JP6256113B2 - 熱電変換材料含有樹脂組成物からなるフィルムの製造方法および熱電変換素子の製造方法 - Google Patents
熱電変換材料含有樹脂組成物からなるフィルムの製造方法および熱電変換素子の製造方法 Download PDFInfo
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- JP6256113B2 JP6256113B2 JP2014045238A JP2014045238A JP6256113B2 JP 6256113 B2 JP6256113 B2 JP 6256113B2 JP 2014045238 A JP2014045238 A JP 2014045238A JP 2014045238 A JP2014045238 A JP 2014045238A JP 6256113 B2 JP6256113 B2 JP 6256113B2
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- 239000000969 carrier Substances 0.000 description 1
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- 125000004093 cyano group Chemical group *C#N 0.000 description 1
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- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
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- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
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- 229910052748 manganese Inorganic materials 0.000 description 1
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- 239000004570 mortar (masonry) Substances 0.000 description 1
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- IBHBKWKFFTZAHE-UHFFFAOYSA-N n-[4-[4-(n-naphthalen-1-ylanilino)phenyl]phenyl]-n-phenylnaphthalen-1-amine Chemical group C1=CC=CC=C1N(C=1C2=CC=CC=C2C=CC=1)C1=CC=C(C=2C=CC(=CC=2)N(C=2C=CC=CC=2)C=2C3=CC=CC=C3C=CC=2)C=C1 IBHBKWKFFTZAHE-UHFFFAOYSA-N 0.000 description 1
- 125000005487 naphthalate group Chemical group 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- 239000002667 nucleating agent Substances 0.000 description 1
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- WCXXBFNWCCIYQO-UHFFFAOYSA-N peropyren Chemical compound C12=C3C4=CC=C2C=CC=C1C=CC3=C1C=CC2=CC=CC3=CC=C4C1=C32 WCXXBFNWCCIYQO-UHFFFAOYSA-N 0.000 description 1
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
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- 239000005015 poly(hydroxybutyrate) Substances 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920001281 polyalkylene Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 239000004631 polybutylene succinate Substances 0.000 description 1
- 229920002961 polybutylene succinate Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 239000004431 polycarbonate resin Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000004633 polyglycolic acid Substances 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002215 polytrimethylene terephthalate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229960000380 propiolactone Drugs 