JP2016528316A - 高い色濃度を有する透明な電気的半導体性干渉顔料 - Google Patents
高い色濃度を有する透明な電気的半導体性干渉顔料 Download PDFInfo
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- JP2016528316A JP2016528316A JP2016520303A JP2016520303A JP2016528316A JP 2016528316 A JP2016528316 A JP 2016528316A JP 2016520303 A JP2016520303 A JP 2016520303A JP 2016520303 A JP2016520303 A JP 2016520303A JP 2016528316 A JP2016528316 A JP 2016528316A
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Classifications
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C09C1/0027—One layer consisting of at least one sub-stoichiometric inorganic compound
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
Description
T=(L*45/90/白色−L*45/90/黒色)/100
(Hofmeister法による隠蔽力HPの決定(Colorimetric evaluation of pearlescent pigments、「Mondial Coleur 85」 congress、Monte carlo、1985、式HP=100/(L*45/90/白色−L*45/90/黒色)に従う))。
ρ=R・π・(d/2)2/L(オーム・cm)
第1の最も単純な実施形態において、本発明による透明なフレーク状干渉顔料は、上述の寸法のフレーク状TiO2−x粒子(式中、0.001≦x<0.05である)からなる。ここで、TiO2−xは、アナターゼ変態およびルチル変態の両方であり得る。そのような顔料の調製のための出発材料は、市販されているフレーク状のTiO2顔料である。この種類のTiO2フレークはまた、WO93/08237に記載の方法に従い生成できる。しかしながら、この方法と同様にして調製されるTiO2顔料は、溶解したまたは溶解していない着色剤を含むべきではない。それらは、ベルトプロセスにおいて、対応する好ましくは無機の前駆体材料から生成され、前駆体は、ベルトに塗布され、酸を使用して酸化形態または酸化物水和物に変換され、固化され、その後ベルトから取り出される。得られた顔料は、乾燥形態で、または空気中における高温での焼成後に、使用される。フレークの幾何学的層厚は、前駆体層の塗布速度または湿潤層厚により調節され、これは非常に正確にできる。本発明によるTiO2からTiO2−xへの変換は、以下に説明される。
T≦550℃、好ましくは≦500℃:還元ガスの割合:5〜10体積%、特に5〜8体積%、
T≦650℃、好ましくは≦600℃:還元ガスの割合:2〜5体積%、
T≦750℃、好ましくは≦700℃:還元ガスの割合:1〜2体積%、
T≦800℃、還元ガスの割合:0.05〜1体積%。
粉砕および分類された雲母(10〜50μm、d9025μm)を、1900mlの脱塩水中に懸濁させる。0.75gの濃HClおよび2.2gのSnCl4の水溶液100mlを、75℃で撹拌しながら、酸性媒体中の懸濁液に徐々に添加する。水酸化ナトリウム溶液の同時添加により、pHを一定に維持する。その後、混合物を75℃でさらに30分間撹拌し、次いで、32%の水酸化ナトリウム溶液を使用してpHを一定に維持しながら、TiCl4水溶液(400g/lのTiCl4)を徐々に添加することにより、pH1.6でTiO2でコーティングする。以下の色の終点に達したら、コーティングを停止する。
実施例1:金
実施例2:赤
実施例3:青
その後、反応混合物を撹拌しながら室温に冷却し、中和する。得られた顔料を吸引フィルタで濾過し、水で洗浄し、140℃で乾燥させる。
実施例4:
光学的に不活性なSiO2中間層を有する顔料の調製:
粉砕および分類された雲母(10〜50μm、d90 25μm)100gを、1900mlの脱塩水中に懸濁させる。0.75gの濃HClおよび2.2gのSnCl4の水溶液100mlを、75℃で撹拌しながら、酸性媒体中の懸濁液に徐々に添加する。水酸化ナトリウム溶液の同時添加により、pHを一定に維持する。その後、混合物を75℃でさらに30分間撹拌し、次いで、32%の水酸化ナトリウム溶液を使用してpHを一定に維持しながら、TiCl4水溶液(400g/lのTiCl4)を徐々に添加することにより、pH1.6でTiO2でコーティングする。二次緑色終点において添加を停止し、混合物をさらに30分間撹拌し、水酸化ナトリウム溶液を使用してpHを7.5に調節する。
コーティングフィルムにおける電気的特性の試験:
表1に従う熱処理後に得られた顔料を、NCラッカー(溶媒混合物中12%のコロジウム/ブチルアクリレート)中に分散させる。PETフィルムをコーティング調合液でコーティングする。乾燥コーティング層中の顔料の濃度は、48.1重量%であり、コーティング層の層厚は、50μmである。コーティング層の乾燥後、スプリングタン(spring−tongue)電極(電極間隔1cm、長さ10cm)を利用して、1000Vの測定電圧で表面抵抗を測定する。結果を表2に示す。導電性顔料を有さない比較コーティングフィルムは、1012オームを超える比抵抗を示す。
