JP2010031158A - Black pigment dispersion, production method and application thereof - Google Patents
Black pigment dispersion, production method and application thereof Download PDFInfo
- Publication number
- JP2010031158A JP2010031158A JP2008195548A JP2008195548A JP2010031158A JP 2010031158 A JP2010031158 A JP 2010031158A JP 2008195548 A JP2008195548 A JP 2008195548A JP 2008195548 A JP2008195548 A JP 2008195548A JP 2010031158 A JP2010031158 A JP 2010031158A
- Authority
- JP
- Japan
- Prior art keywords
- black pigment
- black
- solvent
- dispersion
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000049 pigment Substances 0.000 title claims abstract description 76
- 239000006185 dispersion Substances 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000010936 titanium Substances 0.000 claims abstract description 39
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 39
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 229910010303 TiOxNy Inorganic materials 0.000 claims abstract description 9
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 18
- 239000003021 water soluble solvent Substances 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- 235000012255 calcium oxide Nutrition 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000004220 aggregation Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 230000007774 longterm Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003125 aqueous solvent Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000006722 reduction reaction Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- KELHQGOVULCJSG-UHFFFAOYSA-N n,n-dimethyl-1-(5-methylfuran-2-yl)ethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=C(C)O1 KELHQGOVULCJSG-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- -1 cellosolve acetates Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- 150000002168 ethanoic acid esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 150000003903 lactic acid esters Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 150000003151 propanoic acid esters Chemical class 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Paints Or Removers (AREA)
Abstract
Description
本発明は、顔料の分散性に優れた黒色顔料分散液、および、その製造方法と用途に関する。より詳しくは、本発明は黒色顔料の分散性が長期間安定であり、凝集物を実質的に含まない黒色膜を形成することができる黒色顔料分散液と、その製造方法および用途に関する。 The present invention relates to a black pigment dispersion excellent in pigment dispersibility, and a production method and use thereof. More specifically, the present invention relates to a black pigment dispersion that can form a black film that is stable in dispersibility of the black pigment for a long period of time and is substantially free of aggregates, and a method for producing the black pigment dispersion.
チタン酸窒化物粉末(チタンブラック)は酸化チタンをアンモニア還元して得られる高い黒色度を有する無機顔料であり広い分野で利用されており、例えば、その優れた遮光性を利用して液晶カラーフィルターのブラックマトリックス用黒色顔料として使用されている(特許文献1)。 Titanium oxynitride powder (titanium black) is an inorganic pigment having a high blackness obtained by ammonia reduction of titanium oxide, and is used in a wide range of fields. For example, liquid crystal color filters using its excellent light shielding properties It is used as a black pigment for black matrix (Patent Document 1).
チタンブラックは優れた遮光性を有するが、近年、ブラックマトリックスの低膜厚化が要求されており、遮光性を高めるために樹脂に対するチタンブラックの含有量を著しく高める傾向がある。また、チタンブラックの還元度を高めて黒色度を上げる試みもなされている。 Titanium black has excellent light-shielding properties, but in recent years, a reduction in the thickness of the black matrix has been demanded, and the content of titanium black in the resin tends to be remarkably increased in order to improve the light-shielding properties. Attempts have also been made to increase the blackness by increasing the reduction degree of titanium black.
ところが、樹脂に混合するチタンブラックの配合量を多くすると、相対的に樹脂分が少なくなり、顔料粉末(チタンブラック粉末)の安定性が低下する。また最近、カラーフィルター製造工程のスループット向上のため、高揮発性の低沸点溶剤を多量に使用する傾向にあり、顔料の分散安定性を維持することが厳しくなっている。 However, when the blending amount of titanium black mixed with the resin is increased, the resin content is relatively decreased, and the stability of the pigment powder (titanium black powder) is lowered. Recently, in order to improve the throughput of the color filter manufacturing process, there is a tendency to use a large amount of a highly volatile low-boiling solvent, and it has become strict to maintain the dispersion stability of the pigment.
一方、チタンブラックは表面処理しないものは液中での分散安定性が低く、特に還元反応が進むと表面に存在する活性な窒化物の割合が増え、液中での分散安定性がさらに低下する。このため、分散液を用いて成膜した場合、液中では分散良好に見えても、乾燥過程で異物や凝集物が確認され、使用不能になる場合が多い。この凝集物は一時的には濾過して除去することができるが、再凝集が生じ、長期の使用は困難である。
本発明は、従来の上記問題を解決したものであり、チタンブラック粉末からなる黒色顔料の分散性が長期間安定であり、塗膜を形成したときに凝集物が実質的に発生しない黒色顔料分散液と、その製造方法および用途を提供する。 The present invention solves the above-mentioned conventional problems, the dispersibility of a black pigment made of titanium black powder is stable for a long period of time, and a black pigment dispersion in which aggregates are not substantially generated when a coating film is formed. Provided are liquids, methods for their production and uses.
