JP2005162597A - Mg系フェライト並びに該フェライトを用いた電子写真現像用キャリア及び現像剤 - Google Patents
Mg系フェライト並びに該フェライトを用いた電子写真現像用キャリア及び現像剤 Download PDFInfo
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- JP2005162597A JP2005162597A JP2004264875A JP2004264875A JP2005162597A JP 2005162597 A JP2005162597 A JP 2005162597A JP 2004264875 A JP2004264875 A JP 2004264875A JP 2004264875 A JP2004264875 A JP 2004264875A JP 2005162597 A JP2005162597 A JP 2005162597A
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- based ferrite
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- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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Abstract
【解決手段】 本発明のMg系フェライト材料は、Li, Na, K, Rb, Cs, Ca, Sr, Ba, Y, La, Ti, Zr, Hf, V, Nb, Ta, Al, Ga, Si, Ge, P, Sb, Bi, またはそれらの組み合わせを含み、飽和磁化が30〜80emu/gであり、絶縁破壊電圧が1.5〜5.0 kVである。該Mg系フェライト材料により、高画質化と環境規制への対応を図ることができる。
【選択図】 図1
Description
電子写真法は複写機、プリンタ、FAXなど幅広い分野で用いられているが、さらなる高画質化、高解像度化、並びに階調性及び細線再現性の改善等が求められている。画質低下の原因の一つは、キャリアを介した静電潜像電位のリークである。このリーク現象は、低抵抗のキャリアで起きやすい。しかし、当初は高抵抗のキャリアであっても高電圧を印加することにより絶縁破壊が起き、その結果、リークが起きることがある。
XaMgbFecCadOe (1)
(XはLi, Na, K, Rb, Cs, Sr, Ba, Y, La, Ti, Zr, Hf, V, Nb, Ta, Al, Ga, Si, Ge, P, Sb, Bi, またはそれらの組み合わせであり;
a, b, c, 及びdは
0.001 ≦ R(X) ≦ 0.15,
(ただしR(X)は以下の式:
R(X)= a×(Aw(X) + (n/2)×Aw(O)) / ( a×(Aw(X) + (n/2)×Aw(O)) + b×Fw(MgO) + (c/2)×Fw(Fe2O3) + d×Fw(CaO) )
で表され、;
Aw(X)及びAw(O)はそれぞれX及びOの原子量を表し;
nはXの酸化数を表し;
Fw(A)はAの式量を表す)
0.01 ≦ b/(b+c/2) ≦ 0.85, 及び
0 ≦ R(Ca) ≦ 0.15
(ただしR(Ca)は以下の式:
R(Ca)= d×Fw(CaO) / (a×(Aw(X) + (n/2)×Aw(O)) + b×Fw(MgO) + (c/2)×Fw(Fe2O3) + d×Fw(CaO)) ;
で表され、
Fw(A)はR(X)について記載の通りである)
を充たし、
eはX, Mg, Fe, 及びCaの酸化数により定まる数である)
の組成を有するMg系フェライト材料により解決される。
また上記課題は、該Mg系フェライト材料を含む電子写真現像用キャリア、該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により解決する。
XaMgbFecCadOe (1)
