JP6165004B2 - トナー - Google Patents
トナー Download PDFInfo
- Publication number
- JP6165004B2 JP6165004B2 JP2013193765A JP2013193765A JP6165004B2 JP 6165004 B2 JP6165004 B2 JP 6165004B2 JP 2013193765 A JP2013193765 A JP 2013193765A JP 2013193765 A JP2013193765 A JP 2013193765A JP 6165004 B2 JP6165004 B2 JP 6165004B2
- Authority
- JP
- Japan
- Prior art keywords
- toner
- acid
- charge control
- control agent
- manufactured
- 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.)
- Expired - Fee Related
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- 125000005397 methacrylic acid ester group Chemical group 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 description 1
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- 239000005055 methyl trichlorosilane Substances 0.000 description 1
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- 239000004200 microcrystalline wax Substances 0.000 description 1
- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 150000005673 monoalkenes Chemical class 0.000 description 1
- 235000013872 montan acid ester Nutrition 0.000 description 1
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- WWECJGLXBSQKRF-UHFFFAOYSA-N n,n-dimethylformamide;methanol Chemical compound OC.CN(C)C=O WWECJGLXBSQKRF-UHFFFAOYSA-N 0.000 description 1
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- QYZFTMMPKCOTAN-UHFFFAOYSA-N n-[2-(2-hydroxyethylamino)ethyl]-2-[[1-[2-(2-hydroxyethylamino)ethylamino]-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCNCCO QYZFTMMPKCOTAN-UHFFFAOYSA-N 0.000 description 1
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 1
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- KKFHAJHLJHVUDM-UHFFFAOYSA-N n-vinylcarbazole Chemical compound C1=CC=C2N(C=C)C3=CC=CC=C3C2=C1 KKFHAJHLJHVUDM-UHFFFAOYSA-N 0.000 description 1
- WRYWBRATLBWSSG-UHFFFAOYSA-N naphthalene-1,2,4-tricarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC(C(O)=O)=C21 WRYWBRATLBWSSG-UHFFFAOYSA-N 0.000 description 1
- LATKICLYWYUXCN-UHFFFAOYSA-N naphthalene-1,3,6-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC2=CC(C(=O)O)=CC=C21 LATKICLYWYUXCN-UHFFFAOYSA-N 0.000 description 1
- 150000004780 naphthols Chemical class 0.000 description 1
- HILCQVNWWOARMT-UHFFFAOYSA-N non-1-en-3-one Chemical compound CCCCCCC(=O)C=C HILCQVNWWOARMT-UHFFFAOYSA-N 0.000 description 1
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- HNWJSFBLWQRXIR-UHFFFAOYSA-N octadecanamide;1,3-xylene Chemical compound CC1=CC=CC(C)=C1.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O HNWJSFBLWQRXIR-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
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- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 description 1
- WDAISVDZHKFVQP-UHFFFAOYSA-N octane-1,2,7,8-tetracarboxylic acid Chemical compound OC(=O)CC(C(O)=O)CCCCC(C(O)=O)CC(O)=O WDAISVDZHKFVQP-UHFFFAOYSA-N 0.000 description 1
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 1
- SRSFOMHQIATOFV-UHFFFAOYSA-N octanoyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(=O)CCCCCCC SRSFOMHQIATOFV-UHFFFAOYSA-N 0.000 description 1