実施例25:
色特性の試験:
表1に従う顔料の試料を、実施例24に従いNCラッカー中に分散させる(ラッカー中1.7重量%の顔料)。次いで、500μmの湿潤層厚でラッカーを黒色/白色の厚紙に塗布し、乾燥させる。乾燥した層は、40μmの厚さおよび12.3%の顔料質量濃度(PMC)を有する。次いで、分光光度計(Steag Optik製ETA−Optik)を使用して、以下の角度で反射に関してカードを測定する。
黒色および白色上で45°/90°、および黒色上で75°/95°、90°の角度は、カードの平面に対し垂直を表す。
暗い質感色を有する強還元顔料:
実施例3からの顔料(青色)を、フォーミングガス(5%のH2)下で900℃で45分間焼成すると、暗い紫色の質感色を有する顔料が得られる。顔料の塗料フィルムおよび塗料カードを作製し、実施例24および25に従い測定する。フィルムの抵抗は9.8Mオームであり、白色上のL*値は32である。低いL*値は、顔料の濃い質感色および高い隠蔽力を示す。塗料フィルムの電気抵抗は、本発明による透明干渉顔料を含む塗料フィルムの抵抗よりも、ごく僅かに低い。帯電防止散逸性コーティングのためには、全ての抵抗が十分に低い。
実施例27:
顔料の酸素欠乏度の決定:
顔料試料の質量の変化を、示差熱分析を利用して決定するが、顔料試料は、秤の上で、室温から1000℃まで空気下で10℃/分で加熱される。顔料は、300℃まで、その残留水分を失う。400℃からは、再酸化により、減少した顔料の質量が増加する。酸素欠乏度は、400℃からの質量の増加から計算される。
実施例7(比較) 増加:−0.1%
実施例11(本発明) 増加:0.3%
実施例16(本発明) 増加:0.12%
実施例26(比較) 増加:0.66%
顔料は、約48重量%のTiO2−xを含む。TiO2−x含量に基づいて、重量の増加は、実施例11において0.625%、実施例16において0.25%、実施例26において1.33%である。これにより、以下の組成物が導かれる。
実施例7:TiO2
実施例11:TiO1.96
実施例16:TiO1.98
実施例26:TiO1.93
Claims (20)
- TiO2−x(式中、0.001≦x<0.05である)の層を備える、透明な電気的半導体性フレーク状干渉顔料。
- 前記TiO2−xの層が、透明なフレーク状担体上に位置することを特徴とする、請求項1に記載の干渉顔料。
- 前記フレーク状担体が、天然もしくは合成雲母フレーク、カオリン、絹雲母もしくはタルクフレーク、ガラスフレーク、ホウケイ酸塩フレーク、Al2O3フレークまたはそれらの2種以上の混合物であることを特徴とする、請求項1または2に記載の干渉顔料。
- 前記フレーク状担体、および該担体を包囲するTiO2−xの層からなることを特徴とする、請求項1から3のいずれか一項または複数項に記載の干渉顔料。
- 前記TiO2−xの層が、2つまたは3つの部分層からなり、該部分層は、それぞれの場合において、屈折率n(n<1.8である)を有する透明材料を含む中間層により互いに分離され、該中間層は、それぞれの場合において、15nm以下の幾何学的層厚dを有し、
系が2つの部分層および1つの中間層を備えまたは3つの部分層および2つの中間層を備える場合に、外側最終のTiO2−xの部分層を有する系が、フレーク状担体上に形成されていることを特徴とする、請求項1から3のいずれか一項または複数項に記載の干渉顔料。 - 全てのTiO2−xの部分層において、0.001≦x<0.05であることを特徴とする、請求項5に記載の干渉顔料。
- 外側最終のTiO2−xの部分層においてのみ、0.001≦x<0.05であることを特徴とする、請求項5に記載の干渉顔料。
- 前記中間層が、SiO2、Al2O3、酸化ケイ素水和物、酸化アルミニウム水和物、MgF2、またはそれらの2種以上の混合物からなることを特徴とする、請求項5から7のいずれか一項または複数項に記載の干渉顔料。
- SnO2の追加の層が、前記透明なフレーク状担体と前記TiO2−xの層との間に位置し、該TiO2−xの層は、前記SnO2の層上に直接位置することを特徴とする、請求項2から8のいずれか一項または複数項に記載の干渉顔料。
- 前記TiO2−xの層が、0.1モル%から3モル%のSnでドープされていることを特徴とする、請求項1から9のいずれか一項または複数項に記載の干渉顔料。
- TiO2からなる、または外側表面上にTiO2の層を有するコーティングされた透明なフレーク状担体からなる、透明なフレーク状干渉顔料が、5分から60分の範囲内の時間にわたり、還元ガスの添加のもとに気相中で熱処理され、TiO2がTiO2−xに変換され、0.001≦x<0.05であることを特徴とする、請求項1から10のいずれか一項または複数項に記載の干渉顔料の調製方法。
- 前記熱処理は、還元ガスの割合が0.05体積%から10体積%であるガス混合物中で行われることを特徴とする、請求項11に記載の方法。
- 前記還元ガスが、水素、アンモニアまたはC1〜C4炭化水素化合物であり、ガス混合物が、窒素またはアルゴンをさらに含むことを特徴とする、請求項11または12に記載の方法。
- 前記炭化水素化合物が、メタン、エチレンまたはプロパノンであることを特徴とする、請求項13に記載の方法。
- 前記熱処理が、400℃から800℃の範囲内の温度で行われることを特徴とする、請求項11から14のいずれか一項または複数項に記載の方法。
- 前記ガス混合物中の還元ガスの割合が、800℃の温度で0.05体積%から5体積%未満であり、400℃の温度で5体積%から10体積%であることを特徴とする、請求項15に記載の方法。