本発明は、以下の構成によって上記課題を解決した黒色顔料分散液、その製造方法および用途に関する。
〔1〕一般式TiOxNy(1.0≦x+y≦1.3、2x<y)で表されるチタン酸窒化物からなる黒色顔料粉末、樹脂、および溶剤を含み、該溶剤は水溶性溶剤5%〜50%とエステル系溶剤からなる複合溶剤であり、上記顔料の含有量に対して0.3〜2.0%の水分量を含むことを特徴とする黒色顔料分散液。
〔2〕水溶性溶剤が水溶性のアルコール類またはエーテル類である上記[1]の黒色顔料分散液。
〔3〕分散液の樹脂含有量が黒色顔料量に対して5〜25質量%、分散液の複合溶剤量が60〜90質量%である上記[1]または上記[2]に記載する黒色顔料分散液。
〔4〕粉末分として、チタン酸窒化物と共に、シリカ、アルミナ、ジルコニア、イットリア、カルシア、マグネシア、チタニア、酸化鉄、酸化マンガンなどの酸化物、またはカーボンブラック等の黒色顔料の一種または二種以上を含む上記[1]〜上記[3]の何れかに記載する黒色顔料分散液。
〔5〕上記[1]〜上記[4]の何れかに記載する黒色顔料分散液からなる黒色膜形成用組成物。
〔6〕上記[5]の組成物によって形成された黒色膜。
〔7〕一般式TiOxNy(1.0≦x+y≦1.3、2x<y)で表されるチタン酸窒化物からなる黒色顔料粉末、樹脂、および水溶性溶剤5%〜50%とエステル系溶剤からなる複合溶剤の調合時に水分を添加して、黒色顔料の含有量に対して0.3〜2.0%の水分量になるように調整する黒色膜形成用組成物の製造方法。
The present invention relates to a black pigment dispersion in which the above-described problems are solved by the following configuration, a manufacturing method thereof, and an application.
[1] A black pigment powder composed of a titanium oxynitride represented by the general formula TiOxNy (1.0 ≦ x + y ≦ 1.3, 2x <y), a resin, and a solvent, the solvent being a 5% water-soluble solvent A black pigment dispersion, which is a composite solvent comprising ˜50% and an ester solvent, and contains a water content of 0.3 to 2.0% with respect to the content of the pigment.
[2] The black pigment dispersion of [1] above, wherein the water-soluble solvent is a water-soluble alcohol or ether.
[3] The black pigment as described in [1] or [2] above, wherein the resin content of the dispersion is 5 to 25% by mass relative to the amount of black pigment, and the amount of the composite solvent of the dispersion is 60 to 90% by mass. Dispersion.
[4] As powder, together with titanium oxynitride, one or more kinds of oxides such as silica, alumina, zirconia, yttria, calcia, magnesia, titania, iron oxide, manganese oxide, or black pigments such as carbon black The black pigment dispersion described in any one of [1] to [3] above.
[5] A black film forming composition comprising the black pigment dispersion described in any one of [1] to [4].
[6] A black film formed by the composition of [5] above.
[7] Black pigment powder comprising a titanium oxynitride represented by the general formula TiOxNy (1.0 ≦ x + y ≦ 1.3, 2x <y), a resin, 5% to 50% of a water-soluble solvent, and an ester solvent A method for producing a composition for forming a black film, wherein water is added at the time of preparation of the composite solvent, and the water content is adjusted to 0.3 to 2.0% with respect to the black pigment content.
本発明の分散液は、黒色顔料(チタンブラック)の分散安定性に優れており、具体的には、例えば、調製直後の分散液(A)、および調整後60日経過後の分散液(B)によっておのおの塗膜を形成した場合、何れの塗膜においても凝集物は発生せず、塗膜中の黒色顔料粉末の平均粒子径も殆ど変わらない。また、分散液(A)(B)の粘度も殆ど変わらない。 The dispersion of the present invention is excellent in the dispersion stability of the black pigment (titanium black). Specifically, for example, the dispersion (A) immediately after preparation and the dispersion (B) after 60 days from the preparation. Thus, when each coating film is formed, aggregates are not generated in any coating film, and the average particle diameter of the black pigment powder in the coating film hardly changes. Further, the viscosity of the dispersion liquids (A) and (B) hardly changes.
以下、本発明を実施形態に基づいて具体的に説明する。なお、単位固有の場合を除いて%は質量%である。
〔黒色顔料分散液〕
本発明の分散液は、一般式TiOxNy(1.0≦x+y≦1.3、2x<y)で表されるチタン酸窒化物からなる黒色顔料粉末、樹脂、および溶剤を含み、該溶剤は水溶性溶剤5%〜50%とエステル系溶剤からなる複合溶剤であり、上記顔料の含有量に対して0.3〜2.0%の水分量を含むことを特徴とする黒色顔料分散液。
Hereinafter, the present invention will be specifically described based on embodiments. In addition,% is the mass% except the case intrinsic | native to a unit.
[Black pigment dispersion]
The dispersion of the present invention includes a black pigment powder composed of a titanium oxynitride represented by the general formula TiOxNy (1.0 ≦ x + y ≦ 1.3, 2x <y), a resin, and a solvent. A black pigment dispersion characterized in that it is a composite solvent comprising 5% to 50% of an organic solvent and an ester solvent and contains a water content of 0.3 to 2.0% with respect to the content of the pigment.
