US20220176684A1 - Polymer member/inorganic base composite, production method therefor, and polymer member therefor - Google Patents

Polymer member/inorganic base composite, production method therefor, and polymer member therefor Download PDF

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US20220176684A1
US20220176684A1 US17/435,893 US202017435893A US2022176684A1 US 20220176684 A1 US20220176684 A1 US 20220176684A1 US 202017435893 A US202017435893 A US 202017435893A US 2022176684 A1 US2022176684 A1 US 2022176684A1
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polymer
thermally modified
polymer layer
modified polymer
composite
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Junshi SOEDA
Yoshinori Ikeda
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Teijin Ltd
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Teijin Ltd
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Definitions

  • the present invention relates to a composite of polymer member and inorganic substrate, a method of manufacturing the same, and a polymer member therefor.
  • a polymer member for example a polyolefin-based polymer such as polypropylene, polyethylene, and cyclic olefin, has been widely used in molded articles such as resin films, nonwoven fabrics, automotive parts, electronic equipment parts, and camera lenses because of their excellent lightness, mechanical strength, chemical resistance, and the like.
  • inorganic materials such as metals, semiconductors, or oxides thereof have different mechanical, thermal, optical, and chemical properties than the polymer member.
  • Patent Document 1 proposes a method for producing a composite material comprising an inorganic material and a polyolefin-based resin material, in which a thin film having a thickness of 1 to 50 nm consisting of an organic material with a hydrophilic group is formed on a surface of an inorganic material, and the inorganic material on which the thin film has been formed and a polyolefin-based resin material are irradiated with ultraviolet rays having a wavelength of 100 to 200 nm, respectively, and then the polyolefin-based resin material is laminated on the thin film of the inorganic material to integrate the inorganic material and the polyolefin-based resin material.
  • a polymer member may be preferable to bond a polymer member to an inorganic substrate without using an adhesive. Accordingly, in the present invention, there is provided a method useful for bonding a polymer member to an inorganic substrate without using an adhesive, as well as a polymer member or the like used therefor.
  • the present invention may include the following embodiments.
  • a method for manufacturing a composite of polymer member and inorganic substrate comprising:
  • the polymer member at least comprises inorganic particles and a polymer.
  • the inorganic substrate is selected from a group consisting of metals and metalloids, metal oxides and metalloid oxides, metal nitrides and metalloid nitrides, metal carbides and metalloid carbides, carbon materials, and combinations thereof.
  • a composite of polymer member and inorganic substrate comprising:
  • the polymer member at least comprises inorganic particles and a polymer.
  • thermoly modified polymer layers are formed of an olefin polymer, and the polymer of the polymer member is an olefin polymer.
  • a polymer member at least comprising inorganic particles, a polymer, and a coupling agent.
  • a composite polymer member comprising:
  • a polymer member at least comprising inorganic particles and a polymer
  • an additional polymer member at least comprising a polymer.
  • the composite polymer member according to embodiment 16 which is in the form of a membrane or film.
  • the composite polymer member is in the form of a film.
  • FIG. 1A is a schematic cross-sectional view of a composite of polymer member and inorganic substrate according to the present invention
  • FIG. 1B is a schematic cross-sectional view of a composite of polymer member and inorganic substrate according to the present invention
  • the method for manufacturing a composite of polymer member and inorganic substrate according to the present invention comprises:
  • the polymer member can be bonded directly to the one or more thermally modified polymer layers, or to a thermally unmodified polymer layer on the one or more thermally modified polymer layers.
  • a method for manufacturing a composite of thermally modified polymer layer and inorganic substrate in which one or more thermally modified polymer layers are adhered onto an inorganic substrate may include forming a first polymer layer on an inorganic substrate and then heating the first polymer layer to form a first thermally modified polymer layer, in order to adhere the first thermally modified polymer layer onto the inorganic substrate.
  • the polymer member at least comprises inorganic particles and a polymer, and in particular at least comprises inorganic particles and a cyclic olefin polymer.
  • the polymer member comprises inorganic particles, it is possible to adjust the physical properties, such as the refractive index, of the polymer member.
  • the polymer member at least comprises inorganic particles, a polymer, and a coupling agent, and in particular at least comprises inorganic particles, a cyclic olefin polymer, and a silane coupling agent.
  • the adhesion of the polymer member to the thermally modified polymer layer can be further improved.
  • the adhesion of the polymer member to the thermally modified polymer layer can be further improved, when the adhesion of the polymer member to the thermally modified polymer layer is reduced due to the inclusion of the inorganic particles.
  • the coupling agent in particular the coupling agent adhered to the surface of the inorganic particles, improves the dispersibility of the inorganic particles in the polymer member, and the remaining coupling agent improves the adhesion of the polymer member to the thermally modified polymer layer.
  • the inorganic substrate used in the method of the present invention may be any inorganic substrate, and may be selected from the group consisting of, for example, metals and metalloids, oxides of metals and metalloids, nitrides of metals and metalloids, carbides of metals and metalloids, carbon materials, and combinations thereof.
  • examples of the metal include aluminum, magnesium, titanium, nickel, chromium, iron, copper, gold, silver, tungsten, zirconium, yttrium, indium, iridium, and the like
  • examples of the metalloid include silicon, germanium, GaAs, InGaAs, InAlAs, LiTaOx, NbTaOx, ZnTe, GaSe, GaP, CdTe, diamond, diamond-like carbon, and the like. Therefore, examples of the metal oxide include oxides of these metals, and examples of the metalloid oxide include oxides of these metalloids and the like.
  • Examples of an oxide of silicon includes glass such as quartz glass and soda glass, and examples of an oxide of aluminum include sapphire and the like.
  • the nitride may include aluminum nitride, silicon nitride, and the like.
  • the carbide include silicon carbide. Further, the carbon material includes diamond and the like.
  • the surface of the inorganic substrate in particular the metal or the metalloid, may be subjected to a treatment such as ozonation, ultraviolet treatment, or the like, in order to increase a functional group, e.g., a hydroxyl group, which can be utilized for the bonding with the first thermally modified polymer layer.
  • a treatment such as ozonation, ultraviolet treatment, or the like, in order to increase a functional group, e.g., a hydroxyl group, which can be utilized for the bonding with the first thermally modified polymer layer.
  • an inorganic material having a melting point higher than the thermal modification temperature (thermal denaturation temperature) of the thermally modified polymer layer can be preferably used.
  • the inorganic substrate may be in any form, and may be, for example, in the form of a film, a sheet, a plate, a tube, a rod, a disk, or the like. In addition, the inorganic substrate may be of any size.
