WO2018041007A1 - Matériau macromoléculaire et matériau composite métallique et leur procédé de préparation - Google Patents

Matériau macromoléculaire et matériau composite métallique et leur procédé de préparation Download PDF

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Publication number
WO2018041007A1
WO2018041007A1 PCT/CN2017/098919 CN2017098919W WO2018041007A1 WO 2018041007 A1 WO2018041007 A1 WO 2018041007A1 CN 2017098919 W CN2017098919 W CN 2017098919W WO 2018041007 A1 WO2018041007 A1 WO 2018041007A1
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Prior art keywords
metal
polymer material
porous metal
rubber
composite
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PCT/CN2017/098919
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English (en)
Chinese (zh)
Inventor
韩辉升
丁阳
张红梅
陆婷
施捷
孙强
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南通万德科技有限公司
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Priority to DE112017003833.2T priority Critical patent/DE112017003833B4/de
Publication of WO2018041007A1 publication Critical patent/WO2018041007A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H1/00—Contacts
    • H01H1/02—Contacts characterised by the material thereof
    • H01H1/04—Co-operating contacts of different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2705/00—Use of metals, their alloys or their compounds, for preformed parts, e.g. for inserts

Definitions

  • This invention relates to the field of composite materials, and more particularly to a polymeric material and a metal composite conductive material that can be used to make electrical contacts in conductive plates and buttons.
  • the various rubbers themselves are electrically insulating. To date, all conductive rubbers are not intrinsic. Although conductive plastics are intrinsic, the intrinsic conductive plastics have high production costs, are difficult to produce, and are generally inferior in electrical conductivity and stability to metal conductors, and have not been produced and used in large quantities.
  • the widely used conductive polymer materials are generally composite polymer materials, which are compounded by polymer materials (such as rubber and plastic) and conductive fillers.
  • An antistatic polymer material and a conductive polymer material can be prepared by adding conductive carbon black to the polymer substrate. By adding a metal powder, in particular, a silver powder or a silver-plated powder, to a polymer substrate, a conductive polymer material having better conductivity can be obtained.
  • conductive fibers are added to a polymer material to prepare a conductive polymer material.
  • the conductive fibers used are metallized glass fibers (as described in US Patent No. 4332853 "Conductive plastic with metalized glass fibers retained in partial clumps"), carbon fibers or carbon nanotubes (for example, Chinese Patent Application No. 201210011604.7) Conductive rubber and its preparation method”) and the like. Since the conductive carbon black, the metal powder and the conductive fiber are dispersedly distributed in the conductive rubber, the conductive polymer material prepared from these fillers has a larger volume resistivity and surface resistivity than the common metal conductive material, and the conduction is larger. The ability of current does not appear to be sufficient in some situations.
  • the conductive plastic disclosed in the patent document "A conductive plastic and its processing method and processing device" of the application No. 200510086201.9 comprises 0.1-45 v% of conductive fibers, 55-99 v% of thermoplastics and 0-3 v% of processing aids.
  • the conductive fibers are arranged in a three-dimensional network in the thermoplastic;
  • the plastic fiber is evenly dispersed, the overlap between the fibers is high, and the conductivity is high, so that the shielding performance is improved significantly, the SE value can reach 40-99 dB, and the antistatic and electromagnetic shielding effects are good.
  • the patent document "A Highly Efficient Conductive Material” of the application No. 201110448918.9 discloses an efficient conductive material which can be used as an antenna for satellites, ground radars, directional antennas for broadcasting communication, electromagnetic interference shielding elements for cables, aviation and automobiles,
  • the structure comprises at least one layer of metal fiber non-woven mat which can conduct electricity, heat and electromagnetic at high speed, preferably aluminum fiber non-woven mat; the base body is various plastics, preferably glass fiber reinforced plastic.
  • 201010592410.1 discloses a composite conductive sheet composed of a polymer matrix and a metal foil compounded therein.
  • the metal foil here refers to a nickel foil, a copper foil, an aluminum foil, a stainless steel foil, a gold foil, a silver foil or a woven mesh containing pores
  • the polymer matrix refers to a silicone rubber, a nitrile rubber, an ethylene propylene rubber, a natural rubber, a rubber plastic material. , thermoplastics, thermosets or fiber reinforced plastics.
