WO2020076810A1 - Substrats thermiques - Google Patents

Substrats thermiques Download PDF

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Publication number
WO2020076810A1
WO2020076810A1 PCT/US2019/055168 US2019055168W WO2020076810A1 WO 2020076810 A1 WO2020076810 A1 WO 2020076810A1 US 2019055168 W US2019055168 W US 2019055168W WO 2020076810 A1 WO2020076810 A1 WO 2020076810A1
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WO
WIPO (PCT)
Prior art keywords
dianhydride
outer layer
layer
polyimide
multilayer film
Prior art date
Application number
PCT/US2019/055168
Other languages
English (en)
Inventor
Christopher Banks BECKS
Rosa Irene Gonzalez
Thomas D. Lantzer
Rajesh TRIPATHI
Original Assignee
Dupont Electronics, Inc.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dupont Electronics, Inc. filed Critical Dupont Electronics, Inc.
Priority to KR1020217013837A priority Critical patent/KR20210068129A/ko
Priority to DE112019005062.1T priority patent/DE112019005062T5/de
Priority to JP2021518889A priority patent/JP2022504391A/ja
Priority to CN201980066443.1A priority patent/CN112840747A/zh
Publication of WO2020076810A1 publication Critical patent/WO2020076810A1/fr

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/0313—Organic insulating material
    • H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
    • H05K1/036—Multilayers with layers of different types
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/027—Thermal properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
    • B32B2264/10—Inorganic particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/0213—Electrical arrangements not otherwise provided for
    • H05K1/0254—High voltage adaptations; Electrical insulation details; Overvoltage or electrostatic discharge protection ; Arrangements for regulating voltages or for using plural voltages
    • H05K1/0256—Electrical insulation details, e.g. around high voltage areas
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/0213—Electrical arrangements not otherwise provided for
    • H05K1/0263—High current adaptations, e.g. printed high current conductors or using auxiliary non-printed means; Fine and coarse circuit patterns on one circuit board
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/0313—Organic insulating material
    • H05K1/032—Organic insulating material consisting of one material
    • H05K1/0346—Organic insulating material consisting of one material containing N
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/03—Use of materials for the substrate
    • H05K1/0313—Organic insulating material
    • H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
    • H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/01—Dielectrics
    • H05K2201/0104—Properties and characteristics in general
    • H05K2201/0129—Thermoplastic polymer, e.g. auto-adhesive layer; Shaping of thermoplastic polymer
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/01—Dielectrics
    • H05K2201/0137—Materials
    • H05K2201/0154—Polyimide
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/01—Dielectrics
    • H05K2201/0183—Dielectric layers
    • H05K2201/0191—Dielectric layers wherein the thickness of the dielectric plays an important role
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
    • H05K2201/0206—Materials
    • H05K2201/0209—Inorganic, non-metallic particles
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/09—Shape and layout
    • H05K2201/09209—Shape and layout details of conductors
    • H05K2201/09654—Shape and layout details of conductors covering at least two types of conductors provided for in H05K2201/09218 - H05K2201/095
    • H05K2201/098—Special shape of the cross-section of conductors, e.g. very thick plated conductors

Definitions

  • the field of this disclosure is thermal substrates.
  • thermal substrates in high power density power electronics packaging are rigid boards on which semiconductor dies can be mounted. In addition to mechanical support, these substrates also provide electrical isolation to the circuit and die, as well as a thermally efficient path for heat dissipation.
  • Power module devices such as those found in automobiles, manipulate different forms of current and voltages to control equipment and require large currents flowing though their substrates and a high degree of electrical isolation.
  • thermal substrates take the form of multilayers that include both conducting and insulating layers of dissimilar materials, such as metals (as conductors) and ceramics or polymers (as insulators) and bonding them together in a way that enables a path for heat flow away from the semiconductor die.
  • DRC direct bond copper
  • Organic-based insulating layers such as epoxies
  • epoxies have also been commercialized in recent years for relatively lower power devices (i.e. , for operating temperatures below 150°C).
  • the temperature of the device is limited by the chemical and mechanical stability of the organic component.
  • organic materials must be loaded with thermally conductive fillers to enable acceptable thermal conductivity and are made as thin films to provide a thermal conductivity comparable to ceramic materials. These thin-film epoxies, however, compromise the electrically insulating properties of the thermal substrate.
  • Polyimide films are used in the manufacture of flexible printed circuit boards due to their good electrical insulating properties, mechanical strength, high temperature stability, and chemical resistance properties. Polyimide films are adhered to thin metal foils to form metal-clad laminates, and find broad usage for die pad bonding of flexible print connection boards, semiconductor devices or packaging materials for chip scale package, chip on flex, chip on lead, lead on chip, multi-chip module, ball grid array (or micro- ball grid array), and/or tape automated bonding, among other applications.
