WO2020235070A1 - Corps lié de résine-métal de magnésium et son procédé de fabrication - Google Patents

Corps lié de résine-métal de magnésium et son procédé de fabrication Download PDF

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Publication number
WO2020235070A1
WO2020235070A1 PCT/JP2019/020368 JP2019020368W WO2020235070A1 WO 2020235070 A1 WO2020235070 A1 WO 2020235070A1 JP 2019020368 W JP2019020368 W JP 2019020368W WO 2020235070 A1 WO2020235070 A1 WO 2020235070A1
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WIPO (PCT)
Prior art keywords
magnesium metal
metal member
resin
less
washing
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PCT/JP2019/020368
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English (en)
Japanese (ja)
Inventor
孝 眞 金
修平 三浦
鉄也 藤村
星 衡 李
Original Assignee
ジオネーション株式会社
株式会社東亜電化
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Application filed by ジオネーション株式会社, 株式会社東亜電化 filed Critical ジオネーション株式会社
Priority to KR1020217042145A priority Critical patent/KR102618505B1/ko
Priority to CN201980096719.0A priority patent/CN114207192A/zh
Priority to PCT/JP2019/020368 priority patent/WO2020235070A1/fr
Publication of WO2020235070A1 publication Critical patent/WO2020235070A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
    • B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/70—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by moulding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/72—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined
    • B29C66/723—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined being multi-layered
    • B29C66/7232—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined being multi-layered comprising a non-plastics layer
    • B29C66/72321—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the structure of the material of the parts to be joined being multi-layered comprising a non-plastics layer consisting of metals or their alloys
    • 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
    • C25D11/30—Anodisation of magnesium or alloys based thereon

Definitions

  • the present invention relates to a resin-magnesium metal joint and a method for producing the same, and more particularly to a resin-magnesium metal joint capable of strongly bonding a resin member and a magnesium metal member and a method for producing the same.
  • Patent Document 1 discloses an electrochemical surface treatment method for forming a film of triazinethiol (sulfur organic compound) on the surface of a metal member as a technique for joining a resin member and a metal member.
  • the metal include copper, nickel, aluminum, iron, cobalt, tin and stainless steel.
  • An object of the present invention is to provide a resin-magnesium metal joint body capable of improving the joint strength between a resin member and a magnesium metal member, and to provide a method for producing a resin magnesium metal joint body having good joint strength.
  • the resin magnesium metal joint according to the present invention is a resin magnesium metal joint formed by joining a magnesium metal member and a thermoplastic resin member, and the magnesium metal member and the resin member have a thickness of 50. It is characterized in that it is bonded by an anodic oxide film having a diameter of about 3000 nm.
  • the other resin magnesium metal joint according to the present invention is a resin magnesium metal joint formed by joining a magnesium metal member and a thermoplastic resin member, and the magnesium metal member and the thermoplastic resin member have a thickness. Is bonded by an anodic oxide film in which 50 to 3000 nm triazine thiol is present inside and outside.
  • the anodized film is 1 to 60% by weight of O, 1 to 90% of Mg, 3% or less of S, 20% or less of Al, 3% or less of P, 3% or less of Zn, and Cu. It is characterized by having a component composition of 3% or less, Mn of 3% or less, Ni of 3% or less, Si of 20% or less, and F of 3% or less.
  • the method for producing a resin magnesium metal joint according to the present invention is a production method for producing a resin magnesium metal joint, in which a degreasing step of washing a magnesium metal member with an alkaline solution and a degreasing step of cleaning the magnesium metal member are performed.
  • a thermoplastic resin is inserted into the magnesium metal member on which the anodized film is formed after the washing step of washing the magnesium metal member having the film formed with water at 5 ° C. or higher and lower than 60 ° C. and the washing step. It is characterized in that a step of molding is provided, and the magnesium metal member and a resin member molded of a thermoplastic resin are joined.
  • Another method for producing a resin magnesium metal joint according to the present invention is a method for producing a resin magnesium metal joint, which is a degreasing step of washing a magnesium metal member with an alkaline solution, and a magnesium metal after the degreasing step.
  • An anodic oxide film having a thickness of 50 to 3000 nm is formed on the magnesium metal member by applying a current density of 0.5 A / dm2 or more and less than 5 A / dm2 in a solution containing a triazinethiol derivative at ⁇ 90 ° C.
  • a step of insert-molding a thermoplastic resin is provided, and the magnesium metal member and a resin member molded of the thermoplastic resin are joined.
