JP5967782B2 - 黒色複合微粒子、黒色樹脂組成物、カラーフィルター基板および液晶表示装置 - Google Patents
黒色複合微粒子、黒色樹脂組成物、カラーフィルター基板および液晶表示装置 Download PDFInfo
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- JP5967782B2 JP5967782B2 JP2015133218A JP2015133218A JP5967782B2 JP 5967782 B2 JP5967782 B2 JP 5967782B2 JP 2015133218 A JP2015133218 A JP 2015133218A JP 2015133218 A JP2015133218 A JP 2015133218A JP 5967782 B2 JP5967782 B2 JP 5967782B2
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- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Description
(式中、Xは銅、銀、金、白金、パラジウム及び錫並びにこれらの2種以上の金属の合金から選ばれる少なくとも一種の金属原子、xは0より大きく2未満の数、yは0以上2未満の数、zは0より大きく10未満の数を表す)
で表される黒色複合微粒子であって、チタン窒化物粒子と金属微粒子Xが複合化している黒色複合微粒子(但し、コア/シェル型ナノ粒子を除く)。
(2) 前記黒色複合微粒子の酸素含有量が10質量%未満である(1)記載の黒色複合微粒子。
(3) 前記Xが銀である(1)または(2)記載の黒色複合微粒子。
(4) 前記黒色複合微粒子における銀の含有量が、黒色複合微粒子の全質量に対して5質量%以上50質量%以下である(1)〜(3)のいずれかに記載の黒色複合微粒子。
(5) BET法により測定される比表面積が5m2/g以上100m2/g以下である(1)〜(4)のいずれかに記載の黒色複合微粒子。
(6) 前記黒色複合微粒子は、TiとXが気相状態で混合・凝縮される工程を経て製造されたものである(1)〜(5)のいずれかに記載の黒色複合微粒子。
(7) 前記黒色複合微粒子が、窒素含有ガスをプラズマガスとして用いる熱プラズマにTi粉末とX金属粉末を供することにより製造されたものである(6)記載の黒色複合微粒子。
「金属光沢をもち,電気と熱をよく導き,固体状態では展性,延性に富む物質.水銀以外は室温ですべて固体である.ふつう種々の機械的加工を施すことができる.液化しても光学的・電気的性質は保たれることが多い.単体の金属結晶の大部分は面心立方,六方最密,体心立方のいずれかの構造をとり,通常は微結晶の集合体をなす.結晶中の原子は*金属結合によって結ばれ,電子の一部は自由電子として存在する.金属の性質は金属結合に由来する.単体アンチモン,ビスマスなど自由電子の数が少ない金属を*半金属とよぶ.単体に限らず2種以上の金属元素,または金属元素とある種の非金属元素(ホウ素,炭素など)を含む相にも金属性を示すものがある.なお,金属の電気伝導は温度の上昇とともに減少するが,非金属では増加するので,このことから両者を明確に区別することができる.」
この複合微粒子を遮光材として用いることにより、本発明の樹脂ブラックマトリクスは、黒色樹脂組成中の遮光材濃度を低く保ったまま、高いOD値を達成することが可能となる。その結果、本発明の樹脂ブラックマトリクスは、高密着性を確保することができる。また、本発明の樹脂ブラックマトリクスは、膜厚当たりのOD値が高いため、実用的なOD値(4.0)で膜厚は0.8μm以下となる。その結果、樹脂ブラックマトリクスを用いた場合でも、保護膜無しで平坦性に実用上の問題のないカラーフィルターを得ることができるようになった。
ここで、I0;入射光強度、I;透過光強度となる。
「比表面積」
