.
  • a conductive conductor 14 is formed. It should be noted that the metal layer 35a and the metal 35b are collectively filled with the metal 35.
  • the step of filling the pores 13 of the insulating film 12 with the metal 35b is called a metal filling step.
  • the conductor 14 is not limited to being made of metal, and a conductive substance can be used. Electroplating is used in the metal filling step, and the metal filling step will be described in detail later.
  • the surface 12a of the insulating film 12 corresponds to one surface of the insulating film 12. After the metal filling step, as shown in FIG. 5, a part of the surface 12a of the insulating film 12 on the side where the aluminum substrate 30 is not provided is removed in the thickness direction Dt after the metal filling step, and the insulating film 12 is filled in the metal filling step.
  • the metal 35 is projected from the surface 12a of the insulating film 12.
  • the step of projecting the conductor 14 from the surface 12a of the insulating film 12 is referred to as a surface metal projecting step.
  • the resin layer 16 is formed on the surface 12a of the insulating film 12 on which the projecting portion 14a of the conductor 14 is formed, as shown in FIG. As a result, the surface of the insulating film from which the conductor protrudes is covered with the resin layer, and the structure 18 is obtained.
  • the process of preparing the structure 18 is called a preparation process.
  • the step of forming the resin layer 16 covering the surface of the insulating film 12 on which the conductor 14 protrudes is referred to as a resin layer forming step.
  • the resin layer 16 contains a heat-removable adhesive.
  • the aluminum substrate 30 is removed from the structure 18 as shown in FIG. The step of removing the aluminum substrate 30 is called a substrate removing step.
  • the step of heating the resin layer 16 is called a heating step.
  • a semiconductor wafer heating device used for manufacturing a semiconductor element can be used.
  • the heating step is performed, for example, in a metal container used for heating a semiconductor wafer in a semiconductor manufacturing apparatus.
  • the structure 18 after removing the substrate is placed in the container, and the oxygen partial pressure in the container is set to 10,000 Pa or less.
  • the total pressure and partial pressure of the atmosphere in the heating step can be measured using, for example, a pressure gauge. Thereby, the above-mentioned oxygen partial pressure can be measured.
  • the partial pressure of the inert gas and the partial pressure of the reducing gas which will be described later, can also be measured.
  • the oxygen partial pressure for example, the oxygen partial pressure can be adjusted by degassing.
  • the heating step is not limited to an atmosphere in which the oxygen partial pressure is 10,000 Pa or less. It is preferable that the temperature reached by the resin layer in the heating step is 150 ° C. or lower. When the temperature reached by the resin layer in the heating step is 150 ° C. or lower, the electrical conductivity becomes good.
  • the step of removing the resin layer 16 from the insulating film 12 is referred to as a removal step.
  • the method for removing the resin layer 16 is not particularly limited, and the resin layer 16 is removed using, for example, a tool such as tweezers.
  • the insulating film 12 may be peeled from the resin layer 16 by using a tool such as tweezers.
  • the atmosphere of the removing step does not have to be the same as the atmosphere of the heating step, and may be, for example, an atmospheric atmosphere.
  • FIG. 9 to 11 are schematic cross-sectional views showing another example of the method for manufacturing a metal-filled microstructure according to the embodiment of the present invention in order of steps.
  • the metal 35, that is, the conductor 14, which has been partially removed and filled in the metal filling step, may be projected from the back surface 12b of the insulating film 12. As a result, the protruding portion 14b is obtained.
  • the above-mentioned front surface metal protrusion step and back surface metal protrusion step may have both steps, but may have one of the front surface metal protrusion step and the back surface metal protrusion step.
  • the front surface metal projecting process and the back surface metal projecting process correspond to the "projection process", and the front surface metal projecting process and the back surface metal projecting process are both projecting processes.
  • the structure 18 has a protruding portion 14a and a protruding portion in which the conductor 14 protrudes from the front surface 12a and the back surface 12b of the insulating film 12, that is, from both sides of the insulating film 12 in the thickness direction Dt.
  • a configuration having 14b may be used.
  • a resin layer 16 is formed on the back surface 12b of the insulating film 12 shown in FIG. 9, and resin layers 16 are provided on both sides of the anodic oxide film in the thickness direction Dt.
  • the above-mentioned heating step and the removal step of the resin layer 16 are carried out on the structure 18 to obtain a metal-filled microstructure 10 having the protruding portions 14a and the protruding portions 14b shown in FIG.
  • the barrier layer 31 is not only removed but also the pores 13 are removed by removing the barrier layer using an alkaline aqueous solution containing ions of metal M1 having a higher hydrogen overvoltage than aluminum.
  • a metal layer 35a of the metal M1 that is less likely to generate hydrogen gas than aluminum is formed on the aluminum substrate 30 exposed at the bottom.
  • the in-plane uniformity of the metal filling becomes good. It is considered that this is because the generation of hydrogen gas by the plating solution was suppressed and the metal filling by the electrolytic plating proceeded easily.
  • a holding step of holding the voltage of 95% or more and 105% or less of the voltage (holding voltage) selected from the range of less than 30% of the voltage in the anodic oxidation treatment step for a total of 5 minutes or more is provided. It has been found that the uniformity of metal filling during the plating treatment is greatly improved by combining the application of an alkaline aqueous solution containing the ions of the metal M1. Therefore, it is preferable to have a holding step. Although the detailed mechanism is unknown, in the barrier layer removal step, a layer of metal M1 is formed under the barrier layer by using an alkaline aqueous solution containing ions of metal M1, which damages the interface between the aluminum substrate and the anodic oxide film. It is considered that this is because the reception can be suppressed and the uniformity of dissolution of the barrier layer is improved.
  • a metal layer 35a made of a metal (metal M1) was formed at the bottom of the pores 13, but the present invention is not limited to this, and only the barrier layer 31 is removed to form the pores 13.
  • the aluminum substrate 30 is exposed on the bottom.
  • the aluminum substrate 30 may be used as an electrode for electrolytic plating with the aluminum substrate 30 exposed.
  • an aluminum anodic oxide film is used because pores having a desired average diameter are formed and a conductor is easily formed as described above.
  • the anodic oxide film of aluminum is not limited, and an anodic oxide film of valve metal can be used. Therefore, valve metal is used as the metal substrate.
  • examples of the valve metal include, for example, the above-mentioned aluminum, tantalum, niobium, titanium, hafnium, zirconium, zinc, tungsten, bismuth, antimony and the like.
  • an aluminum anodic oxide film is preferable because it has good dimensional stability and is relatively inexpensive. Therefore, it is preferable to manufacture the structure using an aluminum substrate.
  • the thickness of the anodic oxide film is the same as the thickness ht of the insulating film 12 described above.
  • the metal substrate is used for manufacturing a structure and is a substrate for forming an anodic oxide film.
  • a metal substrate on which an anodic oxide film can be formed is used, and a metal substrate composed of the above-mentioned valve metal can be used.
  • an aluminum substrate is used as the metal substrate because it is easy to form the anodic oxide film as the anodic oxide film.
  • the aluminum substrate used to form the insulating film 12 is not particularly limited, and specific examples thereof include a pure aluminum plate; an alloy plate containing aluminum as a main component and containing a trace amount of a foreign element; low-purity aluminum (for example, for example).
  • the surface of one side of the aluminum substrate on which the anodic oxide film is formed by the anodic oxidation treatment preferably has an aluminum purity of 99.5% by mass or more, more preferably 99.9% by mass or more, and 99. It is more preferably .99% by mass or more. When the aluminum purity is in the above range, the regularity of the micropore arrangement is sufficient.
  • the aluminum substrate is not particularly limited as long as it can form an anodic oxide film, and for example, JIS (Japanese Industrial Standards) 1050 material is used.
  • the surface of one side of the aluminum substrate to be anodized is previously heat-treated, degreased and mirror-finished.