一般に、チタン酸窒化物(酸窒化チタン:チタンブラック)は、未反応原料の二酸化チタン(TiO2)と、還元反応により生成した一酸化チタン(TiO)、および窒化反応により生成した窒化チタン(TiN)との混合物であり、窒素の割合が多く、導電率の高い窒化チタン(TiN)の割合が増加することによって抵抗値が低下する。 In general, titanium oxynitride (titanium oxynitride: titanium black) is composed of unreacted raw material titanium dioxide (TiO 2 ), titanium monoxide (TiO) produced by a reduction reaction, and titanium nitride (TiN produced by a nitriding reaction). ), The ratio of nitrogen is high, and the ratio of titanium nitride (TiN) having a high conductivity increases, so that the resistance value decreases.
従来のチタン酸窒化物は、導電性の低い酸化チタン(TiO2、TiO)の割合が多く、一般式TiOxNyにおいて、窒素量yが酸素量xの2倍未満(2x>y)であり、粉体の抵抗値が高くなり、黒色度が低下する。 Conventional titanium oxynitrides have a high proportion of low-conductivity titanium oxide (TiO 2 , TiO), and in general formula TiOxNy, the amount of nitrogen y is less than twice the amount of oxygen x (2x> y), The resistance value of the body increases and the blackness decreases.
一方、本発明で用いるチタン酸窒化物は窒素の含有量が多く、一般式TiOxNyにおいて、窒素と酸素の割合が2x<yであり、また、酸素と窒素の合計量(x+y)が1.0≦x+y≦1.3である。従って、本発明で用いるチタン酸窒化物は粉体抵抗が低く、黒色度(L値)が高い。 On the other hand, the titanium oxynitride used in the present invention has a high nitrogen content. In the general formula TiOxNy, the ratio of nitrogen to oxygen is 2x <y, and the total amount of oxygen and nitrogen (x + y) is 1.0. ≦ x + y ≦ 1.3. Therefore, the titanium oxynitride used in the present invention has low powder resistance and high blackness (L value).
上記チタン酸窒化物は、リン(P)および/またはケイ素(Si)を0.005〜2.0%含有するものを用いることができる。上記含有量のリンおよび/またはケイ素を含有することによって、窒化チタンの活発な反応性が抑えられ、窒化チタン量が多くても良好な分散性を有し、長期的な分散安定性にも優れる。 As the titanium oxynitride, one containing 0.005 to 2.0% of phosphorus (P) and / or silicon (Si) can be used. By containing phosphorus and / or silicon in the above content, the active reactivity of titanium nitride is suppressed, and even if the amount of titanium nitride is large, it has good dispersibility and excellent long-term dispersion stability. .
リンおよび/またはケイ素を含有するチタン酸窒化物粉末は、酸化チタン粉末を窒化還元処理して一般式TiOxNy(1.0≦x+y≦1.3、2x<y)で表されるチタン酸窒化物粉末からなる黒色導電性粉末を製造する際に、酸化物、窒化物、無機酸、またはアンモニア塩、アルカリ塩のリン化合物および/またはケイ素化合物を、原料の酸化チタン粉末に所定量添加して窒化還元処理することによって得ることができる。 Titanium oxynitride powder containing phosphorus and / or silicon is obtained by subjecting titanium oxide powder to nitridation reduction treatment and represented by the general formula TiOxNy (1.0 ≦ x + y ≦ 1.3, 2x <y) When producing black conductive powder consisting of powder, oxide, nitride, inorganic acid, ammonia salt, phosphorus salt of alkali salt and / or silicon compound is added to raw material titanium oxide powder for nitriding It can be obtained by reduction treatment.
本発明の黒色顔料分散液は、粉末分として、チタン酸窒化物と共に、シリカ、アルミナ、ジルコニア、イットリア、カルシア、マグネシア、チタニア、酸化鉄、酸化マンガンなどの酸化物、またはカーボンブラック等の黒色顔料の一種または二種以上を含むことができる。 The black pigment dispersion of the present invention includes, as a powder component, together with titanium oxynitride, an oxide such as silica, alumina, zirconia, yttria, calcia, magnesia, titania, iron oxide, manganese oxide, or black pigment such as carbon black. 1 type, or 2 or more types can be included.
チタン酸窒化物と共に上記酸化物を含むことによって分散液の安定性を高め、さらには塗膜の絶縁性、密着性、表面粗さを向上させることができる。また、カーボンブラック等の黒色顔料を含むことによって黒色度を高めることができる。上記酸化物およびカーボンブラック等の含有量は上記チタン酸窒化物に対して15%以下が適当である。 By containing the above oxide together with the titanium oxynitride, the stability of the dispersion can be improved, and further, the insulating properties, adhesion, and surface roughness of the coating film can be improved. Moreover, blackness can be raised by including black pigments, such as carbon black. The content of the oxide and carbon black is suitably 15% or less with respect to the titanium oxynitride.