  • a first polymer layer may be formed on an inorganic substrate, and then the first polymer layer may be heated to form a first thermally modified polymer layer, in order to adhere the first thermally modified polymer layer onto the inorganic substrate.
  • a second polymer layer may be formed on the first thermally modified polymer layer, and then the second polymer layer may be heated to form a second thermally modified polymer layer, in order to adhere the second thermally modified polymer layer onto the first thermally modified polymer layer.
  • the degree of thermal modification of the second thermally modified polymer layer may be less than the degree of thermal modification of the first thermally modified polymer layer, so that the first thermally modified polymer layer provides good bonding to the inorganic substrate and the second thermally modified polymer layer provides good bonding to the first thermally modified polymer layer and the polymer member.
  • a third polymer layer may be formed on the second thermally modified polymer layer, and then the third polymer layer may be heated to form a third thermally modified polymer layer, in order to adhere the third thermally modified polymer layer onto the second thermally modified polymer layer.
  • the degree of thermal modification of the third thermally modified polymer layer may be less than the degree of thermal modification of the second thermally modified polymer layer, so that the second thermally modified polymer layer provides good bonding to the first thermally modified polymer layer and the third thermally modified polymer layer provides good bonding to the second thermally modified polymer layer and the polymer member.
  • thermally modified polymer layers such as a fourth thermally modified polymer layer, a fifth thermally modified polymer layer, or the like, can be used in the same manner.
  • the degree of thermal modification of these thermally modified polymer layers can be adjusted by the temperature, time, ambient atmosphere, and the like of the heating for thermal modification.
  • the degree of thermal modification of the first thermally modified polymer layer may be such that the first thermally modified polymer layer adheres onto the inorganic substrate, i.e., such that the adhesion of the first thermally modified polymer layer to the inorganic substrate is greater than the adhesion of the thermally unmodified first polymer layer to the inorganic substrate.
  • the degree of thermal modification of the second thermally modified polymer layer may be such that the second thermally modified polymer layer adheres onto the first thermally modified polymer layer, i.e., such that the adhesion of the second thermally modified polymer layer to the first thermally modified polymer layer is greater than the adhesion of the thermally unmodified second polymer layer to the first thermally modified polymer layer.
  • the degree of thermal modification of the third thermally modified polymer layer may be such that the third thermally modified polymer layer adheres to the second thermally modified polymer layer, i.e., such that the adhesion of the third thermally modified polymer layer to the second thermally modified polymer layer is greater than the adhesion of the thermally unmodified third polymer layer to the second thermally modified polymer layer.
  • the degree of thermal modification of these thermally modified polymer layers can be adjusted, for example, by the heating temperature, the oxygen concentration in an atmosphere for heating, and the like, for the thermal modification of the thermally modified polymer layer.
  • the heating temperature in order to increase the degree of thermal modification, the heating temperature can be increased and/or the oxygen concentration in the atmosphere for heating can be increased.
  • the heating temperature in order to decrease the degree of thermal modification, the heating temperature can be decreased, and/or the oxygen concentration in the atmosphere for heating can be decreased.
  • the heating temperature for thermal modification of the thermally modified polymer layer may be 50° C. or more, 100° C. or more, 140° C. or more, 160° C. or more, 180° C. or more, or 200° C. or more, and may be 500° C. or less, 400° C. or less, 360° C. or less, 320° C. or less, or 280° C. or less. Further, this heating can be performed in an oxygen-containing atmosphere, in particular in air.
  • the degree of thermal modification of these thermally modified polymer layers can be evaluated, for example, using the oxygen content of the thermally modified polymer constituting the thermally modified polymer layer, specifically, the ratio of the number of oxygen atoms contained in the thermally modified polymer layer to the total number of oxygen atoms and carbon atoms contained in the thermally modified polymer layer (number of oxygen atoms/(number of oxygen atoms+number of carbon atoms) ⁇ 100(%)). In this case, it is considered that the larger the ratio, the larger the degree of thermal modification.
  • a method for evaluating the content of oxygen atoms and carbon atoms of the thermally modified polymer layer includes, for example, X-ray photoelectron spectroscopy (XPS).
  • XPS device for this purpose includes a K-Alpha (Thermo Fisher Scientific).
  • ratio (number of oxygen atoms/(number of oxygen atoms+number of carbon atoms) ⁇ 100(%)) is 0.3% or more, 0.5% or more, 1.0% or more, 2.0% or more, or 5.0% or more, and 50% or less, 30% or less, 20% or less, 10% or less, or 8% or less, it is particularly appropriate to use this ratio as an index indicating the degree of thermal modification of the thermally modified polymer layer.
  • the difference in this ratio between neighboring thermally modified polymer layers may be 0.1% or more, 0.2% or more, 0.3% or more, 0.4% or more, 0.5% or more, 0.8% or more, 1.0% or more, 2.0% or more, or 3.0% or more, and may be 10.0% or less, 7.0% or less, 5.0% or less, 3.0% or less, 2.0% or less, 1.0% or less, 0.5% or less, 0.3% or less or 0.1% or less.
  • the ratio of the number of oxygen atoms contained in the second thermally modified polymer layer to the total number of oxygen atoms and carbon atoms contained in the second thermally modified polymer layer may be 0.1% or more and 10.0% or less smaller than the ratio of the number of oxygen atoms contained in the first thermally modified polymer layer to the total number of oxygen atoms and carbon atoms contained in the first thermally modified polymer layer (i.e., the ratio of the number of oxygen atoms/(the number of oxygen atoms+the number of carbon atoms) ⁇ 100(%) for the first thermally modified polymer layer)
  • the degree of thermal modification of these thermally modified polymer layers can be evaluated, for example, by IR absorption spectrum of the thermally modified polymer constituting the thermally modified polymer layer.
  • An IR absorption analyzer for this purpose includes Nicolet 6700 (Thermo Fisher SCIENTIFIC).
  • the degree of thermal modification of the thermally modified polymer layer can be evaluated by the ratio of the intensity of the absorption peak of the C ⁇ O stretching vibration to the intensity of the absorption peak of the C—H stretching vibration (a ratio of the intensity of the absorption peak of C ⁇ O stretching vibration/intensity of the absorption peak of C—H stretching vibration ( ⁇ )). In this case, it is considered that the larger the ratio, the larger the degree of thermal modification.
  • the intensity of the absorption peak can be determined by reading the maximum value of the absorbance value of the absorption peak.