(XはLi, Na, K, Rb, Cs, Sr, Ba, Y, La, Ti, Zr, Hf, V, Nb, Ta, Al, Ga, Si, Ge, P, Sb, Bi, またはそれらの組み合わせであり;
a, b, c, 及びdは
0.001 ≦ R(X) ≦ 0.15,(ただしR(X)は以下の式:
R(X)= a×(Aw(X) + (n/2)×Aw(O)) / (a×(Aw(X) + (n/2)×Aw(O)) + b×Fw(MgO) + (c/2)×Fw(Fe2O3) + d×Fw(CaO) )
で表され、;Aw(X)及びAw(O)はそれぞれX及びOの原子量を表し;nはXの酸化数を表し;Fw(A)はAの式量を表す)
0.01 ≦ b/(b+c/2) ≦ 0.85, 及び
0 ≦ R(Ca) ≦ 0.15(ただしR(Ca)は以下の式
R(Ca)= d×Fw(CaO) / ( a×(Aw(X) + (n/2)×Aw(O)) + b×Fw(MgO) + (c/2)×Fw(Fe2O3) + d×Fw(CaO) )
で表され; Fw(A)はR(X)について記載の通りである)
を充たし、
eはX, Mg, Fe, 及びCaの酸化数により定まる数である)
の組成を有する。
b/(b+c/2)は、Mg系フェライト材料中のMg及びFeのモル量をそれぞれMgO及びFe2O3のモル量に換算した場合のMgO及びFe2O3のモル量の和 (b+c/2) に対するMgOのモル量 ( b ) の割合を表す。従って、b/(b+c/2)が大きい組成はMgリッチ組成に対応し、b/(b+c/2)が小さい組成はFeリッチ組成に対応する。本発明においてb/(b+c/2)は0.01以上、好ましくは0.05以上、より好ましくは0.10以上であり、0.85以下、好ましくは0.70以下である。b/(b+c/2)が上記範囲未満では、過剰のFe2O3の生成によって絶縁破壊電圧が低下する傾向にあり、b/(b+c/2)が上記範囲を超えると、非磁性相(例えばMgO相)が過剰に生成し飽和磁化が低下しやすい。
以上の通り、本発明のMg系フェライト材料では絶縁破壊電圧及び/又は飽和磁化が向上する結果、階調性に優れた高品質の画像を得ることができる。
本発明のMg系フェライト材料の絶縁破壊電圧は、1.5 kV以上、好ましくは2.5 kV以上である。絶縁破壊電圧が低すぎると、現像の際に感光体上の静電潜像電位のリークが生じ、キャリアの寿命低下も起きることがある。キャリアが高い絶縁破壊電圧を有する場合には、高い画質が長期間保持されるため、絶縁破壊電圧の上限に制限はないが、他の特性を充足するために10.0 kV以下、好ましくは7.5 kV以下、さらに好ましくは5.0 kV以下とすることができる。
該Mg系フェライト材料の平均粒径は、0.01μm以上、好ましくは0.1μm以上、2μm以上、好ましくは5μm以上、さらに好ましくは10μm以上であり、200μm以下、好ましくは150μm以下である。粒径が小さすぎると感光体に付着しやすくなり、大きすぎると画像が粗くなり画質が低下する。平均粒径は、各種公知の造粒手段、粉砕手段、及び分級手段により制御することができる。
本発明の製造方法は、混合工程i)に続き、不活性ガス雰囲気下で焼成して粒子を成長させる粒子成長工程ii)と、酸素含有雰囲気下で熱処理を行って金属の酸化数、結晶構造、占有率、磁気構造等を制御するコンディショニング工程iii)との少なくとも2つの加熱工程を含む。そして加熱工程の条件、例えば酸素濃度、焼成温度、焼成時間、熱処理温度及び熱処理時間を調整することにより、絶縁破壊電圧や飽和磁化といった磁性キャリアに求められる特性を制御することが可能である。例えば、工程iii)を工程ii)より高い酸素濃度雰囲気で行い、工程ii)の最高到達温度を工程iii)より高くすることができる。なお、上記の工程ii)の前に仮焼を行ってもよい。工程ii)と工程iii)とは別々の工程としてもよく、連続して行ってもよい。