  • U.S. Patent No. 7,285,321 describes a multilayer laminate having a low glass transition temperature (T g ) polyimide layer, a high T g polyimide layer, and a conductive layer.
  • the high T g polyimide layer is a thermoset polyimide and the low T g polyimide layer is a thermoplastic polyimide.
  • U.S. Patent No. 6,379,784 describes an aromatic polyimide laminate composed of an aromatic polyimide composite film, a metal film and a release film.
  • the aromatic polyimide composite film is composed of an aromatic polyimide substrate film and two thermoplastic aromatic polyimide layers.
  • polyimide films can be made thermally conductive through the addition of thermally conductive fillers.
  • European Patent Application No. 0 659 553 A1 describes a method for providing a coextruded multilayer film that can include thermally conductive particles.
  • Inorganic particles of thermally conductive fillers such as BN, AI2O3, AIN, BeO, ZnO and ShN 4 or their mixtures can be added in either or both of high and low T g polyimide layers.
  • Fillers are typically added in the form of a slurry to the cast solution of the polymer. The solvent of the filler based slurry can be same or different from that used to make the polymer cast solution.
  • a thermal substrate includes a multilayer film, a first conductive layer adhered to the first outer layer of the multilayer film and a second conductive layer adhered to the second outer layer of the multilayer film.
  • the multilayer film includes a first outer layer including a first thermoplastic polyimide, a core layer including a polyimide and a second outer layer including a second thermoplastic polyimide.
  • the multilayer film has a total thickness in a range of from 5 to 150 pm, and the first outer layer, the core layer and the second outer layer each include a thermally conductive filler.
  • the first conductive layer and the second conductive layer each have a thickness in a range of from 250 to 3000 pm.
  • a thermal substrate includes a multilayer film, a first conductive layer adhered to the first outer layer of the multilayer film and a second conductive layer adhered to the second outer layer of the multilayer film.
  • the multilayer film includes a first outer layer including a first thermoplastic polyimide, a core layer including a polyimide and a second outer layer including a second thermoplastic polyimide.
  • the multilayer film has a total thickness in a range of from 5 to 150 pm, and the first outer layer, the core layer and the second outer layer each include a thermally conductive filler.
  • the first conductive layer and the second conductive layer each have a thickness in a range of from 250 to 3000 pm.
  • the first outer layer has a thickness in a range of from 1.5 to 20 pm
  • core layer has a thickness in a range of from 5 to 125 pm
  • the second outer layer has a thickness in a range of from 1.5 to 20 pm.
  • a T g of the core layer is higher than both a T g of the first outer layer and a T g of the second outer layer.
  • the thermally conductive filler of the first outer layer is present in an amount of from greater than 0 to 50 wt% based on the weight of the dry first outer layer
  • the thermally conductive filler of the core layer is present in an amount of from greater than 0 to 60 wt% based on the weight of the dry core layer
  • the thermally conductive filler of the second outer layer is present in an amount of from greater than 0 to 50 wt% based on the weight of the dry second outer layer.
  • a weight percentage of thermally conductive filler in the core layer is higher than that of the first outer layer, the second outer layer, or both the first and second outer layers, based on the dry weight of each layer.
  • the thermally conductive filler of each of the first outer layer, the core layer and the second outer layer are individually selected from the group consisting of BN, AI2O3, AIN, SiC, BeO, diamond, ShN 4 and mixtures thereof.
  • the first thermoplastic polyimide includes an aromatic dianhydride selected from the group consisting of 4, 4'-oxydiphthalic dianhydride, pyromellitic dianhydride, 3, 3', 4,4'- biphenyl tetracarboxylic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride and mixtures thereof; and an aromatic diamine selected from the group consisting of 1 ,3-bis(4-aminophenxoxy) benzene, 2,2-bis-(4-[4- aminophenoxy]phenyl) propane and mixtures thereof.
  • aromatic dianhydride selected from the group consisting of 4, 4'-oxydiphthalic dianhydride, pyromellitic dianhydride, 3, 3', 4,4'- biphenyl tetracarboxylic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride and mixtures thereof.
  • the second thermoplastic polyimide includes an aromatic dianhydride selected from the group consisting of 4,4'-oxydiphthalic dianhydride, pyromellitic dianhydride, 3,3',4,4'-biphenyl tetracarboxylic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride and mixtures thereof; and an aromatic diamine selected from the group consisting of 1 ,3-bis(4-aminophenxoxy) benzene, hexamethylene diamine and mixtures thereof
  • thermoplastic polyimide and second thermoplastic polyimide are the same.