顔料の比表面積は、日本ベル(株)製高精度全自動ガス吸着装置(“BELSORP”36)を用い、100℃で真空脱気後、N2ガスの液体窒素温度(77K)における吸着等温線を測定し、この等温線をBET法で解析し比表面積を求めた。
チタン原子および銀原子の含有量はICP発光分光分析法(セイコーインスツルメンツ社製 ICP発光分光分析装置SPS3000)により測定した。
X線回折は粉末試料をアルミ製標準試料ホルダーに詰め、広角X線回折法(理学電機社製 RU−200R)により測定した。測定条件としては、X線源はCuKα線とし、出力は50kV/200mA、スリット系は1°−1°−0.15mm−0.45mm、測定ステップ(2θ)は0.02°、スキャン速度は2°/分とした。
無アルカリガラス上に膜厚1.0μm或いは0.8μmの樹脂ブラックマトリクスを形成させ、顕微分光器(大塚電子製MCPD2000)を用いて上述の式(8)より求めた。
無アルカリガラス上に膜厚1.0μmの樹脂ブラックマトリクスを形成させ、顕微分光器(大塚電子製MCPD2000)を用いて測定した。この際、リファレンスガラスとしてBK7を用いて測定を行い、絶対反射率を求めた。
TEM 日本電子製JEM−2010F型 電界放射型透過電子顕微鏡を加速電圧200KVにて観察した。またEDSにはノーラン製UTW型Si(Li)半導体検出器(ビーム径1nm、マッピングピクセルサイズ約2.5nm)を用い、元素マッピングを行なった。
上記実施形態に係る黒色複合微粒子の製造方法により、TiとAgから構成される黒色複合微粒子を製造した。なお、ここでは、黒色複合微粒子材料となるTi粒子並びにAg粒子が、熱プラズマ炎中で容易に蒸発するように、Ti粒子は平均粒子径25μm、Ag粒子は平均粒子径5μmの粉末材料を使用した。
ここで、プラズマトーチ12の高周波発振用コイル12bには、約4MHz、約80kVAの高周波電圧を印加し、プラズマガス供給源22からはプラズマガスとしてアルゴンガス50リットル/min、窒素50リットル/minの混合ガスを供給し、プラズマトーチ12内にアルゴン−窒素熱プラズマ炎を発生させた。また、材料供給装置140の噴霧ガス供給源からは10リットル/minのキャリアガスを供給した。
製造例1と同様にして、所定の混合比率で予備混合されたTiとAgの混合粉末を原料として黒色複合微粒子Bk2を得た。黒色複合微粒子Bk2のBET比表面積は30.7m2/gであった。また組成分析を行ったところ、チタン含有量は65.4質量%、窒素含有量は17.7質量%、酸素含有量は5.9質量%、銀含有量は10.5質量%であり、TiN(200)面に由来するピークの回折角2θは42.57°、このピークの半値幅より求めた結晶子サイズは35nm、であった。また、TiO2に起因するX線回折ピークが若干見られた。
製造例1と同様にして、所定の混合比率で予備混合されたTiとAgの混合粉末を原料として黒色複合微粒子Bk3を得た。黒色複合微粒子Bk3のBET比表面積は28.8m2/gであった。また組成分析を行ったところ、チタン含有量は59.8質量%、窒素含有量は17.0質量%、酸素含有量は3.8質量%、銀含有量は18.9質量%であり、TiN(200)面に由来するピークの回折角2θは42.56°、このピークの半値幅より求めた結晶子サイズは37nm、であった。また、TiO2に起因するX線回折ピークは全く見られなかった。
製造例1と同様にして、所定の混合比率で予備混合されたTiとAgの混合粉末を原料として黒色複合微粒子Bk4を得た。黒色複合微粒子Bk4のBET比表面積は23.5m2/gであった。また組成分析を行ったところ、チタン含有量は48.9質量%、窒素含有量は13.6質量%、酸素含有量は3.7質量%、銀含有量は33.5質量%であり、TiN(200)面に由来するピークの回折角2θは42.58°、このピークの半値幅より求めた結晶子サイズは48nm、であった。また、TiO2に起因するX線回折ピークは全く見られなかった。