  • a ratio (a ratio of intensity of absorption peak of C ⁇ O stretching vibration/intensity of absorption peak of C—H stretching vibration ( ⁇ )) is 0.01 or more, 0.02 or more, 0.05 or more, 0.1 or more, 0.15 or more, or 0.20 or more, and 20 or less, 10 or less, or 5 or less, it is particularly appropriate to use the ratio as an index indicating the degree of thermal modification of the thermally modified polymer layer.
  • the difference in this ratio between neighboring thermally modified polymer layers may be 0.1 or more, 0.2 or more, 0.3 or more, 0.4 or more, 0.5 or more, 0.8 or more, 1.0 or more, 2.0 or more, or 3.0 or more, and may be 10.0 or less, 7.0 or less, 5.0 or less, 3.0 or less, 2.0 or less, 1.0 or less, 0.5 or less, 0.3 or less, or 0.1 or less.
  • the ratio of the intensity of the absorption peak of the C ⁇ O stretching vibration of the second thermally modified polymer layer to the intensity of the absorption peak of the C—H stretching vibration of the second thermally modified polymer layer may be 0.1 or more and 20.0 or less smaller than the ratio of the intensity of the absorption peak of the C ⁇ O stretching vibration of the first thermally modified polymer layer to the intensity of the absorption peak of the C—H stretching vibration of the first thermally modified polymer layer (i.e., the ratio of the intensity of the absorption peak of the C ⁇ O stretching vibration/the intensity of the absorption peak of the C—H stretching vibration ( ⁇ ) for the first thermally modified polymer layer).
  • a method for the heating is not particularly limited.
  • the method for the heating may include a method using a heating source such as an oven, a hot plate, infrared rays, a flame, a laser, or a flash lamp.
  • the formation of the polymer layer such as the first polymer layer can be performed by coating and/or thermocompression bonding.
  • a polymer constituting the polymer layer may be dissolved in a solvent to form a solution, a coating may be carried out with this solution, and then the coated solution may be dried to form a polymer layer.
  • a coating method in this case may include methods using a solution, such as a spin coating method, a roll coater method, a spray coating method, a die coater method, an applicator method, an immersion coating method, a brush coating, a spatula coating, a roller coating, a curtain flow coater method and the like.
  • the method may include a step of removing the solvent by heating after the coating of the solution.
  • the heating condition it is possible to select temperature, heating time and atmospheric pressure condition which are sufficient to remove the solvent from the coating film.
  • the coating layer is formed by thermocompression bonding
  • the thickness of the polymer layer such as the first polymer layer may have any thickness, and may have a thickness which ensures that a thermally modified polymer layer to be obtained provides good bonding between the inorganic substrate and the polymer member.
  • the thickness may be, for example, 1 nm or more, 5 nm or more, or 10 nm or more, and may be 100 ⁇ m or less, 30 ⁇ m or less, or 10 ⁇ m or less, or even 1000 nm or less, 500 nm or less, or 100 nm or less.
  • the thermally modified polymer layer is a layer via which the polymer member is bonded to the inorganic substrate. Therefore, this thermally modified polymer layer is preferably composed of the same type of polymer as the polymer constituting the polymer member, in order to promote the bonding between the thermally modified polymer layer and the polymer member.
  • the polymer layer such as the first polymer layer may be formed of an olefin polymer, for example, a cyclic olefin polymer.
  • the olefin polymer means a polymer obtained by polymerizing monomers containing an olefin as the main component; in other words, the olefin polymer means a polymer obtained by polymerizing monomers containing 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, or 95% by mass or more of a monomer portion derived from an olefin.
  • olefin polymer examples include polyethylene, polypropylene, polybutene, polymethylpentene, copolymers of ⁇ -olefin and ethylene or propylene such as propylene-ethylene copolymer and propylene-butene copolymer, styrene-butadiene-styrene block copolymer, styrene-hexadiene-styrene copolymer, styrene-pentadiene-styrene copolymer, ethylene-propylene-diene copolymer (RPDM), cyclic olefin polymer, and the like.
  • RPDM ethylene-propylene-diene copolymer
  • cyclic olefin polymer and the like.
  • these olefin polymers may be used alone, or two or more thereof may be used in combination.
  • olefin polymers mention may be made, in particular, of cyclic olefin polymers.
  • the cyclic olefin polymer is a polymer having a cyclic olefin portion in the polymer main chain.
  • examples of such a cyclic olefin polymer include a ring-opening polymer of a cyclic olefin monomer, an addition polymer of a cyclic olefin monomer, a copolymer of a cyclic olefin monomer and a linear olefin, and the like.
  • the present invention is not limited to these examples.
  • the cyclic olefin monomer is a compound having a ring structure formed of carbon atoms and having a carbon-carbon double bond in the ring structure.
  • Examples of the cyclic olefin monomer include a norbornene-based monomer containing a norbornene ring, such as 2-norbornene, norbornadiene and other bicyclic compounds, dicyclopentadiene, dihydrodicyclopentadiene and other tricyclic compounds, a tetracyclododecene, ethylidene-tetracyclododecene, phenyl-tetracyclododecene and other tetracyclic compounds, tricyclopentadiene and other five-membered ring compounds, tetracyclopentadiene and other seven-membered ring compounds; and a monocyclic cyclic olefin such as cyclobutene, cyclopentene
  • Cyclic olefin polymers are readily available commercially, for example, ZEONEX (trade name) Series and ZEONOR (trade name) Series, etc., from Zeon Corporation; SUMILITE (trade name) Series from Sumitomo Bakelite Co., LTD.; ARTON (trade name) Series from JSR Corporation; APEL Series, Mitsui Chemicals Inc.; TOPAS (trade name) from Ticona; Optolets Series, etc., from Hitachi Chemical Co., LTD.
  • the thermally unmodified polymer layer is preferably the same type of polymer as the thermally modified polymer layer such as the first thermally modified polymer layer and the polymer member.
  • the thermally modified polymer layer such as the first thermally modified polymer layer, the thermally unmodified polymer layer and the polymer member may all be formed of an olefin polymer such as a cyclic olefin polymer.
  • the specific materials and methods for the formation of the polymer member reference may be made to the above description regarding the thermally modified polymer layers such as the first thermally modified polymer layer.
  • the polymer member may be a member of any shape, and may be, for example, in the form of a membrane or film.
  • the bonding of the polymer member may be carried out by coating or thermocompression bonding, in particular by thermocompression bonding.
  • the polymer member at least comprises inorganic particles and a polymer, and particularly preferably at least comprises inorganic particles and a cyclic olefin polymer.
