WO2014065910A1 - Composites de polymère thermoconducteurs contenant du silicate de magnésium et du nitrure de bore - Google Patents

Composites de polymère thermoconducteurs contenant du silicate de magnésium et du nitrure de bore Download PDF

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Publication number
WO2014065910A1
WO2014065910A1 PCT/US2013/050765 US2013050765W WO2014065910A1 WO 2014065910 A1 WO2014065910 A1 WO 2014065910A1 US 2013050765 W US2013050765 W US 2013050765W WO 2014065910 A1 WO2014065910 A1 WO 2014065910A1
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WO
WIPO (PCT)
Prior art keywords
boron nitride
thermally conductive
magnesium silicate
polymer
composite
Prior art date
Application number
PCT/US2013/050765
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English (en)
Inventor
Manjunatha Hosahallli RAMACHANDRAIAH
Srinivasan Duraiswamy
Chitradurga L. Rao ARAVINDA
Sreejith Valiavalappil
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Laird Technologies, 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 Laird Technologies, Inc. filed Critical Laird Technologies, Inc.
Publication of WO2014065910A1 publication Critical patent/WO2014065910A1/fr
Priority to US14/695,361 priority Critical patent/US20150225636A1/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/346—Clay
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives

Definitions

  • the invention in some aspects, relates to thermally conductive plastics, particularly those containing boron nitride, magnesium silicate, and their derivatives.
  • Thermally conductive plastics are polymers with thermally conductive and, frequently, electrically insulating materials used as fillers to achieve desired properties.
  • the final thermoplastic product may provide a means for thermal conductivity while remaining electrically insulating with high dielectric strength.
  • a polymer composite that includes at least one plastic resin, magnesium silicate, and a form of boron nitride, where composite may be injection moldable.
  • the polymer composite comprises at least 2% boron nitride by mass, and about 1% magnesium silicate by volume. In another embodiment, the composite comprises at least 5% boron nitride by volume, and about 2% magnesium silicate by volume.
  • the polymer composite may exhibit a thermal conductivity of above 2 W/m-K and, in specific cases, may be as high as 18 W/m-K and above.
  • the dielectric strength of composites may be above 4 kV/mm, and in specific cases may be as high as 28 KV/mm and above.
  • TCPs may be used in a variety of applications, including in the thermal management of electronic devices and gadgets through, for example, injection molding or thermosetting. Such materials may serve as substitutes for a metal or ceramic article, but where other properties are desired, such as lower density, higher strength and stiffness.
  • TCPs being injection moldable offers flexibility in design, reduces secondary operations, and increases yield.
  • Articles manufactured via conventional injection molding techniques may include, but are not limited to, light emitting diode (LED) heat sinks, electronic housings, mobile phone battery covers, wireless base stations, and other similar applications.
  • LED light emitting diode
  • Magnesium silicate and its derivatives may be used as a component in thermoplastics, including as filler in automotive applications to improve flame retardance.
  • Boron nitride may be used as filler in polymer composites to increase the thermal conductivity.
  • One form of boron nitride used in conventional thermoplastics is hexagonal boron nitride (h-BN).
  • the thermal conductivity of h-BN is directional dependent due to its hexagonal crystal structure.
  • the average thermal conductivity of h-BN can vary between 250 and 300 W/m-K based on processing parameters.
  • h-BN provides a particularly desirable synergistic effect when included in a polymer composite along with certain ratios of magnesium silicate (3MgO, 4Si02, H20).
  • MgO, 4Si02, H20 magnesium silicate
  • these results are both surprising and novel in that the polymer composites exhibit properties that would not be predictable in light of the properties of a polymer composite with only one of either boron nitride or magnesium silicate.
  • the combination of the two materials in the disclosed ratios results in a polymer composite with enhanced injection moldability, which has been a problem when injection molding a polymer composite with only one of either boron nitride or magnesium silicate.
  • h-BN Several types of h-BN are commercially available which are broadly classified as platelet h-BN, agglomerated h-BN or spherical h-BN with various sizes ranging from few microns to several hundreds of microns.
  • Platelet h-BN has plate-like structures of h-BN crystals.