  • the resin member and the magnesium metal member can be bonded well, and the bonding strength is 30 MPa or more. Can be done.
  • the airtightness between the resin member and the magnesium metal member can be reduced to 10-9 Pam 3 / s or less by a leak test using a helium leak. Waterproofness can also be ensured.
  • an anodic oxide film having triazine thiol having a thickness of 50 to 3000 nm present inside and outside was formed on the surface of the magnesium metal member in advance, so that the resin member and the magnesium metal The members can be joined well.
  • the bonding strength is 30 MPa or more, and the airtightness between the resin member and the magnesium metal member can be 10-9 Pam 3 / s or less in a leak test using a helium leak.
  • the anodized film is 1 to 60% O, 1 to 90% Mg, 3% or less S, 20% or less Al, 3% or less P, 3% or less Zn, and Cu in% by weight. Since it contains a component composition of 3% or less, Mn of 3% or less, Ni of 3% or less, Si of 20% or less, and F of 3% or less, the resin member and the magnesium metal member can be satisfactorily bonded.
  • a degreasing step of dipping to remove oil on the surface of a magnesium metal member (b) an acid treatment step of washing with an acidic solution, and (c). ) An activation step of immersing in an alkaline solution and applying a constant voltage, (d) an oxide film forming step of forming an anodic oxide film in an alkaline solution using a magnesium metal member as an anode, and (e) anodization.
  • a washing step of washing the magnesium metal member with water and (f) an insert step of insert-molding the thermoplastic resin and joining the magnesium metal member to the magnesium metal member were provided, so that the resin member and the magnesium metal member are good.
  • the bonding strength can be 30 MPa or more, and the airtightness can be 10-9 Pam 3 / s or less in a leak test using helium leak.
  • a degreasing step of dipping to remove the oil on the surface of the magnesium metal member there are (a) a degreasing step of dipping to remove the oil on the surface of the magnesium metal member, and (b) an acid treatment step of washing with an acidic solution.
  • TRI electrolysis step (Referred to as TRI electrolysis step), (e) a water washing step of washing the magnesium metal member with water after forming an anodized film, and (f) an insert step of insert molding a thermoplastic resin and joining it to the magnesium metal member. Since the above is provided, the bonding strength between the resin member and the magnesium metal member can be 30 MPa or more, and the airtightness can be 10-9 Pam 3 / s or less in the leak test using a helium leak.
  • (A) is a front view
  • (B) is a right side view
  • (C) is a perspective view.
  • FIG. 1 is a flowchart showing a method for producing a resin-magnesium metal joint according to the present invention.
  • the degreasing step (s1) is performed by immersing the magnesium metal member 1 in an aqueous solution prepared by adding a cationic surfactant to NAOH, KOH, or NA 2 CO 3 of the alkaline series for 1 to 10 minutes.
  • the temperature of the solution is in the range of room temperature to 70 ° C. As a result, the oil content on the surface of the magnesium metal member 1 is removed.
  • the acid treatment step (s2) involves adding a magnesium metal member 1 to an acidic aqueous solution of 5 to 50% phosphoric acid, 1 to 20% sulfuric acid or nitric acid, 1 to 5% oxalic acid, and 1 to 5% fluoride in weight%. Is performed by immersing for 1 to 10 minutes. The temperature of the solution is in the range of room temperature to 50 ° C. As a result, the surface of the magnesium metal member 1 is cleaned to remove the oxide film and the like.
  • a small amount of a cationic surfactant is added to an aqueous solution of caustic soda (NaOH) 1 to 30% and sodium carbonate (Na 2 CO 3 ) 1 to 20% by weight, and the solution is added.
  • the magnesium metal member 1 is immersed for 1 to 10 minutes, and a constant voltage of 0.2 to 5 V is applied to the anode or cathode.
  • the temperature of the aqueous solution is room temperature to 50 ° C.
  • a pulse or DC voltage is applied to the electrodes.
  • ultrasonic treatment at 50 Hz and 100 to 2000 watts is also performed for 1 to 10 minutes.
  • the oxide film forming step (s4) is referred to as a TRI electrolysis step.
  • the magnesium metal member 1 is connected as an anode.
  • the temperature of the solution is normal temperature to 90 ° C.
  • a voltage of 4 to 40 V may be applied between the anode and the cathode.
  • Magnesium metal member by electrolysis for 1 to 40 minutes.
  • An anodic oxide film 4 of triazinethiol having a thickness of 50 to 3000 nm is formed on the surface of the anodized film 4.