製造例1と同様にして、所定の混合比率で予備混合されたTiとPdの混合粉末を原料として黒色複合微粒子Bk5を得た。黒色複合微粒子Bk5のBET比表面積は26.9m2/gであった。また組成分析を行ったところ、チタン含有量は61.7質量%、窒素含有量は16.6質量%、酸素含有量は3.8質量%、パラジウム含有量は16.2質量%であり、TiN(200)面に由来するピークの回折角2θは42.58°、このピークの半値幅より求めた結晶子サイズは46nm、であった。また、TiO2に起因するX線回折ピークは全く見られなかった
製造例1と同様にして、所定の混合比率で予備混合されたTiとNiの混合粉末を原料として黒色複合微粒子Bk6を得た。黒色複合微粒子Bk6のBET比表面積は31.5m2/gであった。また組成分析を行ったところ、チタン含有量は66.0質量%、窒素含有量は18.2質量%、酸素含有量は4.4質量%、ニッケル含有量は10.4質量%であり、TiN(200)面に由来するピークの回折角2θは42.56°、このピークの半値幅より求めた結晶子サイズは45nm、であった。また、TiO2に起因するX線回折ピークは全く見られなかった。
製造例1と同様にして、Ti粉末を原料としてチタン窒化物微粒子Bk7を得た。チタン窒化物微粒子Bk7のBET比表面積は36.0m2/gであった。また組成分析を行ったところ、チタン含有量は72.2質量%、窒素含有量は19.4質量%、酸素含有量は6.4質量%であり、TiN(200)面に由来するピークの回折角2θは42.62°、このピークの半値幅より求めた結晶子サイズは29nmであった。また、TiO2に起因するX線回折ピークは全く見られなかった。
特許文献7の製造方法と同様にして、銀微粒子Bk8を得た。銀微粒子Bk8のBET比表面積は9.6m2/gであった。
4,4′−ジアミノフェニルエーテル(0.30モル当量)、パラフェニレンジアミン(0.65モル当量)、ビス(3−アミノプロピル)テトラメチルジシロキサン(0.05モル当量)をγ−ブチロラクトン850g、N−メチル−2−ピロリドン850gと共に仕込み、3,3′,4,4′−オキシジフタルカルボン酸二無水物(0.9975モル当量)を添加し、80℃で3時間反応させた。無水マレイン酸(0.02モル当量)を添加し、更に80℃で1時間反応させ、ポリアミック酸A−1(ポリマー濃度20質量%)溶液を得た。
黒色複合微粒子Bk1(96g)にポリアミック酸溶液A−1(120g)、γ−ブチロラクトン(114g)、N−メチル−2ピロリドン(538g)、3メチル−3メトキシブチルアセテート(132g)をタンクに仕込み、ホモミキサー(特殊機化製)で1時間撹拌し、予備分散液1を得た。その後、0.05mmφジルコニアビーズ(ニッカトー製、YTZボール)を70%充填した遠心分離セパレーターを具備したウルトラアペックスミル(寿工業製)に予備分散液1を供給し、回転速度8m/sで2時間分散を行い、固形分濃度12質量%、顔料/樹脂(質量比)=80/20の顔料分散液1を得た。
使用する遮光材として黒色複合微粒子Bk1の代わりに黒色複合微粒子Bk2を用いた以外は実施例1と同様にして、顔料分散液2および黒色樹脂組成物2を得た。また、黒色樹脂組成物2を用いて実施例1と同様にブラックマトリクス2を作成した。
使用する遮光材として黒色複合微粒子Bk1の代わりに黒色複合微粒子Bk3を用いた以外は実施例1と同様にして、顔料分散液3および黒色樹脂組成物3を得た。また、黒色樹脂組成物3を用いて実施例1と同様にブラックマトリクス3を作成した。
使用する遮光材として黒色複合微粒子Bk1の代わりに黒色複合微粒子Bk4を用いた以外は実施例1と同様にして、顔料分散液4および黒色樹脂組成物4を得た。また、黒色樹脂組成物4を用いて実施例1と同様にブラックマトリクス4を作成した。
使用する遮光材として黒色複合微粒子Bk1の代わりに黒色複合微粒子Bk5を用いた以外は実施例1と同様にして、顔料分散液5および黒色樹脂組成物5を得た。また、黒色樹脂組成物5を用いて実施例1と同様にブラックマトリクス5を作成した。
