JP2013501117A - フルオロポリマーと酸化亜鉛をベースにしたアクリル臭の無い太陽電池用フィルム - Google Patents
フルオロポリマーと酸化亜鉛をベースにしたアクリル臭の無い太陽電池用フィルム Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 37
- 229920002313 fluoropolymer Polymers 0.000 title claims abstract description 35
- 239000004811 fluoropolymer Substances 0.000 title claims abstract description 35
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 66
- 239000002245 particle Substances 0.000 claims abstract description 29
- 239000000945 filler Substances 0.000 claims abstract description 13
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 9
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 38
- 229920001577 copolymer Polymers 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 229920001519 homopolymer Polymers 0.000 claims description 10
- 239000002356 single layer Substances 0.000 claims description 8
- 230000007774 longterm Effects 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000010101 extrusion blow moulding Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 2
- 239000002210 silicon-based material Substances 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims 2
- 238000003825 pressing Methods 0.000 claims 1
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 11
- 239000011256 inorganic filler Substances 0.000 description 10
- 229910003475 inorganic filler Inorganic materials 0.000 description 10
- 239000004594 Masterbatch (MB) Substances 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 7
- 239000006096 absorbing agent Substances 0.000 description 6
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- -1 perfluoroalkyl vinyl ethers Chemical class 0.000 description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 4
- 239000004926 polymethyl methacrylate Substances 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- BLTXWCKMNMYXEA-UHFFFAOYSA-N 1,1,2-trifluoro-2-(trifluoromethoxy)ethene Chemical compound FC(F)=C(F)OC(F)(F)F BLTXWCKMNMYXEA-UHFFFAOYSA-N 0.000 description 2
- MIZLGWKEZAPEFJ-UHFFFAOYSA-N 1,1,2-trifluoroethene Chemical group FC=C(F)F MIZLGWKEZAPEFJ-UHFFFAOYSA-N 0.000 description 2
- YSYRISKCBOPJRG-UHFFFAOYSA-N 4,5-difluoro-2,2-bis(trifluoromethyl)-1,3-dioxole Chemical compound FC1=C(F)OC(C(F)(F)F)(C(F)(F)F)O1 YSYRISKCBOPJRG-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 2
- WFLOTYSKFUPZQB-OWOJBTEDSA-N (e)-1,2-difluoroethene Chemical group F\C=C\F WFLOTYSKFUPZQB-OWOJBTEDSA-N 0.000 description 1
- LGPPATCNSOSOQH-UHFFFAOYSA-N 1,1,2,3,4,4-hexafluorobuta-1,3-diene Chemical compound FC(F)=C(F)C(F)=C(F)F LGPPATCNSOSOQH-UHFFFAOYSA-N 0.000 description 1
- MSHXSYMNYJAOSS-UHFFFAOYSA-N 1,1-dichloro-2-fluoroethene Chemical group FC=C(Cl)Cl MSHXSYMNYJAOSS-UHFFFAOYSA-N 0.000 description 1
- ABADUMLIAZCWJD-UHFFFAOYSA-N 1,3-dioxole Chemical compound C1OC=CO1 ABADUMLIAZCWJD-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- FGEGZNORXGGFML-UHFFFAOYSA-N C(C)C=COF Chemical compound C(C)C=COF FGEGZNORXGGFML-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229920006370 Kynar Polymers 0.000 description 1