本発明のMg系フェライトキャリアは、トナーと所定の比率で混合して2成分現像剤として用いることができる。2成分系現像剤の場合、トナー濃度はキャリアに対し2〜40重量%であることが好ましい。トナーとしては各種公知のトナーを使用することができ、その製造方法も特に制限されるものではなく、粉砕トナーであっても重合トナーでもよい。
[実施例1〜27]
〔Mg系フェライト材料の製造〕
MgO、Fe2O3、CaO、及び表1に記載の添加物を原料として用い、Mg系フェライト材料を製造した。まず、これらの原料を表1に示す組成となるよう秤量した。秤量した原料をバインダー(ポリビニルアルコール)、分散剤、及び消泡剤とともに水に加え、湿式ボールミルで4時間粉砕混合し、スラリーを作製した。スラリー濃度は50重量%であった。スラリー中の原料の総量に対する消泡剤の量は0.1重量%であり、分散剤の量は0.15重量%であった。
<飽和磁化の測定>
飽和磁化測定には振動試料型磁力計(VSMP-lS,東英工業製)を用い、試料を測定用カプセル(0.0565cc)に充填して磁場14kOeで測定した。
<絶縁破壊電圧の測定>
絶縁破壊電圧測定は、N極およびS極を対向させ磁極間間隔8mmとした測定器でおこなった(磁極:表面磁束密度1500G、対向磁極面積10×30mm)。測定器の概要を図1に示す。この磁極間に非磁性の平行平板電極(電極面積10×40mm、電極間隔4mm)を配置し、該電極間に試料を200mg入れ、磁力により電極間に試料を保持した。耐電圧試験器(TOS5051、菊水電子工業製)を用いて交流電圧を印加し、漏れ電流値が110mA以上となる印加電圧値を絶縁破壊電圧とした。
<電気抵抗>
電気抵抗測定には上記の絶縁破壊電圧測定と同様の電極に試料を保持し、絶縁抵抗測定器(TR-8601、武田理研製)を用いて直流電圧100Vを印加して測定した。
[比較例1〜5] MgO、Fe2O3、及びCaOを表2記載の組成となるよう秤量分取し、実施例1〜27と同様の方法によりMg系フェライトを製造した。
[比較例6] MgO、Fe2O3、及びCaOに加えてB2O3も原料として用いた点を除き、比較例1〜5と同様の方法によりMg系フェライトを製造した。
[実施例28]
〔Mg系フェライト材料の製造〕
MgO、Fe2O3、CaO、及び表3に記載の添加物を原料として用い、Mg系フェライト材料を製造した。まず、これらの原料を表3に示す組成となるよう秤量した。秤量した原料をバインダー(ポリビニルアルコール)、分散剤、及び消泡剤とともに水に加え、湿式ボールミルで4時間粉砕混合し、スラリーを作製した。スラリー濃度は50重量%であった。スラリー中の原料の総量に対する消泡剤の量は0.1重量%であり、分散剤の量は0.15重量%であった。
〔コーティングキャリアの製造〕
得られたMg系フェライト材料をコア材としてシリコーン樹脂で被覆し、コーティングキャリアを製造した。被覆処理は、Mg系フェライトにトルエンで希釈したシリコーン樹脂溶液をスプレーコーティングし、続いて200℃で熱処理することにより行った。なお、被覆樹脂量はコア材の1.0重量%とした。
〔コーティング残存率評価〕
コーティングキャリアを市販の2成分系現像用トナー(負荷電性トナー)と混合し、現像剤とした。該現像剤中のトナー濃度は、6重量%であった。混合は市販の複写機の現像槽を用いて行い、該現像剤を回転数400rpmで4時間(常温・常湿環境2時間+高温・高湿環境2時間)撹拌した。常温・常湿環境は温度23℃、湿度55%であり、高温・高湿環境は温度35℃、湿度85%である。撹拌過程でコーティングが残存した割合(コーティング残存率)は、撹拌前と撹拌後のコーティングキャリアについて蛍光X線分析を行い、SiとFeのX線強度から以下の式により算出した。使用した装置は、理学電機製のZSX-100eであった。
(Sif:撹拌後のSiのX線強度;Fef:撹拌後のFeのX線強度;Sii:撹拌前のSiのX線強度;Fei:撹拌前のFeのX線強度)
結果を表3に示す。
酸素濃度20vol.%の窒素雰囲気中における450℃での熱処理を省略した点を除き、実施例28と同様にしてMg系フェライト材料及びMg系フェライトキャリアを製造した。原料の組成は表3に示す通りである。飽和磁化、絶縁破壊電圧、電気抵抗、及びコーティング残存率の測定も、実施例28と同様に行った。