  • the anodic oxide film 4 is 10 to 60% by weight, O is 10 to 90%, Mg is 10 to 90%, and S is 3%.
  • Al is 20% or less
  • P is 3% or less
  • Zn is 3% or less
  • Cu is 3% or less
  • Mn is 3% or less
  • Ni is 3% or less
  • Si 3% or less
  • F is 3% or less. It has a component composition.
  • the water washing step (s5) is a step of washing the magnesium metal member 1 having an anodized film formed on its surface with water having a water temperature of 5 ° C. to 60 ° C.
  • the insert molding step (s6) after the washing step (s5), the magnesium metal member 1 on which the anodic oxide film is formed is loaded into the mold, the thermoplastic resin to be the resin member 2 is injected, and the resin member 2 and magnesium are injected. The metal member 1 is joined to form a resin magnesium metal joint 3.
  • FIG. 1 is a flowchart showing a method for producing a resin-magnesium metal joint according to the present invention.
  • the degreasing step (s1) is performed by immersing the magnesium metal member 1 in an aqueous solution prepared by adding a cationic surfactant to NAOH, KOH, or NA 2 CO 3 of the alkaline series for 1 to 10 minutes.
  • the temperature of the solution is in the range of room temperature to 70 ° C. As a result, the oil content on the surface of the magnesium metal member 1 is removed.
  • the acid treatment step (s2) involves adding a magnesium metal member 1 to an acidic aqueous solution of 5 to 50% phosphoric acid, 1 to 20% sulfuric acid or nitric acid, 1 to 5% oxalic acid, and 1 to 5% fluoride in weight%. Is performed by immersing for 1 to 10 minutes. The temperature of the solution is in the range of room temperature to 50 ° C. As a result, the surface of the magnesium metal member 1 is cleaned to remove the oxide film and the like.
  • a small amount of a cationic surfactant is added to an aqueous solution of caustic soda (NaOH) 1 to 30% and sodium carbonate (Na 2 CO 3 ) 1 to 20% by weight, and the solution is added.
  • the magnesium metal member 1 is immersed for 1 to 10 minutes, and a constant voltage of 0.2 to 5 V is applied to the anode or cathode.
  • the temperature of the aqueous solution is room temperature to 50 ° C.
  • a pulse or DC voltage is applied to the electrodes.
  • ultrasonic treatment at 50 Hz and 100 to 2000 watts is also performed for 1 to 10 minutes.
  • the oxide film forming step (s4) is referred to as a TRI electrolysis step.
  • the magnesium metal member 1 is connected as an anode.
  • the triazine-thiol (triazine thiols) derivatives traces added magnesium metal member 1 into the solution Immersion is performed by applying a constant current density of 1 to 20 A / dm 2 between the anode and the cathode.
  • the temperature of the solution is normal temperature to 90 ° C.
  • a voltage of 4 to 40 V is applied between the anode and the cathode.
  • an anodic oxide film 4 of triazinethiol having a thickness of 50 to 3000 nm is formed on the surface of the magnesium metal member.
  • the anodic oxide film 4 is by weight% and O is 10-60%, Mg 10-90%, S 3% or less, Al 20% or less, P 3% or less, Zn 3% or less, Cu 3% or less, Mn 3% or less, Ni It has a component composition of 3% or less, Si of 3% or less, and F of 3% or less.
  • the washing step (s5) is a step of washing the magnesium metal member 1 having a triazine thiol anodized film formed on its surface with water having a water temperature of 5 ° C. to 60 ° C.
  • the insert molding step (s6) after the washing step (s5), the magnesium metal member 1 on which the anodic oxide film is formed is loaded into the mold, the thermoplastic resin to be the resin member 2 is injected, and the resin member 2 and magnesium are injected. The metal member 1 is joined to form a resin magnesium metal joint 3.
  • triazine thiol is not added to the solution of the TRI electrolysis step.
  • triazine thiol is added to the solution of the TRI electrolysis step.
  • FIG. 2 is a diagram showing the shape of the magnesium metal member 1.
  • A is a front view
  • B is a right side view
  • C is a perspective view.
  • a is a hole having a diameter of 4 mm.
  • f is a plate thickness of 3 mm.
  • the length x width is a plate of 40 mm x 12 mm, and b is 12 mm and e is 40 mm.
  • c is 6 mm and d is 5 mm.
  • FIG. 3 is a table showing the types and components of the magnesium alloy used as the magnesium metal member 1.