  • Agglomerated h-BN may be a collection of h-BN crystals that are bonded together to form an individually identifiable particle, distinct from non-agglomerated particles such as platelets or crystalline domains.
  • Spherical h-BN is also made out of a collection of h-BN crystals in a compressed spherical shape.
  • h-BN has both advantages and disadvantages during the processing of the polymer composites.
  • Agglomerated h-BN has an advantage over others in that it is easy to feed through a conventional hopper in a twin screw extruder.
  • the final composites disclosed herein frequently have h-BN crystals in the platelet form due to high shear rate in processing.
  • Magnesium silicate commonly known as talc (hydrated silicate of magnesium - 3MgO, 4Si02, H20), is commonly used as a thermally insulating material.
  • talc hydrated silicate of magnesium - 3MgO, 4Si02, H20
  • thermal conductivity of about 4 to 6 W/m-K. This value is 10 to 20 times higher than that of some polymers in which the thermal conductivity is limited to 0.2 to 0.4 W/m-K.
  • Talc may be classified into different forms and shapes. As used herein, much of the talc used is in the form of 3MgO, 4Si02, H20. Like h-BN, talc has platelet structure. However, talc platelets have different aspect ratios which can be varied. In h-BN, the aspect ratio is limited due to the hexagonal shape of the platelets. High aspect ratio fillers used in polymer composites can improve the mechanical and thermal properties.
  • One embodiment is an injection moldable composition
  • the plastic resin may be any suitable polymer, such as polyamide 6, polycarbonate, polyphenylene sulfide and liquid crystalline polymers.
  • the term "liquid-crystal polymer” used in various embodiments of the present technology is intended to mean a melt-processable polymer having such properties that the polymer molecular chains are regularly arranged parallel to each other in a molten state.
  • Liquid-crystal polymers (LCPs) are a class of materials that combine properties of polymers with properties of liquid crystals.
  • the particle sizes of the agglomerated boron nitride may range from about 25 ⁇ ⁇ ⁇ to about 250 ⁇ , and are preferably between about 100 ⁇ to about 150 ⁇ .
  • the magnesium silicate (3MgO, 4Si02, H20) has an aspect ratio around 1 referred to as general purpose talc (herein after GP talc).
  • the magnesium silicate (3MgO, 4Si02, H20) is above 2 and referred to as aspect ratio talc (herein after AR talc).
  • aspect ratio refers to the ratio between an object's width to height.
  • thermoplastics include, but are not limited to polyamide-6,6, blends of polycarbonate & acrylonitrile butadiene styrene (PC- ABS), polyether imide, polyether ether ketone, polyether sulfone, polysulfone, polypropylene, and polybutylene terephthalate (PBT).
  • PC- ABS polyamide-6,6, blends of polycarbonate & acrylonitrile butadiene styrene
  • PBT polybutylene terephthalate
  • thermoplastic elastomers are among the thermoplastics embraced by this invention, non-limiting examples of which include polyester- based thermoplastic elastomers, and olefin-based thermoplastic elastomers. Blends of any of the aforementioned thermoplastics or thermoplastic elastomers are embraced by the scope of this disclosure.
  • the magnesium silicate and boron nitride provides a synergistic effect that imparts highly desirable qualities to the polymer compositions.
  • the disclosed fillers enable the polymer to crystallize at an improved level, wherein the thermally conductive fillers achieve optimal spacing from the polymer spherulites. This spacing enables very high thermal conductivity as compared to polymer composites with hexagonal boron nitride or agglomerated boron nitride in the absence of talc. Additionally, this spacing enhances the polymer composite's dielectric properties.
  • one embodiment of the present invention is a composition
  • a composition comprising a polymer that includes magnesium silicate in a total volume fraction of at least 2% and boron nitride in a total volume fraction in an effective amount so as to create a synergistic effect between the boron nitride and the magnesium silicate.
  • a composition comprises a polymer that includes magnesium silicate in a total volume fraction of at least 2% and boron nitride in a total volume fraction of at least 1%. Additional fillers may be added to the thermally conductive composition, including those that are thermally conductive.