使用する遮光材として黒色複合微粒子Bk1の代わりに黒色複合微粒子Bk6を用いた以外は実施例1と同様にして、顔料分散液6および黒色樹脂組成物6を得た。また、黒色樹脂組成物6を用いて実施例1と同様にブラックマトリクス6を作成した。
使用する遮光材として黒色複合微粒子Bk1の代わりにチタン窒化物粒子Bk7を用いた以外は実施例1と同様にして、顔料分散液7および黒色樹脂組成物7を得た。また、黒色樹脂組成物7を用いて実施例1と同様にブラックマトリクス7を作成した。
使用する遮光材として黒色複合微粒子Bk1の代わりに銀微粒子Bk8を用いた以外は実施例1と同様にして、顔料分散液8および黒色樹脂組成物8を得た。また、黒色樹脂組成物8を用いて塗膜厚さが0.5μmとなるようにした以外は実施例1と同様にブラックマトリクス8を作成した。
黒色樹脂組成物7と黒色樹脂組成物8を質量比で90:10となるように混合し、黒色樹脂組成物9を得た。黒色樹脂組成物9を用いて実施例1と同様にブラックマトリクス9を作成した。
黒色樹脂組成物7と黒色樹脂組成物8を質量比で80:20となるように混合し、黒色樹脂組成物10を得た。黒色樹脂組成物10を用いて実施例1と同様にブラックマトリクス10を作成した。
N(r)=r−D
着色樹脂組成物の作製
緑顔料(Pigment Green 36);44g、黄顔料(Pigment Yellow 138);19g、ポリアミック酸A−2;47g、γ−ブチロラクトン;890gをタンクに仕込み、ホモミキサー(特殊機化製)で1時間撹拌し、G顔料予備分散液G1を得た。その後、0.40mmφジルコニアビーズ(東レ(株)製、トレセラムビーズ)を85%充填したダイノーミルKDL(シンマルエンタープライゼス製)に予備分散液G1を供給し、回転速度11m/sで3時間分散を行い、固形分濃度7質量%、顔料/ポリマー(質量比)=90/10のG分散液G1を得た。G分散液G1をポリアミック酸A−2および溶媒で希釈し、緑色樹脂組成物を得た。
得られたカラーフィルター1を中性洗剤で洗浄した後、ポリイミド樹脂からなる配向膜を印刷法により塗布し、ホットプレートで250℃の温度で10分間加熱した。膜厚は0.07μmであった。この後、カラーフィルター基板をラビング処理し、シール剤をディスペンス法により塗布、ホットプレートで90℃、10分間加熱した。一方、ガラス上にTFTアレイを形成した基板も同様に洗浄した後、配向膜を塗布し、加熱した。その後、直径5.5μmの球状スペーサーを散布し、シール剤を塗布したカラーフィルター基板と重ね合わせ、オーブン中で加圧しながら160℃の温度で90分間加熱して、シール剤を硬化させた。このセルを120℃の温度、13.3Paの圧力下で4時間放置し、続いて、窒素中で0.5時間放置した後に、再度真空下において液晶注入を行った。液晶注入は、セルをチャンバに入れて、室温で13.3Paの圧力まで減圧した後、液晶注入口を液晶に漬けて、窒素を用いて常圧に戻すことにより行った。液晶注入後、紫外線硬化樹脂により、液晶注入口を封口した。次に、偏光板をセルの2枚のガラス基板の外側に貼り付け、セルを完成させた。さらに、得られたセルをモジュール化して、液晶表示装置1を完成させた。得られた液晶表示装置1を観察した結果、表示不良はないことがわかった。また、樹脂ブラックマトリクスの遮光性が高いため、コントラストが良好であった。また、同様にして、100台の液晶表示装置を作製したが、樹脂ブラックマトリクスの密着性が高いため、液晶注入時にシール部が、剥がれるなどの不良はまったく発生しなかった。
12 プラズマトーチ
12a 石英管
12b 高周波発振用コイル
12c プラズマガス供給口
15 複合微粒子
16 チャンバ
17 天板
17a 内側部天板部品
17b 外側部天板部品
17c 上部外側部天板部品
17d 通気路
18 分級後複合微粒子
19 サイクロン
19a 入口管
19b 外筒
19c 円錐部
19d 粗大粒子回収チャンバ
19e 内管
20 回収部
20a 回収室
20b バグフィルター
20c 管
22 プラズマガス供給源
24 熱プラズマ炎
26 管
28 気体供給装置
28a 気体射出口
28b 気体射出口