  • AZ91 is a magnesium alloy having a high content of aluminum (Al) and improved corrosion resistance.
  • AZ31 is a magnesium alloy with improved extensibility by reducing aluminum (Al) to 3.5%.
  • FIG. 4 is a photograph of a hanging jig 7 to which a plurality of magnesium metal members 1 can be attached.
  • the hanging jig 7 has hooks at two upper positions and can be hung.
  • Ten magnesium metal members 1 can be attached.
  • FIG. 5 is a photograph of the hanging jig 7 suspended in the degreasing tank.
  • the degreasing tank is filled with an aqueous solution of NAOH, KOH, or NA 2 CO 3 plus a cationic surfactant.
  • FIG. 6 is a photograph of the hanging jig 7 suspended in an acid treatment tank.
  • the acid treatment tank is filled with an acidic aqueous solution of 5 to 50% phosphoric acid, 1 to 20% sulfuric acid or nitric acid, 1 to 5% oxalic acid, and 1 to 5% fluoride.
  • FIG. 7 is a photograph of the TRI electrolysis treatment tank. A plurality of electrodes are prepared in the tank.
  • FIG. 8 is a photograph showing the surface roughness of the magnesium metal member 1.
  • (A) is the untreated surface
  • (B) is the surface after degreasing
  • (C) is the surface after acid treatment
  • (D) is the surface after activation
  • (E) is the surface after TRI electrolysis treatment. is there.
  • the surface roughness is shown by the central average roughness Ra along three straight lines (three lines running from left to right), in units of ⁇ m.
  • Ra of the three straight lines was (0.5, 0.6, 0.6).
  • (B) Ra of the three straight lines was (0.7, 0.8, 1.0).
  • In (C) Ra of the three straight lines was (1.6, 0.7.0.8).
  • (D) Ra of the three straight lines was (0.6, 0.6, 0.6).
  • the black fine powder adhering to the surface is removed by the acid treatment.
  • Ra of the three straight lines was (0.3, 0.4, 0.4).
  • FIG. 9 is a photograph showing a cross section of the anodized film. Film thicknesses of 300 nm and 1.5 ⁇ m are formed on the surface of the anodized film 4. The thickness of the coating can be 50 nm to 3000 nm (3.0 ⁇ m).
  • FIG. 10 is a photograph of the test piece (left side) and a photograph of a test piece for a tensile test manufactured by the manufacturing method shown in FIG. 1 (right side).
  • Specimens are indicated by reference numeral 3 (3a). That is, the test body is a test body 3a for a tensile test.
  • the resin-magnesium metal joint 3 is formed by integrally molding a resin member 2 with a magnesium metal member 1 by insert molding.
  • the magnesium metal member 1 is loaded in the mold, and the thermoplastic resin is press-fitted to integrally mold the magnesium metal member 1 and the resin member 2.
  • the thermoplastic resin polybutylene terephthalate (PBT) and polyphenylene sulfide (PPS) can be used.
  • FIG. 11 is a diagram showing the tensile strength of the test piece.
  • (A) is a bar graph, and (B) is a list. It was measured with 8 test pieces of Nos. 1 to 8. Nos. 1 to 4 are manufactured in Example 1, and Nos. 5 to 8 are manufactured in Example 1.
  • the tensile strength of the resin member 2 and the magnesium metal member 1 can be set to 30 MPa or more from each numerical value of the test piece.
  • FIG. 12 is a photograph showing a test body for an airtightness test. Specimens are indicated by reference numeral 3 (3b). That is, the test body is the test body 3b for the airtightness test of the resin magnesium metal joint 3. In the test body 3b for the airtightness test, the magnesium metal member 1 penetrates the disk-shaped resin member 2 and is integrally joined. A test piece 3b for an airtightness test is loaded in a tubular container, helium gas is sprayed on one side on which the magnesium metal member 1 protrudes, and the other side on which the magnesium metal member 1 protrudes is evacuated to release helium gas. Check for leaks. Test bodies 1-1 to 1-4 were produced in Example 1, and test bodies 2-1 to 2-4 were produced in Example 2.
  • FIG. 13 is a table showing the results of the airtightness test. If the amount of vacuum exhaust is increased or decreased, the amount of leaked helium (He) also increases or decreases, but from the numerical values in the table of FIG. 13, the test bodies 1-1 to 1-4 of Example 1 and the test of Example 2 Any of the bodies 2-1 to 2-4 can be 1 ⁇ 10 -9 Pam 3 / s or less.
