JP5735999B2 - フェライト粒子及びそれを用いた電子写真現像用キャリア、電子写真用現像剤並びにフェライト粒子の製造方法 - Google Patents
フェライト粒子及びそれを用いた電子写真現像用キャリア、電子写真用現像剤並びにフェライト粒子の製造方法 Download PDFInfo
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- JP5735999B2 JP5735999B2 JP2013069622A JP2013069622A JP5735999B2 JP 5735999 B2 JP5735999 B2 JP 5735999B2 JP 2013069622 A JP2013069622 A JP 2013069622A JP 2013069622 A JP2013069622 A JP 2013069622A JP 5735999 B2 JP5735999 B2 JP 5735999B2
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Description
Fe2O3(平均粒径:0.6μm)を71.7wt%、Mn3O4(平均粒径:2μm)を28.3wt%で混合したものを、900℃で2時間、大気中で加熱して仮焼粉を得た。この仮焼粉20.0kgとSrフェライト(平均粒径:1.2μm)1.1kgとを水7.0kg中に分散し、分散剤としてポリカルボン酸アンモニウム系分散剤を239g、還元剤としてカーボンブラックを60.2g添加し、湿式ボールミル(メディア径2mm)により粉砕処理し、混合スラリーを得た。
このスラリーをスプレードライヤーにて約130℃の熱風中に噴霧し、乾燥造粒粉を得た。なお、このとき、目的の粒度分布以外の造粒粉は、ふるいにより除去した。この造粒粉を、電気炉に投入し、1110℃で3時間焼成した。この焼成工程においては、酸素濃度が5000ppmとなる電気炉内の雰囲気で加熱を行い、酸素濃度が15000ppmとなる電気炉内の雰囲気で冷却を行った。得られた焼成物を解粒後にふるいを用いて分級し、平均粒径35μmとした。
さらに、得られた焼成物に対して、440℃、大気下で1時間保持することにより高抵抗化処理を施しフェライト粒子を得た。
得られたフェライト粒子の組成、物性、磁気特性、電気特性、機械的特性を下記に示す方法で測定した。測定結果を表2に示す。また、図1にフェライト粒子のSEM写真を示す。
なお、得られたフェライト粒子において、マンガン組成比を示す上記したいわゆるxの値は、0.8であり、鉄組成比を示す3−xの値については、2.2であった。得られた結晶相は、MnFe 2 O 4 、SrO・nFe 2 O 3 (n=0.5〜6.5)と考えられる。
キーエンス社製「VK-210、VK-X200」を用いて下記手順で測定した。
1.プレパラート上にカーボーンテープを貼り付け、その上にサンプルを固定する。
2.顕微鏡上に25μmスケールバーを表示させ、倍率3000倍で25μm付近の粒子 を数個、撮影できる視野を探す。
3.その後、明るさを自動設定し、画像を取り込む。取り込んだ画像とプロファイルデー タの両方を確認しながら、水平線プロファイルを手動で引き、粒子径を見積もり、2 5μm付近の粒子を解析する。
(凹凸度)
画像の前処理としてピークノイズの除去(カットレベル;通常)を実施する。次に、解析する粒子トップを中心に20μm平方エリアを指定して曲率補正(傾き補正、球面補正(自動))を実行する。そして、解析する粒子トップの中央付近(粒子トップ)φ10μm(内接円の内側)を測定エリアとして指定し、カットオフ(λs0.25μm、λc0.08mm)を実施する。その後、データを出力して1粒子ごとのRz値を凹凸度として測定した。なお、粒子間のばらつきを考慮するため、100個の粒子を測定し、その平均値を凹凸度とした。
(グレインの大きさの標準偏差)
画像の前処理としてピークノイズの除去(カットレベル;通常)を実施する。次に、解析する粒子トップを中心に20μm平方エリアを指定して曲率補正(傾き補正、球面補正(自動))を実行する。次に、
(1)解析する粒子トップの中央付近(粒子トップ10μm平方エリア)を測定エリアとして、長さ10μmの測定ライン10本を定める。
(2)10本の測定ラインについて、光量値をラインスキャンして測定する(カットオフ(λs0.25μm、λc0.08mm))。
(3)各測定ラインについて、以下の測定計算をする。
A:光量レンジの中央値を基準面とし、基準面を超える部分の山の底面(幅)を測定する。
B:測定された複数の幅の長さについて、標準偏差を算出する(各ラインのSD)。
(4)10本についての各ラインのSDの値の平均値を各粒子のSDとする。
(5)100個の粒子について測定し、その平均値を表に記載した結晶サイズのばらつきσとする。
図4に、粒子表面のグレインの大きさの標準偏差σの算出例を示す。
室温専用振動試料型磁力計(VSM)(東英工業株式会社製、VSM−P7)を用いて、外部磁場0〜50000(エルステッド)の範囲で1サイクル連続的に印加して磁化σ1kを測定した。
BET一点法比表面積測定装置(「Macsorb HM model-1208」マウンテック社製)を用いて、サンプル8.500gを容積5mLのセルに充填し、200℃で30分間脱気して測定した。
JIS Z 2504に準拠して測定した。
フェライト粒子9.5g、市販のフルカラー機のトナー0.5gを100mlの栓付きガラス瓶に入れ、25℃、相対湿度50%の環境下で12時間放置して調湿する。調湿したフェライト粒子とトナーを振とう器で30分間振とうし混合する。ここで、振とう器については、株式会社ヤヨイ製のNEW−YS型を用い、200回/分、角度60°で行った。混合したフェライト粒子とトナーを500mg計量し、帯電量測定装置で帯電量を測定した。帯電量測定装置としては、日本パイオテク社製「STC-1-C1型」を用い、吸引圧力5.0kPa、吸引用メッシュはSUS製の795meshを用いた。同一サンプルについて2回の測定を行い、これらの平均値を帯電量とした。帯電量は下記式から算出される。