  • a conductive rubber is prepared by molding a rubber and a metal fiber sintered felt (or a metal nonwoven fabric) by molding or injection, and the metal fiber sintered felt has pores. The pores are at least partially filled with rubber.
  • U.S. Patent 6,475,933, "Highly conductive elastomeric sheet” discloses a highly conductive rubber sheet composed of an electrically conductive mesh and an elastomeric substrate filled with electrically conductive particles, wherein the electrically conductive particles are submicron sized carbonaceous materials.
  • the coefficient of thermal expansion of the polymer material is usually much larger than that of a common metal material, sometimes even as high as ten times or more (for example, the coefficient of thermal expansion of the silicone rubber is approximately It is 15 times that of pure nickel.
  • the polymer material in these composite materials will protrude from the surface of the composite due to the large coefficient of thermal expansion, making the surface contact resistance of the electrical contacts larger, and maybe even The electrical contacts become rendered non-conductive and completely fail.
  • a button containing such an electrical contact if used in a car, may create a safety problem.
  • OBJECT OF THE INVENTION To provide a composite material of a polymer material and a porous metal, and a preparation method thereof, the composite material having a protruding metal material at least on one surface, which is suitable for preparing a conductive function under elevated temperature conditions. Electrical contacts that do not fail.
  • Electrical contacts are a key component of the button and are typically used in conjunction with contact switches on printed circuit boards (PCBs). It must have a low contact resistance. If the contact resistance is too large, the key switch function will be invalid and misjudged.
  • the rubber When used as an electrical contact on a rubber button, the rubber swells and bulges when it is raised from room temperature to 80 °C. Due to the phenomenon of the surface of the electrical contact, the conduction is affected, and the contact resistance is raised from 0.4 ⁇ to more than 2 ⁇ , and is even non-conductive. As shown in Figure 1.
  • the reason for the rubber bulging is due to the large coefficient of thermal expansion of the rubber. For example, the coefficient of thermal expansion of silicone rubber is about 15 times that of metallic nickel.
  • the present invention discloses a composite material and a preparation process thereof: by combining a polymer material containing an extractable substance and a porous metal, the composite method includes thermosetting molding, thermal vulcanization molding, radiation curing molding, thermoplastic molding, and the like. , producing a polymer material containing an extractable substance and porous A molded article of a metal, in particular, a molded article in which a polymer material having an extractable substance and a metal material are simultaneously exposed on at least one surface. The pores in the porous metal in the molded body are partially or completely filled in the composite material during the composite molding, and then the extractables in the molded product are extracted by a solvent, thereby causing the molded body to be in the molded body.
  • the volume shrinkage of the polymer material and the surface of the polymer material in the molded body collapse, thereby producing a composite material of a polymer material and a porous metal in which the porous metal protrudes from at least one surface.
  • the composite material can be a sheet, a bar, a tube or a profile.
  • the porous metal in the present invention refers to a metal material or a metal material having pores and holes, and includes a metal sheet having a plurality of uniformly distributed or randomly distributed pores, a metal mesh, a sintered metal mesh, and a metal plate. Net, metal foam or metal fiber sintered felt, etc., or a multilayer metal structure containing them.
  • the metal mesh and the sintered metal mesh may be a single layer or a plurality of layers, and the metal mesh and the metal mesh are formed into a porous metal by a specific vacuum sintering process.
  • the pores in the porous metal are independent or interconnected, and at least a portion of the pores are exposed on the surface of the porous metal so that the polymer material can penetrate into the pores.
  • the holes may be of a regular cylindrical shape, for example, all holes in the metal mesh may have a diameter of 0.25 mm or may be irregular. The diameter of the cross-sectional area of the hole may be in the range of 1 ⁇ m to 3.0 mm.
  • the porous metal may be a metal mesh having a uniformly distributed pores, a pore diameter of 50 ⁇ m to 1.0 mm, a pore spacing of 25 ⁇ m to 1.0 mm, and a circular shape, a regular polygon or other geometric shape.
  • the material of the porous metal can be varied.
  • the porous metal may be composed of aluminum, iron, cobalt, nickel, copper, zinc, tin, manganese, tungsten, silver, gold or alloys thereof.
  • the alloys include Hastelloy, Monel, Inconel, and the like.