  • FIG. 14 is a diagram showing the tensile strength of the test piece manufactured in Example 1 before and after the thermal shock test.
  • the temperature was changed between -40 ° C and 80 ° C every 30 minutes, and 150 cycles were repeated.
  • the column of MPa is the value when the joint cross section is 36 mm 2
  • the column of N is the value obtained by multiplying the value of MPa by 36.
  • the tensile strength avg was 41.84 MPa before the thermal shock test, but increased to 50.12 MPa after the thermal shock test.
  • FIG. 15 is a diagram showing the tensile strength of the test piece manufactured in Example 2 before and after the thermal shock test.
  • the temperature was changed between -40 ° C and 80 ° C every 30 minutes, and 150 cycles were repeated.
  • the column of MPa is the value when the joint cross section is 36 mm 2
  • the column of N is the value obtained by multiplying the value of MPa by 36.
  • the tensile strength avg was 45.60 MPa before the thermal shock test, but increased to 51.32 MPa after the thermal shock test.
  • FIG. 16 is a diagram showing the tensile strength of the test piece produced in Example 1 before and after the high temperature and high humidity test.
  • the high temperature and high humidity test was carried out at a temperature of 80 ° C., a humidity of 95%, and a test time of 200 hours.
  • the tensile strength after this test was lower than the tensile strength of the test piece not subjected to the load test.
  • the tensile strength avg was 42.82 MPa before the test, but decreased to 30.39 MPa after the test.
  • FIG. 17 is a diagram showing the tensile strength of the test piece produced in Example 2 before and after the high temperature and high humidity test.
  • the high temperature and high humidity test was carried out at a temperature of 80 ° C., a humidity of 95%, and a test time of 200 hours.
  • the tensile strength after this test was lower than the tensile strength of the test piece not subjected to the load test.
  • the tensile strength avg was 42.82 MPa before the test, but decreased to 30.39 MPa after the test.
  • FIG. 18 is a surface photograph and a component analysis table of the Mg material (AZ91) after the TRI electrolysis treatment.
  • the surface has an uneven shape.
  • magnesium oxide (MgO) is formed because Mg is 32.33% and O is 39.59% in weight%.
  • FIG. 19 is a surface photograph and a component analysis table of the Mg material (AZ31) after the TRI electrolysis treatment.
  • the surface has an uneven shape, and a large number of holes are formed.
  • magnesium oxide (MgO) is formed because Mg is 64.32% and O is 31.98% by weight.
  • the resin-magnesium metal joint of the present invention and the method for manufacturing the same are for integrally joining the metal member and the resin member, and are suitable for reducing the weight of the parts.

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Abstract

Corps lié de résine-métal de magnésium présente une force de liaison exceptionnelle, et procédé de fabrication du corps lié de résine-métal de magnésium. Procédé de fabrication d'un corps lié de résine-métal de magnésium comprenant : une étape de dégraissage consistant à laver un élément en métal de magnésium avec une solution alcaline ; une étape de traitement à l'acide consistant à laver l'élément en métal de magnésium avec une solution acide ; une étape de traitement d'activation consistant à immerger l'élément en métal de magnésium dans une solution alcaline et à appliquer une tension constante à une électrode ; une étape d'application d'une densité de courant prédéfinie dans une solution alcaline à l'aide de l'élément en métal de magnésium en tant qu'électrode positive pour former un film de revêtement d'oxyde d'électrode positive sur l'élément en métal de magnésium ; une étape de lavage à l'eau consistant à laver l'élément en métal de magnésium ayant le film de revêtement d'oxyde d'électrode positive formé sur celui-ci avec de l'eau ; et une étape consistant à former une résine thermoplastique par moulage par insertion sur l'élément en métal de magnésium sur lequel est formé le film de revêtement d'oxyde d'électrode positive.
PCT/JP2019/020368 2019-05-23 2019-05-23 Corps lié de résine-métal de magnésium et son procédé de fabrication WO2020235070A1 (fr)

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KR1020217042145A KR102618505B1 (ko) 2019-05-23 2019-05-23 수지와 마그네슘계 금속의 접합체 및 그 제조 방법
CN201980096719.0A CN114207192A (zh) 2019-05-23 2019-05-23 树脂金属镁接合体及其制造方法
PCT/JP2019/020368 WO2020235070A1 (fr) 2019-05-23 2019-05-23 Corps lié de résine-métal de magnésium et son procédé de fabrication

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