  • the heat treatment, the degreasing treatment, and the mirror finish treatment the same treatments as those described in paragraphs [0044] to [0054] of JP-A-2008-270158 can be applied.
  • the mirror finish treatment before the anodic oxidation treatment is, for example, electrolytic polishing, and for the electrolytic polishing, for example, an electrolytic polishing liquid containing phosphoric acid is used.
  • anodizing process For the anodizing treatment, a conventionally known method can be used, but from the viewpoint of increasing the regularity of the micropore arrangement and ensuring the anisotropic conductivity of the structure, a self-regular method or a constant voltage treatment should be used. Is preferable.
  • the self-regularization method and the constant voltage treatment of the anodizing treatment the same treatments as those described in paragraphs [0056] to [0108] and [FIG. 3] of JP-A-2008-270158 are performed. Can be applied.
  • the method for manufacturing the structure may include a holding step.
  • the holding step is a voltage of 95% or more and 105% or less of the holding voltage selected from the range of 1 V or more and less than 30% of the voltage in the above-mentioned anodizing treatment step after the above-mentioned anodizing treatment step for a total of 5 minutes or more.
  • the holding step is a total of 95% or more and 105% or less of the holding voltage selected from the range of 1 V or more and less than 30% of the voltage in the above-mentioned anodizing treatment step after the above-mentioned anodizing treatment step.
  • This is a step of performing electrolytic treatment for 5 minutes or more.
  • the "voltage in the anodizing treatment” is a voltage applied between the aluminum and the counter electrode, and for example, if the electrolysis time by the anodizing treatment is 30 minutes, the voltage maintained for 30 minutes. The average value.
  • the voltage in the holding step is 5% or more and 25% or less of the voltage in the anodizing process. It is preferably present, and more preferably 5% or more and 20% or less.
  • the total holding time in the holding step is preferably 5 minutes or more and 20 minutes or less, more preferably 5 minutes or more and 15 minutes or less, and 5 minutes or more. It is more preferably 10 minutes or less.
  • the holding time in the holding step may be 5 minutes or more in total, but is preferably 5 minutes or more continuously.
  • the voltage in the holding step may be set by continuously or stepwise reducing the voltage from the voltage in the anodic oxidation treatment step to the voltage in the holding step, but for the reason of further improving the in-plane uniformity, the anodic oxidation treatment is performed. It is preferable to set the voltage to 95% or more and 105% or less of the above-mentioned holding voltage within 1 second after the completion of the step.
  • the above-mentioned holding step can also be performed continuously with the above-mentioned anodizing treatment step, for example, by lowering the electrolytic potential at the end of the above-mentioned anodizing treatment step.
  • the same electrolytic solution and treatment conditions as those of the above-mentioned conventionally known anodizing treatment can be adopted.
  • the anodic oxide film having a plurality of micropores has a barrier layer (not shown) at the bottom of the micropores as described above. It has a barrier layer removing step for removing the barrier layer.
  • the barrier layer removing step is a step of removing the barrier layer of the anodic oxide film by using, for example, an alkaline aqueous solution containing ions of a metal M1 having a hydrogen overvoltage higher than that of aluminum.
  • the barrier layer removing step described above the barrier layer is removed, and a conductor layer made of the metal M1 is formed at the bottom of the micropores.
  • the hydrogen overvoltage means the voltage required for hydrogen to be generated.
  • the hydrogen overvoltage of aluminum (Al) is ⁇ 1.66 V (Journal of the Chemical Society of Japan, 1982, (8)). , P1305-1313).
  • Metal M1 having a higher hydrogen overvoltage than that of aluminum and the value of the hydrogen overvoltage thereof are shown below.
  • the barrier layer is removed as described above because it causes a substitution reaction with the metal M2 to be filled in the anodizing treatment step described later and has less influence on the electrical characteristics of the metal to be filled inside the micropores.
  • the metal M1 used in the step is preferably a metal having a higher ionization tendency than the metal M2 used in the metal filling step described later.
  • examples of the metal M1 used in the barrier layer removing step described above include Zn, Fe, Ni, Sn and the like. Above all, it is preferable to use Zn and Ni, and it is more preferable to use Zn.
  • examples of the metal M1 used in the barrier layer removing step described above include Zn and Fe, and among them, Zn is preferably used.
  • the method of removing the barrier layer using such an alkaline aqueous solution containing the metal M1 is not particularly limited, and examples thereof include the same methods as those of conventionally known chemical etching treatments.
  • ⁇ Chemical etching process> To remove the barrier layer by chemical etching treatment, for example, the structure after the above-mentioned anodic oxidation treatment step is immersed in an alkaline aqueous solution, the inside of the micropores is filled with the alkaline aqueous solution, and then the micropores of the anodic oxide film are opened. Only the barrier layer can be selectively dissolved by a method of contacting the surface on the portion side with a pH buffer solution or the like.
  • the alkaline aqueous solution containing the above-mentioned metal M1 it is preferable to use at least one alkaline aqueous solution selected from the group consisting of sodium hydroxide, potassium hydroxide and lithium hydroxide.
  • the concentration of the alkaline aqueous solution is preferably 0.1 to 5% by mass.
  • the temperature of the alkaline aqueous solution is preferably 10 to 60 ° C, more preferably 15 to 45 ° C, and further preferably 20 to 35 ° C. Specifically, for example, 50 g / L, 40 ° C. phosphoric acid aqueous solution, 0.5 g / L, 30 ° C.
  • sodium hydroxide aqueous solution 0.5 g / L, 30 ° C. potassium hydroxide aqueous solution and the like are preferably used. Be done.
  • a buffer solution corresponding to the above-mentioned alkaline aqueous solution can be appropriately used.
  • the immersion time in the alkaline aqueous solution is preferably 5 to 120 minutes, more preferably 8 to 120 minutes, still more preferably 8 to 90 minutes, and preferably 10 to 90 minutes. Especially preferable. Of these, 10 to 60 minutes is preferable, and 15 to 60 minutes is more preferable.
  • the pores 13 can also be formed by expanding the diameter of the micropores and removing the barrier layer.
  • pore wide processing is used to increase the diameter of the micropores.
  • the pore-wide treatment is a treatment in which the anodic oxide film is immersed in an acid aqueous solution or an alkaline aqueous solution to dissolve the anodic oxide film and expand the pore size of the micropores.
  • An aqueous solution of an inorganic acid such as hydrochloric acid or a mixture thereof, or an aqueous solution of sodium hydroxide, potassium hydroxide, lithium hydroxide or the like can be used.
  • the barrier layer at the bottom of the micropores can also be removed by the pore wide treatment, and by using the sodium hydroxide aqueous solution in the pore wide treatment, the diameter of the micropores is expanded and the barrier layer is removed.
  • the metal to be filled as a conductor in the pores 13 described above to form a conductor and the metal constituting the metal layer are made of a material having an electrical resistivity of 103 ⁇ ⁇ cm or less. It is preferable to have.
  • Specific examples of the above-mentioned metals are preferably gold (Au), silver (Ag), copper (Cu), aluminum (Al), magnesium (Mg), nickel (Ni), and zinc (Zn). ..
  • copper (Cu), gold (Au), aluminum (Al), nickel (Ni) are preferable, and copper (Cu) and gold (Au) are preferable from the viewpoint of electrical conductivity and formation by a plating method. ) Is more preferable, and copper (Cu) is further preferable.
  • ⁇ Plating method> As the plating method for filling the inside of the pores with metal, for example, an electrolytic plating method or an electroless plating method can be used. Here, it is difficult to selectively deposit (grow) a metal in the pores with a high aspect ratio by a conventionally known electrolytic plating method used for coloring or the like. It is considered that this is because the precipitated metal is consumed in the pores and the plating does not grow even if electrolysis is performed for a certain period of time or longer. Therefore, when metal is filled by the electrolytic plating method, it is necessary to allow a rest time during pulse electrolysis or constant potential electrolysis. The rest time is required to be 10 seconds or more, preferably 30 to 60 seconds. It is also desirable to add ultrasonic waves to promote the agitation of the electrolyte.
