JP2020523448A - 熱伝導度が向上したポリイミドフィルム及びその製造方法 - Google Patents
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Abstract
Description
[数式1]
熱伝導度(k)=比熱(C)×密度(ρ)×熱拡散度(α)
前記式において、C、ρ及びαは、それぞれポリイミドフィルムの比熱(J/g・K)、密度(g/cm3)及び熱拡散度(mm2/sec)を示す。
[化学式1]
[数式1]
熱伝導度(k)=C×ρ×α
前記数式1において、C、ρ及びαは、それぞれポリイミドフィルムの比熱(J/g・K)、密度(g/cm3)及び熱拡散度(mm2/sec)を示す。
[化学式1]
窒素気流が流れる攪拌機内に有機溶媒NMP(N−メチル−2−ピロリドン)80gを満たした後、反応器の温度を25℃に保持した状態でアニリン18.99g(0.204mol)を溶解させた。前記アニリン溶液に3,3',4,4'−ビフェニルカルボン酸二無水物(s−BPDA)30.0g(0.102mol)とNMP 93.7gとを同じ温度で添加して、一定時間溶解しながら撹拌した後、化学式3の化合物を合成した。
[化学式3]
窒素気流が流れる攪拌機内に有機溶媒NMP(N−メチル−2−ピロリドン)100gを満たした後、反応器の温度を25℃に保持した状態でパラフェニレンジアミン(p−PDA)6.192g(57.259mmol)を溶解させた。前記p−PDA溶液に3,3',4,4'−ビフェニルカルボン酸二無水物(s−BPDA)16.661g(56.629mmol)とNMP 56.96gとを同じ温度で添加して、一定時間溶解しながら撹拌した後、ポリアミド酸を重合した。
化学式4の化合物を使用したことを除いては、実施例1と同様に厚さ10μmであるポリイミドフィルムを製造した。
窒素気流が流れる攪拌機内に有機溶媒NMP(N−メチル−2−ピロリドン)100gを満たした後、反応器の温度を25℃に保持した状態でパラフェニレンジアミン(p−PDA)6.243g(57.726mmol)を溶解させた。前記p−PDA溶液に3,3',4,4'−ビフェニルカルボン酸二無水物(s−BPDA)16.797g(57.091mmol)とNMP 56.96gとを同じ温度で添加して、一定時間溶解しながら撹拌した後、ポリイミド前駆体を製造した。
前記製造されたそれぞれのポリイミドフィルムに対して、下記のような方法で、熱分解温度(Td 1%)、透過度、熱拡散度及び熱伝導度を測定して、表1に示した。
TA instruments社のDiscovery TGAを用いて窒素雰囲気、30〜00℃の区間でTGA評価進行、初期重量(100%)で1%の重量損失が発生した温度を示す。
◎:Td 1% 565℃以上
○:Td 1% 545〜564℃
X:Td 1% 545℃以下
透過度は、JIS K 7105に基づいて透過率計(モデル8453 UV−visible Spectrophotometer、Agilent Technologies製造)で380〜780nmの波長に対する透過率の平均を測定した。
◎:60%以上
○:50〜60%
X:50%以下
ポリイミドフィルムの比熱(J/g・K)は、DSC法で測定し、密度(g/cm3)は、アルキメデス法で測定した。
図4に示されたNETZSCH社のLFA 467装置を使用して熱拡散度を測定した。サンプルは、フィルムを10mm×12.7mmサイズの四角形に切り、図5に示したように、サンプルの両側面に金を250〜500nmの厚さに蒸着して準備した。
下記数式1によって熱伝導度を求めた。
[数式1]
熱伝導度(k)=比熱(C)×密度(ρ)×熱拡散度(α)
実施例1と比較例とで製造したポリイミドフィルムに対して、Td 1%、透過度、熱拡散度、密度、比重及び熱伝導度の測定結果を表1に示した。
Claims (12)
- イミド単分子化合物を有機フィラーとして含み、下記数式1によって定義される熱伝導度(k)が0.2W/m・K以上であるポリイミドフィルム:
[数式1]
熱伝導度(k)=比熱(C)×密度(ρ)×熱拡散度(α)
前記数式1において、C、ρ及びαは、それぞれポリイミドフィルムの比熱(J/g・K)、密度(g/cm3)及び熱拡散度(mm2/sec)を示す。 - 前記ポリイミドフィルムは、3,3',4,4'−ビフェニルカルボン酸二無水物(s−BPDA)及び4,4'−パラフェニレンジアミン(pPDA)を重合成分とする請求項1に記載のポリイミドフィルム。
- 前記3,3',4,4'−ビフェニルカルボン酸二無水物(s−BPDA)及び4,4'−パラフェニレンジアミン(pPDA)のmol比が、0.98:1〜0.99:1である請求項3に記載のポリイミドフィルム。
- 前記ポリイミドフィルムは、10μmの厚さで測定した比熱1.5J/g・K以上、密度1.5g/cm3以上、熱拡散度が0.07mm2/sec以上である請求項1から5のいずれか一項に記載のポリイミドフィルム。
- 重合溶媒に4,4'−パラフェニレンジアミン(pPDA)1molに対して3,3',4,4'−ビフェニルカルボン酸二無水物(s−BPDA)を1mol未満に含む重合成分を添加してポリイミド前駆体を製造する段階と、
前記ポリイミド前駆体溶液にイミド単分子化合物を有機フィラーとして添加する段階と、
前記ポリイミド前駆体溶液を基板上に塗布する段階と、
前記塗布されたポリイミド前駆体溶液を乾燥及び加熱する段階と、
を含むポリイミドフィルムの製造方法。 - 前記イミド単分子化合物を前駆体溶液総重量を基準に0.1〜10重量%に含む請求項7から9のいずれか一項に記載のポリイミドフィルムの製造方法。
- 前記ポリイミド前駆体溶液の乾燥及び加熱を通じる硬化工程において、
最終硬化温度が450℃以上である請求項7から10のいずれか一項に記載のポリイミドフィルムの製造方法。 - 請求項1から請求項6のうち何れか一項に記載のポリイミドフィルムを基板として含むフレキシブルディスプレイ素子。
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CN110753721A (zh) | 2020-02-04 |
US11649354B2 (en) | 2023-05-16 |
EP3620483A1 (en) | 2020-03-11 |
US20210147679A1 (en) | 2021-05-20 |
TWI791748B (zh) | 2023-02-11 |
KR102338871B1 (ko) | 2021-12-13 |
JP6938838B2 (ja) | 2021-09-22 |
KR20190098042A (ko) | 2019-08-21 |
CN110753721B (zh) | 2022-08-16 |
EP3620483A4 (en) | 2020-06-24 |
TW201945445A (zh) | 2019-12-01 |
EP3620483B1 (en) | 2022-09-28 |
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