- 229920007450 Kynar® 710 Polymers 0.000 description 1
- 229920007457 Kynar® 720 Polymers 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920000995 Spectralon Polymers 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000004428 fluoroalkoxy group Chemical group 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- UGFMBZYKVQSQFX-UHFFFAOYSA-N para-methoxy-n-methylamphetamine Chemical compound CNC(C)CC1=CC=C(OC)C=C1 UGFMBZYKVQSQFX-UHFFFAOYSA-N 0.000 description 1
- FOKCKXCUQFKNLD-UHFFFAOYSA-N pent-1-enyl hypofluorite Chemical compound C(CC)C=COF FOKCKXCUQFKNLD-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229920005609 vinylidenefluoride/hexafluoropropylene copolymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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Abstract
【解決手段】本発明の組成物で充填剤は0.1〜10%、好ましくは0.5〜6%の重量比率で存在し、ZnO粒子は粒径が25〜40nm、好ましくは30〜35nmであり、この粒子は表面処理され、に関する。組成物はアクリルポリマーを含まない。
Description
本発明はさらに、上記組成物から製造されたフィルムに関するものである。本発明フィルムは可視領域で透明で、紫外線に対して不透明であるので、太陽電池のフロントシートとして利用される。
上記組成物に混和されるZnO粒子は粒径が25〜40nm、好ましくは30〜35nmであることを特徴とする。この特定のナノメートルサイズにすることよって、コンパウンディング段階および成形段階でポリマー体が溶融状態にあるときに、ポリマーに損傷を引き起こさずに、ポリマー中に粒子を十分に分散させることができる。ZnO粒子の表面は表面処理して化学的に不活性にするのが有利であり、それによってフルオロポリマーとの相溶性が高まり、均一で、経時的に安定な懸濁液が得られる。さらに、本発明組成物はアクリルポリマーを含まないので、成形中に不快臭が生成する危険はない。
本発明のさらに別の対象は、一変形例として300kg/時の流量で押出−ブロー成形段階を含むか、別の一変形例としてフラットシート押出成形段階を含む、いずれの操作も220〜240℃の温度で操作される本発明フィルムの製造方法にある。
本発明の利点は添付図面を参照した以下の説明からより良く理解できよう。
(1)フルオロポリマーが二フッ化ビニリデンのホモポリマーまたは二フッ化ビニリデンと少なくとも一種の他のフルオロモノマーとのコポリマーであり、
(2)ZnO粒子は粒径が25〜40nm、好ましくは30〜35nmであり、
(3)ZnO粒子は表面処理を有し、それによってZnO粒子は化学的に不活性になり、
(4)上記組成物はアクリルポリマーを含まない。
X1はHまたはFを表し、
X2およびX3はH、F、Cl、式CnFmHp-のフルオロアルキル基またはフルオロアルコキシ基CnFmHpO-を表し、nは1〜10の整数、mは1〜(2n+1)の整数であり、pは2n+1−mに等しい)
HFPはVDFと良く共重合し、優れた熱機械的特性を与えるので、コモノマーはHFPであるのが有利である。コポリマーはVDFとHFPのみを含むのが好ましい。
好ましい一実施例では、PVDFと粒径が30〜35nmのZnO粒子とから成り、この充填剤の重量含有率は0.5〜6%である。
(1)厚さ=10〜100μm、有利には15〜90μm、好ましくは20〜80μm(両限界値を含む)、
(2)密度=1.79〜1.86g/cm3(両限界値を含む)、
(3)単位面積当たりの重量=17.9〜186g/m2(両限界値を含む)、
(4)破断点伸び(%):
縦方向:50〜500%、
横方向:50〜500%、
(5)引張強度(MPa):
縦方向:30〜70MPa、
横方向:20〜60MPa、
(6)150℃のオーブンに30分間通した後の寸法変化(%):
縦方向:<1%、
横方向:<1%。
本発明フィルムは、第1実施例では240〜260℃の温度での管状(バブル)押出ブロー成形(インフレーションフィルム)によって製造する。この方法では熱可塑性ポリマーを環状ダイに通して一般に下から上に共押出する。押出物は延伸装置によって縦方向に通常はロールの形で延伸し、それと同時にダイと延伸装置と管壁との間に閉じ込められた一定容量の空気で膨張させる。この膨張管を一般にダイ出口で送風リングによって冷却する。
(1)220〜260℃、好ましくは240℃の温度で、溶融フルオロポリマー中にナノメートルZnOをカレンダ混練する、
(2)このブレンド物を(220〜230℃の温度で)ホットプレスし、最初に厚さが厚い(例えば150μmの厚さの)フィルムを作り、次いで、このフィルムを再プレスし、各種厚さの、例えば厚さが20〜80μmの最初より薄いフィルムにする。
(1)ナノフィラーによるPVDF中の「永久的」な可視透明性および紫外線不透明性、すなわち、有機紫外線吸収剤とは異なり、消費されることがなく、マイグレーションや浸出もなく、従って、長期間性能が維持される、
(2)透明性、耐薬品性、耐溶剤性、温度安定性および長期紫外線保護を組み合わせた単層フィルムを可能にする。
本発明の上記以外の特徴および利点は以下の実施例からより良く理解できよう。
カレンダで混練操作した後にフィルムをプレス
ブレンド物S1−A、C、D、Eを、1〜6%の「表面処理済みナノメートルZnO」(Zano20)を溶融カイナー740中に導入して、240℃の二本のカレンダで調製する。ブレンド物S1−Bは下記のようにして得る:20%の「表面処理済みナノメートルZnO」(Zano20)をカイナー740中に含むマスターバッチを同じ条件下に調製し、このマスターバッチをカイナー740を用いて5%濃度に希釈し、ブレンド物S1−Aと同じ最終組成が得られるようにする。冷却後、これらのブレンド物は全て白く見え、気泡を含まない。