  • the electrolytic voltage is usually 20 V or less, preferably 10 V or less, but it is preferable to measure the precipitation potential of the target metal in the electrolytic solution to be used in advance and perform constant potential electrolysis within the potential of + 1 V.
  • constant potential electrolysis it is desirable that cyclic voltammetry can be used in combination, and potentiometer devices such as Solartron, BAS, Hokuto Denko, and IVIUM can be used.
  • plating liquid As the plating solution, a conventionally known plating solution can be used. Specifically, when precipitating copper, an aqueous solution of copper sulfate is generally used, but the concentration of copper sulfate is preferably 1 to 300 g / L, more preferably 100 to 200 g / L. preferable. Further, the precipitation can be promoted by adding hydrochloric acid to the electrolytic solution. In this case, the hydrochloric acid concentration is preferably 10 to 20 g / L. When depositing gold, it is desirable to use a sulfuric acid solution of tetrachlorogold and perform plating by AC electrolysis.
  • the plating solution preferably contains a surfactant.
  • a surfactant known ones can be used.
  • Sodium lauryl sulfate which is conventionally known as a surfactant to be added to the plating solution, can be used as it is.
  • Both ionic (cationic / anionic / bidirectional) and nonionic (nonionic) hydrophilic portions can be used, but the point of avoiding the generation of bubbles on the surface of the object to be plated.
  • a cation beam activator is desirable.
  • the concentration of the surfactant in the plating solution composition is preferably 1% by mass or less. In the electroless plating method, it takes a long time to completely fill the pores composed of pores having a high aspect with metal, so it is desirable to fill the pores with metal by using the electrolytic plating method.
  • the substrate removing step is a step of removing the above-mentioned aluminum substrate after the metal filling step.
  • the method for removing the aluminum substrate is not particularly limited, and for example, a method for removing by melting is preferable.
  • a treatment liquid that is difficult to dissolve the anodic oxide film and easily dissolves aluminum.
  • a treatment liquid preferably has a dissolution rate in aluminum of 1 ⁇ m / min or more, more preferably 3 ⁇ m / min or more, and further preferably 5 ⁇ m / min or more.
  • the dissolution rate for the anodic oxide film is preferably 0.1 nm / min or less, more preferably 0.05 nm / min or less, and even more preferably 0.01 nm / min or less.
  • a pH hydrogen ion index
  • the treatment liquid for dissolving aluminum is based on an acid or alkaline aqueous solution, for example, manganese, zinc, chromium, iron, cadmium, cobalt, nickel, tin, lead, antimony, bismuth, copper, mercury, silver, palladium, platinum.
  • a gold compound for example, platinum chloride acid
  • these fluorides, these chlorides and the like are preferably blended.
  • an acid aqueous solution base is preferable, and a chloride blend is preferable.
  • a treatment liquid obtained by blending a hydrochloric acid aqueous solution with mercury chloride (hydrochloric acid / mercury chloride) and a treatment liquid obtained by blending a hydrochloric acid aqueous solution with copper chloride (hydrochloric acid / copper chloride) are preferable from the viewpoint of treatment latitude.
  • the composition of the treatment liquid for dissolving aluminum is not particularly limited, and for example, a bromine / methanol mixture, a bromine / ethanol mixture, aqua regia, or the like can be used.
  • the acid or alkali concentration of the treatment liquid for dissolving aluminum is preferably 0.01 to 10 mol / L, more preferably 0.05 to 5 mol / L. Further, the treatment temperature using the treatment liquid for dissolving aluminum is preferably ⁇ 10 ° C. to 80 ° C., preferably 0 ° C. to 60 ° C.
  • the above-mentioned melting of the aluminum substrate is performed by bringing the aluminum substrate after the above-mentioned plating step into contact with the above-mentioned treatment liquid.
  • the contact method is not particularly limited, and examples thereof include a dipping method and a spraying method. Above all, the dipping method is preferable.
  • the contact time at this time is preferably 10 seconds to 5 hours, more preferably 1 minute to 3 hours.
  • a support may be provided on the insulating film 12, for example.
  • the support preferably has the same outer shape as the insulating film 12. By attaching a support, handleability is increased.
  • an acid aqueous solution or an alkaline aqueous solution that does not dissolve the metal constituting the conductor 14 but dissolves the insulating film 12 that is, aluminum oxide (Al 2 O 3 ) is used. ..
  • the insulating film 12 is partially removed by bringing the above-mentioned aqueous acid solution or alkaline aqueous solution into contact with the insulating film 12 having the pores 13 filled with metal.
  • the method of bringing the above-mentioned acid aqueous solution or alkaline aqueous solution into contact with the insulating film 12 is not particularly limited, and examples thereof include a dipping method and a spraying method. Of these, the dipping method is preferable.
  • an aqueous acid solution When an aqueous acid solution is used, it is preferable to use an aqueous solution of an inorganic acid such as sulfuric acid, phosphoric acid, nitric acid and hydrochloric acid, or a mixture thereof. Of these, an aqueous solution containing no chromic acid is preferable because it is excellent in safety.
  • the concentration of the aqueous acid solution is preferably 1 to 10% by mass.
  • the temperature of the aqueous acid solution is preferably 25 to 60 ° C.
  • an alkaline aqueous solution it is preferable to use at least one alkaline aqueous solution selected from the group consisting of sodium hydroxide, potassium hydroxide and lithium hydroxide.
  • the concentration of the alkaline aqueous solution is preferably 0.1 to 5% by mass.
  • the temperature of the alkaline aqueous solution is preferably 20 to 35 ° C. Specifically, for example, a 50 g / L, 40 ° C. phosphoric acid aqueous solution, a 0.5 g / L, 30 ° C. sodium hydroxide aqueous solution, or a 0.5 g / L, 30 ° C. potassium hydroxide aqueous solution is preferably used. ..
  • the immersion time in the acid aqueous solution or the alkaline aqueous solution is preferably 8 to 120 minutes, more preferably 10 to 90 minutes, and even more preferably 15 to 60 minutes.
  • the soaking time means the total of each soaking time when the soaking treatment for a short time is repeated.
  • a cleaning treatment may be performed between the immersion treatments.
  • the metal 35 that is, the conductor 14 is projected from the front surface 12a or the back surface 12b of the insulating film 12, but the conductor 14 is preferably projected from the front surface 12a or the back surface 12b of the insulating film 12 by 10 nm to 1000 nm. It is more preferable to project from 50 nm to 500 nm. That is, the amount of protrusion of the insulating film 12 of the protruding portion 14a from the front surface 12a and the amount of protrusion of the conductor 14 from the back surface 12b of the insulating film 12 of the protruding portion 14b are preferably 10 nm to 1000 nm, more preferably 50 nm to 500 nm, respectively. be.
  • the cross section of the metal-filled microstructure 10 is observed with an electrolytic discharge scanning electron microscope at a magnification of 20,000 times, and the height of the protrusions of the conductor is 10 points. The measured average value.
  • the inside of the pore 13 is filled with a conductive substance such as metal, and then the insulating film 12 and the end portion of the conductive substance such as metal are formed. It is preferable to selectively remove the anodic oxide film after processing the particles so that they have the same planar shape.
  • heat treatment can be performed for the purpose of reducing the distortion in the conductor 14 generated by the metal filling.
  • the heat treatment is preferably carried out in a reducing atmosphere from the viewpoint of suppressing the oxidation of the metal, specifically, the oxygen concentration is preferably 20 Pa or less, and more preferably carried out under vacuum.