- NZIDBRBFGPQCRY-UHFFFAOYSA-N octyl 2-methylprop-2-enoate Chemical compound CCCCCCCCOC(=O)C(C)=C NZIDBRBFGPQCRY-UHFFFAOYSA-N 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- 229920002601 oligoester Polymers 0.000 description 1
- 239000004209 oxidized polyethylene wax Substances 0.000 description 1
- 235000013873 oxidized polyethylene wax Nutrition 0.000 description 1
- HDBWAWNLGGMZRQ-UHFFFAOYSA-N p-Vinylbiphenyl Chemical compound C1=CC(C=C)=CC=C1C1=CC=CC=C1 HDBWAWNLGGMZRQ-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- UCUUFSAXZMGPGH-UHFFFAOYSA-N penta-1,4-dien-3-one Chemical class C=CC(=O)C=C UCUUFSAXZMGPGH-UHFFFAOYSA-N 0.000 description 1
- 229940059574 pentaerithrityl Drugs 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
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- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
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- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 description 1
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- 230000000704 physical effect Effects 0.000 description 1
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- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- YPVDWEHVCUBACK-UHFFFAOYSA-N propoxycarbonyloxy propyl carbonate Chemical compound CCCOC(=O)OOC(=O)OCCC YPVDWEHVCUBACK-UHFFFAOYSA-N 0.000 description 1
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- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- JOUDBUYBGJYFFP-FOCLMDBBSA-N thioindigo Chemical class S\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2S1 JOUDBUYBGJYFFP-FOCLMDBBSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
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- 238000012546 transfer Methods 0.000 description 1
- CAPIMQICDAJXSB-UHFFFAOYSA-N trichloro(1-chloroethyl)silane Chemical compound CC(Cl)[Si](Cl)(Cl)Cl CAPIMQICDAJXSB-UHFFFAOYSA-N 0.000 description 1
- FLPXNJHYVOVLSD-UHFFFAOYSA-N trichloro(2-chloroethyl)silane Chemical compound ClCC[Si](Cl)(Cl)Cl FLPXNJHYVOVLSD-UHFFFAOYSA-N 0.000 description 1
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- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
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- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 229940096522 trimethylolpropane triacrylate Drugs 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- GRPURDFRFHUDSP-UHFFFAOYSA-N tris(prop-2-enyl) benzene-1,2,4-tricarboxylate Chemical group C=CCOC(=O)C1=CC=C(C(=O)OCC=C)C(C(=O)OCC=C)=C1 GRPURDFRFHUDSP-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- HBOUJSBUVUATSW-UHFFFAOYSA-N undec-1-enylbenzene Chemical compound CCCCCCCCCC=CC1=CC=CC=C1 HBOUJSBUVUATSW-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- FUSUHKVFWTUUBE-UHFFFAOYSA-N vinyl methyl ketone Natural products CC(=O)C=C FUSUHKVFWTUUBE-UHFFFAOYSA-N 0.000 description 1
- JLQFVGYYVXALAG-CFEVTAHFSA-N yasmin 28 Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1.C([C@]12[C@H]3C[C@H]3[C@H]3[C@H]4[C@@H]([C@]5(CCC(=O)C=C5[C@@H]5C[C@@H]54)C)CC[C@@]31C)CC(=O)O2 JLQFVGYYVXALAG-CFEVTAHFSA-N 0.000 description 1