帯電量(μC/g)=実測電荷(nC)×10 3 ×係数(1.0083×10 −3 )÷トナー重量
(式中、トナー重量=(吸引前重量(g)−吸引後重量(g)))
フェライト粒子の表面を樹脂で被覆したキャリアの帯電量は、フェライト粒子の帯電量と同様にして測定した。なお、測定は温度25℃、湿度50%RHの雰囲気下で行った。
フェライト粒子30gを、サンプルミル(「SK−M10型」協立理工株式会社製)に投入し、回転数14000rpmで60秒間撹拌する。次いで、レーザー回折式粒度分布測定装置(「マイクロトラックModel9320−X100」日機装社製)を用いて、粒径22μm以下の累積粒子頻度を測定する。そして、サンプルミルによる処理前後の、粒径22μm以下の累積粒子頻度の増加率(%)を算出し、粒子強度の指標とした。増加率が小さいほど、粒子の強度は高いこと意味する。
フェライト粒子及びSrフェライト粒子の平均粒径は、日機装社製「マイクロトラック Model9320-X100」を用いて測定した。
シリコーン樹脂(東レダウコーニング社製SR2411)を、トルエンに溶解させてコーティング樹脂溶液を準備した。そして、フェライト粒子と樹脂溶液とを重量比で9:1で撹拌機に装填し、温度150℃〜250℃で3時間加熱撹拌した。次いで、熱風循環式加熱装置に投入し温度250℃で5時間加熱を行い、被覆樹脂層を硬化させてキャリアを作製した。
このキャリア95重量部と平均粒径5μm程度のトナー5重量部とを、ポットミルを用いて所定時間混合し電子写真用現像剤を作製した。この二成分系の電子写真用現像剤を、デジタル反転現像方式の60cpm機相当の評価機に投入して、初期、100k枚、200k枚の画像形成の後、目視により下記基準で画像評価した。
◎:試験画像を非常によく再現している。
○:試験画像をほぼ再現している。
△:試験画像をほとんど再現していない。
×:試験画像を全く再現していない。
原料として平均粒径2.5μmのSrフェライトを用いた以外は、実施例1と同様にしてフェライト粒子を得た。そして、実施例1と同様にして物性等を測定した。測定結果を表2に合わせて示す。
実施例1のフェライト粒子と組成が同じになるように、原料として平均粒径2.5μmのSrフェライトを0.55kg配合した以外は、実施例1と同様にしてフェライト粒子を得た。そして、実施例1と同様にして物性等を測定した。測定結果を表2に合わせて示す。
実施例1のフェライト粒子と組成が同じになるように、原料として平均粒径2.5μmのSrフェライトを2.2kg配合した以外は、実施例1と同様にしてフェライト粒子を得た。そして、実施例1と同様にして物性等を測定した。測定結果を表2に合わせて示す。
実施例1のフェライト粒子と組成が同じになるように、Srフェライト粒子に換えてSrCO3を146g配合した以外は、実施例1と同様にしてフェライト粒子を得た。そして、実施例1と同様にして物性等を測定した。測定結果を表2に合わせて示す。
実施例1のフェライト粒子と組成が同じになるように、原料として平均粒径5.0μmのSrフェライトを1.1kg配合した以外は、実施例1と同様にしてフェライト粒子を得た。そして、実施例1と同様にして物性等を測定した。測定結果を表2に合わせて示す。
Claims (5)
- Mnフェライトを主相とし、Srフェライトを含有するフェライト粒子であって、粒子表面の凹凸度が2.5μm〜4.5μmの範囲であり、粒子表面に現れているグレインの大きさの標準偏差が1.5μm〜3.5μmの範囲であることを特徴とするフェライト粒子。
- 請求項1記載のフェライト粒子の表面を樹脂で被覆したことを特徴とする電子写真現像用キャリア。
- 請求項2記載の電子写真現像用キャリアとトナーとを含む電子写真用現像剤。
- Fe成分原料、Mn成分原料、体積平均粒径が1.0μm〜4.5μmのSrフェライト粒子を分散媒中に投入してスラリーを得る工程と、前記スラリーを噴霧乾燥して造粒物を得る工程と、前記造粒物を焼成して焼成物を得る工程とを有することを特徴とするフェライト粒子の製造方法。
- Srフェライト粒子の添加量がFe成分原料とMn成分原料の総量に対して2.5wt%〜15wt%の範囲である請求項4記載のフェライト粒子の製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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JP2013069622A JP5735999B2 (ja) | 2013-03-28 | 2013-03-28 | フェライト粒子及びそれを用いた電子写真現像用キャリア、電子写真用現像剤並びにフェライト粒子の製造方法 |
US14/773,973 US9507285B2 (en) | 2013-03-28 | 2014-02-26 | Ferrite particles and electrophotographic development carrier using same, electrophotographic developer and method of manufacturing ferrite particles |
EP14775103.6A EP2980023A4 (en) | 2013-03-28 | 2014-02-26 | FERRITE PARTICLES AND ELECTROPHOTOGRAPHIC REVELATING MEDIUM EMPLOYING THEM, ELECTROPHOTOGRAPHIC DEVELOPER AND PROCESS FOR PRODUCTION OF FERRITE PARTICLES |