本発明の黒色顔料分散液は上記チタン酸窒化物粉末と共に分散樹脂および溶剤を含む。樹脂はアミノ基、アミド基、カルボキシル基等顔料表面に吸着する吸着基を有するものが有効であり、市販の分散剤を使用することができる。具体的には、ポリエステル系、ポリウレタン系、エポキシ系、シリコーン系、アクリル系等が挙げられる。また、これらを二種以上混合して使用することもできる。また、カチオン系、アニオン系、ノニオン系、両性、シリコーン系、フッ素系等の界面活性剤を単独、もしくは併用して使用することもできる。 The black pigment dispersion of the present invention contains a dispersion resin and a solvent together with the titanium oxynitride powder. As the resin, those having an adsorbing group that adsorbs to the pigment surface such as an amino group, an amide group, or a carboxyl group are effective, and a commercially available dispersant can be used. Specific examples include polyester, polyurethane, epoxy, silicone, and acrylic. Moreover, these can also be used in mixture of 2 or more types. Moreover, surfactants such as cationic, anionic, nonionic, amphoteric, silicone, and fluorine can be used alone or in combination.
分散液の樹脂含有量は黒色顔料(チタン酸窒化物)量に対して5〜25%が好ましく、10%〜20%がより好ましい。樹脂の含有量が5%より少ないと顔料表面への吸着が不十分であり安定した分散液が得られない。一方、樹脂の含有量が25%より多いと樹脂どうしの反応が起こりやすく高粘度となりやはり安定した分散状態が得られない。 The resin content of the dispersion is preferably from 5 to 25%, more preferably from 10% to 20%, based on the amount of black pigment (titanium oxynitride). If the resin content is less than 5%, adsorption to the pigment surface is insufficient and a stable dispersion cannot be obtained. On the other hand, if the resin content is more than 25%, the reaction between the resins tends to occur and the viscosity becomes high, and a stable dispersion state cannot be obtained.
本発明の黒色顔料分散液に用いる溶剤は、水溶性溶剤5%〜50%とエステル系溶剤からなる複合溶剤である。水溶性溶剤とエステル系溶剤とを含む複合溶剤を用いることによって分散液の安定性が得られると共に、薄膜形成時の塗布性、乾燥性、薄膜の緻密性、表面平滑性、密着性が良好となる。 The solvent used for the black pigment dispersion of the present invention is a composite solvent comprising a water-soluble solvent 5% to 50% and an ester solvent. By using a composite solvent containing a water-soluble solvent and an ester solvent, the stability of the dispersion can be obtained, and the coating property, drying property, thin film denseness, surface smoothness, and adhesion during film formation are good. Become.
水溶性溶剤としては、OH基を有する有機系溶剤であって、例えば、エタノールやプロパノール等のアルコール類、グリコールエーテル等のエーテル類、エチレングリコールやプロピレングリコール等のグリコール類、メチルセロソルブ、エチルセロソルブ等のセロソルブ類等、N−メチルピロリドン、N,Nジメチルホルムアミド等のアミド類を用いることができる。 The water-soluble solvent is an organic solvent having an OH group, for example, alcohols such as ethanol and propanol, ethers such as glycol ether, glycols such as ethylene glycol and propylene glycol, methyl cellosolve, ethyl cellosolve, etc. , And other amides such as N-methylpyrrolidone and N, N dimethylformamide can be used.
エステル系溶剤としては、例えば、酢酸ブチル、酢酸プロピルなどの酢酸エステル、プロピレングリコールモノメチルエーテルアセテート(PMA)等のグリコールエーテルエステルを用いることができる。これらの酢酸エステルおよびグリコールエーテルエステルは、黒色インキ液、ブラックマトリックスを形成する塗膜などの溶剤として用いられている。また、酢酸エステル、グリコールエーテルエステルの他にプロピオン酸エステル類、乳酸エステル類、セロソルブアセテート類、ケトン類、炭化水素系溶剤、ベンゼン系溶剤などを用いることができる。これらは単独でも使用可能であるが、2種類以上組み合わせても良く、またケトン類、炭化水素系溶剤、ベンゼン系溶剤を一部置換しても良い。 Examples of ester solvents that can be used include acetate esters such as butyl acetate and propyl acetate, and glycol ether esters such as propylene glycol monomethyl ether acetate (PMA). These acetate esters and glycol ether esters are used as solvents for black ink liquids, coating films that form black matrices, and the like. In addition to acetic acid esters and glycol ether esters, propionic acid esters, lactic acid esters, cellosolve acetates, ketones, hydrocarbon solvents, benzene solvents and the like can be used. These can be used alone or in combination of two or more, and ketones, hydrocarbon solvents, and benzene solvents may be partially substituted.
複合溶剤中の水溶性溶剤の量は5〜50%が好ましい。水溶性溶剤の量が5%より少ないと、複合溶剤を用いる上記効果が乏しくなる。一方、水溶性溶剤の含有量が10%より多いと乾燥性が悪くなり、緻密で表面平滑性に優れた薄膜が得られ難くなる。 The amount of the water-soluble solvent in the composite solvent is preferably 5 to 50%. When the amount of the water-soluble solvent is less than 5%, the above effect using the composite solvent becomes poor. On the other hand, if the content of the water-soluble solvent is more than 10%, the drying property is deteriorated, and it is difficult to obtain a thin film having a fine and excellent surface smoothness.