- 239000001060 yellow colorant Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- KRJOFJHOZZPBKI-KSWODRSDSA-N α-defensin-1 Chemical compound C([C@H]1C(=O)N[C@H]2CSSC[C@H]3C(=O)N[C@H](C(N[C@@H](C)C(=O)NCC(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CC=4C=CC(O)=CC=4)C(=O)NCC(=O)N[C@H](C(=O)N[C@@H](CSSC[C@H](NC(=O)[C@H](CC=4C=CC(O)=CC=4)NC(=O)[C@H](CSSC[C@H](NC2=O)C(O)=O)NC(=O)[C@H](C)N)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H]([C@@H](C)CC)C(=O)N2[C@@H](CCC2)C(=O)N[C@@H](C)C(=O)N3)C(=O)N[C@H](C(=O)N[C@@H](CC=2C=CC(O)=CC=2)C(=O)N[C@@H](CCC(N)=O)C(=O)NCC(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CC=2C3=CC=CC=C3NC=2)C(=O)N[C@@H](C)C(=O)N1)[C@@H](C)CC)[C@@H](C)O)=O)[C@@H](C)CC)C1=CC=CC=C1 KRJOFJHOZZPBKI-KSWODRSDSA-N 0.000 description 1
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/097—Plasticisers; Charge controlling agents
- G03G9/09733—Organic compounds
- G03G9/09775—Organic compounds containing atoms other than carbon, hydrogen or oxygen
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/0827—Developers with toner particles characterised by their shape, e.g. degree of sphericity
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/097—Plasticisers; Charge controlling agents
- G03G9/09733—Organic compounds
- G03G9/09758—Organic compounds comprising a heterocyclic ring
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G9/00—Developers
- G03G9/08—Developers with toner particles
- G03G9/097—Plasticisers; Charge controlling agents
- G03G9/09783—Organo-metallic compounds
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Developing Agents For Electrophotography (AREA)
Description
該荷電制御剤は、
i)下記式〔1〕で表される化合物であり、
ii)ブラッグ角をθとしたとき、2θが10°以上40°以下の範囲で得られるCuKαのX線回折スペクトルにおいて、15.000°±0.150°及び20.100°±0.150°にピークを有し、且つ前記ピークの一方が最大強度のピークであり、他方が2番目の強度のピークであることを特徴とするトナーに関する。
<1>25℃で1時間保持
<2>11時間かけて45℃まで直線的に温度を上げる
<3>45℃で1時間保持
<4>11時間かけて25℃まで直線的に温度を下げる
円形度C=2×(π×S)1/2/L
SiCl4+2H2+O2→SiO2+4HCl
トナーの重量平均粒径(D4)は、以下のようにして算出する。測定装置としては、100μmのアパーチャーチューブを備えた細孔電気抵抗法による精密粒度分布測定装置「コールター・カウンター Multisizer 3」(登録商標、ベックマン・コールター社製)を用いる。測定条件の設定及び測定データの解析は、付属の専用ソフト「ベックマン・コールター Multisizer 3 Version3.51」(ベックマン・コールター社製)を用いる。尚、測定は実効測定チャンネル数2万5千チャンネルで行う。
(1)Multisizer 3専用のガラス製250ml丸底ビーカーに前記電解水溶液約200mlを入れ、サンプルスタンドにセットし、スターラーロッドの撹拌を反時計回りで24回転/秒にて行う。そして、専用ソフトの「アパーチャーのフラッシュ」機能により、アパーチャーチューブ内の汚れと気泡を除去しておく。
(2)ガラス製の100ml平底ビーカーに前記電解水溶液約30mlを入れる。この中に分散剤として「コンタミノンN」(非イオン界面活性剤、陰イオン界面活性剤、有機ビルダーからなるpH7の精密測定器洗浄用中性洗剤の10質量%水溶液、和光純薬工業社製)をイオン交換水で約3質量倍に希釈した希釈液を約0.3ml加える。
(3)発振周波数50kHzの発振器2個を位相を180度ずらした状態で内蔵し、電気的出力120Wの超音波分散器「Ultrasonic Dispension System Tetora150」(日科機バイオス社製)を準備する。超音波分散器の水槽内に約3.3lのイオン交換水を入れ、この水槽中にコンタミノンNを約2ml添加する。
(4)前記(2)のビーカーを前記超音波分散器のビーカー固定穴にセットし、超音波分散器を作動させる。そして、ビーカー内の電解水溶液の液面の共振状態が最大となるようにビーカーの高さ位置を調整する。
(5)前記(4)のビーカー内の電解水溶液に超音波を照射した状態で、トナー約10mgを少量ずつ前記電解水溶液に添加し、分散させる。そして、さらに60秒間超音波分散処理を継続する。尚、超音波分散にあたっては、水槽の水温が10℃以上40℃以下となる様に適宜調節する。
(6)サンプルスタンド内に設置した前記(1)の丸底ビーカーに、ピペットを用いてトナーを分散した前記(5)の電解質水溶液を滴下し、測定濃度が約5%となるように調整する。そして、測定粒子数が50000個になるまで測定を行う。
(7)測定データを装置付属の前記専用ソフトにて解析を行い、重量平均粒径(D4)を算出する。尚、前記専用ソフトでグラフ/体積%と設定したときの、「分析/体積統計値(算術平均)」画面の「平均径」が重量平均粒径(D4)である。
トナーの平均円形度は、フロー式粒子像分析装置「FPIA−3000」(シスメックス社製)によって、校正作業時の測定及び解析条件で測定した。
荷電制御剤のX線回折測定は、測定装置「RINT−TTRII」(株式会社リガク社製)と、装置付属の制御ソフト及び解析ソフトを用いる。
X線:Cu/50kV/300mA
ゴニオメータ:ロータ水平ゴニオメータ(TTR−2)
アタッチメント:標準試料ホルダー
フィルタ:不使用
インシデントモノクロ:不使用
カウンタモノクロメータ:不使用
発散スリット:解放
発散縦制限スリット:10.00mm
散乱スリット:開放
受光スリット:開放
カウンタ:シンチレーションカウンタ
走査モード:連続
スキャンスピード:4.0000°/min.
サンプリング幅:0.0200°
走査軸:2θ/θ
走査範囲:10.0000乃至40.0000°
θオフセット:0.0000°
X線のノイズによるプロファイルの乱れを除去するために行う。小さなノイズを回折ピークとして検知すると、膨大な量の回折ピークが現れてしまうこと、さらに本発明で重要な1番目、2番目の強度のピークに対しても、正確なピーク位置を算出できない可能性がある。一般的な処理方法として、平滑化処理方法は加重平均法を用い、パラメータ決定方法は自動処理を用いる。
回折ピークの強度は、バックグラウンドの位置からピーク位置までの高さを計算する。そのため回折ピークの強度を正確に算出するために、バックグラウンド除去を行う。バックグラウンド除去には、Sonnevelt−Visser法を用いる。Sonnevelt−Visser法は、強度のしきい値とピークしきい値を設定することで、バックグラウンドの値を自動的に見積もる方法である。強度のしきい値は10、ピーク幅しきい値は0.5に設定する。
入射X線Kαは強度比2:1の2成分Kα1、Kα2から成っている。これをどちらかの成分だけにして真のプロファイルを知るために、得られた回折線からKα2成分を除去する。強度比は0.5に設定する。
回折ピークを検出する。ピークサーチは手動を選択し、強度のしきい値は60、ピーク幅しきい値は0.5に設定する。
荷電制御剤の温度77KにおけるN2分子の吸着−脱着等温線は、細孔分布測定装置Tristar3000(島津製作所社製)を用いて、試料表面に窒素ガスを吸着させるガス吸着法により測定したものである。測定の概略は、島津製作所社発行の操作マニュアルに記載されており、以下の通りである。測定前には、試料管にサンプル0.3乃至0.5gを入れ、23℃で24時間真空引きを行う。真空引き終了後サンプル質量を精秤し、サンプルを得た。得られたサンプルを上記細孔分布測定装置を用いて、温度77KにおけるN2分子の吸着−脱着等温線を得た。得られた、吸着−脱着等温線より、相対圧p/p0(p0:飽和蒸気圧)が0.4の時の吸着過程の吸着量M1(cm3/g)と、相対圧p/p0が0.4の時の脱着過程の吸着量M2(cm3/g)との差(M2−M1)を算出した。
ポリエステルモノマーを下記比率で混合する。
・テレフタル酸:1.200mol
・フマル酸:3.500mol
・エチレングリコール:4.450mol
・ネオペンチルグリコール:0.600mol
ポリエステルモノマーを下記比率で混合する。
・前記式〔2〕で表されるビスフェノール誘導体(R:プロピレン基,x+yの平均値:2.2):1.250mol
・テレフタル酸:0.430mol
・イソフタル酸:0.400mol
・ドデセニル無水琥珀酸:0.170mol
スチレン70部、アクリル酸n−ブチル24部、マレイン酸モノブチル6部、ジ−t−ブチルパーオキサイド1部をキシレン200部中に4時間かけて滴下した。更に、キシレン還流下で重合を完了した。この後、昇温して有機溶剤を留去し、室温まで冷却後、粉砕し、結着樹脂(A−3)(Tg60.0℃、酸価8.5mgKOH/g)を得た。
荷電制御剤(C−1)乃至(C−6)としては、以下の特徴を持つものを使用した。
・結着樹脂(A−1):100部
・磁性酸化鉄粒子:90部
(平均粒径0.20μm、Hc=11.5kA/m、σs=85Am2/kg、σr=16Am2/kg)
・フィッシャートロプッシュワックス(サゾール社製、C105、融点105℃):2部
・荷電制御剤(C−1):1部
上記材料をヘンシェルミキサーで前混合した後、PCM−30(池貝鉄工所社製)を用い、吐出口における溶融物温度が150℃になるように、温度を設定し、溶融混練した。得られた混練物を冷却し、ハンマーミルで粗粉砕した後、粉砕機としてターボミルT250(ターボ工業社製)を用いて微粉砕した。この時の微粉砕温度は48℃であった。微粉砕温度は、粉砕機内からトナーが排出される部分で測定された温度を指す。得られた微粉砕粉末をコアンダ効果を利用した多分割分級機を用いて分級した。
<1>25℃で1時間保持
<2>11時間かけて45℃まで直線的に温度を上げる
<3>45℃で1時間保持
<4>11時間かけて25℃まで直線的に温度を下げる
トナーを所定のプロセスカートリッジに充填した。印字率2%となる横線パターンを2枚/1ジョブとして、ジョブとジョブの間にマシンがいったん停止してから次のジョブが始まるように設定したモードで、計1000枚の画出し試験を実施し、1000枚目での画像濃度を測定した。評価は常温常湿下(25.0℃,60%RH)と、トナーの帯電性能が顕著に表れやすい低温低湿下(10℃,30%RH)で行った。画像濃度は、反射濃度計であるマクベス濃度計(マクベス社製)でSPIフィルタを使用して、5mm丸のベタ黒画像の反射濃度を測定することにより測定した。数値が大きいほど現像性が良いことを示す。
現像性の評価において、1000枚耐久後の画像の白地部反射濃度最悪値をDs、画像形成前の転写材の反射平均濃度をDrとし、Dr−Dsをカブリ値とした。白地部反射濃度の測定には、反射濃度計(リフレクトメーター モデル TC−6DS 東京電色社製)を用いた。数値が小さいほどカブリ抑制が良いことを示す。
トナーを所定のプロセスカートリッジに充填し、低温低湿環境下(10℃,30%RH)で3時間調湿した。A4の75g/m2紙を用いて、画像の前半半分がベタ黒、後半半分が白地の静電オフセット試験用チャートを用いて連続100枚の画出しを行った。得られた画像の白地部を目視にて観察し、白地部にオフセットした画像が見られるかを確認した。評価基準を以下に示す。
A:1枚目から100枚目まで全く見られない。
B:1枚目からわずかに見られ、10枚目以降では全く見られない。
C:1枚目からわずかに見られ、50枚目以降では全く見られない。
D:1枚目からわずかに見られ、100枚目まで消失しない。
E:1枚目から明らかなオフセット画像が見られる。
図1に示す表面改質装置により熱処理を行う代わりに、ファカルティF−600型(ホソカワミクロン社製)を用いて機械的表面処理を行った以外は、実施例1と同様にしてトナー2を得た。ファカルティF−600型の分散ローター回転数は100s-1(回転周速を140m/sec)で15秒間処理を行った。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
図1に示す表面改質装置により表面改質を行わなかった以外は、実施例1と同様にしてトナー3を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
荷電制御剤C−2を用いた以外は、実施例3と同様にしてトナー4を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
荷電制御剤C−3を用いた以外は、実施例3と同様にしてトナー5を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
微粉砕温度を40℃とした以外は、実施例5と同様にしてトナー6を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
結着樹脂A−2を用いた以外は、実施例6と同様にしてトナー7を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
結着樹脂A−3を用いた以外は、実施例6と同様にしてトナー8を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
用いる荷電制御剤を表2のようにした以外は、実施例6と同様にして比較用トナー1乃至3を得た。得られたトナーに対して、実施例1と同様の評価を実施した。結果を表3及び表4に示す。
Claims (3)
- 該荷電制御剤の温度77KにおけるN2分子の吸着−脱着等温線において、相対圧p/p0が0.4の時の吸着過程の吸着量M1が3.0cm3/g以上8.0cm3/g以下であり、且つM1と相対圧p/p0が0.4の時の脱着過程の吸着量M2(cm3/g)との差(M2−M1)が0.4cm3/g以下である請求項1に記載のトナー。
- 該トナーは、平均円形度が0.940以上である請求項1または2に記載のトナー。
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2013
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- 2013-09-18 EP EP13838321.1A patent/EP2898373B1/en not_active Not-in-force
- 2013-09-18 KR KR1020157009292A patent/KR20150056596A/ko not_active Application Discontinuation
- 2013-09-18 TW TW102133878A patent/TWI512414B/zh active
- 2013-09-18 US US14/421,782 patent/US20150220013A1/en not_active Abandoned
- 2013-09-18 WO PCT/JP2013/075964 patent/WO2014046295A1/en active Application Filing
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US20150220013A1 (en) | 2015-08-06 |
KR20150056596A (ko) | 2015-05-26 |
TWI512414B (zh) | 2015-12-11 |
WO2014046295A1 (en) | 2014-03-27 |
CN104685419A (zh) | 2015-06-03 |
JP2014078003A (ja) | 2014-05-01 |
EP2898373A4 (en) | 2016-04-27 |
EP2898373A1 (en) | 2015-07-29 |
TW201413404A (zh) | 2014-04-01 |
EP2898373B1 (en) | 2017-03-29 |
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