  • the thickness thereof is preferably 1 cm or less, 5 mm or less, 2 mm or less, 1 mm or less, 500 ⁇ m or less, 200 ⁇ m or less, 100 ⁇ m or less, or 50 ⁇ m or less, and 1 ⁇ m or more, 2 ⁇ m or more, 5 ⁇ m or more, 10 ⁇ m or more, or 15 ⁇ m or more.
  • the polymer member preferably further comprises a coupling agent, in particular a silane coupling agent.
  • Such a polymer member may be an optical member, in particular an anti-reflection film.
  • the polymer member may consist of a plurality of portions, and in particular, the polymer member may be a composite film which is a laminate of a plurality of layers.
  • the number of layers of the laminate is preferably 2 or more, and preferably 500 or less, 100 or less, 80 or less, 60 or less, 40 or less, 30 or less, 20 or less, 10 or less, or 5 or less.
  • the thermally modified polymer layer such as the first thermally modified polymer layer and the polymer member are preferably the same type of polymer.
  • the thermally modified polymer layer such as the first thermally modified polymer layer and the polymer member may be formed of an olefin polymer such as a cyclic olefin polymer.
  • the specific polymers and methods for the formation of the polymer member reference may be made to the above description regarding the thermally modified polymer layers such as the first thermally modified polymer layers.
  • the inorganic particles in the present invention may include any inorganic particles which can be dispersed in the polymer member, and examples of such inorganic particles include particles of metal or metalloid, particles of an oxide or fluoride of metal or metalloid, and particles of compounds containing metal or metalloid.
  • the metal or the metalloid at least one selected from the group consisting of Si, Ge, Al, Mg, Ti, Ni, Cr, Fe, Cu, Au, Ag, W, Zr, Y, In, and Ir may be preferably used, and Si and Ge may be particularly preferably used.
  • the oxide and the fluoride of the metal or the metalloid at least one selected from the group consisting of MgO, Al 2 O 3 , Bi 2 O 3 , CaF 2 , In 2 O 3 , In 2 O 3 .SnO 2 , HfO 2 , La 2 O 3 , MgF 2 , Sb 2 O 5 , Sb 2 O 5 .SnO 2 , SiO 2 , SnO 2 , TiO 2 , Y 2 O 3 , ZnO and ZrO 2 may be preferably used, and MgO, Al 2 O 3 , SiO 2 , TiO 2 may be particularly preferably used.
  • the compound containing the metal or the metalloid includes GaAs, InGaAs, InAlAs, LiTaOx, NbTaOx, ZnTe, GaSe, GaP, CdTe, diamond, diamond-like carbon, SiC, and the like.
  • the inorganic particles may be silicon particles obtained by a laser pyrolysis method, in particular, a laser pyrolysis method using a CO 2 laser.
  • the above inorganic particles may contain impurity elements such that the concentration of each impurity element is 1000 ppm or less, 500 ppm or less, 300 ppm or less, 100 ppm or less, 50 ppm or less, 10 ppm or less, or 1 ppm or less, in order to obtain good optical properties.
  • impurities include elements in Group 13 and Group 15.
  • the average primary particle diameter of the inorganic particles is 1 nm or more, or 3 nm or more, and 10000 nm or less, 5000 nm or less, 2000 nm or less, 1000 nm or less, 500 nm or less, 200 nm or less, 100 nm or less, 50 nm or less, 30 nm or less, 20 nm or less, or 10 nm or less.
  • the average primary particle diameter of the particles may be obtained as the number average primary particle diameter, by taking images of the particles with a scanning electron microscope (SEM), a transmission electron microscope (TEM) or the like, by measuring the particle diameter directly based on the images, and by analyzing a group of particles of 100 or more.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • the content ratio of the inorganic particles may be, for example, such that the volume ratio of the polymer to the inorganic particles is 1:99 to 99:1, 5:95 to 95:5, 10:90 to 85:15, 20:80 to 80:20, 30:70 to 75:25, or 40:60 to 70:30.
  • the degree of adjustment of the refractive index and the like of the polymer member may be reduced, and when the content of the inorganic particles is too high, the strength and the like as the polymer member may not be maintained.
  • the polymer member is composed of a plurality of portions as described above, it is preferable that a portion of the polymer member to be bonded to a composite of thermally modified polymer layer and inorganic substrate satisfies the above-described volume ratio of the polymer and the inorganic particles.
  • the polymer member is a composite film which is a laminate of a plurality of layers, it is preferable that a layer of the composite film to be bonded to a composite of thermally modified polymer layer and inorganic substrate satisfies the above-described volume ratio of the polymer and the inorganic particles.
  • any coupling agent which can be combined with the inorganic particles may be used.
  • a silane coupling agent, a titanate coupling agent, or an aluminate coupling agent may be used, and in particular, a silane coupling agent may be used.
  • an olefin polymer such as a cyclic olefin polymer
  • a coupling agent with a functional group exhibiting good miscibility to these polymers for example, a coupling agent with an alkyl chain, a cyclohexyl group, or a benzene ring, and more specifically, a coupling agent with an alkyl chain having 1 to 30, 1 to 25, or 1 to 20 carbon atoms, a cyclohexyl group, or a benzene ring.
  • the coupling agent and/or a hydrolytic condensate of the coupling agent may be used alone or in combination of two or more.
  • the coupling agent includes octadecyltriethoxysilane (OTS), octyltriethoxysilane, triethoxyphenylsilane, 3-phenylpropyltriethoxysilane, cyclohexyltrimethoxysilane, octadecyltrimethoxysilane, octadecyltrichlorosilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, ⁇ -(2-aminoethyl)aminopropyltrimethoxysilane, ⁇ -(2-aminoethyl)aminopropyltriethoxysilane, ⁇ -(2-aminoethyl)aminopropylmethyldimethoxysilane, ⁇ -(2-aminoethyl)aminopropylmethyldiethoxysilane
  • the content ratio of the coupling agent may be, for example, such that the mass ratio of the inorganic particles to the coupling agent is 1:99 to 99:1, 5:95 to 95:5, 10:90 to 90:10, 20:80 to 80:20, 30:70 to 70:30, or 40:60 to 60:40.
  • the content of the coupling agent is too low, the adhesion between the polymer member and the thermally modified polymer layer may be insufficient, and when the content of the coupling agent is too high, strength and the like as the polymer member may not be maintained.
  • the one or more thermally modified polymer layers are adhered to the inorganic substrate.
  • the polymer member is adhered to the inorganic substrate via the one or more thermally modified polymer layers of the composite of thermally modified polymer layer and inorganic substrate of the present invention.