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- LNKHTYQPVMAJSF-UHFFFAOYSA-N pyranthrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC3=C(C=CC=C4)C4=CC4=CC=C1C2=C34 LNKHTYQPVMAJSF-UHFFFAOYSA-N 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical compound C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000021286 stilbenes Nutrition 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/856—Thermoelectric active materials comprising organic compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/01—Manufacture or treatment
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Description
本発明に係る熱念変換材料含有樹脂組成物(以下、樹脂組成物とも記す。)は、(A)絶縁性樹脂と、(B)無機熱電変換材料と、(C)電荷輸送材料とを含む。また、樹脂組成物は、(S)有機溶剤を含む液状の組成物であってもよい。さらに、樹脂組成物は、(A)絶縁性樹脂、(B)無機熱電変換材料、(C)電荷輸送材料、及び(S)有機溶剤の以外に、(D)他の成分として、従来から種々の樹脂組成物に配合されている、強化材、充填材、及び添加剤を含んでいてもよい。
以下、樹脂組成物が含む、必須又は任意の成分について説明する。
(A)絶縁性樹脂は、フィルム状に製膜可能なものであれば特に限定されず、従来からフィルム形成用途に用いられている絶縁性の樹脂から適宜選択することができる。(A)絶縁性樹脂は、当業者に一般的に絶縁性の材料であると認識されているものであれば特に限定されない。(A)絶縁性樹脂の電導率は、1S/cm以下が好ましい。また、(A)絶縁性樹脂の熱伝導率は、0.5W/mK以下が好ましく、0.3W/mK以下がより好ましい。
(B)無機熱電変換材料は、従来から当業者に熱電変換能を有する無機材料であると認識されているものであれば特に限定されない。このような、材料の具体例としては、単層カーボンナノチューブ;酸化亜鉛、酸化スズ、チタン酸ストロンチウム、チタン酸バリウム、(Zn,Al)O、NaCo2O4、Ca3Co4O9、Bi2Sr2Co2Oy、及び硫化銀等の金属の酸化物や硫化物;Bi、Sb、Ag、Pb、Ge、Cu、Sn、As、Se、Te、Fe、Mn、Co、及びSiから選択される少なくとも2種以上の元素を含む金属元素複合材料が挙げられる。金属元素複合材料の好適な例としては、BiTe系、BiSb系、BiSbTe系、BiSbSe系、CoSb系、PbTe系、TeSe系、及びSiGe系の材料や、マグネシウムシリサイド系材料(Mg2Si系材料)が挙げられる。
上記の平均粒子径、平均長、及び平均径は、粒子状の無機変換材料の電子顕微鏡観察画像から求められる数平均値である。
(C)電荷輸送材料は、電子又は正孔を輸送するか、輸送を促進させる物質であって、樹脂組成物を用いて形成されるフィルムの熱電変換の効率を高める。樹脂組成物が、(C)電荷輸送材料を含むことにより、樹脂組成物を用いて形成されるフィルムの導電性及びパワーファクターが高まる。
樹脂組成物を用いてキャストフィルムを形成する場合、樹脂組成物は(S)有機溶剤を含んでいてもよい。(S)有機溶剤の種類、(A)絶縁性樹脂を均一に溶解可能なものであれば特に限定されない。このため(S)有機溶剤の種類は、(A)絶縁性樹脂の種類に応じて適宜選択される。なお、(B)無機熱電変換材料、及び(C)電荷輸送材料は、必ずしも(S)有機溶剤に可溶である必要はない。
樹脂組成物は、多様な目的で使用されている種々の樹脂組成物に従来から配合されている強化材や充填材、及び種々の添加剤から選択される1種以上の成分を含んでいてもよい。添加剤の具体例としては可塑剤、分散剤、着色剤、紫外線吸収剤、酸化防止剤、造核剤、及び難燃剤等が挙げられる。これらの強化材、充填材、及び添加剤の使用量は、フィルムを形成する際の製膜性等を考慮しつつ、従来の樹脂組成物におけるこれらの強化材、充填材、及び添加剤の使用量の範囲内で適宜選択される。
樹脂組成物の製造方法は、以上説明した成分を均一に混合できれば特に限定されない。樹脂組成物が(S)有機溶剤を含まない場合、(A)絶縁性樹脂と、(A)絶縁性樹脂以外の成分とを、二本ロール、三本ロール、加圧ニーダー、バンバリーミキサー、単軸押出機、及び二軸押出機等の溶融混練装置を用いて均一に混合して、樹脂組成物が得られる。
以上説明した樹脂組成物を用いてフィルムを形成する方法は特に限定されない。フィルムの製造方法は、樹脂組成物の性状や、樹脂組成物に含まれる樹脂の種類に応じて、公知の方法から適宜選択される。
(ポリ(ニッケル 1,1,2,2−エテンテトラチオラート)(可溶化PETT)の調製)
1,3,4,6−テトラチアペンタレン−2,5−ジオン(TPD、試薬、東京化成工業株式会社製)1g、ナトリウムメトキシド(試薬、和光純薬工業株式会社製)1.2g、及びドデシルトリメチルアンモニウムブロマイド(DTAB、試薬、和光純薬工業株式会社)6.8gを、メタノール200mL中に溶解させた。得られた溶液を、12時間加熱還流させた。次いで、溶液中に塩化ニッケル(II)無水(試薬、和光純薬工業株式会社製)0.63gを加えた。塩化ニッケル(II)無水の添加後、さらに、溶液を12時間加熱還流させた。12時間還流後、溶液を室温下に12時間静置し、沈殿を生成させた。生成した黒色の沈殿物を吸引ろ過により回収した。回収された沈殿物を、メタノール2L、水2L、及びジエチルエーテル50mLを順に用いて洗浄した後、乾燥させて、可溶化PETTを得た。