  • the vacuum means a state of a space in which at least one of the gas density and the atmospheric pressure is lower than that of the atmosphere. Further, it is preferable that the heat treatment is performed while applying stress to the insulating film 12 for the purpose of straightening.
  • this is a step of forming a resin layer that covers the surface of the insulating film from which the conductor protrudes.
  • the resin layer is provided to protect the conductor and to improve the transportability.
  • the resin layer forming step is a step to be carried out after the above-mentioned metal filling step, after the surface metal projecting step, and before the substrate removing step.
  • the resin layer contains a heat-removable adhesive as described above.
  • the resin layer is more preferably a film with an adhesive layer whose adhesiveness is weakened by heat treatment and which can be peeled off.
  • the method of attaching the above-mentioned film with an adhesive layer is not particularly limited, and the film can be attached using a conventionally known surface protective tape affixing device or laminator.
  • Examples of the film with an adhesive layer whose adhesiveness is weakened by the above-mentioned heat treatment and which can be peeled off include a heat-peelable resin layer.
  • the heat-peeling type resin layer has adhesive strength at room temperature and can be easily peeled off only by heating, and most of them mainly use effervescent microcapsules or the like.
  • Specific examples of the adhesive constituting the adhesive layer include a rubber adhesive, an acrylic adhesive, a vinyl alkyl ether adhesive, a silicone adhesive, a polyester adhesive, and a polyamide adhesive. , Urethane-based pressure-sensitive adhesives, styrene-diene block copolymerization-based pressure-sensitive adhesives, and the like.
  • the heating step is a step for facilitating the removal of the resin layer in order to remove the resin layer. Moreover, when the resin layer is simply heated, it may be oxidized depending on the metal species constituting the conductor and the electric resistance may increase. Therefore, when a metal-filled microstructure is used as an anisotropic conductive member and a semiconductor chip is electrically connected, the electrical conductivity may decrease. However, by carrying out the heating step in an atmosphere having an oxygen partial pressure of 10,000 Pa or less, an increase in electrical resistance is suppressed, and when a semiconductor chip is electrically connected, electrical conductivity is improved. In the heating step, the oxygen partial pressure of the atmosphere is 10,000 Pa or less, but it is preferably 1.0 Pa or less. When the oxygen partial pressure is 10,000 Pa or less, the oxidation of the conductor is suppressed, but the smaller the oxygen partial pressure is, the more preferable it is because the oxidation is suppressed regardless of the metal type of the conductor.
  • the heating step can have the atmosphere shown below.
  • the partial pressure of the inert gas in the atmosphere is preferably 85% or more of the total pressure of the atmosphere.
  • the oxygen partial pressure can be relatively reduced and the oxidation of the conductor can be suppressed.
  • the partial pressure of the inert gas for example, the partial pressure of the inert gas can be adjusted by adjusting the supply amount of the inert gas into the container in which the heating step is carried out.
  • the partial pressure of the reducing gas in the atmosphere is preferably 85% or more of the total pressure of the atmosphere. If the partial pressure of the reducing gas in the atmosphere is 85% or more of the total pressure, the oxygen partial pressure can be relatively reduced, and the oxidation of the conductor can also be suppressed.
  • the reducing gas is preferably a gas that has a small reaction with the conductor.
  • the partial pressure of the reducing gas can be adjusted by adjusting the supply amount of the reducing gas into the container in which the heating step is carried out.
  • the inert gas is not particularly limited, but is, for example, a rare gas such as helium gas, neon gas, and argon gas, or nitrogen gas.
  • the inert gas the above-mentioned various gases may be used alone, or at least two gases may be mixed.
  • the reducing gas is not particularly limited, but is, for example, hydrogen gas, carbon monoxide gas, or a hydrocarbon gas such as CH 4 , C 3 H 8 , or C 4 H 10 .
  • the reducing gas the above-mentioned various gases may be used alone, or at least two gases may be mixed.
  • the total pressure of the atmosphere in the heating step is preferably 5.0 Pa or less.
  • the oxygen partial pressure of the atmosphere becomes small and the oxidation of the conductor can be suppressed, which is preferable.
  • the total pressure of the atmosphere can be reduced to 5.0 Pa or less by, for example, reducing the pressure in the container using a vacuum pump.
  • the oxygen partial pressure may be lowered by degassing as described above, the atmosphere may be replaced by the inert gas or the reducing gas, or the atmosphere may be replaced by the inert gas and the reducing gas. It may be replaced.
  • the heating conditions in the heating step are preferably 80 to 350 ° C., more preferably 90 to 250 ° C., and most preferably 100 to 200 ° C.
  • the temperature reached by the resin layer in the heating step is preferably 150 ° C. or lower. In the heating step, if the temperature is lower than the above temperature range, it becomes difficult to peel off the resin layer. On the other hand, if the temperature is high, the filling metal is oxidized, that is, the conductor is oxidized, and defects such as cracks or cracks in the structure are caused.
  • the removal step is not particularly limited as long as the resin layer can be removed. Further, the removal step does not have to have the same atmosphere as the heating step, and after heating the resin layer, for example, it may be taken out from the container used in the heating step and carried out in an atmospheric atmosphere.
  • a part of the surface of the aluminum substrate may be anodized using a mask layer having a desired shape.
  • the structure 18 shown in FIG. 7 from which the substrate has been removed is an embodiment intended to be supplied in a state of being wound around the winding core 21 in a roll shape.
  • the metal-filled microstructure 10 is used as an anisotropic conductive member
  • the resin layer 16 is removed by carrying out the above-mentioned heating step and the removal step of the resin layer 16.
  • the metal-filled microstructure 10 can be used as the anisotropic conductive member.
  • a winding step of winding the metal-filled microstructure 10 into a roll shape with the above-mentioned resin layer 16 after the above-mentioned arbitrary resin layer forming step It is preferable to have.
  • the winding method in the above-mentioned winding step is not particularly limited, and examples thereof include a method of winding on a winding core 21 (see FIG. 12) having a predetermined diameter and a predetermined width.
  • the average thickness of the metal-filled microstructure 10 excluding the resin layer 16 is preferably 30 ⁇ m or less, preferably 5 to 20 ⁇ m. Is more preferable.
  • the metal-filled microstructure 10 excluding the resin layer is machined by FIB (Focused Ion Beam) in the thickness direction, and the cross section thereof is surfaced by a field emission scanning electron microscope (FE-SEM). It can be calculated by taking a photograph (magnification 50,000 times) and using it as an average value measured at 10 points.
  • the production method of the present invention includes a polishing step, a surface smoothing step, a protective film forming treatment, and a washing treatment described in paragraphs [0049] to [0057] of International Publication No. 2015/029881. You may have.
  • various processes and types as shown below can be applied from the viewpoint of handling in manufacturing and the use of the metal-filled microstructure 10 as an anisotropic conductive member.
  • the substrate removing step described above there may be a step of fixing the metal-filled microstructure on a silicon wafer using wax and thinning the layer by polishing. Then, after the step of thinning, after thoroughly cleaning the surface, the above-mentioned surface metal projecting step can be performed. Next, a temporary adhesive is applied to the surface on which the metal is projected and fixed on the silicon wafer, and then the wax is melted by heating to peel off the silicon wafer, and the surface on the side of the peeled metal-filled microstructure is peeled off. On the other hand, the above-mentioned back surface metal protrusion step can be performed. Although solid wax may be used, sky coat (manufactured by Nikka Seiko Co., Ltd.) or the like can be used to improve the uniformity of coating thickness.
  • the aluminum substrate is subjected to a rigid substrate (for example, a silicon wafer, a glass substrate) using a temporary adhesive, wax or a functional adsorption film. Etc.), it may have a step of thinning the surface of the above-mentioned anodic oxide film on the side where the above-mentioned aluminum substrate is not provided by polishing. Then, after the step of thinning, after thoroughly cleaning the surface, the above-mentioned surface metal projecting step can be performed.