  • the polymer members 30 , 31 , 32 are bonded to the inorganic substrate 10 via the one or more thermally modified polymer layers 20 , 21 , 22 of the composites of thermally modified polymer layer and inorganic substrate 110 , 120 .
  • the polymer member according to the present disclosure may form a composite polymer member together with an additional polymer member at least comprising a polymer.
  • additional polymer member reference may be made to the description relating to the polymer member, except that the additional polymer member may not contain inorganic particles.
  • a laminate which has, on a silicon substrate 10 , first and second thermally modified polymer layers 21 , 22 and first and second anti-reflection layers 31 , 32 as polymer members in this order, as shown in FIG. 1B .
  • the adhesion of the anti-reflection composite film composed of the first and second anti-reflection layers to the silicon substrate was evaluated.
  • Comparative Example 1 a laminate was formed which has, on a silicon substrate, first and second anti-reflection layers as polymer members in this order. For this laminate, the adhesion of the anti-reflection composite film composed of the first and second anti-reflection layers to the silicon substrate was evaluated.
  • a cyclic olefin polymer (COP) (ZEONEXTM 480R; from Zeon Corporation; glass transition temperature of 138° C.) was used as a material for both the thermally modified polymer layer and the polymer member.
  • COP cyclic olefin polymer
  • a COP solution A was obtained by mixing and stirring 7% by mass of COP and 93% by mass of toluene at room temperature.
  • a COP solution B1 was obtained by mixing and stirring 35% by mass of COP and 65% by mass of toluene at room temperature
  • Silicon particles were prepared by laser pyrolysis (LP) method using carbon dioxide laser, using monosilane gas as a raw material. Further, the metal impurity content of the obtained silicon particles was measured using an inductively coupled plasma mass spectrometer (ICP-MS). As a result, the content of Fe was 15 ppb, the content of Cu was 18 ppb, the content of Ni was 10 ppb, the content of Cr was 21 ppb, the content of Co was 13 ppb, the content of Na was 20 ppb, and the content of Ca was 10 ppb. The average primary particle diameter of the inorganic particles was 100 nm.
  • Silicon particles and octadecyltriethoxysilane (OTS) were placed in a sealed container in an amount such that a ratio of silicon particles and OTS was 1:1 (mass ratio), and then, after mixing, heated to 120° C. and held for 3 hours, to obtain OTS-treated silicon particles.
  • a COP solution was obtained by mixing and stirring 10% by mass of COP and 90% by mass of toluene at room temperature. To this COP solution, the OTS-treated silicon particles were added and mixed such that the volume ratio of the COP and the silicon particles was 65:35. Further, by homogenizing this mixture in a homogenizer for 15 minutes, a COP solution B2 containing the OTS-treated silicon particles was prepared.
  • the COP solution B1 obtained as described above was coated on a glass substrate using a doctor blade to obtain a coating film, and the solvent in the coating film was removed by heating at 110° C., in order to obtain a second anti-reflection layer having a thickness of 25 ⁇ m on the glass plate.
  • the COP solution B2 obtained as described above was coated on the second anti-reflection layer using a doctor blade to obtain a coating film, and the solvent in the coating film was removed by heating at 110° C., in order to form a first anti-reflection layer having a thickness of 20 ⁇ m on the second anti-reflection layer having a thickness of 25 ⁇ m.
  • the first and second anti-reflection layers obtained as described above were peeled off from the glass plate to obtain an anti-reflection composite film (a composite polymer member) having the first and second anti-reflection layers.
  • a silicon substrate was used as an inorganic substrate, and a COP solution A was spin-coated on the silicon substrate.
  • the spin coating was performed by maintaining the rotation speed at 2000 rpm for 20 seconds.
  • the silicon substrate coated with the COP solution A in this manner was held on a hot plate heated to 120° C. and dried to obtain a silicon substrate having a first polymer layer.
  • the first polymer layer was thermally modified (thermally denatured) by holding the substrate on a hot plate heated to 280° C. over a period of 1 minutes, in order to form a first thermally modified polymer layer having a film thickness of 23 nm, which was adhered to the silicon substrate.
  • a COP solution A was spin-coated on the first thermally modified polymer layer of the silicon substrate obtained as described above.
  • the spin coating was performed by maintaining the rotation speed at 2000 rpm for 20 seconds.
  • the silicon substrate coated with COP solution A in this manner was held on a hot plate heated to 120° C. and dried to form a second polymer layer on the first thermally modified polymer layer.
  • the second polymer layer was thermally modified by holding the substrate on a hot plate heated to 200° C. for 2 minutes, in order to form a second thermally modified polymer layer having a film thickness of 23 nm, which was adhered onto the first thermally modified polymer layer.
  • the anti-reflection composite film obtained as described above was adhered onto the second thermally modified polymer layer of the silicon substrate obtained as described above such that the first anti-reflection layer was in contact with the second thermally modified polymer layer, and thermocompression bonding was performed at 115° C. and 0.2 MPa pressure for 60 minutes to adhere the anti-reflection composite film onto the second thermally modified polymer layer.
  • the obtained evaluation laminate had, on the silicon substrate, the first thermally modified polymer layer, the second thermally modified polymer layer, the first anti-reflection layer, and the second anti-reflection layer in this order.
  • the evaluation laminate obtained as described above was subjected to a cross-cut test.
  • cuts were made at 1 mm intervals to reach the silicon substrate using a utility knife. After six cuts were made, six more cuts were made orthogonal to these cuts, in order to form grid-like cuts.
  • Scotch-Mending Tape manufactured by 3M Company; 810, 24-mm wide
  • 3M Company 810, 24-mm wide
  • Evaluation laminates of Examples 2 to 8 having first and second thermally modified polymer layers and first and second anti-reflection layers on a silicon substrate were obtained in the same manner as in Example 1 except that a spray method was used as the method of forming the second anti-reflection layer (Example 2) and the volume ratio of the COP and the silicon particles was changed in the COP solution for preparing COP solution B2 (Examples 3 to 8).
  • the evaluation laminates of Examples 2 to 8 were evaluated in the same manner as in Example 1.
  • the preparation conditions and evaluation results of the evaluation laminates according to Examples 2 to 8 are shown in Table 1 below.
  • An evaluation laminate having first and second thermally modified polymer layers and first and second anti-reflection layers on a silicon substrate was obtained in the same manner as in Example 1, except that the COP solution B2′ (containing non-OTS-treated silicon particles) was obtained without performing surface treatment of the silicon particles using OTS in the manufacturing process of the COP solution B2, and that this COP solution B2′ was used instead of the COP solution B2.