ここで用いるカイナー740はPVDFホモポリマーである。
従って、これらのブレンド物にはプレスも光学的特性の分析もしない。
上記フィルムの吸光度および透過率を、積分球を備えたVarian社のCary 300分光光度計(角度8°)で測定した。積分球の入口にフィルム保持器を取り付け、サンプル反射口にはSpectralonを配置する。ベースラインを空のフィルム保持器で記録する。フィルムの紫外スペクトルを下記のパラメータによって得る:
(1)モジュールスペクトル
(2)範囲:200〜800nm
(3)速度:12nm/分
(4)ランプの交換:350nm
(5)モード:透過
(6)SBW:2.0nm
押出機で混練操作した後にフィルムを押出す
7.5%の「表面処理済みナノメートルZnO」(Zano20)をカイナー1000HD(PVDFホモポリマー)中に含むマスターバッチを下記条件下で、共回転二軸押出機(直径27mm、L/D=44)で調製した:原料は溶融領域へ供給、設定温度230℃、スクリュー速度250回転/分、流量20kg/時。白色で平滑なロッドが得られ、これを続いてペレット化する。顆粒は中心に収縮ボイドを示すことがあるが、微細分解気泡は含まない。
このマスターバッチを続いて、カイナー1000HDまたはカイナーフレックス3120-50に顆粒ドライブレンディングで混和し、それぞれブレンド物S2−A(カイナー1000HD)およびS2−B〜S2−F(カイナーフレックス3120-50)を作る。マスターバッチの混和度によって、[表2]に示すように、最終ブレンド物中の「表面処理済みナノメートルZnO」(Zano20)の濃度が定義される。カイナーフレックス3120-50はVDF−HFPコポリマーである。
次いで、これらのブレンド物の顆粒を管状インフレーションフィルム一軸押出機(スクリュー径30nm、L/D=25、ダイ径50mm、ギャップ1.2mm)で下記条件下に押し出す:温度250℃、延伸速度5.4m/分、BUR2.55。
Claims (15)
- 充填剤が組成物中に0.1〜10重量%、好ましくは0.5〜6重量%の重量比率で存在する、フルオロポリマーと酸化亜鉛(ZnO)とを含むポリマー組成物において、
フルオロポリマーが二フッ化ビニリデンのホモポリマーまたは二フッ化ビニリデンVDFと少なくとも一種の他のフルオロモノマーとのコポリマーであり、ZnO粒子が表面処理され、その粒径が25〜40nm、好ましくは30〜35nmであり、アクリルポリマーを含まないことを特徴とする組成物。 - ZnO粒子がシリコンベースの化合物で被覆されている請求項1に記載の組成物。
- フルオロポリマーがPVDFホモポリマーである請求項1または2に記載の組成物。
- フルオロコポリマーがVDFと少なくとも一種の他のフルオロモノマーとのコポリマーであり、少なくとも50重量%、有利には少なくとも75重量%、好ましくは少なくとも90重量%のVDFを含む請求項1または2に記載の組成物。
- 上記の他のフルオロモノマーがHFPである請求項4に記載の組成物。
- PVDFとZnOとを含み、ZnO粒子の粒径が30〜35nmで、充填剤の重量含有率が0.5〜6%である請求項1〜5のいずれか一項に記載の組成物。
- 紫外線に対して不透明で、可視領域で透明で且つ長期安定性を有する請求項1〜6のいずれか一項に記載の組成物から成る単層フィルム。
- 厚さが10〜100μm、有利には15〜90μm、好ましくは20〜80μmである請求項7に記載のフィルム。
- フロントシートおよび/またはバックシートが請求項7または8に記載のフィルムから成る太陽電池パネル。
- 太陽電池パネル内のフロントシートの製造での請求項7または8に記載のフィルムの使用。
- 太陽電池パネル内のバックシートの製造での請求項7または8に記載のフィルムの使用。
- 充填剤をフルオロポリマーに溶融経路で混和する段階を含む、紫外線に対して不透明で、可視領域で透明なフィルムを製造するための請求項1〜6のいずれか一項に記載の組成物の製造方法。
- 240〜260℃の温度で押出−ブロー成形する請求項7または8に記載の単層フィルムの製造方法。
- 240〜260℃の温度でフラットシート押出成形する請求項7または8に記載の単層フィルムの製造方法。
- 下記(1)および(2)の段階を有する請求項7または8に記載の単層フィルムの製造方法:
(1)220〜260℃、好ましくは240℃の温度で、溶融フルオロポリマー中にナノメートルZnOをカレンダ混練する、
(2)得られたブレンド物を220〜230℃の温度でホットプレスし、最初に厚さが150μmのフィルムを作り、次いで、このフィルムを再プレスして厚さが10〜100μmのフィルムにする。
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WO2017115812A1 (ja) * | 2015-12-28 | 2017-07-06 | 旭硝子株式会社 | フルオロエラストマー組成物および架橋物の製造方法 |
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JP7042377B1 (ja) * | 2021-03-31 | 2022-03-25 | 大日精化工業株式会社 | フッ素樹脂用マスターバッチ、その製造方法、フッ素樹脂組成物、及び成形体 |
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FR2948943A1 (fr) | 2011-02-11 |
US20130053498A1 (en) | 2013-02-28 |
CN102977525A (zh) | 2013-03-20 |
EP2462185A1 (fr) | 2012-06-13 |
CN102575030A (zh) | 2012-07-11 |
FR2948943B1 (fr) | 2012-03-16 |
US20120186636A1 (en) | 2012-07-26 |
KR20120125992A (ko) | 2012-11-19 |
TW201129578A (en) | 2011-09-01 |
KR20120089264A (ko) | 2012-08-09 |
TWI461438B (zh) | 2014-11-21 |
WO2011015785A1 (fr) | 2011-02-10 |
EP2719718A1 (fr) | 2014-04-16 |
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