  • the polyimide of the core layer includes an aromatic dianhydride selected from the group consisting of 3,3’,4,4’-biphenyl tetracarboxylic dianhydride, 4,4'-oxydiphthalic dianhydride, pyromellitic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride, bisphenol A dianhydride, 1 ,2,5,6-naphthalene tetracarboxylic dianhydride, 1 ,4,5,8-naphthalene tetracarboxylic dianhydride, and 2,3,6,7- naphthalene tetracarboxylic dianhydride and mixtures thereof; and an aromatic diamine selected from the group consisting of p-phenylenediamine, 4,4'-diaminodiphenyl ether, 3,4'-diaminodiphenyl ether, 2,2'-
  • the first thermoplastic polyimide and the second thermoplastic polyimide each have a T g in the range of from 150 to 320°C.
  • a core layer for a multilayer film includes a polyimide synthesized by a poly-condensation reaction, involving the reaction of a first aromatic dianhydride with a first aromatic diamine.
  • the polyimide can include one or more additional aromatic dianhydrides, one or more additional aromatic diamines, or both one or more additional aromatic dianhydrides and one or more additional aromatic diamines.
  • an aromatic dianhydride can be selected from the group consisting of 3,3’,4,4’-biphenyl tetracarboxylic dianhydride, 4,4'- oxydiphthalic dianhydride, pyromellitic dianhydride, 3,3',4,4'-benzophenone tetracarboxylic dianhydride, bisphenol A dianhydride, 1 ,2,5,6-naphthalene tetracarboxylic dianhydride, 1 ,4,5,8-naphthalene tetracarboxylic dianhydride, and 2,3,6,7-naphthalene tetracarboxylic dianhydride.
  • an aromatic diamine can be selected from the group consisting of p- phenylenediamine, 4,4'-diaminodiphenyl ether (ODA), 3,4'-diaminodiphenyl ether, 2,2'-bis(trifluoromethyl) benzidine (TFMB), m-phenylenediamine (MPD) and 4,4'-diaminodiphenylmethane (MDA).
  • the polyimide can include an aliphatic diamine.
  • the core layer can be a thermoset polyimide.
  • the core layer can include a polyimide with some thermoplastic properties.
  • a first outer layer for a multilayer film includes a first thermoplastic polyimide.
  • the first thermoplastic polyimide can be synthesized by a poly-condensation reaction, involving the reaction of an aromatic dianhydride and an aromatic diamine.
  • the first thermoplastic polyimide can include one or more additional aromatic dianhydrides, one or more additional aromatic diamines, or both additional aromatic dianhydrides and additional aromatic diamines.
  • a second outer layer for a multilayer film includes a second thermoplastic polyimide.
  • the second thermoplastic polyimide can be synthesized by a poly-condensation reaction, involving the reaction of an aromatic dianhydride and an aromatic diamine.
  • the second thermoplastic polyimide can include one or more additional aromatic dianhydrides, one or more additional aromatic diamines, or both additional aromatic dianhydrides and additional aromatic diamines.
  • the first outer layer, the second outer layer, or both the first and the second outer layers can include one or more aliphatic diamines, which may be useful to lower the T g of the outer layers, if desired.
  • the first thermoplastic polyimide and the second thermoplastic polyimide can be the same or different.
  • the first thermoplastic polyimide and the second thermoplastic polyimide each have a T g in the range of from about 150 to about 320°C.
  • an“aromatic diamine” is intended to mean a diamine having at least one aromatic ring, either alone (i.e. , a substituted or unsubstituted, functionalized or unfunctionalized benzene or similar-type aromatic ring) or connected to another (aromatic or aliphatic) ring, and such an amine is to be deemed aromatic, regardless of any non-aromatic moieties that might also be a component of the diamine.
  • an aromatic diamine backbone chain segment is intended to mean at least one aromatic moiety between two adjacent imide linkages.
  • an“aliphatic diamine” is intended to mean any organic diamine that does not meet the definition of an aromatic diamine.
  • diamine as used herein is intended to mean: (i) the unreacted form (i.e., a diamine monomer); (ii) a partially reacted form (i.e., the portion or portions of an oligomer or other polyimide precursor derived from or otherwise attributable to diamine monomer) or (iii) a fully reacted form (the portion or portions of the polyimide derived from or otherwise attributable to diamine monomer).
  • the diamine can be
  • diamine is not intended to be limiting (or interpreted literally) as to the number of amine moieties in the diamine component.
  • (ii) and (iii) above include polymeric materials that may have two, one, or zero amine moieties.
  • the diamine may be functionalized with additional amine moieties (in addition to the amine moieties at the ends of the monomer that react with dianhydride to propagate a polymeric chain). Such additional amine moieties could be used to crosslink the polymer or to provide other functionality to the polymer.