  • a rigid substrate for example, a silicon wafer, a glass substrate
  • a resin material for example, epoxy resin, polyimide resin, etc.
  • a rigid substrate for example, epoxy resin, polyimide resin, etc.
  • For pasting with a resin material select one whose adhesive strength is greater than the adhesive strength with a temporary adhesive or the like, and after pasting with the resin material, the rigid substrate pasted first is peeled off, and the above-mentioned substrate is attached.
  • the removal step, the polishing step, and the back surface metal protrusion processing step can be performed in order.
  • Q-chuck registered trademark
  • the functional adsorption film Q-chuck (registered trademark) (manufactured by Maruishi Sangyo Co., Ltd.) or the like can be used.
  • the metal-filled microstructure is provided as a product in a state of being attached to a rigid substrate (for example, a silicon wafer, a glass substrate, etc.) by a peelable layer.
  • a rigid substrate for example, a silicon wafer, a glass substrate, etc.
  • the metal-filled microstructure is used as a joining member, the surface of the metal-filled microstructure is temporarily adhered to the device surface, the rigid substrate is peeled off, and then the device to be connected is attached.
  • the upper and lower devices can be joined by a metal-filled microstructure by installing in an appropriate place and heat-pressing.
  • a heat peeling layer may be used, or a photopeeling layer may be used in combination with a glass substrate.
  • each of the above-mentioned steps can be performed on a single sheet, or can be continuously processed on a web using an aluminum coil as a raw material. Further, in the case of continuous treatment, it is preferable to install an appropriate cleaning step and drying step between each step.
  • a metal-filled microstructure in which a metal is filled inside a through hole derived from a micropore provided in an insulating base material made of an anodic oxide film of an aluminum substrate.
  • the body is obtained.
  • the anisotropic conductive member described in JP-A-2008-270158 that is, in an insulating base material (anodized film of an aluminum substrate having micropores).
  • the insulating film 12 is formed of a conductor and makes a plurality of conductors 14 electrically insulated from each other.
  • the insulating film has an electrical insulating property.
  • the insulating film 12 has a plurality of pores 13 on which the conductor 14 is formed.
  • the insulating film is made of, for example, an inorganic material.
  • As the insulating film for example, one having an electrical resistivity of about 10 14 ⁇ ⁇ cm can be used.
  • the insulating film is composed of, for example, an anodic oxide film.
  • the insulating film may be made of, for example, a metal oxide, a metal nitride, glass, silicon carbide, ceramics such as silicon nitride, a carbon base material such as diamond-like carbon, polyimide, a composite material thereof, or the like. ..
  • a ceramic material or an inorganic material containing 50% by mass or more of a carbon material may be formed on an organic material having through holes.
  • the length of the insulating film 12 in the thickness direction Dt is preferably in the range of 1 to 1000 ⁇ m, more preferably in the range of 5 to 500 ⁇ m, and in the range of 10 to 300 ⁇ m. It is more preferable to be inside. When the thickness of the insulating film 12 is within this range, the handleability of the insulating film 12 is improved.
  • the thickness ht of the insulating film 12 is preferably 30 ⁇ m or less, and more preferably 5 to 20 ⁇ m, from the viewpoint of ease of winding.
  • the thickness of the anodic oxide film is determined by cutting the anodic oxide film with a focused ion beam (FIB) in the thickness direction Dt and taking a surface photograph (magnification 5) of the cross section with a field emission scanning electron microscope (FE-SEM). It is a value calculated as an average value measured at 10 points by taking a picture (10,000 times).
  • the distance between the conductors 14 in the insulating film 12 is preferably 5 nm to 800 nm, more preferably 10 nm to 200 nm, and even more preferably 20 nm to 60 nm. When the distance between the conductors 14 in the insulating film 12 is within the above range, the insulating film 12 sufficiently functions as an electrically insulating partition wall of the conductor 14.
  • the distance between the conductors means the width between the adjacent conductors
  • the cross section of the metal-filled microstructure 10 is observed with an electrolytic discharge scanning electron microscope at a magnification of 200,000 times, and the distance between the adjacent conductors is observed.
  • the average diameter of the pores is preferably 1 ⁇ m or less, more preferably 5 to 500 nm, further preferably 20 to 400 nm, even more preferably 40 to 200 nm, and even more preferably 50 to 100 nm. Most preferably.
  • the conductor 14 having the above average diameter can be obtained.
  • the average diameter of the pores 13 is obtained by photographing the surface of the insulating film 12 from directly above at a magnification of 100 to 10000 times using a scanning electron microscope.
  • the magnification in the above range can be appropriately selected so that a photographed image capable of extracting 20 or more pores can be obtained.
  • the maximum value of the distance between the ends of the pore portions was measured. That is, since the shape of the opening of the pore is not limited to a substantially circular shape, when the shape of the opening is non-circular, the maximum value of the distance between the ends of the pore portion is set as the opening diameter. Therefore, for example, even in the case of a pore having a shape in which two or more pores are integrated, this is regarded as one pore, and the maximum value of the distance between the ends of the pore portions is set as the opening diameter. ..
  • the plurality of conductors 14 are provided in the anodic oxide film in a state of being electrically insulated from each other.
  • the plurality of conductors 14 have electrical conductivity.
  • the conductor is composed of a conductive substance.
  • the conductive substance is not particularly limited, and examples thereof include metals. Specific examples of the metal preferably include gold (Au), silver (Ag), copper (Cu), aluminum (Al), magnesium (Mg), nickel (Ni) and the like. From the viewpoint of electrical conductivity, copper, gold, aluminum, and nickel are preferable, copper and gold are more preferable, and copper is most preferable.
  • copper is a base metal, but it may be a base metal.
  • Base metals are easily oxidized in the air, but in the method for producing a metal-filled microstructure, even if the conductor is made of a base metal, a metal-filled microstructure having good electrical conductivity can be obtained.
  • oxide conductive substances can be mentioned. Examples of the oxide conductive substance include tin oxide (ITO) doped with indium.
  • ITO tin oxide
  • the conductor may be made of a conductive resin containing nanoparticles such as Cu or Ag.
  • the height H of the conductor 14 in the thickness direction Dt is preferably 10 to 300 ⁇ m, more preferably 20 to 30 ⁇ m.
  • the plurality of conductors preferably have a conductor having a cross-sectional area of 20 ⁇ m 2 or less in the longitudinal direction of the conductor, that is, a cross section perpendicular to the thickness direction Dt of the insulating film 12.
  • a conductor having a cross-sectional area of 20 ⁇ m 2 or less has a diameter d of about 3.99 ⁇ m or less.
  • the average diameter d of the conductor 14 is more preferably 1 ⁇ m or less, further preferably 5 to 500 nm, further preferably 20 to 400 nm, and even more preferably 40 to 200 nm. Most preferably, it is 50 to 100 nm.
  • the density of the conductor 14 is preferably 20,000 pieces / mm 2 or more, more preferably 2 million pieces / mm 2 or more, further preferably 10 million pieces / mm 2 or more, and 50 million pieces / mm 2. It is particularly preferable that it is / mm 2 or more, and most preferably 100 million pieces / mm 2 or more.
  • the distance p between the centers of the adjacent conductors 14 is preferably 20 nm to 500 nm, more preferably 40 nm to 200 nm, and further preferably 50 nm to 140 nm.
  • the average diameter of the conductor is obtained by photographing the surface of the anodic oxide film from directly above at a magnification of 100 to 10000 times using a scanning electron microscope.
  • the magnification in the photographed image, at least 20 conductors having an annular shape around them are extracted, the diameters thereof are measured and used as the opening diameter, and the average value of these opening diameters is calculated as the average diameter of the conductors.
  • the magnification in the above range can be appropriately selected so that a photographed image capable of extracting 20 or more conductors can be obtained.