- 塗料、コーティング、印刷インク、プラスチック、センサ、セキュリティ用途、床の敷物、織物、フィルム、セラミック材料、ガラス、紙における;レーザマーキングのための;熱保護における;光半導体としての;顔料含有調合物、顔料調製物および乾燥調製物における、請求項1から10のいずれか一項または複数項に記載の透明で電気的半導体性フレーク状干渉顔料の使用。
- 前記干渉顔料が、有機および/もしくは無機着色剤、ならびに/または電気伝導性材料、ならびに/または非電気伝導性効果顔料との混合物として使用されることを特徴とする、請求項17に記載の使用。
- 前記干渉顔料が、電磁場の影響に曝されるセキュリティ製品において使用されることを特徴とする、請求項17または18に記載の使用。
- 請求項1から10のいずれか一項または複数項に記載の干渉顔料を含有するセキュリティ製品。
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US (1) | US9850384B2 (ja) |
EP (1) | EP3010979A1 (ja) |
JP (1) | JP6608813B2 (ja) |
KR (1) | KR20160020549A (ja) |
CN (1) | CN105308127B (ja) |
AU (1) | AU2014283735B2 (ja) |
MX (1) | MX2015017041A (ja) |
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JP2016528317A (ja) * | 2013-06-17 | 2016-09-15 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングMerck Patent Gesellschaft mit beschraenkter Haftung | 電気的半導体特性を有する、透明で光学的に可変の干渉顔料 |
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JP6841088B2 (ja) * | 2017-03-01 | 2021-03-10 | 堺化学工業株式会社 | 導電性材料及び電極材料 |
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US11579348B2 (en) * | 2018-11-20 | 2023-02-14 | The Regents Of The University Of Michigan | Decorative near-infrared transmission optical filter devices |
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- 2014-05-28 EP EP14728828.6A patent/EP3010979A1/de not_active Withdrawn
- 2014-05-28 WO PCT/EP2014/001435 patent/WO2014202179A1/de active Application Filing
- 2014-05-28 US US14/899,314 patent/US9850384B2/en not_active Expired - Fee Related
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- 2014-05-28 CN CN201480034214.9A patent/CN105308127B/zh not_active Expired - Fee Related
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JP2016528317A (ja) * | 2013-06-17 | 2016-09-15 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングMerck Patent Gesellschaft mit beschraenkter Haftung | 電気的半導体特性を有する、透明で光学的に可変の干渉顔料 |
Also Published As
Publication number | Publication date |
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WO2014202179A1 (de) | 2014-12-24 |
US9850384B2 (en) | 2017-12-26 |
MX2015017041A (es) | 2016-04-21 |
CN105308127B (zh) | 2018-03-23 |
JP6608813B2 (ja) | 2019-11-20 |
RU2658842C2 (ru) | 2018-06-25 |
KR20160020549A (ko) | 2016-02-23 |
AU2014283735A1 (en) | 2016-02-11 |
AU2014283735B2 (en) | 2017-06-22 |
CN105308127A (zh) | 2016-02-03 |
RU2016101117A (ru) | 2017-07-20 |
US20160137846A1 (en) | 2016-05-19 |
EP3010979A1 (de) | 2016-04-27 |
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