  • dianhydride as used herein is intended to mean the component that reacts with (is complimentary to) the diamine and in combination is capable of reacting to form an intermediate polyamic acid (which can then be cured into a polyimide).
  • anhydride as used herein can mean not only an anhydride moiety per se, but also a precursor to an anhydride moiety, such as: (i) a pair of carboxylic acid groups (which can be converted to anhydride by a de-watering or similar- type reaction); or (ii) an acid halide (e.g., chloride) ester functionality (or any other functionality presently known or developed in the future which is) capable of conversion to anhydride functionality.
  • an acid halide e.g., chloride
  • dianhydride can mean: (i) the unreacted form (i.e. a dianhydride monomer, whether the anhydride functionality is in a true anhydride form or a precursor anhydride form, as discussed in the prior above paragraph); (ii) a partially reacted form (i.e., the portion or portions of an oligomer or other partially reacted or precursor polyimide composition reacted from or otherwise attributable to dianhydride monomer) or (iii) a fully reacted form (the portion or portions of the polyimide derived from or otherwise attributable to dianhydride monomer).
  • the dianhydride can be functionalized with one or more moieties, depending upon the particular embodiment selected in the practice of the present invention.
  • the term“dianhydride” is not intended to be limiting (or interpreted literally) as to the number of anhydride moieties in the dianhydride component.
  • (i), (ii) and (iii) include organic substances that may have two, one, or zero anhydride moieties, depending upon whether the anhydride is in a precursor state or a reacted state.
  • the dianhydride component may be
  • additional anhydride type moieties in addition to the anhydride moieties that react with diamine to provide a polyimide.
  • additional anhydride moieties could be used to crosslink the polymer or to provide other functionality to the polymer.
  • the terms“comprises,”“comprising,” “includes,” “including,” “has,” “having” or any other variation thereof, are intended to cover a non- exclusive inclusion.
  • a method, process, article, or apparatus that comprises a list of elements is not necessarily limited only those elements but may include other elements not expressly listed or inherent to such method, process, article, or apparatus.
  • "or” refers to an inclusive or and not to an exclusive or. For example, a condition A or B is satisfied by any one of the following: A is true (or present) and B is false (or not present), A is false (or not present) and B is true (or present), and both A and B are true (or present).
  • Useful organic solvents for the synthesis of the polyimides of the present invention are preferably capable of dissolving the polyimide precursor materials.
  • Such a solvent should also have a relatively low boiling point, such as below 225°C, so the polymer can be dried at moderate (i.e. , more convenient and less costly) temperatures.
  • a boiling point of less than 210, 205, 200, 195, 190, or 180°C is preferred.
  • Solvents of the present invention may be used alone or in combination with other solvents (i.e., co-solvents).
  • Useful organic solvents include: N- methylpyrrolidone (NMP), dimethylacetamide (DMAc), N,N’-dimethyl- formamide (DMF), dimethyl sulfoxide (DMSO), tetramethyl urea (TMU), diethyleneglycol diethyl ether, 1 ,2-dimethoxyethane (monoglyme), diethylene glycol dimethyl ether (diglyme), 1 ,2-bis-(2-methoxyethoxy) ethane (triglyme), bis [2-(2-methoxyethoxy) ethyl)] ether (tetraglyme), gamma-butyrolactone, and bis-(2-methoxyethyl) ether, tetrahydrofuran.
  • preferred solvents include N-methylpyrrolidone (NMP) and dimethylace
  • Co-solvents can generally be used at about 5 to 50 weight percent of the total solvent, and useful such co-solvents include xylene, toluene, benzene, "Cellosolve” (glycol ethyl ether), and "Cellosolve acetate"
  • Aromatic Diamines (hydroxyethyl acetate glycol monoacetate).