  • a composite includes a ratio of polymer, boron nitride, and magnesium silicate sufficient to generate a synergistic effect whereby the composite is thermally conductive.
  • the composite is additionally dielectric and injection moldable.
  • Example 1 LCP based thermally conductive composites
  • Case la A thermally conductive composite was prepared by melt mixing based on the formulation given in Table 1 a.
  • composition A comprises 60 V% agglomerated h-BN in 40 V% liquid crystalline polymer (LCP).
  • LCP liquid crystalline polymer
  • the resultant melt mixed composite, at 290 degrees Celsius, may not be suitable for injection molding. However, the composite is suitable for compression molding, providing a thermal conductivity of about 16 W/m-K.
  • Case lb A thermally conductive composite was prepared by melt mixing based on the formulation given in Table lb.
  • composition B comprises 60 V% GP talc in 40 V% liquid crystalline polymer (LCP).
  • LCP liquid crystalline polymer
  • the resultant melt mixed composite, at 290 degrees Celsius, may not be suitable for injection molding. However, it is suitable for compression molding.
  • the resultant sample shows a thermal conductivity of about 2 W/m-K.
  • Case lc A thermally conductive composite was prepared by melt mixing based on the formulation given in Table lc.
  • composition C comprises 45 V% of agglomerated h-BN and 15 V% of GP talc in 40 V% liquid crystalline polymer (LCP).
  • LCP liquid crystalline polymer
  • the resultant melt mixed composite at 290 degrees Celsius was found to be suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 18 W/m-K.
  • composition A comprising Agglomerated BN but no talc
  • Composition B comprising talc but no Agglomerated h-BN
  • After compression molding, samples show a thermal conductivity of only 2 W/m-K. This is because talc is a less thermally conductive material (5 W/m-K) compared to boron nitride (-300 W/m- K), when measured through the plane of a hexagonal boron nitride crystal.
  • Composition C comprising 45 V% of the agglomerated h-BN with 15 V% of the GP talc, is injection moldable and the resultant samples show an enhanced thermal conductivity of about 18 W/m-K.
  • Replacing the 15 V% of highly thermally conductive BN with the poor thermally conductive talc makes the composite injection moldable, and provides a marginal enhancement in the thermal conductivity, when compared to Composition A.
  • Example 2 Polyamide based thermally conductive composites
  • Case 2a A thermally conductive composite was prepared by melt mixing based on the formulation given in Table 2a.
  • composition D comprises 15 V% agglomerated h-BN in 85 V% polyamide 6.
  • the resultant melt mixed composite at 270 degrees Celsius is suitable for injection molding.
  • the resultant samples show a thermal conductivity of about 4.7 W/m-K.
  • Case 2b A thermally conductive composite was prepared by melt mixing based on the formulation given in Table 2b.
  • composition E comprises 15 V% agglomerated h-BN and 23 V% of GP talc in 62 V% polyamide 6.
  • the resultant melt mixed composite at 270 degrees Celsius is suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 8 W/m-K.
  • Example 2 In the two formulations seen in Example 2, the agglomerated h-BN volume percentage was kept constant as 15. However, adding 23 V% of GP talc along with 15 V% of agglomerated h-BN enhances the thermal conductivity of the resultant injection moldable material, that being Composition E, by about 70% compared to that of agglomerated h-BN only Composition D.
  • Example 3 PC-ABS based thermally conductive composite
  • thermally conductive composite was prepred by melt mixing based on the formulation given in Table 3, where PC-ABS is Polycarbonate / Acrylonitrile Butadiene Styrene.
  • composition F comprises 15 V% agglomerated h-BN and 23 V% of GP talc in 62 V% PC-ABS.
  • the resultant melt mixed composite at 270 degrees Celsius is suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 8 W/m-K.
  • Example 4 Polyphenylene sulfide based thermally conductive composite
  • a thermally conductive composite was prepared by melt mixing based formulation given in Table 4.
  • composition G comprises 15 V% agglomerated h-BN and 23 V% of GP talc in 62 V% Polyphenylene sulfide.
  • the resultant melt mixed composite at 290 degrees Celsius is suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 8 W/m-K.