  • Stainless steel, nickel or a nickel alloy is preferred. This is because stainless steel, nickel or nickel alloys have relatively stable chemical properties at room temperature and are inexpensive and readily available.
  • the porous metal is composed of a homogeneous or non-homogeneous metal material; further, the outer surface of the porous metal and the pores thereof may be coated with a metal, and the metal plating may be partially or partially covered with a porous layer.
  • Gold plating or silver plating is preferred.
  • Gold and silver have A relatively good electrical conductivity, as a coating of the outer layer of the metal material, can improve the surface conductivity of the electrical contact, reduce the contact resistance of the electrical contact, and improve the electrical conductivity and service life of the electrical contact.
  • the porous metal is free or contains a metal plating; the metal plating completely or partially covers the surface of the porous metal and the inner surface of the porous metal hole.
  • the outer surface of the porous metal or the inner surface of the pore may be coated with an adhesion promoter, a coupling agent or a primer having an average thickness of not more than 1 ⁇ m to increase the bonding strength between the porous metal and the polymer material.
  • the adhesion promoter, coupling agent or primer to be applied should not be too thick, and the average thickness of the coating should not exceed 1 ⁇ m, otherwise the contact resistance of the porous metal may be significantly increased, thereby affecting the electrical conductivity of the electrical contact.
  • the porous metal may be various, and the selection range of the polymer material in the present invention is also broad, and the composite material of the polymer material and the metal and the preparation process thereof are characterized in that the polymer material is: It is a thermosetting rubber, thermoplastic rubber, thermoplastic, thermosetting plastic, radiation curable material, adhesive, ink or coating.
  • thermosetting rubber liquid or solid diene rubber, olefin liquid rubber, polyurethane rubber, acrylate rubber, polysulfide rubber, silicone rubber, fluororubber, fluorosilicone rubber, etc. can be used and porous metal.
  • a conductive composite is prepared.
  • liquid rubber is that the viscosity of the liquid rubber is lower than that of the solid rubber, which facilitates the compounding of the rubber and the porous metal by various methods. But this is not to say that solid rubber is not available.
  • the solid raw rubber and the porous metal can be combined together, for example, the solid raw rubber and the porous metal (such as a metal mesh) are stacked together, and then placed in a mold cavity and pressed by a flat vulcanizer. The solid rubber is infiltrated into the pores of the porous metal, and the solid rubber and the porous metal are combined and vulcanized at a high temperature.
  • the formulation of the polymer material may contain various additives such as pigments, fillers or conductive fillers.
  • the present invention differs from the formulation of a general polymer material in that an extractable substance must be added to the formulation of the polymer material.
  • the purpose of adding an extractable material to a polymer material formulation is not to allow the extractable material to remain in the polymer material after molding the polymer material, but to pass the polymer material after molding.
  • the extraction method drives the extractable material out of the polymer material to shrink the polymer matrix in the composite material of the polymer material and the porous metal, so that the polymer matrix in the pore of the porous metal in the composite material occurs. Collapse.
  • the content of the extractable material in the polymer material is from 1 to 95% by weight before being compounded with the porous metal.
  • These extractables are low molecular weight, oligomeric or uncrosslinked polymers that are compatible or partially compatible with the polymeric material.
  • the polymer material and the extractable material contained therein need to be compatible or partially compatible, so that when the extractable material is extracted from the polymer material, the volume of the polymer material shrinks instead of Holes are formed in the polymer material so that no or substantially no shrinkage occurs.
  • liquid silicone rubber or solid silicone rubber is used to prepare a composite material of a polymer material and a metal
  • various silicone oils liquid paraffin waxes, paraffin wax, chlorinated paraffin, naphthalene, tetralin, decalin, tetramethylbenzene
  • a substance such as tetramethylbenzene, hexamethylbenzene or a high-boiling solvent oil is added as an extractable substance to a liquid silicone rubber or a solid silicone rubber, and after the silicone rubber and the metal are composite-molded, some or all of these extractables are extracted.
  • the preparation method of the composite material in the present invention is also various. Can be superimposed by means of lamination, pad printing, silk screen printing, brush coating, roller brushing, blade coating, spray coating, dip coating, shower coating, and draw coating.