  • any number of suitable aromatic diamines can be included in the core layer polyimide, including p-phenylenediamine (PPD), m- phenylenediamine (MPD), 2,5-dimethyl-1 ,4-diaminobenzene, trifluoromethyl- 2,4-diaminobenzene, trifluoromethyl-3,5-diaminobenzene, 2,5-dimethyl-1 ,4- phenylenediamine (DPX), 2,2-bis-(4-aminophenyl) propane, 4,4'- diaminobiphenyl, 4,4'-diaminobenzophenone, 4,4'-diaminodiphenylmethane (MDA), 4,4'-diaminodiphenyl sulfide, 4,4'-diaminodiphenyl sulfone, 3,3'- diaminodiphenyl sulfone, bis-(4-(4-(4-
  • aromatic diamines include 2,2'-bis(trifluoromethyl) benzidine (TFMB), 1 ,2-bis-(4-aminophenoxy)benzene, 1 ,3-bis-(4- aminophenoxy) benzene, 1 ,2-bis-(3-aminophenoxy)benzene, 1 ,3-bis-(3- aminophenoxy) benzene, 1 -(4-aminophenoxy)-3-(3-aminophenoxy) benzene, 1 ,4-bis-(4-aminophenoxy) benzene, 1 ,4-bis-(3-aminophenoxy) benzene, 1 -(4- aminophenoxy)-4-(3-aminophenoxy) benzene, 2,2-bis-(4-[4- aminophenoxy]phenyl) propane (BAPP), 2,2'-bis-(4-aminophenyl)-hexafluoro propane (6F diamine), 2,2'-bis-
  • useful aromatic diamines include the isomers of bis-aminophenoxybenzenes (APB), aminophenoxyphenylpropane (BAPP), dimethylphenylenediamine (DPX), bisaniline P, and combinations thereof, and the use of these particular aromatic diamines can lower the lamination temperature of the polyimide, and can increase the peel strength of the polyimide when adhered to other materials, especially metals.
  • APIB bis-aminophenoxybenzenes
  • BAPP aminophenoxyphenylpropane
  • DPX dimethylphenylenediamine
  • bisaniline P bisaniline P
  • thermoplastic polyimide of the outer layers can include one or more of any of the aromatic diamines listed above for the core layer.
  • any aromatic dianhydride, or combination of aromatic dianhydrides can be used as dianhydride monomers in forming the core layer polyimide.
  • the dianhydrides can be used in their tetra-acid form (or as mono, di, tri, or tetra esters of the tetra acid), or as their diester acid halides (chlorides).
  • the dianhydride form can be preferred, because it is generally more reactive than the acid or the ester.
  • aromatic dianhydrides examples include 3,3',4,4'-biphenyl tetracarboxylic dianhydride (BPDA), 1 ,2,5,6-naphthalene tetracarboxylic dianhydride, 1 ,4,5,8-naphthalene tetracarboxylic dianhydride, 2, 3,6,7- naphthalene tetracarboxylic dianhydride, 2-(3',4'-dicarboxyphenyl) 5,6- dicarboxybenzimidazole dianhydride, 2-(3',4'-dicarboxyphenyl) 5,6- dicarboxybenzoxazole dianhydride, 2-(3',4'-dicarboxyphenyl) 5,6- dicarboxybenzothiazole dianhydride, 2,2',3,3'-benzophenone tetracarboxylic dianhydride, 2,3,3',4'-benzophenone tetracarboxylic
  • thermoplastic polyimide of the outer layers can include one or more of any of the aromatic dianhydrides listed above for the core layer.
  • thermally conductive fillers while being thermally conducting, must also be electrically insulating to preserve the electrically insulating nature of the multilayer film.
  • Example of fillers that are both thermally conducting and electrically insulating include BN, AIN, AI2O3, ShN 4 , ZnO, MgC03, MgO, BeO, diamond, SiC, many other oxide, nitride and carbide compounds and mixtures thereof.
  • a core-shell type filler can include one of these filler materials coated by a coating of a second filler material.
  • These thermally conductive fillers can be of any shape or size and can have an average primary particle size (D50) in a range of from about 0.001 to about 8 pm.
  • Polyimide film layers according to the present invention can be produced by combining the diamine and dianhydride (monomer or other polyimide precursor form) together with a solvent to form a polyamic acid (also called a polyamide acid) solution.
  • the dianhydride and diamine can be combined in a molar ratio of about 0.90 to 1.10.
  • the molecular weight of the polyamic acid formed therefrom can be adjusted by adjusting the molar ratio of the dianhydride and diamine.
  • a polyamic acid casting solution is derived from the polyamic acid solution.
  • the polyamic acid casting solution preferably comprising the polyamic acid solution, can optionally be combined with conversion chemicals like: i.) one or more dehydrating agents, such as, aliphatic acid anhydrides (acetic anhydride, etc.) and/or aromatic acid anhydrides; and ii.) one or more catalysts, such as, aliphatic tertiary amines (triethyl amine, etc.), aromatic tertiary amines (dimethyl aniline, etc.) and heterocyclic tertiary amines (pyridine, picoline, isoquinoline, etc.).
  • dehydrating agents such as, aliphatic acid anhydrides (acetic anhydride, etc.) and/or aromatic acid anhydrides
  • catalysts such as, aliphatic tertiary amines (triethyl amine, etc.), aromatic tertiary amines (d
  • the anhydride dehydrating material it is often used in molar excess compared to the amount of amide acid groups in the polyamic acid.
  • the amount of acetic anhydride used is typically about 2.0 to 4.0 moles per equivalent (repeat unit) of polyamic acid.
  • a comparable amount of tertiary amine catalyst is used.