KR1020157024631A KR101940594B1 (ko) | 2013-03-28 | 2014-02-26 | 페라이트 입자 및 이것을 사용한 전자 사진 현상용 캐리어, 전자 사진용 현상제 및 페라이트 입자의 제조 방법 |
PCT/JP2014/054591 WO2014156437A1 (ja) | 2013-03-28 | 2014-02-26 | フェライト粒子及びそれを用いた電子写真現像用キャリア、電子写真用現像剤並びにフェライト粒子の製造方法 |
CN201480018910.0A CN105073644B (zh) | 2013-03-28 | 2014-02-26 | 铁氧体颗粒及使用其的电子照相显影用载体、电子照相用显影剂以及铁氧体颗粒的制造方法 |
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JP (1) | JP5735999B2 (ja) |
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JP6631200B2 (ja) * | 2015-11-27 | 2020-01-15 | 株式会社リコー | キャリア、二成分現像剤、補給用現像剤、プロセスカートリッジ、画像形成装置および画像形成方法 |
JP6757284B2 (ja) * | 2017-03-31 | 2020-09-16 | Dowaエレクトロニクス株式会社 | キャリア芯材並びにそれを用いた電子写真用キャリア及び電子写真用現像剤 |
JP6302123B1 (ja) * | 2017-08-25 | 2018-03-28 | パウダーテック株式会社 | 電子写真現像剤用磁性芯材、電子写真現像剤用キャリア及び現像剤 |
JP7099902B2 (ja) * | 2018-08-07 | 2022-07-12 | Dowaエレクトロニクス株式会社 | キャリア芯材 |
JP7151413B2 (ja) * | 2018-11-22 | 2022-10-12 | 株式会社リコー | 電子写真画像形成用キャリア、電子写真画像形成用現像剤、電子写真画像形成方法、電子写真画像形成装置およびプロセスカートリッジ |
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JP2001022123A (ja) * | 1999-07-09 | 2001-01-26 | Fujitsu Ltd | 電子写真用トナー及び画像形成方法 |
JP2006053201A (ja) * | 2004-08-10 | 2006-02-23 | Ricoh Co Ltd | 電子写真用キャリア、現像剤及び画像形成装置 |
JP4544099B2 (ja) * | 2005-08-26 | 2010-09-15 | 富士ゼロックス株式会社 | 静電潜像現像用キャリア及び静電潜像現像用現像剤 |
US7824833B2 (en) | 2005-11-30 | 2010-11-02 | Powdertech Co., Ltd. | Resin-coated ferrite carrier for electrophotographic developer, its production method, and electrophotographic developer using the resin-coated ferrite carrier |
US20090197190A1 (en) * | 2008-02-01 | 2009-08-06 | Canon Kabushiki Kaisha | Two-component developer, replenishing developer, and image-forming method using the developers |
JP2011141542A (ja) * | 2009-12-11 | 2011-07-21 | Fuji Xerox Co Ltd | 静電潜像現像用キャリア、及び静電潜像現像用現像剤 |
EP2555056B1 (en) | 2010-03-31 | 2017-01-25 | DOWA Electronics Materials Co., Ltd. | Carrier core material for electrophotographic developing agent, carrier for electrophotographic developing agent, and electrophotographic developing agent |
JP5742319B2 (ja) * | 2011-03-11 | 2015-07-01 | 株式会社リコー | トナー、現像剤及び画像形成方法 |
JP2013035737A (ja) * | 2011-08-11 | 2013-02-21 | Dowa Electronics Materials Co Ltd | フェライト粒子の製造方法 |
JP5650773B2 (ja) * | 2013-02-25 | 2015-01-07 | Dowaエレクトロニクス株式会社 | 電子写真現像剤用キャリア芯材の製造方法、電子写真現像剤用キャリア芯材、電子写真現像剤用キャリア、および電子写真現像剤 |
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KR101940594B1 (ko) | 2019-01-21 |
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