複合溶剤は沸点140℃以下が好ましい。沸点が140℃以上になると乾燥速度が遅くなるため緻密な膜が得られなくなり、生産性が著しく低下するためコスト高となり好ましくない。また、分散液中の複合溶剤量は60〜90%が好ましい。60%より少ないと粘度が分散液の高すぎて扱いにくくなり、90%より多いと顔料割合が低すぎて目的とする膜厚の膜が得られなくなる。 The composite solvent preferably has a boiling point of 140 ° C. or lower. When the boiling point is 140 ° C. or higher, the drying rate is slow, so that a dense film cannot be obtained, and the productivity is remarkably lowered, resulting in an increase in cost. Further, the amount of the composite solvent in the dispersion is preferably 60 to 90%. If it is less than 60%, the viscosity is too high for the dispersion liquid to be difficult to handle, and if it is more than 90%, the pigment ratio is too low to obtain a film having the desired film thickness.
本発明の黒色顔料分散液は、黒色顔料(チタン酸窒化物)量に対して0.3〜2.0%の水分を含む。この範囲の水分量を含むことによって、黒色顔料の分散安定性が格段に向上し、被膜を形成したときに凝集物が大幅に少なくなる。水分量が0.3%より少ないと、顔料の凝集を十分に抑制することができず、液の保存後に形成した被膜中に凝集物が生じるようになり、また液の保存期間中に粘性が高くなるなど、分散液の保存安定性が低い。一方、水分量が2.0%を上回ると、顔料の凝集は抑えられるものの、樹脂の加水分解を招き、分散液の粘性が次第に高くなる。 The black pigment dispersion of the present invention contains 0.3 to 2.0% of water with respect to the amount of black pigment (titanium oxynitride). By including the water content in this range, the dispersion stability of the black pigment is remarkably improved, and aggregates are greatly reduced when a film is formed. When the water content is less than 0.3%, the aggregation of the pigment cannot be sufficiently suppressed, and aggregates are formed in the film formed after storage of the liquid, and the viscosity is reduced during the storage period of the liquid. The storage stability of the dispersion is low. On the other hand, if the water content exceeds 2.0%, the aggregation of the pigment is suppressed, but the resin is hydrolyzed and the viscosity of the dispersion becomes gradually higher.
〔製造方法〕
本発明の黒色顔料分散液は、上記チタン酸窒化物からなる黒色顔料粉末、樹脂、および上記複合溶剤を調合し、この調合時に水分を添加し、黒色顔料の含有量に対して0.3〜2.0%の水分量になるように調整することによって製造することができる。具体的には、黒色顔料、および溶剤に含まれる水分量をあらかじめ測定し、不足分の水分量を調合時に添加すると良い。
〔Production method〕
The black pigment dispersion of the present invention is prepared by preparing a black pigment powder composed of the above titanium oxynitride, a resin, and the above composite solvent, adding water at the time of preparation, and adding 0.3 to the content of the black pigment. It can be manufactured by adjusting the water content to 2.0%. Specifically, the amount of water contained in the black pigment and the solvent is measured in advance, and the insufficient amount of water may be added during preparation.
〔黒色膜〕
本発明の黒色顔料分散液は、ブラックマトリックスなどの黒色膜を形成する塗液として好適である。本発明の黒色顔料分散液を用いて形成した塗膜には異物(顔料の凝集物等)が殆ど存在せず、顔料が均一に分散した高品質の黒色膜を得ることができる。
[Black film]
The black pigment dispersion of the present invention is suitable as a coating liquid for forming a black film such as a black matrix. The coating film formed using the black pigment dispersion of the present invention has almost no foreign matter (such as pigment aggregates), and a high-quality black film in which the pigment is uniformly dispersed can be obtained.
以下に本発明の実施例を比較例と共に示す。なお、分散液中の顔料の平均粒子径はコールター測定器(N4plus)を用いて測定した。成膜中の凝集物の有無は100倍の光学顕微鏡観察を用いた肉眼観察によって判定した。分散液の粘度はE型粘度計(トキメック社製)によって測定した。実施例の結果を表1に示し、比較例の結果を表2に示した。 Examples of the present invention are shown below together with comparative examples. The average particle size of the pigment in the dispersion was measured using a Coulter measuring device (N4plus). The presence or absence of aggregates during film formation was determined by visual observation using 100-fold optical microscope observation. The viscosity of the dispersion was measured with an E-type viscometer (manufactured by Tokimec). The results of the examples are shown in Table 1, and the results of the comparative examples are shown in Table 2.