  • the polyamic acid solution, and/or the polyamic acid casting solution is dissolved in an organic solvent at a concentration from about 5.0 or 10 % to about 15, 20, 25, 30, 35 and 40 % by weight.
  • a thermally conductive filler is dispersed or suspended in a polar, aprotic solvent, such as, DMAC or other solvent compatible with polyamic acid.
  • the thermally conductive filler can be dispersed in an organic solvent at a concentration from about 5, 10 or 15 % to about 20, 30, 40, 50 and 75 % by weight.
  • the solvent used for the dispersion or suspension of the thermally conductive filler is the same or different as the solvent used for the polyamic acid solution. The dispersion or suspension of thermally conductive filler can then be added to the polyamic acid casting solution to achieve the desired filler loading of the final film.
  • the first outer layer can contain thermally conductive filler in an amount of from greater than 0 to about 50 wt% of the dry film.
  • the core layer can contain thermally conductive filler in an amount of from greater than 0 to about 60 wt% of the dry film.
  • the second outer layer can contain thermally conductive filler in an amount of from greater than 0 to about 50 wt% of the dry film.
  • the first outer layer, the core layer and the second outer layer can each have the same or different amount of thermally conductive filler, based on weight percentage of the dry film, as the other layers in the multilayer film.
  • the weight percentage of thermally conductive filler in the core layer can be higher than that of the first outer layer, the second outer layer, or both the first and second outer layers. In another embodiment, the weight percentage of thermally conductive filler in the core layer can be lower than that of the first outer layer, the second outer layer, or both the first and second outer layers.
  • the solvated mixture (the polyamic acid casting solution with thermally conductive filler) can then be cast or applied onto a support, such as an endless belt or rotating drum, to give a film.
  • the solvent containing-film can be converted into a self-supporting film by heating at an appropriate temperature (thermal curing) together with conversion chemical reactants (chemical curing).
  • the film can then be separated from the support, oriented such as by tentering, with continued thermal and chemical curing to provide a polyimide film.
  • Useful methods for producing polyimide film in accordance with the present invention can be found in U.S. Patent Nos. 5,166,308 and 5,298,331 , which are incorporate by reference into this specification for all teachings therein. Numerous variations are also possible, such as,
  • diamine and dianhydride components (contrary to (a) above) (c.) A method wherein diamines are exclusively dissolved in a solvent and then dianhydrides are added thereto at such a ratio as allowing to control the reaction rate.
  • each polyimide layer may be adjusted, depending on the intended purpose of the film or final application specifications.
  • the multilayer film has a total thickness of from about 5 to about 150 pm, or from about 15 to about 100 pm, or from about 25 to about 75 pm.
  • the thickness of the core layer is in a range of from about 5 to about 125 pm , or from about 10 to about 100 pm , or from about 15 to about 75 pm, or from about 15 to about 40 pm.
  • the thickness of the outer layers is in a range of from about 1.5 to about 20 pm for each of the outer layers, or from about 3 to about 15 pm, or from about 3 to about 12 pm, or from about 3 to about 6 pm for each of the outer layers.
  • a minimum thickness of the outer layers with thermoplastic polyimide is needed to provide sufficient adhesion to metal layers to form a useful thermal substrate for power electronics applications.
  • a minimum thickness of the core layer is needed to maintain the mechanical integrity of the multilayer film.
  • the multilayer film As a thermal substrate for high power density semiconductor devices (such as insulated gate bipolar transistors), the multilayer film might experience rapid temperature changes from room temperature to temperature as high as 200°C. Actual drive cycle condition of a power module in an automobile might exert these temperature changes in a fast and repeating pattern requiring quick heat dissipation and high mechanical integrity. Under these conditions, a low T g organic layer, such as an epoxy, is susceptible to adhesion loss and delamination.
  • the core layer and the outer layers of the multilayer film can be simultaneously solution cast by co-extrusion.
  • the polyimides can be in the form of a polyamic acid solution.
  • the cast solutions form an uncured polyamic acid film that is later cured to a polyimide.
  • the adhesion strength of such laminates can be improved by employing various techniques for elevating adhesion strength.
  • a finished polyamic acid solution is filtered and pumped to a slot die, where the flow is divided in such a manner as to form the first outer layer and the second outer layer of a three-layer coextruded film.
  • a second stream of polyimide is filtered, then pumped to a casting die, in such a manner as to form the middle polyimide core layer of a three-layer coextruded film. The flow rates of the solutions can be adjusted to achieve the desired layer thickness.
  • the multilayer film is prepared by
  • the layers are extruded through a single or multi-cavity extrusion die.