  • the evaluation laminate according to Example 9 was evaluated in the same manner as in Example 1. The preparation conditions and evaluation results of the evaluation laminate according to Example 9 are shown in Table 1 below.
  • Example 9 An evaluation laminate having first and second anti-reflection layers on a silicon substrate was obtained in the same manner as in Example 9 except that the first and second thermally modified polymer layers were not formed.
  • This evaluation laminate according to Comparative Example 1 was evaluated in the same manner as in Example 1.
  • the preparation conditions and evaluation results of the evaluation laminate according to Comparative Example 1 are shown in Table 1 below.
  • a coating film was obtained by applying a COP solution B1 on a glass plate using a doctor blade, and a solvent in the coating film was removed by heating at 110° C. to obtain a fourth anti-reflection layer having a thickness of 25 ⁇ m on the glass plate;
  • This evaluation laminate according to Example 10 was evaluated in the same manner as in Example 1.
  • the preparation conditions and evaluation results of the evaluation laminate according to Example 10 are shown in Table 2 below.
  • a coating film was obtained by coating a COP solution B1 on a glass plate using a doctor blade, and a solvent in the coating film was removed by heating at 110° C. to obtain a third anti-reflection layer having a thickness of 25 ⁇ m on the glass plate;
  • a coating film was obtained by applying the COP solution B2′ used in Example 9, i.e., the COP solution containing silicon particles not subjected to a surface treatment with OTS, on the third anti-reflection layer using a doctor blade, and a solvent in the coating film was removed by heating at 110° C. to obtain a second anti-reflection layer having a thickness of 15 ⁇ m on the third anti-reflection layer;
  • This evaluation laminate according to Example 11 was evaluated in the same manner as in Example 1.
  • the preparation conditions and evaluation results of the evaluation laminate according to Example 11 are shown in Table 2 below.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 Inorganic substrate Si Si Si Si
  • Example 6 Example 7
  • Example 8 Example 9
  • Example 1 Inorganic substrate Si Si Si Si
  • Example 10 Example 11 Inorganic substrate Si Si First thermally Polymer COP COP modified polymer Thermal 280° C. 280° C. layer modification temp. Second thermally Polymer COP COP modified polymer Thermal 200° C. 200° C. layer modification temp.
  • First anti- Polymer COP COP reflection layer Filler Si particles Si particles Filler content 35 vol % 35 vol % Coupling agent OTS OTS Preparation method Blade coating Blade coating Thickness 20 ⁇ m 5 ⁇ m Second anti- Polymer COP COP reflection layer Filler — Si particles Filler content — 35 vol % Coupling agent — — Preparation method Blade coating Blade coating Thickness 25 ⁇ m 15 ⁇ m Third anti- Polymer COP COP reflection layer Filler Si particles — Filler content 5 vol % — Coupling agent OTS — Preparation method Blade coating Blade coating Thickness 20 ⁇ m 25 ⁇ m Fourth anti- Polymer COP — reflection layer Filler — — Filler content — — Coupling agent — — Preparation method Blade coating — Thickness 25 ⁇ m — Bonding method for anti-reflection ( ⁇ ) ( ⁇ ) composite film Evaluation result A A ( ⁇ ) Thermocompression bonding
  • COP1 Cyclic olefin polymer (ARTONTM (JSR Corporation))
  • COP2 Cyclic olefin polymer (Zeon Corporation, ZEONEXTM 480R, glass transition temperature 138° C.)
  • COP1 was used as a material for both thermally modified polymer layers and polymer members.
  • thermally modified polymer layers were not used, and COP1 was used as a material of a polymer member.
  • a solution for thermally modified polymer layer was obtained by mixing and stirring 7% by mass of COP1 and 93% by mass of chloroform at room temperature.
  • a silicon substrate was used as inorganic substrate, and the solution for thermally modified polymer layer was spin-coated on the silicon substrate.
  • the spin coating was performed by maintaining the rotation speed at 2000 rpm for 20 seconds.
  • the silicon substrate coated with the solution for thermally modified polymer layer in this manner was held on a hot plate heated to 120° C. to dry the solution for thermally modified polymer layer, in order to obtain a silicon substrate with a first polymer layer, and then the first polymer layer was thermally modified (thermally denatured) by holding the substrate on a hot plate heated to 280° C. for 1 minutes to obtain a silicon substrate with a first thermally modified polymer layer having a film thickness of 23 nm.
  • the solution for thermally modified polymer layer was spin-coated on the first thermally modified polymer layer of the silicon substrate obtained as described above.
  • the spin coating was performed by maintaining the rotation speed at 2000 rpm for 20 seconds.
  • the silicon substrate coated with the solution for thermally modified polymer layer in this manner was held on a hot plate heated to 120° C. to dry the solution for thermally modified polymer layer, in order to form a second polymer layer on the first thermally modified polymer layer.
  • the second polymer layer was thermally modified by holding the substrate on a hot plate heated to 200° C. for 2 minutes to obtain a second thermally modified polymer layer having a film thickness of 23 nm, which was adhered onto the first thermally modified polymer layer.
  • a composite of thermally modified polymer layer and inorganic substrate thus obtained was used as the composite of thermally modified polymer layer and inorganic substrate according to Reference Example 1.
  • a solution for polymer member was obtained by mixing and stirring 7% by mass of COP1 and 93% by mass of chloroform at room temperature.
  • the solution for polymer member was spin-coated on the second thermally modified polymer layer obtained as described above.
  • the spin coating was performed by maintaining the rotation speed at 2000 rpm for 20 seconds.
  • the silicon substrate coated with the solution for polymer member in this manner was held on a hot plate heated to 140° C. for 10 minutes to dry the solution for polymer member, in order to bond a polymer member having a film thickness of 23 nm onto the second thermally modified polymer layer.
  • a composite of polymer member and inorganic substrate thus obtained was used as the composite of polymer member and inorganic substrate according to Reference Example 1.
  • cuts reaching the silicon substrate were made at 1 mm intervals by using a utility knife. After six cuts were made, six more cuts were made orthogonal to these cuts to form grid-like cuts.
  • Scotch-Mending Tape (3M Company; 810, 24-mm wide) was applied to the surfaces of the polymer member, and after finger-rubbing the tape from above to adhere it, the tape was peeled off. The area where the tape was stuck and peeled off in this way was observed by a stereomicroscope.
  • Composites of polymer member and inorganic substrate according to Reference Examples 2 to 8 was prepared in the same manner as in Reference Example 1, except that the concentration of the polymer in the solution for thermally modified polymer layer was changed (Reference Examples 2 and 3), the spin coating condition of the solution for thermally modified polymer layer was changed (Reference Example 4), or the temperature of thermal modification of the first thermally modified polymer was changed (Reference Examples 5 to 8), as in Tables R1 and R2.