  • the maximum value of the distance between the ends of the conductor portion was measured. That is, since the shape of the opening of the conductor is not limited to a substantially circular shape, when the shape of the opening is non-circular, the maximum value of the distance between the ends of the conductor portion is set as the opening diameter. Therefore, for example, even in the case of a conductor having a shape in which two or more conductors are integrated, this is regarded as one conductor, and the maximum value of the distance between the ends of the conductor portions is set as the opening diameter.
  • the protrusion is part of the conductor and is columnar.
  • the protruding portion is preferably cylindrical because it can increase the contact area with the object to be joined.
  • the average protruding length of the protruding portion 14a and the average length of the protruding portion 14b are preferably 30 nm to 500 nm, and the upper limit is more preferably 100 nm or less.
  • a cross-sectional image of the protrusion is obtained using a field emission scanning electron microscope as described above, and the height of the protrusion is determined based on the cross-sectional image. It is the average value measured by measuring 10 points each.
  • the resin layer is provided on at least one of the front surface and the back surface of the anodic oxide film, and for example, the protruding portion of the conductor is embedded. That is, the resin layer covers the end portion of the conductor protruding from the anodic oxide film and protects the protruding portion.
  • the resin layer preferably exhibits fluidity in a temperature range of, for example, 50 ° C to 200 ° C and cures at 200 ° C or higher. The resin layer will be described in detail later.
  • the average protruding length of the conductor 14 is preferably less than the average thickness of the resin layer 16. If the average protrusion length of the protrusion 14a and the average length of the protrusion 14b of the conductor 14 are both less than the average thickness of the resin layer 16, the protrusions 14a and 14b are both the resin layer of the resin layer 16. It is embedded in the portion 20a, and the conductor 14 is protected by the resin layer 16.
  • the average thickness of the resin layer 16 is the average distance from the front surface 12a of the insulating film 12 or the average distance from the back surface 12b of the insulating film 12.
  • the resin layer 16 is cut in the thickness direction Dt of the metal-filled microstructure 10, and a cross-sectional observation of the cut cross section is performed using a field emission scanning electron microscope (FE-SEM).
  • the distances from the surface 12a of the insulating film 12 are measured at 10 points corresponding to the resin layer, and the average value of the measured values at 10 points is used. Further, the distances from the back surface 12b of the insulating film 12 are measured at 10 points corresponding to the resin layer, and the average value of the measured values at 10 points is used.
  • the average thickness of the resin layer is preferably 200 to 1000 nm, more preferably 400 to 600 nm. When the average thickness of the resin layer is 200 to 1000 nm as described above, the effect of protecting the protruding portion of the conductor 14 can be sufficiently exhibited.
  • the metal-filled microstructure 10 is cut in the thickness direction Dt, and a field emission scanning electron microscope (FE-SEM) is used. It is an average value obtained by observing the cross section of the cut cross section and measuring 10 points corresponding to each size.
  • FE-SEM field emission scanning electron microscope
  • FIG. 14 is a schematic view showing an example of a laminated device using the metal-filled microstructure of the embodiment of the present invention.
  • the laminated device 40 shown in FIG. 14 uses the above-mentioned metal-filled microstructure 10 (see FIGS. 8 and 11) as an anisotropic conductive member 45 exhibiting anisotropic conductivity.
  • the semiconductor element 42, the anisotropic conductive member 45, and the semiconductor element 44 are joined in this order in the stacking direction Ds and electrically connected.
  • the conductor 14 see FIGS. 8 and 11 of the metal-filled microstructure 10 (see FIGS.
  • the laminated device 40 is in the form of joining one semiconductor element 44 to one semiconductor element 42, but is not limited thereto. It may be in the form of joining three semiconductor elements via an anisotropic conductive member 45. In this case, the laminated device is composed of three semiconductor elements and two anisotropic conductive members 45.
  • the laminated device 40 is not limited to the one having a semiconductor element, and may be a substrate having an electrode.
  • the substrate having an electrode is, for example, a wiring board, an interposer, or the like.
  • the form of the laminated device is not particularly limited, and for example, SoC (System on a chip), SiP (System in Package), PoP (Package on Package), PiP (Package in Package), CSP (Chip). Scale Package), TSV (Through Silicon Via) and the like.
  • the laminated device 40 may have a semiconductor element that functions as an optical sensor.
  • a semiconductor element and a sensor chip (not shown) are laminated in the stacking direction Ds.
  • the sensor chip may be provided with a lens.
  • the semiconductor element is formed with a logic circuit, and its configuration is not particularly limited as long as it can process the signal obtained by the sensor chip.
  • the sensor chip has an optical sensor that detects light.
  • the optical sensor is not particularly limited as long as it can detect light, and for example, a CCD (Charge Coupled Device) image sensor or a CMOS (Complementary Metal Oxide Semiconductor) image sensor is used.
  • the configuration of the lens is not particularly limited as long as it can condense light on the sensor chip, and for example, a lens called a microlens is used.
  • the semiconductor element 42, the semiconductor element 44, and the semiconductor element 46 described above those having an element region (not shown) can be used.
  • the element region will be described later.
  • An element constituent circuit or the like is formed in the element region, and the semiconductor element is provided with, for example, a rewiring layer (not shown).
  • a semiconductor element having a logic circuit and a semiconductor element having a memory circuit can be combined. Further, all the semiconductor elements may have a memory circuit, or all the semiconductor elements may have a logic circuit.
  • the combination of the semiconductor elements in the laminated device 40 may be a combination of a sensor, an actuator, an antenna or the like, a memory circuit and a logic circuit, and is appropriately determined according to the application of the laminated device 40 and the like.
  • the semiconductor element As the object to be joined of the structure, the semiconductor element is exemplified as described above, but for example, the object has an electrode or an element region.
  • the device having an electrode include a semiconductor device that exerts a specific function by itself, but also includes a device in which a plurality of devices are gathered to exert a specific function. Further, those that only transmit electric signals such as wiring members are included, and printed wiring boards and the like are also included in those having electrodes.
  • the element region is an region in which various element constituent circuits and the like for functioning as an electronic element are formed.
  • a memory circuit such as a flash memory
  • MEMS Micro Electro Mechanical Systems
  • MEMS Micro Electro Mechanical Systems
  • sensors include sensors, actuators, antennas and the like.
  • Sensors include various sensors such as acceleration, sound, and light.
  • an element component circuit or the like is formed in the element region, and an electrode (not shown) is provided for electrically connecting the semiconductor chip to the outside.
  • the element region has an electrode region on which an electrode is formed.
  • the electrode in the element region is, for example, a Cu post.
  • the electrode region is basically a region including all the formed electrodes. However, if the electrodes are provided separately, the region where each electrode is provided is also referred to as an electrode region.
  • the form of the structure may be a single piece such as a semiconductor chip, a form such as a semiconductor wafer, or a form of a wiring layer. Further, the structure is bonded to the object to be bonded, but the object to be bonded is not particularly limited to the above-mentioned semiconductor element or the like, for example, a semiconductor element in a wafer state, a semiconductor element in a chip state, or a printed wiring. Plates, heat sinks, etc. are the objects to be joined.
  • semiconductor element 42 and semiconductor element 44 may include, for example, a logic LSI (Large Scale Integration) (for example, ASIC (Application Specific Integrated Circuit), FPGA (Field Programmable Gate Array), ASSP (Application Specific).