[実施例29]
〔Mg系フェライト材料の製造〕
MgO、Fe2O3、CaO、及び表4に記載の添加物を原料として用い、Mg系フェライト材料を製造した。まず、これらの原料を表4に示す組成となるよう秤量した。秤量した原料をバインダー(ポリビニルアルコール)、分散剤、及び消泡剤とともに水に加え、湿式ボールミルで4時間粉砕混合し、スラリーを作製した。スラリー濃度は50重量%であった。スラリー中の原料の総量に対する消泡剤の量は0.1重量%であり、分散剤の量はO.15重量%であった。得られたスラリーをスプレードライヤにて造粒乾燥し、球状ペレットとした。この球状ペレットを電気炉にて窒素雰囲気中において130O℃で焼成した。窒素雰囲気中の酸素濃度は1000ppm以下となるように調整した。さらに、この焼成物を酸素濃度20vo1.%の窒素雰囲気中において450℃で熱処理した。その後、解砕、分級して平均粒径35μmのMg系フェライトを得た。得られたMg系フェライトの飽和磁化、絶縁破壊電圧、及び電気抵抗を表4に示す。
〔コーティングキャリアの製造〕
得られたMg型フェライト材料をコア材としてシリコーン樹脂で被覆し、コーティングキャリアを製造した。被覆処理は、Mg系フェライトにトルエンで希釈したシリコーン樹脂溶液をスプレーコーティングし、続いて200℃で熱処理することにより行った。被覆樹脂量は、コア材の1.0重量%とした。
〔帯電量変化率測定〕
100ccのガラスビンにコーティングキャリア47.5gと市販の2成分系現像用トナー(負荷電性トナー)2.5gとを入れ、常温常湿下にてボールミル(110rpm)で撹拌し、現像剤とした。該現像材剤中のトナー濃度は5重量%であった。コーティングキャリア及びトナーの撹拌を開始してから30秒後と2時間後に、帯電量を測定した。帯電量の変化は、撹拌から30秒後の帯電量(A)と撹拌から2時間後の帯電量(B)の測定値に基づき、帯電量変化率として以下の式で評価した。
結果を表4に示す。
酸素濃度20vol.%の窒素雰囲気中における450℃での熱処理を省略した点を除き、実施例29と同様にしてMg系フェライト材料及びMg系フェライトキャリアを製造した。原料の組成は表4に示す通りである。飽和磁化、絶縁破壊電圧、電気抵抗、及び帯電量変化率の測定も、実施例28と同様に行った。
以上の実施例では、Caを含有するMg系フェライト材料についてLi, Na, Sr, B, Al, Si, P, K, Ti, V, Y, Zr, Bi, 又はLaの添加による効果を示すが、かかる効果はCaを含有するMg系フェライト材料に限定されるものではない。
2:真鍮
3磁極
4:テフロン(登録商標)支持台
Claims (17)
- 式(1):
XaMgbFecCadOe (1)
(XはLi, Na, K, Rb, Cs, Sr, Ba, Y, La, Ti, Zr, Hf, V, Nb, Ta, Al, Ga, Si, Ge, P, Sb, Bi, またはそれらの組み合わせであり;
a, b, c, 及びdは
0.001 ≦ R(X) ≦ 0.15,
(ただしR(X)は以下の式:
R(X)= a×(Aw(X) + (n/2)×Aw(O)) / ( a×(Aw(X) + (n/2)×Aw(O)) + b×Fw(MgO) + (c/2)×Fw(Fe2O3) + d×Fw (CaO) )
で表され、;
Aw(X)及びAw(O)はそれぞれX及びOの原子量を表し;
nはXの酸化数を表し;
Fw(A)はAの式量を表す)
0.01 ≦ b/(b+c/2) ≦ 0.85, 及び
0 ≦ R(Ca) ≦ 0.15
(ただしR(Ca)は以下の式
R(Ca)= d×Fw(CaO) / ( a×(Aw(X) + (n/2)×Aw(O)) + b×Fw(MgO) + (c/2)×Fw(Fe2O3) + d×Fw (CaO))
で表され ;
Fw(A)はR(X)について記載の通りである)
を充たし、
eはX, Mg, Fe, 及びCaの酸化数により定まる数である)