  • the composites thus prepared were evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results of these composite materials are shown in Tables R1 and R2 below.
  • a first thermally modified polymer layer and a second thermally modified polymer were formed on a silicon substrate in the same manner as in Reference Example 1, except that the temperature of thermal modification for the first thermally modified polymer was 300° C., and the temperature of thermal modification for the second thermally modified polymer was 280° C. and the treatment was performed for 1 minute.
  • the solution for thermally modified polymer layer was spin-coated on the second thermally modified polymer layer obtained as described above.
  • the spin coating was performed by maintaining the rotation speed at 2000 rpm for 20 seconds.
  • the silicon substrate coated with the solution for thermally modified polymer layer in this manner was held on a hot plate heated to 120° C. to dry the solution for thermally modified polymer layer, in order to form a third polymer layer on the second thermally modified polymer layer.
  • the third polymer layer was thermally modified by holding the substrate on a hot plate heated to 200° C. for 2 minutes to obtain a third thermally modified polymer layer having a film thickness of 23 nm, which was adhered onto the second thermally modified polymer layer.
  • a composite of thermally modified polymer layer and inorganic substrate thus obtained was used as the composite of thermally modified polymer layer and inorganic substrate of Reference Example 3A
  • the composite of polymer member and inorganic substrate according to Reference Example 3A was prepared by performing bonding of the polymer member in the same manner as in Reference Example 1.
  • the composite of polymer member and inorganic substrate according to Reference Comparative Example 1 was prepared in the same manner as in Reference Example 1, except that first and second thermally modified polymer layers were not formed on a silicon substrate which was used as an inorganic substrate, and that COP1 was spin-coated directly on the silicon substrate.
  • the obtained composite was evaluated in the same manner as in Reference Example 1.
  • the preparation conditions and evaluation results of this composite material are shown in Tables R1 and R2 below.
  • the composite of polymer member and inorganic substrate according to Reference Example 9 was prepared and evaluated in the same manner as in Reference Example 1, except that instead of spin-coating the cyclic olefin polymer during bonding of the polymer member, a film of COP1 (with a thickness of 100 ⁇ m) was placed on the second thermally modified polymer layer and held at 50 MPa pressure and 140° C. for 2 hours for the thermocompression-bonding of the film and the second thermally modified polymer layer.
  • Table R3 The preparation conditions and evaluation results of this composite material are shown in Table R3 below.
  • the composite polymer member and inorganic substrate according to Reference Comparative Example 2 was prepared in the same manner as in Reference Example 9, except that first and second thermally modified polymer layer were not formed on a silicon substrate which was used as an inorganic substrate, and a film of COP1 (thickness: 100 ⁇ m) was bonded directly onto the silicon substrate by thermocompression-bonding.
  • the obtained composite was evaluated in the same manner as in Reference Example 1.
  • the preparation conditions and evaluation results of this composite material are shown in Table R3 below.
  • Composites of polymer member and inorganic substrate according to Reference Examples 10 to 14 were prepared in the same manner as in Reference Examples 5, 6, 1, 7 and 8, respectively, except that after the first thermally modified polymer layer was formed on the silicon substrate which was used as an inorganic substrate, a solution for polymer member was spin-coated directly on the first thermally modified polymer layer without forming a second thermally modified polymer layer.
  • the obtained composites were evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results for these composite materials are shown in Table R4 below.
  • COP2 was used as a material for both the thermally modified polymer layer and the film of the polymer member.
  • the thermally modified polymer layer was not used, and COP2 was used as a material of the film of the polymer member.
  • the composite of polymer member and inorganic substrate according to Reference Example 15 was prepared in the same manner as in Reference Example 1, except that in the preparation of both the solution for thermally modified polymer layer and the solution for polymer member, a solution for thermally modified polymer layer was obtained by mixing and stirring 10% by mass of COP2 and 90% by mass of toluene at room temperature.
  • the obtained composite was evaluated in the same manner as in Reference Example 1. The conditions and evaluation results of this composite material are shown in Table R5 below.
  • the composite of polymer member and inorganic substrate according to Reference Example 16 was prepared in the same manner as in Reference Example 15, except that the concentration of polymer in the solution for forming thermally modified polymer layer was changed from 10% by mass to 1% by mass.
  • the obtained composite was evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results of this composite are shown in Table R5 below.
  • the composite of polymer member and inorganic substrate according to Reference Comparative Example 3 was prepared in the same manner as in Reference Example 15, except that first and second thermally modified polymer layers were not formed on the silicon substrate which was used as an inorganic substrate, and that COP2 was spin-coated directly on the silicon substrate.
  • the obtained composite was evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results for this composite material are shown in Table R5 below.
  • Composites of polymer member and inorganic substrate according to Reference Examples 17 to 20 were prepared in the same manner as in Reference Example 15, except that the temperature of thermal modification for the first thermally modified polymer was changed as in Table R6.
  • the obtained composites were evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results for these composite materials are shown in Table R6 below.
  • a polyethylene (PE) film (thickness: 30 ⁇ m) was used as a material for both the thermally modified polymer layer and the polymer member.
  • the thermally modified polymer layer was not used, and a polyethylene film (thickness: 30 ⁇ m) was used as a material of the polymer member.
  • a silicone substrate as inorganic substrate having a polyethylene film (30 ⁇ m thickness) thereon was heated to 120° C. and held for 1 minute to obtain a silicon substrate with a polyethylene film, and then the polyethylene film was thermally modified by holding the substrate on a hot plate heated to 280° C. for 1 minute, in order to obtain a silicon substrate with a first thermally modified polymer layer.
  • a polyethylene film (thickness: 30 ⁇ m) was placed on the first thermally modified polymer layer of the silicon substrate obtained as described above, and the substrate was heated to 120° C. and held for 1 minute to adhere the polyethylene film onto the first thermally modified polymer layer. Then, the polyethylene film was thermally modified by holding the substrate on a hot plate heated to 200° C. for 2 minutes, in order to obtain a second thermally modified polymer layer, which was adhered onto the first thermally modified polymer layer.
  • a composite of thermally modified polymer layer and inorganic substrate thus obtained was used as the composite of thermally modified polymer layer and inorganic substrate according to Reference Example 21.