  • LSI Large Scale Integration
  • ASIC Application Specific Integrated Circuit
  • FPGA Field Programmable Gate Array
  • ASSP Application Specific
  • Microprocessor for example, CPU (Central Processing Unit), GPU (Graphics Processing Unit), etc.), Memory (for example, DRAM (Dynamic Random Access Memory), HMC (Hybrid Memory Cube), MRAM (MagneticRAM: Magnetic memory) and PCM (Phase-Change Memory), ReRAM (Resistive RAM), FeRAM (Ferroelectric RAM: ferroelectric memory), flash memory (NAND (Not AND) flash), etc.) , LED (Light Emitting Diode), (for example, microflash of mobile terminal, in-vehicle, projector light source, LCD backlight, general lighting, etc.), power device, analog IC (Integrated Circuit), (for example, DC (Direct Current)) )-DC (Direct Current) converters, isolated gate bipolar transistors (IGBTs), etc.), MEMS (Micro Electro Mechanical Systems), (eg, acceleration sensors, pressure sensors, oscillators, gyro sensors, etc.), wireless (eg, GPS (eg, GPS (eg, GPS (
  • the semiconductor element is, for example, one complete, and the semiconductor element alone exhibits a specific function such as a circuit or a sensor.
  • the semiconductor element may have an interposer function. Further, for example, it is possible to stack a plurality of devices such as a logic chip having a logic circuit and a memory chip on a device having an interposer function. Further, in this case, even if the electrode size is different for each device, the bonding can be performed.
  • the laminated device is not limited to a one-to-many form in which a plurality of semiconductor elements are bonded to one semiconductor element, but is a form in which a plurality of semiconductor elements and a plurality of semiconductor elements are bonded. It may be in a plurality of to multiple forms.
  • the present invention is basically configured as described above. Although the method for producing the metal-filled microstructure of the present invention has been described in detail above, the present invention is not limited to the above-described embodiment, and various improvements or changes have been made without departing from the gist of the present invention. Of course, it is also good.
  • a TEG chip (daisy chain pattern) and an interposer manufactured by Waltz Co., Ltd. were prepared, and these were installed above and below the chip bonder, and the alignment was adjusted in advance. After adjusting the alignment, the prepared metal-filled microstructures were superposed on the Cu post side of the interposer installed on the lower side, and a room temperature joining device (WP-100 (model), manufactured by PMT Co., Ltd.) was used. Heat crimping was performed under the conditions of a temperature of 250 ° C. for 1 minute and 6 MPa, and the bonding was performed. For the sample after joining, the electrical resistance between the chip wirings was measured.
  • Example 1 The metal-filled microstructure of Example 1 will be described.
  • [Metal-filled microstructure] ⁇ Manufacturing of aluminum substrate> Si: 0.06% by mass, Fe: 0.30% by mass, Cu: 0.005% by mass, Mn: 0.001% by mass, Mg: 0.001% by mass, Zn: 0.001% by mass, Ti: A molten metal containing 0.03% by mass, the balance of which is Al and an aluminum alloy of unavoidable impurities is prepared, and after the molten metal treatment and filtration are performed, an ingot having a thickness of 500 mm and a width of 1200 mm is DC (Direct Chill). ) Made by the casting method.
  • the surface was scraped to an average thickness of 10 mm by a surface mill, kept at 550 ° C for about 5 hours, and when the temperature dropped to 400 ° C, the thickness was 2.7 mm using a hot rolling mill. It was made into a rolled plate. Further, after heat treatment was performed at 500 ° C. using a continuous annealing machine, the thickness was finished to 1.0 mm by cold rolling to obtain an aluminum substrate of JIS (Japanese Industrial Standards) 1050 material. After making this aluminum substrate 1030 mm wide, each of the following treatments was performed.
  • JIS Japanese Industrial Standards
  • the above-mentioned aluminum substrate was subjected to electrolytic polishing treatment using an electrolytic polishing liquid having the following composition under the conditions of a voltage of 25 V, a liquid temperature of 65 ° C., and a liquid flow rate of 3.0 m / min.
  • the cathode was a carbon electrode, and the power supply was GP0110-30R (manufactured by Takasago Seisakusho Co., Ltd.).
  • the flow velocity of the electrolytic solution was measured using a vortex flow monitor FLM22-10PCW (manufactured by AS ONE Corporation).
  • Electrolytic polishing liquid composition ⁇ 85% by mass phosphoric acid (reagent manufactured by Wako Pure Chemical Industries, Ltd.) 660 mL ⁇ Pure water 160mL ⁇ Sulfuric acid 150mL ⁇ Ethylene glycol 30mL
  • the aluminum substrate after the electrolytic polishing treatment was subjected to anodizing treatment by a self-regularization method according to the procedure described in JP-A-2007-204802.
  • the aluminum substrate after the electrolytic polishing treatment was subjected to pre-anodizing treatment for 5 hours with an electrolytic solution of 0.50 mol / L oxalic acid under the conditions of a voltage of 40 V, a liquid temperature of 16 ° C., and a liquid flow velocity of 3.0 m / min. ..
  • the pre-anodized aluminum substrate was subjected to a film removal treatment by immersing it in a mixed aqueous solution of 0.2 mol / L chromic anhydride and 0.6 mol / L phosphoric acid (liquid temperature: 50 ° C.) for 12 hours. Then, a reanodizing treatment was performed for 3 hours and 45 minutes with an electrolytic solution of 0.50 mol / L oxalic acid under the conditions of a voltage of 40 V, a liquid temperature of 16 ° C., and a liquid flow rate of 3.0 m / min, and an anode having a film thickness of 30 ⁇ m. An oxide film was obtained.
  • the cathode was a stainless steel electrode, and GP0110-30R (manufactured by Takasago Seisakusho Co., Ltd.) was used as the power source.
  • a NeoCool BD36 manufactured by Yamato Kagaku Co., Ltd.
  • a pair stirrer PS-100 manufactured by EYELA Tokyo Rika Kikai Co., Ltd. was used as the stirring and heating device.
  • the flow velocity of the electrolytic solution was measured using a vortex type flow monitor FLM22-10PCW (manufactured by AS ONE Corporation).
  • etching treatment was performed in which zinc oxide was dissolved in an aqueous sodium hydroxide solution (50 g / l) so as to have a concentration of 2000 ppm and immersed at 30 ° C. for 150 seconds to perform an etching treatment on the anodized film.
  • the barrier layer at the bottom of the micropores was removed and zinc was simultaneously deposited on the surface of the exposed aluminum substrate.
  • the average thickness of the anodic oxide film after the barrier layer removing step was 30 ⁇ m.
  • ⁇ Metal filling process> an aluminum substrate was used as a cathode and platinum was used as a cathode to perform electrolytic plating. Specifically, a copper plating solution having the composition shown below was used and constant current electrolysis was performed to prepare a metal-filled microstructure in which nickel was filled inside the micropores.
  • a plating apparatus manufactured by Yamamoto Plating Tester Co., Ltd. is used, and a power source (HZ-3000) manufactured by Hokuto Denko Co., Ltd. is used to perform cyclic voltammetry in the plating solution for precipitation. After confirming the potential, the treatment was performed under the conditions shown below.
  • ⁇ Surface metal protrusion process> The structure after the metal filling step is immersed in an aqueous sodium hydroxide solution (concentration: 5% by mass, liquid temperature: 20 ° C.), and the immersion time is adjusted so that the height of the protruding portion is 400 nm, and the aluminum anode is used. The surface of the oxide film was selectively melted to prepare a structure in which copper, which is a filling metal, was projected.
  • an aqueous sodium hydroxide solution concentration: 5% by mass, liquid temperature: 20 ° C.
  • ⁇ Substrate removal process> the aluminum substrate was dissolved and removed by immersing it in a mixed solution of copper chloride / hydrochloric acid to prepare a metal-filled microstructure having an average thickness of 30 ⁇ m.
  • the diameter of the conduction path in the produced metal-filled microstructure was 60 nm
  • the pitch between the conduction paths was 100 nm
  • the density of the conduction path was 57.7 million pieces / mm 2 .
  • ⁇ Back side metal protrusion process> The structure after the metal filling step is immersed in an aqueous sodium hydroxide solution (concentration: 5% by mass, liquid temperature: 20 ° C.), and the immersion time is adjusted so that the height of the protruding portion is 400 nm, and the aluminum anode is used. The surface of the oxide film was selectively melted to prepare a structure in which copper, which is a filling metal, was projected.