〔実施例1〕
チタンブラック粉末(TiO0.24N0.92)100重量部と市販の塩基性分散樹脂10重量部、混合溶剤(酢酸ブチル:イソプロパノール=8:2)390重量部を調合した。このときチタンブラックに含まれる水分量0.3%、混合溶剤に含まれる水分量0.01%であったので、分散液の水分量がチタンブラック量に対して0.7%になるよう純水を添加した。調合した分散液を循環型サンドミルで分散処理し、最終的に顔料濃度25%になるように上記複合溶剤を加えて希釈した。
作製した分散液を1ミクロンフィルターで濾過した後に、ガラス基板にスピンコート成膜し、この成膜を100倍の光学顕微鏡で観察し、異物の有無を調べた。この結果、上記成膜には異物が存在せず均一な膜であった。また、液中に分散しているチタンブラックの平均粒子径は120nmであった。
上記分散液を60日間、25℃に保管した後に、濾過せずにガラス基板にスピンコート成膜した。この成膜には異物が存在せず均一な膜であった。また、液中に分散しているチタンブラックの平均粒子径は120nmであった。
[Example 1]
100 parts by weight of titanium black powder (TiO 0.24 N 0.92 ), 10 parts by weight of a commercially available basic dispersion resin, and 390 parts by weight of a mixed solvent (butyl acetate: isopropanol = 8: 2) were prepared. At this time, the amount of water contained in the titanium black was 0.3% and the amount of water contained in the mixed solvent was 0.01%, so that the water content of the dispersion was 0.7% with respect to the amount of titanium black. Water was added. The prepared dispersion was dispersed in a circulating sand mill, and diluted by adding the above composite solvent so that the final pigment concentration was 25%.
The prepared dispersion was filtered through a 1 micron filter, and then a spin coat film was formed on a glass substrate. This film formation was observed with a 100 × optical microscope to examine the presence of foreign matter. As a result, the film formation was uniform with no foreign matter present. The average particle size of titanium black dispersed in the liquid was 120 nm.
The dispersion was stored at 25 ° C. for 60 days, and then spin-coated on a glass substrate without filtration. This film was a uniform film with no foreign matter present. The average particle size of titanium black dispersed in the liquid was 120 nm.
〔実施例2〜9〕
実施例1と同様な方法によって黒色顔料の分散液を調製した。使用顔料、溶剤、樹脂、水分量を表1に示した。この分散液を用いて黒色膜を形成した。この結果を表1に示した。
[Examples 2 to 9]
A black pigment dispersion was prepared in the same manner as in Example 1. Table 1 shows the pigment, solvent, resin, and amount of water used. A black film was formed using this dispersion. The results are shown in Table 1.
表1に示すように、実施例1〜9の分散液は、調製直後の分散液を用いた形成した成膜には異物が存在せず、顔料の良好な分散性を示している。また、60日経過後の分散液についてみると、液中に分散しているチタンブラックの平均粒子径、液の粘度は調製直後の分散液と殆ど変わらず、成膜にも異物は観察されず、液の保存期間を通じて分散液が安定に維持されている。 As shown in Table 1, the dispersions of Examples 1 to 9 showed no dispersibility in the formed film using the dispersion immediately after preparation, and showed good dispersibility of the pigment. Also, when looking at the dispersion after 60 days, the average particle diameter of the titanium black dispersed in the liquid, the viscosity of the liquid is almost the same as the dispersion immediately after the preparation, no foreign matter is observed in the film formation, The dispersion is kept stable throughout the storage period of the liquid.
〔比較例1〜4〕
表2に示す条件に従い、その他は実施例1と同様にして黒色顔料分散液を調製し、この分散液を用いて黒色膜を形成した。この結果を表2に示す。
[Comparative Examples 1-4]
According to the conditions shown in Table 2, a black pigment dispersion was prepared in the same manner as in Example 1, and a black film was formed using this dispersion. The results are shown in Table 2.
比較例1〜4の分散液は、何れも60日経過後において液の粘性が大幅に高くなり、比較例2を除いて、60日経過後の分散液を用いて形成した成膜中に異物が観察された。 In all of the dispersions of Comparative Examples 1 to 4, the viscosity of the liquid was significantly increased after 60 days had elapsed, and, except for Comparative Example 2, foreign matter was observed during film formation using the dispersion after 60 days. It was done.
Claims (7)
A black pigment powder composed of a titanium oxynitride represented by the general formula TiOxNy (1.0 ≦ x + y ≦ 1.3, 2x <y), a resin, and a solvent, the solvent being a water-soluble solvent 5% to 50% A black pigment dispersion characterized by containing a 0.3 to 2.0% water content with respect to the pigment content.
The black pigment dispersion according to claim 1, wherein the water-soluble solvent is a water-soluble alcohol or ether.
The black pigment dispersion according to claim 1 or 2, wherein the resin content of the dispersion is 5 to 25% by mass with respect to the amount of black pigment, and the amount of the composite solvent of the dispersion is 60 to 90% by mass.
Claims containing, as a powder component, one or more of oxides such as silica, alumina, zirconia, yttria, calcia, magnesia, titania, iron oxide, manganese oxide, and black pigments such as carbon black, together with titanium oxynitride The black pigment dispersion according to any one of claims 1 to 3.
The composition for black film formation which consists of a black pigment dispersion liquid in any one of Claims 1-4.