  • Composition G maintains the same ratio of base polymer to agglomerated h/BN to talc as that of Composition F and Composition E, but is distinguished from those other compositions in that polyamide 6 was replaced with high heat polypheneylene sulfide. As can be seen in Table 4, this substitution did not affect the thermal conductivity and injection moldability. This infers that observed synergetic effect between talc and BN is not only independent of polymer, but is suitable for all high heat polymer matrices and their blends.
  • a thermally conductive composite was prepared by melt mixing based formulation given in Table 5.
  • composition H comprises 15 V% platelet h-BN and 23 V% of GP talc in 62 V% polyamide 6.
  • the resultant melt mixed composite at 270 degrees Celsius is suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 8 W/m-K.
  • Composition H maintains the same ratio of elements as that of Composition E of Example 2, except that the type of h-BN is changed. Replacing the agglomerated h-BN with non-agglomerated platelet h-BN in the same volume percentage did not affect the thermal conductivity and injection moldability. This infers that observed synergetic effect between talc and BN is independent of h-BN types. It is suitable for all types of h- BN and their combinations.
  • a thermally conductive composite was prepared by melt mixing based on the formulation given in Table 6.
  • composition I comprises 15 V% platelet h-BN and 23 V% of AR talc in 62 V% polyamide 6.
  • the resultant melt mixed composite at 270 degrees Celsius is suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 8 W/m-K.
  • Composition I the ratio of the elements is kept the same as that of Composition E of Example 2, but the type of the talc in the composition is changed.
  • Replacing the GP talc with high aspect ratio AR talc in the same volume percentage did not affect the thermal conductivity and injection moldability. This infers that observed synergetic effect between talc and BN is independent of talc types. It is suitable for all types of talc and their combinations. Further, the AR talc enhances the mechanical properties due to their high aspect ratio.
  • Example 7 Polycarbonate based thermally conductive composites with low filler loadings
  • a thermally conductive composite was prepared by melt mixing based on the formulation given in Table 7.
  • composition J comprises 5 V% of agglomerated h-BN and 2 V% of AR talc in 93 V% polycarbonate.
  • the resultant melt mixed composite at 280 degrees Celsius is suitable for injection molding.
  • the injection molded samples show a thermal conductivity of about 4 W/m-K.
  • thermally conductive composite was prepared by melt mixing based on the formulation given in Table 8.
  • compositions maintain high dielectric strength, as can be seen by the examples shown in Table 9 below.
  • compositions A and B provided highly effective dielectric strength results.
  • theoretically calculated dielectric strength of compositions A and B are in the range of 12 to 15 KV/mm.
  • An added advantage of some of the embodiments described above is the flexibility with respect to the color of the molded thermoplastic article.
  • Many of the compositions disclosed herein are white in color, and various known colorants may be added to the thermoplastic composite with no loss of thermal or dielectric performance.
  • Articles manufactured via conventional injection molding techniques may include, but are not limited to, light emitting diode (LED) heat sinks, electronic housings, mobile phone battery covers, wireless base stations, and other similar applications.
  • Composites manufactured in accordance with the teachings herein meet most industry standard requirements for electronic applications, and additionally possess a low coefficient of thermal expansion.
  • Articles manufactured from the thermally conductive dielectric composites of the present disclosure may be formed using manufacturing processes such as extrusion, injection molding, and compression molding, though it is preferred that the present composites be formed through injection molding.
  • injection molding allows the present composites to be formed into many different shapes and sizes using available equipment and systems.
  • These fabrication processes may also be performed in a continuous fashion (e.g., using a twin-screw extruder) providing benefits with respect to production time and cost- effectiveness.
  • the words "preferred” and “preferably” refer to embodiments of the technology that afford certain benefits, under certain circumstances. But other embodiments may also be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, and is not intended to exclude other embodiments from the scope of the technology.
  • compositional percentages are by weight of the total composition, unless otherwise specified.
  • the word “comprise”, “include,” and variants thereof are intended to be non-limiting, such that recitation of items in a list is not to the exclusion of other like items that may also be useful in the materials, compositions, devices, and methods of this technology.