(電荷移動錯体(TTF−TCNQ)の調製)
7,7,8,8−テトラシアノキノジメタン(TCNQ、試薬、東京化成工業株式会社製)1020.87mgを、アセトニトリル250mLに加え、室温下で12時間撹拌してTCNQのアセトニトリル溶液を得た。次いで、テトラチアフルバレン(TTF、試薬、東京化成工業株式会社製)1021.88mgをアセトニトリル60mgに加えた後、室温で10分間超音波を照射して、TTFのアセトニトリル溶液を得た。
得られたTCNQのアセトニトリル溶液と、TTFのアセトニトリル溶液と混合した後、室温で30分間撹拌した。撹拌により、アセトニトリル中に黒色の沈殿が生成した。沈殿をろ過により回収した後、乾燥させた。乾燥させた沈殿をアセトニトリルで洗浄した後、80℃で15時間真空下に乾燥させて、電荷移動錯体(TTF−TCNQ)1905.50mg(収率93.3%)を得た。
PVC:ポリ塩化ビニル(試薬、和光純薬工業株式会社製)
PI:ポリイミド(Solpit A、ソルピー工業株式会社製)
B1:単層カーボンナノチューブ(Pure Tubes(商品名)、Aldrich社製、平均長1μm、平均径1.4nm)を用いた。
B2:単層カーボンナノチューブ(Single−Walled Carbon Nanotubes、平均径0.8nm、Aldrich社製)
C1:調製例1で得られたPETT
C2:調製例2で得られた電荷移動錯体(TTF−TCNQ)
C3:テトラチアフルバレン(TTF、試薬、東京化成工業株式会社製)
まず、フィルム、又はシートをメタノール中に30分間浸漬させた。次いで、フィルム、又はシートをメタノール中から引き揚げ、70℃のホットプレート上で15分間加熱して、フィルム又はシート乾燥させた。
試薬として購入したシート状のB1を、4mm×16mmの大きさに切り取り、石英基板に張り付けて、ZEM−3で熱電特性を測定した。膜の厚さは18μmであった。
比較例1で得たシートについてはメタノール処理を施さず、比較例2で得たシートについてはメタノール処理を施した。
(A)成分の含有量と、(C)成分の含有量との比率が、表1に記載の比率であり、分散液中の(A)成分の含有量と、(C)成分の含有量との合計が0.5質量%となるように、(A)成分及び(C)成分を、N−メチル−2−ピロリドンと均一に混合して、分散液を得た。(A)成分及び(C)成分としては、表1に記載の種類のものを用いた。得られた分散液を石英基板上にキャストした後、石英基板を60℃で10時間加熱して、膜厚8μmのフィルムを得た。
比較例3で得たシートについてはメタノール処理を施さず、比較例4で得たシートについてはメタノール処理を施した。
(A)成分の含有量と、(B)成分の含有量との比率が、表1に記載の比率であり、分散液中の(A)成分の含有量と、(B)成分の含有量の合計が0.5質量%となるように、(A)成分及び(B)成分を、N−メチル−2−ピロリドンと均一に混合して、分散液を得た。(A)成分及び(B)成分としては、表1に記載の種類のものを用いた。得られた分散液を石英基板上にキャストした後、石英基板を60℃で10時間加熱して、膜厚7μmのフィルムを得た。
比較例5及び6で得たシートについてはメタノール処理を施さず、比較例7で得たシートについてはメタノール処理を施した。
熱伝導率κを測定する際、フィルムの比熱Cp(J/gK、25℃)は、示差走査熱量計(DSC 204 F1 Phoenix、ネッチジャパン社製)を用いて測定した。フィルムの熱拡散率α(mm2/S、25℃)は、ナノフラッシュアナライザ−(LFA 447/2−4/InSb NanoFlash Xe、ネッチジャパン社製)を用いて測定した。フィルムの密度ρ(g/cm3)は、アルキメデス法で測定した。測定された各値は、以下の通りである。
Cp:0.88(J/gK、25℃)
α:0.079(mm2/S、25℃)
ρ:0.83(g/cm3)
(熱伝導率算出式)
κ=α×Cp×ρ
(無次元性能指数算出式)
ZT=(S2×σ×T)÷κ(Tは絶対温度)
調製例2で得られた電荷移動錯体(TTF−TCNQ、C2)をめのう乳鉢で粉砕した。電荷移動錯体(C2)110.34mgを、ペレット作成用の金型に充填した後、電荷移動錯体(C2)の粉末をプレス機でプレスして、10mm×3.0mm×2.3mmのブロック状のペレットを得た。比較例8ではペレットを作成委したため、製膜性の評価を行わなかった。
比較例8で得たペレットについてはメタノール処理を施さなかった。
(B)成分(単層カーボンナノチューブ、B1)4.22mg、及び(C)成分(TTF、C3)5.27mgを、N,N−ジメチルホルムアミド2mLと均一に混合して分散液を得た。得られた分散液を石英基板上にキャストした後、石英基板を80℃で2時間加熱した。次いで、石英基板を110℃で30分間加熱して、膜厚6.3μmのフィルムを得た。
比較例9で得たペレットについてはメタノール処理を施さなかった。
(A)成分の含有量と、(B)成分の含有量と、(C)成分の含有量との比率が、表1に記載の比率であり、分散液中の(A)成分の含有量と、(B)成分の含有量と、(C)成分の含有量との合計が0.5質量%となるように、(A)成分、(B)成分、及び(C)成分を、N−メチル−2−ピロリドンと均一に混合して、分散液を得た。(A)成分、(B)成分、及び(C)成分としては、表1に記載の種類のものを用いた。得られた分散液を石英基板上にキャストした後、石英基板を60℃で10時間加熱して、膜厚6.8μmのフィルムを得た。
実施例1で得たシートについてはメタノール処理を施さず、実施例2及び3で得たシートについてはメタノール処理を施した。