A black film formed by the composition of claim 5.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2008195548A JP5424591B2 (en) | 2008-07-29 | 2008-07-29 | Black pigment dispersion, its production method and use |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2008195548A JP5424591B2 (en) | 2008-07-29 | 2008-07-29 | Black pigment dispersion, its production method and use |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2010031158A true JP2010031158A (en) | 2010-02-12 |
JP5424591B2 JP5424591B2 (en) | 2014-02-26 |
Family
ID=41736025
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2008195548A Active JP5424591B2 (en) | 2008-07-29 | 2008-07-29 | Black pigment dispersion, its production method and use |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP5424591B2 (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102372949A (en) * | 2010-08-09 | 2012-03-14 | 曾炽涛 | Aqueous pigment slurry and preparation method thereof |
JP2013035917A (en) * | 2011-08-05 | 2013-02-21 | Mitsubishi Chemicals Corp | Pigment dispersion, colored resin composition, color filter, liquid crystal display device and organic el display |
CN104212246A (en) * | 2014-09-10 | 2014-12-17 | 张家港格瑞特化学有限公司 | Ferric oxide oily color paste |
KR20160136271A (en) * | 2014-03-27 | 2016-11-29 | 미쓰비시마테리알덴시카세이가부시키가이샤 | Black titanium oxynitride pigment, method for producing same, and semiconductor-sealing resin compound using black titanium oxynitride pigment |
CN109181375A (en) * | 2018-08-31 | 2019-01-11 | 吴丰容 | A kind of black body radiation energy-saving coatings and preparation method thereof |
JPWO2018061644A1 (en) * | 2016-09-30 | 2019-09-05 | 富士フイルム株式会社 | Metal nitride-containing particles, dispersion composition, curable composition, cured film, and production method thereof, color filter, solid-state imaging device, solid-state imaging device, infrared sensor |
WO2023204314A1 (en) * | 2022-04-22 | 2023-10-26 | 三菱ケミカル株式会社 | Pigment dispersion, photosensitive resin composition, cured product, black matrix, and image display device |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6437408A (en) * | 1987-08-03 | 1989-02-08 | Toray Industries | Black powder of titanium nitride |
JPH01141963A (en) * | 1987-11-30 | 1989-06-02 | Dainippon Toryo Co Ltd | Coating composition |
JPH0762323A (en) * | 1993-08-27 | 1995-03-07 | Asahi Glass Co Ltd | Coating liquid for forming colored film, colored film and preparation thereof |
JP2002361063A (en) * | 2001-06-08 | 2002-12-17 | Mitsubishi Materials Corp | Dispersant for black pigment, black pigment dispersed composition and black film |
JP2004004651A (en) * | 2002-03-28 | 2004-01-08 | Toray Ind Inc | Resin black matrix, color filter, liquid crystal display device and black coating film composition |
JP2004217805A (en) * | 2003-01-15 | 2004-08-05 | Yoshiyuki Nagae | Pigment, coating, and method for manufacturing pigment and coating |
JP2004281056A (en) * | 2002-03-25 | 2004-10-07 | Sumitomo Metal Mining Co Ltd | Process for producing noble-metal-containing fine-particle dispersion and coating liquid for forming transparent conductive layer, as well as transparent conductive substrate and display device |
JP2004354845A (en) * | 2003-05-30 | 2004-12-16 | Toray Ind Inc | Color filter for liquid crystal display device, and liquid crystal display device |
JP2005135722A (en) * | 2003-10-30 | 2005-05-26 | Sumitomo Metal Mining Co Ltd | Coating liquid for forming transparent conductive layer and transparent conductive substrate |
JP2008266045A (en) * | 2007-04-17 | 2008-11-06 | Mitsubishi Materials Corp | High resistance black powder and its dispersed liquid, paint and black film |
JP2008269820A (en) * | 2007-04-17 | 2008-11-06 | Mitsubishi Materials Corp | Conductive black powder, and its manufacturing method, and its black film |
JP2010030842A (en) * | 2008-07-29 | 2010-02-12 | Mitsubishi Materials Corp | Black titanium oxynitride powder and its producing method and usage |
-
2008
- 2008-07-29 JP JP2008195548A patent/JP5424591B2/en active Active
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6437408A (en) * | 1987-08-03 | 1989-02-08 | Toray Industries | Black powder of titanium nitride |
JPH01141963A (en) * | 1987-11-30 | 1989-06-02 | Dainippon Toryo Co Ltd | Coating composition |
JPH0762323A (en) * | 1993-08-27 | 1995-03-07 | Asahi Glass Co Ltd | Coating liquid for forming colored film, colored film and preparation thereof |
JP2002361063A (en) * | 2001-06-08 | 2002-12-17 | Mitsubishi Materials Corp | Dispersant for black pigment, black pigment dispersed composition and black film |
JP2004281056A (en) * | 2002-03-25 | 2004-10-07 | Sumitomo Metal Mining Co Ltd | Process for producing noble-metal-containing fine-particle dispersion and coating liquid for forming transparent conductive layer, as well as transparent conductive substrate and display device |
JP2004004651A (en) * | 2002-03-28 | 2004-01-08 | Toray Ind Inc | Resin black matrix, color filter, liquid crystal display device and black coating film composition |
JP2004217805A (en) * | 2003-01-15 | 2004-08-05 | Yoshiyuki Nagae | Pigment, coating, and method for manufacturing pigment and coating |