  • the molecular material and the porous metal are combined together, and then solidified by a thermoplastic molding process, a thermosetting molding process or a radiation curing process to obtain a composite material containing an extractable polymer material and a porous metal, and then impregnated with a volatile solvent.
  • the molding process depends on the type of polymer material.
  • the composite material can be die cut into small discs having a diameter of 1.0 to 10.0 or other geometrical pieces after pumping or extraction.
  • the composite material described in the present invention is punched into a small wafer having a diameter of 1.0 to 10.0 mm, which has good electrical conductivity and a contact resistance of less than 1 ⁇ , and can be used as an electrical contact in a rubber button.
  • the surface of the electrical contact prepared by using the composite material shrinks and collapses after the extraction of the polymer material, and the material of the porous metal protrudes from the surface of the composite material, so that the electrical contact has good dust resistance and resistance. Oil stain performance and good electrical conductivity when temperature rises.
  • the thermal expansion coefficient of polymer materials is usually larger than that of metal materials
  • the shrinkage and collapse of polymer materials in composite materials can offset the thermal expansion of polymer materials due to the large thermal expansion coefficient of polymer materials, preventing polymer materials from protruding in composites.
  • the surface of the material affects the electrical conductivity of the contacts.
  • Figure 1 is a schematic view showing the surface of a composite material prepared from a rubber and a metal mesh when the temperature is raised in the present invention; wherein, 1-rubber, 2-metal mesh;
  • FIG. 2 is a schematic view showing the shrinkage of rubber in a porous metal hole in the present invention; wherein, 3-nickel mesh, 4-rubber;
  • Figure 3 is a schematic view showing the shrinkage of the rubber in the porous metal hole in the present invention; wherein, 5-nickel mesh, 6-rubber;
  • Formulation A a mixture of methyl vinyl silicone rubber containing fumed silica (SE 4705U from Dow Corning) 100 (parts by weight, the same below), dimethyl silicone oil (selected Dow Corning's Xiameter PMX-200) , 1000cs) 50, vinyl tri-tert-butylperoxysilane (VTPS) 1, dicumyl peroxide (DCP) 0.5.
  • SE 4705U fumed silica
  • DCP dicumyl peroxide
  • Formulation B SE 4705U 100, VTPS 1, DCP 0.5.
  • the mixed film of Formulation A and Formula B was laminated with a nickel mesh (nickel purity of not less than 99.5%) having a thickness of 0.25 mm, a pore diameter of 0.5 mm, and a hole pitch of 0.25 mm, and placed on a Teflon coating.
  • the mold cavity of the layer was vulcanized and molded at a temperature of 175 ° C for 10 minutes to form a sheet having a thickness of 0.25 mm.
  • the sheet was die cut into small discs having a diameter of 3.0 mm.
  • the small discs prepared from Formulation A and Formulation B were separately extracted with ethanol as a solvent for 3 hours using a Soxhlet extractor. It is then dried at 60 ° C to a substantially constant weight.
  • the small wafer obtained by Formulation B is used as an electrical contact.
  • the contact resistance between the electrical contact and the PCB electrical contact with it is increased from no more than 0.5 ⁇ to more than 2 ⁇ . Not even conductive.
  • the surface of the small disc obtained by using the formula A due to the extraction of the silicone oil, causes the rubber in the metal hole to shrink and collapse (as shown in Fig. 2).
  • the small disc has good dust resistance and oil resistance, and can overcome the disadvantage that the thermal expansion coefficient of the silicone rubber is large and the resistance becomes large or non-conductive at high temperature. Warm The scope of application. At elevated temperatures, the contact resistance is still below 0.5.
  • One side of the nickel mesh in the first embodiment was attached with a 0.025 mm thick polyimide (PI) self-adhesive film, and then a compound of the formula A and a nickel mesh were combined to form a 0.8 mm thick composite sheet. material.
  • the PI was removed from the mucosa and punched into small discs having a diameter of 2.0-5.0 mm. Soaking with solvent gasoline, the silicone oil contained in the small round silicone rubber is extracted, and the rubber in the nickel mesh cavity shrinks (Fig. 3).
  • These small wafers act as electrical contacts and also have good electrical conductivity when the ambient temperature rises. This is because, when the temperature is raised, such as from 25 ° C to 80 ° C, the rubber in the porous metal hole does not protrude from the surface of the porous metal even if it has a lower expansion coefficient (as shown in FIG. 4 ).
  • the addition of polyvinyl butyral is to improve the adhesion of PVC to metals.