  • an aqueous sodium hydroxide solution concentration: 5% by mass, liquid temperature: 20 ° C.
  • the structure was placed in the container. After that, when the total pressure was 100%, the partial pressure of each gas was 80% nitrogen and 20% oxygen, and the total pressure was 4.0 ⁇ 10 ⁇ 2 Pa.
  • the resin layer was heated at a temperature of 120 ° C. for 2 minutes using a heater, and then the resin layer was peeled off.
  • the pressure inside the container was reduced using a vacuum pump to adjust the total pressure.
  • Example 2 In Example 2, when the total pressure is 100%, the partial pressure of each gas is 80% nitrogen and 20% oxygen, except that the total pressure is 4.0 Pa. It was produced in the same manner as above. (Example 3) In Example 3, when the total pressure is 100%, the partial pressure of each gas is 80% nitrogen and 20% oxygen, except that the total pressure is 1.0 ⁇ 10 4 Pa. Was produced in the same manner as in Example 1. (Example 4) In Example 4, when the total pressure is 100%, the partial pressure of each gas is 99.8% nitrogen and 0.2% oxygen, and the total pressure is 1.0 ⁇ 106 Pa. It was produced in the same manner as in Example 1 except that. (Example 5) In Example 5, when the total pressure is 100%, the partial pressure of each gas is 99.8% argon and 0.2% oxygen, and the total pressure is 1.0 ⁇ 106 Pa. It was produced in the same manner as in Example 1 except that.
  • Example 6 In Example 6, when the total pressure is 100%, the partial pressure of each gas is 99.8% hydrogen and 0.2% oxygen, and the total pressure is 1.0 ⁇ 10 6 Pa. It was produced in the same manner as in Example 1 except that.
  • Example 7 (Example 7) In Example 7, when the total pressure is 100%, the partial pressure of each gas is 99.998% nitrogen and 0.002% oxygen, except that the total pressure is 4.0 Pa. was produced in the same manner as in Example 1.
  • Example 8 In Example 8, when the total pressure is 100%, the partial pressure of each gas is 99.998% argon and 0.002% oxygen, except that the total pressure is 4.0 Pa. was produced in the same manner as in Example 1.
  • Example 9 In Example 9, when the total pressure is 100%, the partial pressure of each gas is 99.998% for hydrogen and 0.002% for oxygen, except that the total pressure is 4.0 Pa. Was produced in the same manner as in Example 1.
  • Example 10 In Example 10, the heat-peeling type resin base material with an adhesive layer was changed to Riva Alpha (registered trademark) 3195VS (manufactured by Nitto Denko KK) in the resin layer forming step. Regarding the atmosphere of the heating step, when the total pressure was 100%, the partial pressure of each gas was 80% nitrogen and 20% oxygen, and the total pressure was 1.0 ⁇ 10 4 Pa. The resin layer was heated at a temperature of 170 ° C. for 2 minutes to prepare the same as in Example 1 except that the resin layer was peeled off.
  • Riva Alpha registered trademark
  • 3195VS manufactured by Nitto Denko KK
  • Example 11 In Example 11, when the total pressure is 100%, the partial pressure of each gas is 99.998% nitrogen and 0.002% oxygen, except that the total pressure is 4.0 Pa. was produced in the same manner as in Example 10.
  • Example 12 Example 12 was produced in the same manner as in Example 3 except that the heat-peeling type resin base material with an adhesive layer was changed to SomaTac TE PS-2021TE (manufactured by SOMAR Corporation) in the resin layer forming step.
  • Comparative Example 1 Comparative Example 1 was produced in the same manner as in Example 12 except that the total pressure of the atmosphere in the heating step was 1.0 ⁇ 10 6 Pa.
  • Examples 1 to 12 had lower electrical resistance and better electrical conductivity than Comparative Example 1.
  • Comparative Example 1 the oxygen partial pressure exceeded 10,000 Pa in the atmosphere of the heating step, and the electric resistance became large.
  • Examples 1, 2, 7 to 9 and 11 the oxygen partial pressure was 1.0 Pa or less, the electric resistance was further small, and the electric conductivity was further good. From Examples 1 to 3, the lower the total pressure, the smaller the electric resistance and the better the electric conductivity. From Examples 3 and 10 and Examples 7 and 11, the lower the heating temperature, the smaller the electric resistance and the better the electric conductivity.
  • Metal-filled microstructure 12 Insulation film 12a Surface 12b Back surface 13 Pore 14 Conductor 14a Projection 14b Projection 15 Anodized oxide film 16 Resin layer 18 Structure 21 Winding core 30 Aluminum substrate 30a Surface 31 Barrier layer 32c Bottom 32d Surface 35 Metal 35a Metal layer 35b Metal 40 Laminated device 42 Semiconductor element 44 Semiconductor element 45 Anotropically conductive member Ds Laminating direction Dt Thickness direction H Height d Average diameter ht Thickness p Center-to-center distance

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Abstract

L'invention concerne un procédé de fabrication d'une microstructure remplie de métal ayant une bonne conductivité électrique. Le procédé de fabrication d'une microstructure remplie de métal comprend : une étape de préparation pour préparer une structure ayant une pluralité de conducteurs et une couche de résine, les conducteurs étant disposés dans un état de pénétration d'un film diélectrique dans une direction d'épaisseur et étant isolés électriquement les uns des autres, les conducteurs dépassant à partir d'une face du film diélectrique dans la direction de l'épaisseur, la face du film diélectrique, où les conducteurs dépassent, étant recouverte par la couche de résine ; une étape de chauffage pour chauffer au moins la couche de résine dans une atmosphère où une pression partielle d'oxygène est de 10 000 Pa maximum ; et une étape de retrait pour retirer la couche de résine chauffée dans l'étape de chauffage du film diélectrique. La couche de résine comprend un adhésif pouvant être retiré à la chaleur.
PCT/JP2021/026287 2020-08-24 2021-07-13 Procédé de fabrication d'une microstructure remplie de métal WO2022044585A1 (fr)

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KR1020237006062A KR20230043153A (ko) 2020-08-24 2021-07-13 금속 충전 미세 구조체의 제조 방법

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220165619A1 (en) * 2019-08-16 2022-05-26 Fujifilm Corporation Method for manufacturing structure

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011090865A (ja) * 2009-10-22 2011-05-06 Shinko Electric Ind Co Ltd 導電フィルムおよびその製造方法、並びに半導体装置およびその製造方法
WO2017057150A1 (fr) * 2015-09-29 2017-04-06 富士フイルム株式会社 Procédé de fabrication d'un dispositif à microstructure remplie de métal
WO2018037805A1 (fr) * 2016-08-24 2018-03-01 富士フイルム株式会社 Procédé de stockage
WO2019039071A1 (fr) * 2017-08-25 2019-02-28 富士フイルム株式会社 Structure, procédé de fabrication de structure, stratifié et boîtier semi-conducteur

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011090865A (ja) * 2009-10-22 2011-05-06 Shinko Electric Ind Co Ltd 導電フィルムおよびその製造方法、並びに半導体装置およびその製造方法
WO2017057150A1 (fr) * 2015-09-29 2017-04-06 富士フイルム株式会社 Procédé de fabrication d'un dispositif à microstructure remplie de métal
WO2018037805A1 (fr) * 2016-08-24 2018-03-01 富士フイルム株式会社 Procédé de stockage
WO2019039071A1 (fr) * 2017-08-25 2019-02-28 富士フイルム株式会社 Structure, procédé de fabrication de structure, stratifié et boîtier semi-conducteur

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220165619A1 (en) * 2019-08-16 2022-05-26 Fujifilm Corporation Method for manufacturing structure

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