  • the multilayer film is produced using a single-cavity die. If a single-cavity die is used, the laminar flow of the streams should be of high enough viscosity to prevent comingling of the streams and to provide even layering. By using a co-extrusion process, a multilayer film with good interlayer adhesion can be made without the use of adhesives layers.
  • the multilayer film can be formed by any conventional technique used in the formation of polyimide films.
  • the outer layers can be applied to the core layer during an intermediate manufacturing stage of making polyimide film such as to gel film or to green film.
  • a lamination process may be used to form a thermal substrate with a multilayer film adhered to first and second conductive layers.
  • a first outer layer of the multilayer film including a first thermoplastic polyimide
  • a second outer layer including a second thermoplastic polyimide
  • a second conductive layer is placed in contact with the second outer layer on a side opposite the core layer.
  • the conductive layer(s) is a metal layer(s).
  • a metal layer is a metal sheet having a thickness in a range of from about 250 to about 3000 pm, or from about 250 to about 2000 pm, or from about 300 to about 1000 pm.
  • the polyimide film prior to the step of applying the multilayer film of the present invention onto a conductive layer, can be subjected to a pre-treatment step.
  • Pre-treatment steps can include, heat treatment, corona treatment, plasma treatment under atmospheric pressure, plasma treatment under reduced pressure, treatment with coupling agents like silanes and titanates, sandblasting, alkali-treatment, acid-treatments, and coating polyamic acids.
  • coupling agents like silanes and titanates
  • sandblasting alkali-treatment
  • acid-treatments and coating polyamic acids.
  • the conductive layer surface may be treated with various organic and inorganic treatments. These treatments include using silanes, imidazoles, triazoles, oxide and reduced oxide treatments, tin oxide treatment, and surface cleaning/roughening (called micro-etching) via acid or alkaline reagents.
  • the term“conductive layers” mean metal layers (compositions having at least 50% of the electrical conductivity of a high- grade copper). Metal layers do not have to be used as elements in pure form; they may also be used as metal alloys, such as copper alloys containing nickel, chromium, iron, and other metals. Particularly suitable metal layers are rolled, annealed copper or rolled, annealed copper alloy. In many cases, it has proved to be advantageous to pre-treat the metallic layer before adhering the multilayer film.
  • This pre- treatment may include, but is not limited to, electro-deposition or immersion- deposition on the metal of a thin layer of copper, zinc, chrome, tin, nickel, cobalt, other metals, and alloys of these metals.
  • the pre-treatment may consist of a chemical treatment or a mechanical roughening treatment.
  • an organic direct bond copper (ODBC) system can include the multilayer film and a first copper layer adhered to an outer surface of the first outer layer of the multilayer film.
  • a ODBC system can include a second copper layer adhered to an outer surface of the second outer layer of the multilayer film.
  • the first copper layer and the second copper layer are the same thickness.
  • the first copper layer and the second copper layer are the same thickness and are in a range of from about 300 pm to about 1000 pm thick.
  • the first copper layer is thicker than the second copper layer.
  • the first copper layer is 500 pm thick and the second copper layer is 2000 pm thick.
  • an outer layer of the first copper layer includes microchannels. These microchannels can provide improved heat dissipation for the thermal substrate.
  • the copper layers can be laminated to the multilayer film using a static press or autoclave, as conventionally used to form metal-clad laminates with polyimide films for flex circuit applications.
  • An ODBC structure using the multilayer film and conductive layers of the present invention maintains good adhesion strength due to the thermoplastic nature of the outer layers of the multilayer film, and thus the effects of CTE mismatch are minimized. This contrasts with ceramic-metal bonding in DBC structures, in which bond rigidity in combination with the CTE difference between the ceramic and metal results in large thermomechanical stresses during power module operation.
  • ODBC thermal substrates using the multilayer film and conductive layers of the present invention can be used for high power density power electronics packaging, operating at temperatures of up to 200°C.
  • the polyimide films of the present invention generally also have a low loss-tangent value. Loss-tangent is typically measured at 10 GHz and is used to measure a dielectric material’s degradation of a nearby digital signal that is passing through a metal circuit trace. Different loss-tangent values exist for different dielectric materials. The lower the loss-tangent value for a given dielectric material, the (increasingly) superior a material is for digital circuitry applications.
  • the polyimides of the present invention exhibit excellent, low loss-tangent values. In one embodiment, the loss-tangent value for the polyimide layers was less than 0.010, about 0.004, at 10 GHz.
  • the polyimides of present invention may also be used in applications ranging from 1 to 100 GHz, with 1 to 20 GHz being most common.
  • the multilayer films of the present invention exhibit excellent
  • the polyimides of the present invention can often exhibit an attenuation value, measured in decibels per inch, of about 0.3 at 10 GHz using a 50-ohm micro strip.