  • the materials are put into a high-speed mixer for mixing and mixing, the time is controlled at about 15 minutes, the temperature reaches 110-120 ° C, and the PVC powder absorbs the plasticizer without being sticky, and is placed in a low-speed cooling mixer while stirring. Cooling; when cooled to about 25 ° C, the material is discharged.
  • the material is applied to a multi-layer stainless steel sintering net made by a 5-layer 80-mesh AISI 304 stainless steel wire plain weave through special lamination pressing and vacuum sintering, or by a two-roll mill at 160 ° C.
  • a 1.5 mm thick sheet was placed on a multi-layer stainless steel sintered wire, placed in a Teflon-coated mold cavity at 175 ° C, and hot-pressed and formed on a flat vulcanizing machine to make a 1.5 mm thick sheet. .
  • the sheet or the small circular piece having a diameter of 2.5-10 mm which is die-cut from the sheet is extracted by a solvent gasoline soaking method of 120 or by a Soxhlet extractor for 5-120 minutes, wherein Part of low molecular weight such as trioctyl trimellitate and epoxidized soybean oil or Almost all drawn up.
  • the extraction time and other parameters can be determined according to the degree of collapse of the resin in the multi-layer stainless steel sintered mesh.
  • the composite material of the polyvinyl chloride-stainless steel sintered mesh obtained by this method the polyvinyl chloride shrinks to the inside of the material, and the stainless steel material protrudes from the surface.
  • This composite material can be used as a conductive material, a shielding material, or as an electrical contact having good high-temperature electrical conductivity.
  • the preparation of a composite material of a polymer material and a porous metal by extraction is advantageous for environmental protection because the extracted plasticizer can be recycled without being discharged to the environment.
  • This embodiment prepares a composite of a polymer material and a porous metal as in Example 1, wherein the polymer material is based on Formulation A in Example 1, and the porous material used is the surface and hole inner surface plating in Example 3.
  • a gold plating having an average thickness of 0.05-0.75 ⁇ m and a purity greater than 99.0%. Gold plating reduces the surface contact resistance of the composite and keeps the contact resistance at 0.3 ⁇ .
  • the preparation method was the same as in Example 1, and a small wafer having a diameter of 2 to 10 mm was obtained. After the small wafer was subjected to an extraction process, 0.1 ⁇ m of gold was plated by electroless plating. Compared with the embodiment 4, the composite material or the electrical contact obtained in the embodiment consumes less gold, and the surface contact resistance of the composite material or the electrical contact is substantially the same as that of the embodiment 1. The surface contact resistance of the composite or electrical contacts is the same or similar.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention concerne un matériau macromoléculaire et un matériau composite métallique et leur procédé de préparation : dans certaines conditions, la réalisation d'un moulage composite d'un métal poreux et d'un matériau macromoléculaire contenant de la matière extractible, la préparation d'un matériau en feuille, puis la réalisation d'une extraction par solvant sur le matériau en feuille obtenu de sorte que la matière extractible en son sein soit extraite, et ainsi la préparation d'un matériau composite ayant un matériau macromoléculaire rétracté ou plié. Dans un matériau composite préparé à l'aide dudit procédé, le métal poreux fait saillie à partir de la surface du matériau composite électroconducteur, de telle sorte que le matériau composite est approprié pour une utilisation en tant que matériau de contact électrique.
PCT/CN2017/098919 2016-08-30 2017-08-24 Matériau macromoléculaire et matériau composite métallique et leur procédé de préparation WO2018041007A1 (fr)

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DE112017003833.2T DE112017003833B4 (de) 2016-08-30 2017-08-24 Verbundwerkstoff aus einem hochmolekularen Material und einem Metall und Verfahren zu dessen Herstellung

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CN201610780383.8 2016-08-30

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Publication number Priority date Publication date Assignee Title
EP3540009A1 (fr) * 2018-03-15 2019-09-18 Shark Solutions ApS Modification de polymères de construction recyclés et/ou vierges, à l'aide de poly vinyl butyral (pvb) ou de pvb recyclé à partir de flux de déchets industriels et copolymère d'alliage
WO2019174700A1 (fr) * 2018-03-15 2019-09-19 Shark Solutions Aps Modification de polymères de construction vierges et/ou recyclés en utilisant du polybutyral de vinyle (pvb) ou du pvb recyclé à partir de flux de déchets industriels et un copolymère d'alliage
US11453769B2 (en) 2018-03-15 2022-09-27 Shark Solutions Aps Modification of virgin and/or recycled construction polymers, using poly vinyl butyral (PVB), or recycled PVB from industrial waste streams and an alloying copolymer

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DE112017003833B4 (de) 2024-03-21

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