28c コンプレッサ
28d 気体供給源
28e 管
140 複合微粒子原料供給装置
140a 供給管
142 貯蔵槽
144 予備混合済複合微粒子原料
146 攪拌軸
148 攪拌羽根
150a、150b オイルシール
152a、152b 軸受け
154a、154b モータ
160 スクリューフィーダ
162 スクリュー
164 軸
166 ケーシング
170 分散部
172 外管
174 粉体分散室
176 回転ブラシ
178 気体供給口
180 気体通路
182 搬送管
Claims (7)
- 組成式:TiNxOy・zX
(式中、Xは銅、銀、金、白金、パラジウム及び錫並びにこれらの2種以上の金属の合金から選ばれる少なくとも一種の金属原子、xは0より大きく2未満の数、yは0以上2未満の数、zは0より大きく10未満の数を表す)
で表される黒色複合微粒子であって、チタン窒化物粒子と金属微粒子Xが複合化している黒色複合微粒子(但し、コア/シェル型ナノ粒子を除く)。 - 前記黒色複合微粒子の酸素含有量が10質量%以下である請求項1記載の黒色複合微粒子。
- 前記Xが銀である請求項1または2記載の黒色複合微粒子。
- 前記黒色複合微粒子における銀の含有量が、黒色複合微粒子の全質量に対して5質量%以上50質量%以下である請求項1〜3のいずれか1項に記載の黒色複合微粒子。
- BET法により測定される比表面積が5m2/g以上100m2/g以下である請求項1〜4のいずれか1項に記載の黒色複合微粒子。
- 前記黒色複合微粒子は、TiとXが気相状態で混合・凝縮される工程を経て製造されたものである請求項1〜5のいずれか1項に記載の黒色複合微粒子。
- 前記黒色複合微粒子が、窒素含有ガスをプラズマガスとして用いる熱プラズマにTi粉末とX金属粉末を供することにより製造されたものである請求項6記載の黒色複合微粒子。
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JP5136139B2 (ja) | 2007-03-20 | 2013-02-06 | 東レ株式会社 | 樹脂ブラックマトリクス用黒色樹脂組成物、樹脂ブラックマトリクス、カラーフィルターおよび液晶表示装置 |
JP4915664B2 (ja) | 2007-04-17 | 2012-04-11 | 三菱マテリアル株式会社 | 高抵抗黒色粉末およびその分散液、塗料、黒色膜 |
JP2009058946A (ja) * | 2007-08-03 | 2009-03-19 | Toray Ind Inc | 黒色樹脂組成物、樹脂ブラックマトリクス、カラーフィルターおよび液晶表示装置 |
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CN102459084B (zh) | 2015-03-18 |
EP2444376A1 (en) | 2012-04-25 |
WO2010147098A1 (ja) | 2010-12-23 |
TW201114849A (en) | 2011-05-01 |
JPWO2010147098A1 (ja) | 2012-12-06 |
JP2015227282A (ja) | 2015-12-17 |
TWI483999B (zh) | 2015-05-11 |
KR20120030068A (ko) | 2012-03-27 |
JP5875179B2 (ja) | 2016-03-02 |
EP2444376B1 (en) | 2017-01-25 |
CN102459084A (zh) | 2012-05-16 |
SG176863A1 (en) | 2012-02-28 |
US20120128898A1 (en) | 2012-05-24 |
EP2444376A4 (en) | 2015-08-12 |
KR101833352B1 (ko) | 2018-02-28 |
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