の組成を有するMg系フェライト材料。 - XがLi, Na, K, Sr, Y, La, Ti, Zr, V, Al, Si, P, Bi, またはそれらの組み合わせである請求項1に記載のMg系フェライト材料。
- 絶縁破壊電圧が1.5〜5.0kVである請求項1又は2に記載のMg系フェライト材料。
- 飽和磁化が30〜80emu/gである請求項1〜3の何れかに記載のMg系フェライト材料。
- b及びcが
0.01 ≦ b/(b+c/2) ≦ 0.30
を充たす請求項1〜4の何れかに記載のMg系フェライト材料。 - 平均粒子径が0.01〜150μmである請求項1〜5のいずれかに記載のMg系フェライト材料。
- 請求項1〜6の何れかに記載のMg系フェライト材料を含む電子写真現像用キャリア。
- 樹脂で被覆された請求項1〜6の何れかに記載のMg系フェライト材料を含む電子写真現像用キャリア。
- 請求項7又は8に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。
- キャリアに対するトナーの重量比が2〜40重量%である請求項9記載の電子写真用現像剤。
- i)原料を混合する工程とii)最高到達温度が800〜1500℃である粒子成長工程とiii)最高到達温度が300〜1000℃である酸素含有雰囲気でのコンディショニング工程とを含む、請求項1乃至6の何れかに記載のMg系フェライトの製造方法。
- 工程iii)の雰囲気の酸素濃度が工程ii)の雰囲気の酸素濃度よりも高い、請求項11記載の方法。
- 工程iii)の雰囲気が酸素濃度0.05〜25.0vol.%の不活性ガス雰囲気である請求項11又は12に記載の方法。
- 工程ii)の雰囲気が酸素濃度0.001〜10.0vol.%の不活性ガス雰囲気である請求項11〜13の何れかに記載の方法。
- 原料混合工程i)がMg含有化合物及びFe含有化合物を含むスラリーを作成する工程と該スラリーを造粒乾燥する工程とを含む、請求項11〜14の何れかに記載の方法。
- Mg含有化合物及びFe含有化合物を含むスラリーが、Li, Na, K, Rb, Cs, Sr, Ba, Y, La, Ti, Zr, Hf, V, Nb, Ta, Al, Ga, Si, Ge, P, Sb, Bi, Ca又はそれらの組み合わせを含有する化合物をさらに含む、請求項15に記載の方法。
- Mg含有化合物及びFe含有化合物を含むスラリーがバインダーをさらに含み、スラリー中の原料の総量に対するバインダーの量が0.1〜5重量%である、請求項15又は16に記載の方法。
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PCT/JP2004/016811 WO2005048276A2 (en) | 2003-11-12 | 2004-11-05 | An mg-based ferrite, an electrophotographic development carrier containing the ferrite, and developer containing the carrier |
US10/578,901 US7476482B2 (en) | 2003-11-12 | 2004-11-05 | Mg-based ferrite, an electrophotographic development carrier containing the ferrite, and developer containing the carrier |
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JP4668574B2 (ja) | 2011-04-13 |
WO2005048276A3 (en) | 2008-01-10 |
US7476482B2 (en) | 2009-01-13 |
WO2005048276A2 (en) | 2005-05-26 |
US20070087282A1 (en) | 2007-04-19 |
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