  • the terms “can” and “may” and their variants are intended to be non-limiting, such that recitation that an embodiment can or may comprise certain elements or features does not exclude other embodiments of the present technology that do not contain those elements or features.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Injection Moulding Of Plastics Or The Like (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne et revendique une composition de polymère, la composition comprenant un polymère, du nitrure de bore et du silicate de magnésium, la composition présentant une certaine conductivité thermique et des propriétés diélectriques. En outre, la composition peut être moulable par injection.
PCT/US2013/050765 2012-10-26 2013-07-16 Composites de polymère thermoconducteurs contenant du silicate de magnésium et du nitrure de bore WO2014065910A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150184055A1 (en) * 2012-09-19 2015-07-02 Momentive Performance Materials Inc. Thermally conductive plastic compositions, extrusion apparatus and methods for making thermally conductive plastics
WO2016106410A1 (fr) * 2014-12-24 2016-06-30 Momentive Performance Materials Inc. Compositions plastiques thermoconductrices, appareil d'extrusion et procédés de fabrication de plastiques thermonconducteurs
US9685598B2 (en) 2014-11-05 2017-06-20 Novation Iq Llc Thermoelectric device

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US5844036A (en) * 1995-06-09 1998-12-01 Hoechst Celanese Corp. Highly filled injection moldable polyetherketones
WO2001021393A1 (fr) * 1999-09-21 2001-03-29 Saint-Gobain Ceramics And Plastics, Inc. Materiaux thermoconducteur d'un compose hydrophobe devant etre soumis a une gestion thermique
US20050197436A1 (en) * 2004-03-05 2005-09-08 Saint-Gobain Performance Plastics Corporation Flame resistant thermal interface material
US20100009109A1 (en) * 2008-07-11 2010-01-14 Polymatech Co., Ltd. Thermally conductive sheet composite and method for manufacturing the same
US20110159296A1 (en) * 2008-08-18 2011-06-30 Sekisui Chemical Co., Ltd. Insulating sheet and laminated structure
US8029694B2 (en) * 2007-04-24 2011-10-04 E.I. Du Pont De Nemours And Company Thermally conductive and electrically resistive liquid crystalline polymer composition

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Publication number Priority date Publication date Assignee Title
US5844036A (en) * 1995-06-09 1998-12-01 Hoechst Celanese Corp. Highly filled injection moldable polyetherketones
WO2001021393A1 (fr) * 1999-09-21 2001-03-29 Saint-Gobain Ceramics And Plastics, Inc. Materiaux thermoconducteur d'un compose hydrophobe devant etre soumis a une gestion thermique
US20050197436A1 (en) * 2004-03-05 2005-09-08 Saint-Gobain Performance Plastics Corporation Flame resistant thermal interface material
US8029694B2 (en) * 2007-04-24 2011-10-04 E.I. Du Pont De Nemours And Company Thermally conductive and electrically resistive liquid crystalline polymer composition
US20100009109A1 (en) * 2008-07-11 2010-01-14 Polymatech Co., Ltd. Thermally conductive sheet composite and method for manufacturing the same
US20110159296A1 (en) * 2008-08-18 2011-06-30 Sekisui Chemical Co., Ltd. Insulating sheet and laminated structure

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150184055A1 (en) * 2012-09-19 2015-07-02 Momentive Performance Materials Inc. Thermally conductive plastic compositions, extrusion apparatus and methods for making thermally conductive plastics
US9434870B2 (en) * 2012-09-19 2016-09-06 Momentive Performance Materials Inc. Thermally conductive plastic compositions, extrusion apparatus and methods for making thermally conductive plastics
US9685598B2 (en) 2014-11-05 2017-06-20 Novation Iq Llc Thermoelectric device
WO2016106410A1 (fr) * 2014-12-24 2016-06-30 Momentive Performance Materials Inc. Compositions plastiques thermoconductrices, appareil d'extrusion et procédés de fabrication de plastiques thermonconducteurs
JP2018502198A (ja) * 2014-12-24 2018-01-25 モーメンティブ・パフォーマンス・マテリアルズ・インク 熱伝導性プラスチック組成物、熱伝導性プラスチックを製造するための押出装置および方法

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