JP2004354845A (en) * | 2003-05-30 | 2004-12-16 | Toray Ind Inc | Color filter for liquid crystal display device, and liquid crystal display device |
JP2005135722A (en) * | 2003-10-30 | 2005-05-26 | Sumitomo Metal Mining Co Ltd | Coating liquid for forming transparent conductive layer and transparent conductive substrate |
JP2008266045A (en) * | 2007-04-17 | 2008-11-06 | Mitsubishi Materials Corp | High resistance black powder and its dispersed liquid, paint and black film |
JP2008269820A (en) * | 2007-04-17 | 2008-11-06 | Mitsubishi Materials Corp | Conductive black powder, and its manufacturing method, and its black film |
JP2010030842A (en) * | 2008-07-29 | 2010-02-12 | Mitsubishi Materials Corp | Black titanium oxynitride powder and its producing method and usage |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102372949A (en) * | 2010-08-09 | 2012-03-14 | 曾炽涛 | Aqueous pigment slurry and preparation method thereof |
JP2013035917A (en) * | 2011-08-05 | 2013-02-21 | Mitsubishi Chemicals Corp | Pigment dispersion, colored resin composition, color filter, liquid crystal display device and organic el display |
KR20160136271A (en) * | 2014-03-27 | 2016-11-29 | 미쓰비시마테리알덴시카세이가부시키가이샤 | Black titanium oxynitride pigment, method for producing same, and semiconductor-sealing resin compound using black titanium oxynitride pigment |
KR102330139B1 (en) | 2014-03-27 | 2021-11-22 | 미쓰비시마테리알덴시카세이가부시키가이샤 | Black titanium oxynitride pigment, method for producing same, and semiconductor-sealing resin compound using black titanium oxynitride pigment |
CN104212246A (en) * | 2014-09-10 | 2014-12-17 | 张家港格瑞特化学有限公司 | Ferric oxide oily color paste |
JPWO2018061644A1 (en) * | 2016-09-30 | 2019-09-05 | 富士フイルム株式会社 | Metal nitride-containing particles, dispersion composition, curable composition, cured film, and production method thereof, color filter, solid-state imaging device, solid-state imaging device, infrared sensor |
JP2022079500A (en) * | 2016-09-30 | 2022-05-26 | 富士フイルム株式会社 | Metal nitride-containing particles, dispersion composition, curable composition, curable film, production method thereof, color filter, solid-state imaging element, solid-state imaging device, and infrared sensor |
JP7373000B2 (en) | 2016-09-30 | 2023-11-01 | 富士フイルム株式会社 | Metal nitride-containing particles, dispersion compositions, curable compositions, cured films, and methods for producing them, color filters, solid-state imaging devices, solid-state imaging devices, infrared sensors |
CN109181375A (en) * | 2018-08-31 | 2019-01-11 | 吴丰容 | A kind of black body radiation energy-saving coatings and preparation method thereof |
WO2023204314A1 (en) * | 2022-04-22 | 2023-10-26 | 三菱ケミカル株式会社 | Pigment dispersion, photosensitive resin composition, cured product, black matrix, and image display device |
Also Published As
Publication number | Publication date |
---|---|
JP5424591B2 (en) | 2014-02-26 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5424591B2 (en) | Black pigment dispersion, its production method and use | |
EP3263651B1 (en) | Dispersion of titanium oxide particles in organic solvent, and production method for same | |
US9976036B2 (en) | Organic solvent dispersion of zirconium oxide particles and method for producing same | |
EP3263527B1 (en) | Method for producing organic solvent dispersion of titanium oxide particles | |
CN110643214B (en) | High-dispersity precipitated silica anti-settling agent for coating and preparation method thereof | |
JP5264351B2 (en) | Black titanium oxynitride powder and production method and use thereof | |
CN114736548A (en) | Photo-curable nano zirconium oxide dispersion liquid, preparation method thereof and optical film | |
JP2012031353A (en) | Coating composition and optical member | |
JP6631656B2 (en) | Inorganic oxide dispersion with high transparency | |
KR20140046796A (en) | Titanium oxide dispersion sol composition and method of preparing titanium oxide dispersion sol composition | |
JP6105281B2 (en) | Aluminum pigment composition and method for producing the same | |
JP5212589B2 (en) | Black fine composite particle powder, dispersion containing the black fine composite particle powder, and method for producing black fine composite particle powder | |
WO2024161873A1 (en) | Dispersion body including strontium titanate spherical fine particle powder and method for producing same | |
KR102397564B1 (en) | Titania dispersion composition and preparation method thereof | |
TW202120435A (en) | Inorganic oxide dispersion and paint | |
JP5339020B2 (en) | Method for producing dispersion of inorganic particles |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20110727 |
|
A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20121227 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20130116 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20130315 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20130807 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20131003 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20131030 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20131126 |
|
R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 Ref document number: 5424591 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313117 |
|
R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |