JP2005070756A - トナー - Google Patents
トナー Download PDFInfo
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- JP2005070756A JP2005070756A JP2004219543A JP2004219543A JP2005070756A JP 2005070756 A JP2005070756 A JP 2005070756A JP 2004219543 A JP2004219543 A JP 2004219543A JP 2004219543 A JP2004219543 A JP 2004219543A JP 2005070756 A JP2005070756 A JP 2005070756A
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- HNEGQIOMVPPMNR-UHFFFAOYSA-N methylfumaric acid Natural products OC(=O)C(C)=CC(O)=O HNEGQIOMVPPMNR-UHFFFAOYSA-N 0.000 description 4
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- YLLIGHVCTUPGEH-UHFFFAOYSA-M potassium;ethanol;hydroxide Chemical compound [OH-].[K+].CCO YLLIGHVCTUPGEH-UHFFFAOYSA-M 0.000 description 4
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 3
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
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- Developing Agents For Electrophotography (AREA)
Abstract
【解決手段】円相当径3μm以上400μm以下のトナー粒子における平均円形度が0.935以上0.970未満、該トナー粒子の平均面粗さが5.0nm以上35.0nm未満、ポリエステル樹脂またはビニル系重合体ユニットとポリエステルユニットとのハイブリッド樹脂を含有し、トナーのTHF可溶分のGPCの分子量分布において、分子量1万未満の成分M1が40〜70質量%、分子量1万乃至5万の成分M2の含有量が25〜50質量%、分子量5万を超える成分M3の含有量が2〜25質量%、分子量10万以上の成分の含有量が10質量%末満で、かつ分子量1万未満の成分の含有量をM1とし、分子量1万乃至5万の成分の含有量をM2とし、分子量5万を超える成分の含有量をM3としたときにM1≧M2>M3を満足する。
【選択図】 なし
Description
該トナー粒子のフロー式粒子像測定装置で計測される円相当径3μm以上400μm以下のトナー粒子における平均円形度が0.935以上0.970未満であり、該トナー粒子の走査型プローブ顕微鏡で測定される平均面粗さが5.0nm以上35.0nm未満であることを特徴とし、
前記結着樹脂は、ポリエステル樹脂またはビニル系重合体ユニットとポリエステルユニットとを有するハイブリッド樹脂を少なくとも含有し、
トナーのテトラヒドロフラン可溶分のゲルパーミエーションクロマトグラフィーの分子量分布において、分子量1万未満の成分M1の含有量が40〜70質量%であり、分子量1万乃至5万の成分M2の含有量が25〜50質量%であり、分子量5万を超える成分M3の含有量が2〜25質量%であり、分子量10万以上の成分の含有量が10質量%末満であり、
かつ分子量1万未満の成分の含有量をM1とし、分子量1万乃至5万の成分の含有量をM2とし、分子量5万を超える成分の含有量をM3としたときにM1≧M2>M3を満足することを特徴とするトナーに関する。
円形度a=L0/L (1)
〔式中、L0は粒子像と同じ投影面積を持つ円の周囲長を示し、Lは512×512の画像処理解像度(0.3μm×0.3μmの画素)で画像処理した時の粒子投影像の周囲長を示す。〕
UH−150(株式会社エス・エム・テー社製)
OUTPUT レベル:5
コンスタントモード
プローブステーション:SPI3800N(セイコーインスツルメンツ(株)製)
測定ユニット:SPA400
測定モード:DFM(共振モード)形状像
カンチレバー:SI−DF40P
解像度:Xデータ数 256
Yデータ数 128
1)トナー45mgをサンプル瓶に入れ、メタノールを10ml加える。
2)超音波洗浄機で1分間試料を分散させて外添剤を分離させる。
3)吸引ろ過(10μmメンブランフィルター)してトナー粒子と外添剤を分離する。磁性体を含むトナーの場合は、磁石をサンプル瓶の底にあててトナー粒子を固定して上澄み液だけ分離させても構わない。
4)上記2)、3)を計3回行い、得られたトナー粒子を真空乾燥機で室温で十分に乾燥させる。
・平均面粗さ(Ra)
JIS B0601で定義されている中心線平均粗さRaを、測定面に対して適用できるよう三次元に拡張したもの。基準面から指定面までの偏差の絶対値を平均した値で次式で表される。
S0:指定面が理想的にフラットであると仮定したときの面積
Z0:指定面内のZデータ(指定面に対して垂直方向のデータ)の平均値
指定面とは、本発明においては1μm四方の測定エリアを意味する。
指定面内におけるZデータの最大値と最小値の差。
・表面積(S)
指定面の表面積。
下記1)〜5)の操作により求められる。基本操作はJIS K−0070に属する。
1)試料はあらかじめ結着樹脂(重合体成分)以外の添加物を除去して使用するか、試料の結着樹脂以外の成分の含有量を求めておく。トナー又は結着樹脂の粉砕品0.5〜2.0gを精秤する。このときの結着樹脂成分をWgとする。
2)300(ml)のビーカーに試料を入れ、トルエン/エタノール(4/1)の混合液150(ml)を加え溶解する。
3)0.1mol/lのKOHのエタノール溶液を用いて、電位差滴定測定装置を用いて測定する。この滴定には、例えば、京都電子株式会社の電位差的定測定装置AT−400(win workstation)とABP−410電動ビュレットとを用いての自動滴定が利用できる。
4)この時のKOH溶液の使用量をS(ml)とする。同時にブランクを測定して、この時のKOHの使用量をB(ml)とする。
5)下記式により酸価を計算する。なお下記式中のfはKOHのファクターである。
酸価(mgKOH/g)={(S−B)×f×5.61}/W
下記1)〜8)の操作により求められる。基本操作はJIS K−0070に属する。
1)試料はあらかじめ結着樹脂(重合体成分)以外の添加物を除去して使用するか、試料の結着樹脂以外の成分の含有量を求めておく。トナー又は結着樹脂の粉砕品0.5〜2.0gを200ml平底フラスコに精秤する。
2)これにアセチル化試薬(無水酢酸25gを全量フラスコ(100ml)に取り、ピリジンを加えて全量を100mlにし、十分撹拌する)を5mlを加える。なお試料が溶解しにくい場合は、少量のピリジンを追加するか、キシレン又はトルエンを加え溶解する。
3)フラスコの口に小さなロートを置き、温度95〜100℃のグリセリン浴中に低部約1cmを浸して加熱する。フラスコの首がグリセリン浴の熱を受けて温度が上がるのを防ぐために、中に丸い穴をあけた厚紙の円板をフラスコの首の付け根に被せる。
4)1時間後フラスコにグリセリン浴から取り出し、放冷後ロートから水1mlを加えて振り動かし無水酢酸を分解する。
5)さらに分解を完全にするため、再びフラスコをグリセリン浴中で10分間加熱し、放冷後エタノール5mlでロート及びフラスコ壁を洗う。
6)フェノールフタレイン溶液数滴を指示薬として加え、0.5kmol/m3水酸化カリウムエタノール溶液で滴定し、指示薬の薄い紅色が焼く30秒間続いたときを終点とする。
7)樹脂を入れないで2)〜6)を空試験として行う。
8)下記式により水酸基価を計算する。
A=[{(B−C)×28.05×f}/S]+D
(但し、Aは水酸基価(mgKOH/g)であり、Bは空試験に用いた0.5kmol/m3水酸化カリウムエタノール溶液の量(ml)であり、Cは滴定に用いた0.5kmol/m3水酸化カリウムエタノール溶液の量(ml)であり、fは0.5kmol/m3水酸化カリウムエタノール溶液のファクターであり、
Sは試料中に含まれる結着樹脂の量(g)であり、Dは試料の酸価である。なお式中「28.05」は水酸化カリウムの式量(56.11×1/2)である。)
(1)ビニル系重合体とポリエステル樹脂を別々に製造した後、有機溶剤に溶解/膨潤させ、エステル化触媒、必要に応じてアルコール類を添加して、加熱することによりエステル化反応又は/及びエステル交換反応を行った後、有機溶媒を留去する。この製造方法では前記反応時にワックス類を添加しても良い。
(2)ビニル系重合体の存在下に、ポリエステル系モノマーを添加し、重合並びにビニル系重合体とのエステル化反応又は/及びエステル交換反応を行う。この製造方法では、反応時に、必要に応じてさらにビニル系モノマーを添加し重合しても良い。また、この製造方法では、有機溶剤が適宜使用される。また、この製造方法では、前記(1)と同様に、反応時にワックス類を添加しても良い。
(3)ポリエステル樹脂の存在下に、ビニル系モノマーを添加し、重合並びにエステル化反応又は/及びエステル交換反応を行う。この製造方法では、反応時に、必要に応じてさらにポリエステル系モノマーを添加し重合しても良い。また、この製造方法では、前記(2)と同様に有機溶剤を適宜使用することができ、前記(1)と同様に反応時にワックスを添加しても良い。
(4)ビニル系重合体及びポリエステル樹脂存在下に、ビニル系モノマー及び/又はポリエステル系モノマーを添加し、重合並びにエステル化反応又は/及びエステル交換反応を行う。この製造方法でも、前記(2)と同様に有機溶剤を適宜使用することができ、前記(1)と同様に反応時にワックスを添加しても良い。
(5)ビニル系モノマー及びポリエステル系モノマーを混合して付加重合及び縮重合反応並びにエステル化反応又は/及びエステル交換反応を行う。この製造方法でも、前記(2)と同様に有機溶剤を適宜使用することができ、前記(1)と同様に反応時にワックスを添加しても良い。
(6)上記(1)〜(5)で製造されたハイブリッド樹脂成分を含有する樹脂を、さらにビニル系重合体及び/又はポリエステル系樹脂と、例えば有機溶剤に溶解/膨潤させるなどして混合して、有機溶剤を留去する。
(7)上記(1)〜(5)で製造されたハイブリッド樹脂成分を含有する樹脂の存在下に、さらにビニル系モノマー及び/又はポリエステル系モノマーを添加し、重合並びにエステル化反応又は/及びエステル交換反応を行う。この製造方法でも、前記(2)と同様に有機溶剤を適宜使用することができ、前記(1)と同様に反応時にワックスを添加しても良い。
・ガラス転移点(Tg)
昇温時のDSC曲線において比熱変化の現われる前後のベースラインの中間点を結ぶ線とDSC曲線の交点の温度。
前記結着樹脂が、ポリエステル樹脂またはビニル系重合体ユニットとポリエステルユニットとを有するハイブリッド樹脂を少なくとも含有し、
トナーのテトラヒドロフラン可溶分のゲルパーミエーションクロマトグラフィーの分子量分布において、分子量1万未満の成分の含有量が40〜70質量%であり、分子量1万乃至5万の成分の含有量が25〜50質量%であり、分子量5万を超える成分の含有量が2〜25質量%であり、分子量10万以上の成分の含有量が10質量%末満であり、
かつ分子量1万未満の成分の含有量をM1とし、分子量1万乃至5万の成分の含有量をM2とし、分子量5万を超える成分の含有量をM3としたときにM1≧M2>M3を満足することを特徴とすること
を同時に満たすことが現像スリーブへのトナー融着現象の発生を抑制する点で好ましい。
で表わされるモノマーの単重合体:前述したスチレン、アクリル酸エステル、メタクリル酸エステルの如き重合性モノマーとの共重合体を正荷電性制御剤として用いることができる。この場合これらの荷電制御剤は、結着樹脂(の全部または一部)としての作用をも有する。
BPA−PO(ビスフェノールA プロピレンオキサイド付加物(2mol付加))
30mol%
BPA−EO(ビスフェノールA エチレンオキサイド付加物(2mol付加))
13mol%
TPA(テレフタル酸) 39mol%
TMA(トリメリット酸無水物) 17mol%
上記ポリエステル系モノマーをジブチルチンオキサイド7.0mmolとともにオートクレーブに仕込み、減圧装置、水分離装置、窒素ガス導入装置、温度測定装置及び撹拌装置を装着し、窒素雰囲気下にて減圧しながら常法にしたがって210℃まで加熱し、縮重合反応を行うことにより、ポリエステル樹脂aを得た。結着樹脂aの物性を表3に示す。
ポリエステル系モノマーの組成を表3のようにして、ポリエステル樹脂製造例と同様にして各ポリエステル樹脂を得た。各結着樹脂の物性を表3に示す。
BPA−PO 35mol%
BPA−EO 15mol%
TPA 11mol%
TMA 22mol%
FA 17mol%
ポリエステル系モノマーの組成を上記のようにして、ポリエステル樹脂製造例と同様にしてポリエステル樹脂Dを得た。
ポリエステル系モノマーの組成を表3のようにして、ポリエステル樹脂製造例と同様にして各ポリエステル樹脂を得た。
スチレン83質量%と、アクリル酸−n−ブチル17質量%とを付加重合してスチレン−アクリル樹脂を得た。これを結着樹脂nとする。
・結着樹脂a 100質量部
・磁性体 95質量部
・アルミ化合物(構造式(I)) 0.5質量部
・モノアゾ鉄錯体 2質量部
・低分子ポリエチレン1 2質量部
上記混合物をヘンシェルミキサーで前混合した後、130℃に加熱された2軸エクストルーダで溶融混練し、冷却した混練物をハンマーミルで粗粉砕してトナー粗粉砕物を得た。得られた粗粉砕物を、機械式粉砕機ターボミル(ターボ工業社製;回転子および固定子の表面に炭化クロムを含有したクロム合金めっきでコーティング(めっき厚150μm、表面硬さHV1050))を用いて、表4の条件表に基づき、エアー温度を調整して機械式粉砕させて微粉砕し、得られた微粉砕物をコアンダ効果を利用した多分割分級装置(日鉄鉱業社製エルボジェット分級機)で微粉及び粗粉を同時に分級除去した。そこで得られた原料トナー粒子のコールターカウンター法で測定される重量平均粒径(D4)は6.5μm、4μm未満のトナー粒子の個数平均分布の累積値は26.3%であった。
用いる結着樹脂、磁性体、ワックスを表4のようにして、更にターボミルの微粉砕条件を表5に示すように変更し、多分割分級装置での分級条件を変更し、更に表面改質装置の条件を表4に示すようにした以外はトナー1と同様にしてトナー2〜8を得た。トナー粒子2〜10の、FPIA2100で測定された物性、及び走査型プローブ顕微鏡測定値を表7に示す。また、トナー樹脂に関するDSC、THF不溶分、GPCの分析結果を表6に示す。
用いる結着樹脂、磁性体、ワックスを表4のようにして、更にターボミルの微粉砕条件を表5に示すように変更し、多分割分級装置での分級条件を変更し、得られたトナー粒子を300℃の熱風中を瞬間的に通過させる処理を行った以外はトナー1と同様にしてトナー13及び15を得た。トナー粒子13及び15の、FPIA2100で測定された物性、及び走査型プローブ顕微鏡測定値を表7に示す。また、トナー樹脂に関するDSC、THF不溶分、GPCの分析結果を表6に示す。トナー13の、FPIA2100で測定された円相当径3μm以上400μm以下のトナーにおける平均円形度は0.934であり、走査型プローブ顕微鏡で測定されるトナー13の平均面粗さは44.2nmであった。
用いる結着樹脂、磁性体、ワックスを表4のようにして、更にターボミルの微粉砕条件を表5に示すように変更し、多分割分級装置での分級条件を変更し、更に表面改質装置による表面改質を行わなかった以外はトナー1と同様にしてトナー16を得た。トナー粒子16の、FPIA2100で測定された物性、及び走査型プローブ顕微鏡測定値を表7に示す。また、トナー樹脂に関するDSC、THF不溶分、GPCの分析結果を表6に示す。
次に、調製されたトナーを用いて、以下に示すような方法によって評価を行った。評価結果を表8及び表9に示す。
低温低湿環境下(15℃,10%RH)、高温高湿環境下(32.5℃,80%RH)の各環境下で、プロセススピードが1.1倍になるように本体を改造し、連続印字にて、印字比率5%で複写機用普通紙(A4サイズ:75g/m2)に8000枚の画出し試験を行い、一日放置して再び8000枚、計16000枚の画出し試験を行った。結果を表8に示す。
常温常湿環境下(23℃,60%RH)で印字比率4%の画像で複写機用普通紙(A4サイズ:75g/m2)に5000枚の画出し試験を行う前後で、トナー容器内のトナー量を測定し、画像1枚あたりのトナー消費量を測定した。結果を表8に示す。
通常の複写機用普通紙(A4サイズ:75g/m2)に、低温低湿環境下(15℃,10%RH)で16000枚プリントアウトし、4000枚ごとにスリーブネガゴーストの評価を行った。ゴーストに関する画像評価には、スリーブ一周分だけベタ黒の帯を出力した後ハーフトーンの画像を出力した。パターンの概略図を図3に示す。評価方法は、一枚のプリント画像のうち、スリーブ2周目で、1周目で黒画像が形成された場所(黒印字部)と、されない場所(非画像部)での、マクベス濃度反射計により測定された反射濃度の差を下記のごとく算出した。ネガゴーストは、一般的にスリーブ2周目で出る画像において、スリーブ1周目に黒印字部だった部分の画像濃度が、スリーブ1周目に非画像部だった部分の画像濃度よりも低く、1周目で出したパターンの形がそのまま現れるゴースト現象である。ここの濃度差を、反射濃度差を測定することにより評価を行った。
反射濃度差=反射濃度(像形成されない場所)−反射濃度(像形成された場所)
反射濃度差 0.00以上0.02未満:A
0.02以上0.04未満:B
0.04以上0.06未満:C
0.06以上 :D
低温低湿環境下での耐久において、初期と16000枚時に100μm(潜像)ラインでの格子パターン(1cm間隔)をプリントし、その飛び散りを光学顕微鏡を用いて目視で評価した。結果を表8に示す。
A:ラインが非常にシャープで飛び散りはほとんどない
B:わずかに飛び散っている程度でラインは比較的シャープ
C:飛び散りがやや多くラインがぼんやりした感じになる
D:Cのレベルに満たない
低温定着性については、前記評価装置の定着ユニットを取り出し通常の1.2倍のプロセススピードにおいて評価できるよう改造を加えた。加熱定着装置において150〜240℃温度範囲で加熱用ヒータの温度を5℃おきに制御し、定着ローラーの表面の温度が一定になってから、未定着トナー像が形成された記録材を定着ニップ部に挿入し、得られた画像を、4.9kPaの荷重をかけたシルボン紙で5往復摺擦を行い、摺擦前後の画像濃度の濃度低下率が10%以下になる定着温度を低温定着性とした。この温度が低いほど低温定着性に優れたトナーである。未定着画像としては、普通紙(75g/m2)を用い、紙上のトナー現像量を0.6mg/cm2に設定したベタ黒画像の定着を行った。
高温高湿環境における耐久後の現像剤担持体表面を目視で観察し、現像剤汚染の程度を下記の基準で評価した。
A:軽微な汚染が観察される。
B:やや汚染が観察される。
C:部分的に汚染が観察される。
D:著しい汚染が観察される。
32 微粉回収
33 原料供給口
34 ライナー
35 冷風導入口
36 分散ローター
37 製品排出口
38 排出弁
39 ガイドリング
40 角型ディスク
41 第一の空間
42 第二の空間
Claims (10)
- 結着樹脂、着色剤を少なくとも含有するトナー粒子と無機微粒子からなるトナーにおいて、
該トナー粒子のフロー式粒子像測定装置で計測される円相当径3μm以上400μm以下のトナー粒子における平均円形度が0.935以上0.970未満であり、該トナー粒子の走査型プローブ顕微鏡で測定される平均面粗さが5.0nm以上35.0nm未満であることを特徴とし、
前記結着樹脂は、ポリエステルユニットを少なくとも含有し、
トナーのテトラヒドロフラン可溶分のゲルパーミエーションクロマトグラフィーの分子量分布において、分子量1万未満の成分M1の含有量が40〜70質量%であり、分子量1万乃至5万の成分M2の含有量が25〜50質量%であり、分子量5万を超える成分M3の含有量が2〜25質量%であり、分子量10万以上の成分の含有量が10質量%末満であり、
かつ分子量1万未満の成分の含有量をM1とし、分子量1万乃至5万の成分の含有量をM2とし、分子量5万を超える成分の含有量をM3としたときにM1≧M2>M3を満足することを特徴とするトナー。 - 該トナー粒子のフロー式粒子像測定装置で計測される円相当径0.6μm以上400μm以下のトナー粒子における個数基準粒径分布において、0.6μm以上3μm未満のトナー粒子比率が0個数%以上20個数%未満であることを特徴とする請求項1に記載のトナー。
- 前記着色剤の含有量が結着樹脂100質量部に対して30〜200質量部であることを特徴とする請求項1又は2に記載のトナー。
- 該トナー粒子の円形度0.960未満のトナー粒子の個数累積値が20個数%以上70個数%未満であることを特徴とする請求項1乃至3のいずれかに記載のトナー。
- 該トナー粒子の走査型プローブ顕微鏡で測定される最大高低差が50nm以上250nm未満であることを特徴とする請求項1乃至4のいずれかに記載のトナー。
- 該トナー粒子の走査型プローブ顕微鏡で測定される、トナー粒子の表面の1μm四方のエリアを測定した時の表面積が1.03μm2以上1.33μm2未満であることを特徴とする請求項1乃至5のいずれかに記載のトナー。
- 前記結着樹脂は、ポリエステル樹脂、ハイブリッド樹脂の混合物、ポリエステル樹脂とハイブリッド樹脂との混合物、ビニル系樹脂とハイブリッド樹脂との混合物、及びポリエステル樹脂とビニル系樹脂とハイブリッド樹脂との混合物、からなるグループから選択される混合物であることを特徴とする請求項1乃至6のいずれかに記載のトナー。
- 前記結着樹脂は、ポリエステル樹脂またはポリエステル樹脂とハイブリッド樹脂との混合物を含有し、かつトナーのテトラヒドロフラン不溶分の含有量が1〜50質量%であることを特徴とする請求項1乃至7のいずれかに記載のトナー。
- 前記結着樹脂は、二種以上のハイブリッド樹脂の混合物を含有し、かつトナーのテトラヒドロフラン不溶分の含有量が25質量%以下であることを特徴とする請求項1乃至7のいずれかに記載のトナー。
- 該トナーのフロー式粒子像測定装置で計測される円相当径3μm以上400μm以下のトナーにおける平均円形度が0.935以上0.970未満であり、該トナーの走査型プローブ顕微鏡で測定される平均面粗さが10.0nm以上26.0nm未満であることを特徴とする請求項1乃至9のいずれかに記載のトナー。
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JP2007279400A (ja) * | 2006-04-07 | 2007-10-25 | Canon Inc | トナー及び画像形成方法 |
US7608379B2 (en) | 2005-08-18 | 2009-10-27 | Sharp Kabushiki Kaisha | Toner and manufacturing method thereof |
US7939231B2 (en) | 2005-04-22 | 2011-05-10 | Canon Kabushiki Kaisha | Magnetic toner |
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US7939231B2 (en) | 2005-04-22 | 2011-05-10 | Canon Kabushiki Kaisha | Magnetic toner |
US7608379B2 (en) | 2005-08-18 | 2009-10-27 | Sharp Kabushiki Kaisha | Toner and manufacturing method thereof |
JP2007279400A (ja) * | 2006-04-07 | 2007-10-25 | Canon Inc | トナー及び画像形成方法 |
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