  • a polyimide precursor for a core layer and polyimide precursors for first and second outer layers are cast simultaneously (using a multi-port die) to form a multilayer polyimide film (after curing of the polyamic acid layers).
  • This multilayer film is then bonded to metal layer(s) using the thermoplastic polyimide of the outer layer(s) as the bonding layer to the metal layer(s).
  • a thermal substrate formed comprises the multilayer film and at least one conductive layer.
  • Polyamic acid solutions for producing the core layer and outer layers were separately prepared by a chemical reaction between the appropriate molar equivalents of the monomers in dimethylacetamide (DMAc) solvent.
  • DMAc dimethylacetamide
  • the diamine dissolved in DMAc was stirred under nitrogen, and the dianhydride was added as a solid over a period of several minutes. Stirring was continued to obtain maximum viscosity of the polyamic acid. The viscosity was adjusted by controlling the amount of dianhydride in the polyamic acid composition.
  • thermally conductive filler a 25 wt% dispersion of BN in DMAc was made and then added to the polyamic acid solutions so that the multilayer film would have 50 wt% BN in the core layer and 25 wt% BN in the outer layers of the dried film.
  • Multilayer films were cast by co-extrusion. Three separate polyamic polymer streams were simultaneously extruded through a multi-cavity extrusion die onto a heated moving belt to form a co-extruded three-layer polyimide film. The thicknesses of the polyimide core layer and the top and bottom thermoplastic polyimide outer layers were adjusted by varying the amounts of polyamic acids fed to the extruder.
  • the extruded multilayer film was dried at an oven temperature in the range of from about 95 to about 150°C.
  • the self-supporting film was peeled from the belt and heated with radiant heaters in a tenter oven at a
  • the radiant heating set point temperature used to cure the film was 805°C.
  • the core layer polymer composition contained a polyimide derived from an approximately 1 :1 molar ratio of PMDA to ODA.
  • the thermoplastic outer layers also contained a polyimide derived from an approximately 1 :1 molar ratio of dianhydride to diamine.
  • the dianhydride composition contained the monomers PMDA and ODPA in a 20:80 molar ratio and the diamine composition was 100 mole % RODA monomer.
  • the flow rates of the polyamic acid solutions were adjusted to yield a three-layer film in which the thermoplastic outer layers were approximately 3 pm thick, and the core layer was approximately 19 pm thick.
  • a cross sectional scanning electron microscope (SEM) image of the three-layer film was obtained to determine the thicknesses of the multilayer film and the individual core and outer layers. To obtain this image, a film sample was cut and mounted in an epoxy and allowed to dry overnight.
  • the sample was then polished using a Buehler variable speed grinder/polisher and placed into a desiccator for about two hours to ensure dryness.
  • the image was captured using a Hitachi S-3400 SEM (Hitachi High Technologies America, Inc., Schaumburg, IL) under variable pressure.
  • the total thickness of the multilayer film was approximately 25 pm.
  • the multilayer film was used to prepare a series of ODBC thermal substrates. 1000 pm copper sheet was laminated to both sides of the multilayer film using a vacuum assisted static press at temperatures with a maximum temperature of 330°C. The substrates were evaluated for thermal and reliability performance by conducting inspections periodically during accelerated testing.
  • any change in thermal performance of the package was measured by a transient thermal tester.
  • a diode in a TO-247 package was attached to the top of the substrate under test with thermal grease.
  • the thermal grease also adhered the substrate to a cold plate.
  • a transient power pulse was applied to the package, and the decay of the temperature in the diode was monitored over time. This, coupled with transient 1 D conduction analysis, helps establish the resistance-capacitance network for the package.
  • the resistance measurements were monitored for any changes between a new substrate and a substrate that had completed an accelerated test. Thermal resistance measurements, as shown in Table 1 , demonstrate that the ODBC substrates show good stability in all three of the accelerated tests.

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Laminated Bodies (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

La présente invention concerne un substrat thermique comprenant un film multicouche, une première couche conductrice collée à la première couche externe du film multicouche et une seconde couche conductrice collée à la seconde couche externe du film multicouche. Le film multicouche comprend une première couche externe comprenant un premier polyimide thermoplastique, une couche centrale comprenant un polyimide, et une seconde couche externe comprenant un second polyimide thermoplastique. Le film multicouche a une épaisseur totale comprise entre 5 et 150 µm, et la première couche externe, la couche centrale et la seconde couche externe comprennent chacune une élément de remplissage thermiquement conducteur. La première couche conductrice et la seconde couche conductrice ont chacune une épaisseur comprise entre 250 et 3 000 µm.
PCT/US2019/055168 2018-10-09 2019-10-08 Substrats thermiques WO2020076810A1 (fr)

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