  • a polyethylene film (thickness: 30 ⁇ m) was placed on the second thermally modified polymer layer obtained as described above, and the substrate was heated to 120° C. and held for 1 minute, and further heated to 140° C. and held for 10 minutes, to bond the polyethylene film as polymer member onto the first thermally modified polymer layer.
  • a composite of polymer member and inorganic substrate thus obtained was used as the composite of polymer member and inorganic substrate according to Reference Example 21, and evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results for this composite material are shown in Table R7 below.
  • the composite of polymer member and inorganic substrate according to Reference Comparative Example 4 was prepared in the same manner as in Reference Example 21, except that first and second thermally modified polymer layer were not formed on a silicon substrate which was used as an inorganic substrate, and a polyethylene film as polymer member was bonded directly onto the silicon substrate.
  • the obtained composite was evaluated in the same manner as in Reference Example 1.
  • the preparation conditions and evaluation results for this composite material are shown in Table R7 below.
  • a silicon substrate was used as an inorganic substrate, and, as in Reference Example 1, COP1 was used to form first and second thermally modified polymer layers on the silicon substrate.
  • a silicon substrate was used as an inorganic substrate, and as in Reference Example 15, COP2 was used to form first and second thermally modified polymer layers on the silicon substrate.
  • a silicon substrate was used as an inorganic substrate, and as in Reference Example 21, a polyethylene film (thickness: 30 ⁇ m) was used to form first and second thermally modified polymer layer on the silicon substrate.
  • Composites of polymer member and inorganic substrate according to Reference Examples 28 to 30 were prepared in the same manner as in Reference Example 15, except that a silicon substrate with an SiN layer formed on the surface thereof (Reference Example 28), a copper plate (Reference Example 29), and an aluminum plate (Reference Example 30) were used as an inorganic substrate, respectively, instead of a silicon substrate.
  • the obtained composites were evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results of these composite materials are shown in Table R9 below.
  • Composites of polymer member and inorganic substrate according to Reference Comparative Examples 5 to 7 were prepared in the same manner as in Reference Examples 28 to 30, respectively, except that the thermally modified polymer layer was not used. The obtained composites were evaluated in the same manner as in Reference Example 1. The preparation conditions and evaluation results of these composite materials are shown in the following table.
  • a silicon substrate as inorganic substrate was treated with a silane coupling agent, and a polymer member was bonded to this treated surface.
  • An OTS-treated silicon substrate was obtained by treating a silicon substrate as an inorganic substrate with ultraviolet and ozone (UV/O 3 treatment), and then by holding the substrate for 3 hours in a saturated vapor pressure atmosphere at 150° C. of octadecyltriethoxysilane (OTS) as a silane coupling agent.
  • UV/O 3 treatment ultraviolet and ozone
  • OTS octadecyltriethoxysilane
  • Composites of polymer member and inorganic substrate according to Reference Comparative Examples 10 to 11 were prepared in the same manner as in Reference Comparative Examples 8 and 9, respectively, except that 3-phenylpropyltriethoxysilane (PTS) was used as a silane coupling agent instead of octadecyltriethoxysilane (OTS).
  • PTS 3-phenylpropyltriethoxysilane
  • OTS octadecyltriethoxysilane
  • Composites of polymer member and inorganic substrate according to Reference Comparative Examples 12 to 13 were prepared in the same manner as in Reference Comparative Examples 8 and 9, respectively, except that 3-aminopropyltriethoxysilane (ATS) was used as a silane coupling agent instead of octadecyltriethoxysilane (OTS).
  • ATS 3-aminopropyltriethoxysilane
  • OTS octadecyltriethoxysilane
  • COP1 is a cyclic olefin polymer (JSR Corporation, ARTON TM) * 3 COP2 is a cyclic olefin polymer (Zeon Corporation, Zeonex TM 480R) * 4 PE film is a polyethylene film (thickness of 30 ⁇ m) ( ⁇ ) Thermocompression bonding
  • ATS treated PE film ( ⁇ ) C Ex. 13 Si * 3 COP2 is a cyclic olefin polymer (Zeon Corporation, Zeonex TM 480R) * 4 PE film is a polyethylene film (thickness of 30 ⁇ m) ( ⁇ ) Thermocompression bonding
  • a silicon substrate was used as an inorganic substrate, and a silicon substrate with thermally modified polymer layer was obtained on the silicon substrate in the same manner as in Reference Example 1, except that a solution for thermally modified polymer layer was obtained by mixing and stirring 20% by mass of COP1 and 80% by mass of chloroform at room temperature, and the temperature of the hot plate for thermal modification was changed to 400° C. (Reference Example 31), 320° C. (Reference Example 32), 280° C. (Reference Example 33), 240° C. (Reference Example 34), 200° C. (Reference Example 35), and 160° C. (Reference Example 36).
  • a ratio of the number of oxygen atoms contained in the thermally modified polymer layer to the total number of oxygen atoms and carbon atoms contained in the thermally modified polymer layer was determined using an XPS device (K-Alpha (from Thermo Fisher Scientific)).
  • Measurement was performed using monochromatized AlK ⁇ rays as an X-ray source and with a photoelectron extraction angle of 0 degree.
  • the O1s peak area was determined by drawing a baseline according to Shirley method in the range of 527 to 537 eV
  • the C1s peak area was determined by drawing a baseline according to Shirley method in the range of 280 to 290 eV.
  • the oxygen concentration and carbon concentration on the surface of the film were obtained by correcting the above-mentioned O1s peak area and C1s peak area with a sensitivity coefficient inherent to respective devices.
  • infrared transmission absorption spectrum ranging from 4000 to 500 cm ⁇ 1 was measured using an IR absorption spectrometer (Nicolet 6700 (from Thermo Fisher Scientific)) to determine the ratio of the absorption peak intensity of C ⁇ O stretching vibration peaking at 1732 cm ⁇ 1 to the absorption peak intensity of C—H stretching vibration peaking at 2947 cm ⁇ 1 (ratio of the absorption peak intensity of C ⁇ O stretching vibration/the absorption peak intensity of C—H stretching vibration ( ⁇ )).
  • the absorption peak intensity was determined by reading the maximum value of the absorbance value of the absorption peak.

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US6525126B1 (en) * 1999-06-04 2003-02-25 Chisso Corporation Method for producing reinforced thermoplastic resin composition and melt-kneading apparatus
US20010030059A1 (en) * 1999-12-20 2001-10-18 Yasuhiro Sugaya Circuit component built-in module, radio device having the same, and method for producing the same
US11320569B2 (en) * 2018-09-28 2022-05-03 Hamamatsu Photonics K.K. Optical element for terahertz waves and manufacturing method of the same

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