PVCを、PIに変えることの他は、実施例2と同様にして、CNTと、PETTと、樹脂とを、実施例2と同濃度でNMP中に含む塗布液を得た。得られた塗布液を用いて、実施例2と同様にして、フィルム形成と、フィルムのメタノール処理とを行った。
(A)成分(PVC)1.36mgと、(B)成分(単層カーボンナノチューブ、B2)3.61mg、及び(C)成分(TTF、C3)4.52mgを、N,N−ジメチルホルムアミド2mLと均一に混合して分散液を得た。得られた分散液を石英基板上にキャストした後、石英基板を80℃で2時間加熱した。次いで、石英基板を110℃で30分間加熱して、膜厚4.8μmのフィルムを得た。
実施例4で得たフィルムについてはメタノール処理を施さなかった。
(A)成分(PVC)1.36mgと、(B)成分(単層カーボンナノチューブ、B1)3.61mg、及び(C)成分(TTF−TCNQ、C2)4.52mgを、N,N−ジメチルホルムアミド2mLと均一に混合して分散液を得た。得られた分散液を石英基板上にキャストした後、石英基板を80℃で2時間加熱した。次いで、石英基板を110℃で30分間加熱して、膜厚6.7μmのフィルムを得た。
実施例5で得たフィルムについてはメタノール処理を施さなかった。
Claims (7)
- (A)絶縁性樹脂と、(B)無機熱電変換材料と、(C)電荷輸送材料とを含む、熱電変換材料含有樹脂組成物からフィルムを形成する工程と、
前記フィルムに対して、脂肪族アルコール類、芳香族溶媒、エーテル類、糖類の水溶液、及び酸又は塩基を含む水溶液からなる群より選択される処理液を接触させる工程と、
を含む、
熱電変換材料含有樹脂組成物からなるフィルムの製造方法。 - 前記(B)無機熱電変換材料の形態が、平均径が0.5〜3000nmであり、アスペクト比(平均長/平均径)が10以上のチューブ又はワイヤーである、請求項1に記載のフィルムの製造方法。
- 前記(B)無機熱電変換材料が単層カーボンナノチューブである、請求項2に記載のフィルムの製造方法。
- 前記(A)絶縁性樹脂がポリオレフィン、及びハロゲン化ポリオレフィンからなる群より選択される1種以上である、請求項1〜3のいずれか1項に記載のフィルムの製造方法。
- 前記(A)絶縁性樹脂がポリ塩化ビニルである、請求項4に記載のフィルムの製造方法。
- 前記処理液が、脂肪族アルコール類である、請求項1〜5のいずれか1項に記載のフィルムの製造方法。
- 請求項1〜6のいずれか1項に記載のフィルムの製造方法に従って形成されたフィルムを用いる、熱電変換素子の製造方法。
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JP4895293B2 (ja) * | 2007-01-26 | 2012-03-14 | 新日鐵化学株式会社 | フレキシブル熱電変換素子及びその製造方法 |
CN101631744A (zh) * | 2007-03-13 | 2010-01-20 | 东洋炭素株式会社 | 含有碳纳米管的碳材料的精制方法及由该精制方法得到的碳材料、以及使用该碳材料的树脂成型体、纤维、散热器、滑动材料、电场电子释放源材料、电极的导电助剂、担载有催化剂的材料及导电性膜 |
EP2754690B1 (en) * | 2007-05-10 | 2017-12-13 | Plastipak Packaging, Inc. | Oxygen scavenging molecules, articles containing same, and methods of their use |
JP2010245299A (ja) * | 2009-04-06 | 2010-10-28 | Three M Innovative Properties Co | 複合材熱電材料及びその製造方法 |
CN101931043B (zh) * | 2009-06-19 | 2013-03-20 | 清华大学 | 热电转换材料 |
JP5713472B2 (ja) * | 2011-03-04 | 2015-05-07 | 独立行政法人産業技術総合研究所 | 熱電変換材料及び該材料を用いたフレキシブル熱電変換素子 |
US20120234204A1 (en) * | 2011-03-17 | 2012-09-20 | Bayer Materialscience Ag | Vapor phase functionalization of carbon nanotubes |
JP2014029932A (ja) * | 2012-07-31 | 2014-02-13 | Nippon Valqua Ind Ltd | 熱電変換材料、熱電変換シートおよびその製造方法ならびに熱電変換モジュール |
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EP3128566A1 (en) | 2017-02-08 |
WO2015133536A1 (ja) | 2015-09-11 |
KR20160130383A (ko) | 2016-11-11 |
US20170069812A1 (en) | 2017-03-09 |
US10084124B2 (en) | 2018-09-25 |
KR102269045B1 (ko) | 2021-06-23 |
CN106165133B (zh) | 2018-12-21 |
EP3128566A4 (en) | 2017-11-08 |
EP3128566B1 (en) | 2019-07-31 |
JP2015170766A (ja) | 2015-09-28 |
CN106165133A (zh) | 2016-11-23 |
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