JPH07106910B2 - Magnetoplumbite-type ferrite particle powder for magnetic card and method for producing the same - Google Patents
Magnetoplumbite-type ferrite particle powder for magnetic card and method for producing the sameInfo
- Publication number
- JPH07106910B2 JPH07106910B2 JP62017621A JP1762187A JPH07106910B2 JP H07106910 B2 JPH07106910 B2 JP H07106910B2 JP 62017621 A JP62017621 A JP 62017621A JP 1762187 A JP1762187 A JP 1762187A JP H07106910 B2 JPH07106910 B2 JP H07106910B2
- Authority
- JP
- Japan
- Prior art keywords
- magnetoplumbite
- magnetic
- particle powder
- ferrite particle
- magnetic card
- 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
Links
- 239000002245 particle Substances 0.000 title claims description 90
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 43
- 239000000843 powder Substances 0.000 title claims description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 32
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 17
- 238000010304 firing Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 229910052788 barium Inorganic materials 0.000 claims description 8
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 7
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 150000003438 strontium compounds Chemical class 0.000 claims description 4
- 239000000696 magnetic material Substances 0.000 description 13
- 238000009826 distribution Methods 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 8
- 239000006247 magnetic powder Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 4
- 229910052712 strontium Inorganic materials 0.000 description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、磁気カード用マグネトプランバイト型フェラ
イト粒子粉末及びその製造法に関するものである。The present invention relates to a magnetoplumbite ferrite particle powder for magnetic cards and a method for producing the same.
従来から、磁気カード用磁性材料としてマグネトプラン
バイト型フェライト粒子粉末が使用されている。マグネ
トプランバイト型フェライト粒子粉末は、バリウム、ス
トロンチウム及び鉛からなる群より選ばれた少なくとも
１種の金属元素の化合物と酸化鉄とを所定のモル比にな
るよう混合配合し、焼成、粉砕するという製法によって
得られるものであり、従前は主にモーター、発電機等の
励磁界用磁石材料等永久磁石材料として用いられていた
が、最近では、その高保磁力に着目して粒度調整を施し
た上で、磁気カード用の磁性材料として使用されてい
る。Conventionally, magnetoplumbite-type ferrite particle powder has been used as a magnetic material for magnetic cards. The magnetoplumbite type ferrite particle powder is said to be obtained by mixing and compounding at least a compound of at least one metal element selected from the group consisting of barium, strontium and lead and iron oxide in a predetermined molar ratio, followed by firing and crushing. It was obtained by a manufacturing method, and it was used as a permanent magnet material such as a magnet material for exciting magnetic field of motors and generators in the past. It is used as a magnetic material for magnetic cards.
近年、各種交通切符、グレジットカード等の磁気カード
応用製品の普及は目覚ましく、磁気カード応用製品に対
する高記録密度化の要求が益々高まってきている。In recent years, magnetic card application products such as various types of traffic tickets and credit cards have been remarkably spread, and demands for high recording density of magnetic card application products are increasing more and more.
磁気カードの高記録密度化の条件、即ち、所望の保磁力
を有し、且つ角型比が高く、しかも塗膜の表面性が優れ
ているという条件を備えた磁気カードを得るためには、
磁性材料として使用される磁性粉末の粒度分布が狭く、
適度の粒子サイズを有し、配向性が優れていることが必
要である。To obtain a magnetic card having a high recording density condition, that is, a magnetic card having a desired coercive force, a high squareness ratio, and excellent coating surface properties,
The particle size distribution of magnetic powder used as a magnetic material is narrow,
It is necessary to have an appropriate particle size and excellent orientation.
磁気カード角型比は、磁性粉末の粒度分布、粒子サイズ
及び配向性に影響を受け、特に配向性の影響は大きく、
磁性粉末の配向性が向上する程高くなる傾向にあるとさ
れている。The squareness ratio of the magnetic card is affected by the particle size distribution, particle size and orientation of the magnetic powder, and the orientation is particularly large.
It is said that the higher the orientation of the magnetic powder, the higher the tendency.
この現象は、例えば日経エレクトロニクス（日経マグロ
ウヒル社発光）1976.5.3第85頁の「角型比を高くするに
は、粒子の大きさが揃っており、針状比が大きく、磁場
配向性に優れている磁性粉が有利である。」なる記載か
ら明らかである。This phenomenon can be seen, for example, in Nikkei Electronics (Nikkei McGraw-Hill Inc.) 1976.5.3 page 85 "To increase the squareness ratio, the particles are of uniform size, the acicular ratio is large, and the magnetic field orientation is excellent. Magnetic powders are advantageous. "
この関係は、粒子形状が不定形のマグネトプランバイト
型フェライト粒子粉末についても同様に言えることなの
である。This relationship can be similarly applied to the magnetoplumbite type ferrite particle powder having an irregular particle shape.
現在、磁気カード用として用いられているマグネトプラ
ンバイト型フェライト粒子粉末は、粒子サイズが0.8μ
ｍ程度、配向度が0.75〜0.90程度のものであり、これを
磁気カード用の磁性材料として使用した場合、磁気カー
ドの角型比は0.70〜0.80程度のものとなっている。もっ
とも高い角型比を有した磁気カードを得る為の対応策と
して、ボンド磁石用に用いられているフェライト粒子粉
末を使用して角型比の高い磁気カードを得ようと検討さ
れてはいるが、この場合には用いる磁性粉末の粒子サイ
ズが１〜1.5μｍ程度と大きく、カード表面に塗布した
時、表面性の悪い塗膜となり、高記録密度の磁気カード
を得ることは困難である。また、磁気カード用の磁性材
料として平均粒径0.7〜0.9μｍ程度のマグネトプランバ
イト型フェライト粒子粉末も使用されてはいるが、周知
の通り、加熱焼成→粉砕して製造される従来のマグネト
プランバイト型フェライト粒子粉末は粗大粒子と超微粒
子とが混在している所謂粒度分布の拡いものであり、こ
のような磁性粉末を磁気カード用の磁性材料として使用
した場合、結果的には角型比が低く、しかも表面性の悪
い磁気カードしか得られなかったのである。Magnetoplumbite type ferrite particle powder currently used for magnetic cards has a particle size of 0.8μ.
m, and the degree of orientation is about 0.75 to 0.90. When this is used as a magnetic material for a magnetic card, the squareness ratio of the magnetic card is about 0.70 to 0.80. As a countermeasure to obtain a magnetic card with the highest squareness ratio, it is considered to obtain a magnetic card with a high squareness ratio by using the ferrite particle powder used for bond magnets. In this case, the particle size of the magnetic powder used is as large as about 1 to 1.5 μm, and when applied on the surface of the card, it becomes a coating film having poor surface properties, and it is difficult to obtain a magnetic card with high recording density. Also, as a magnetic material for magnetic cards, magnetoplumbite ferrite particle powder with an average particle size of 0.7 to 0.9 μm is also used, but as is well known, it is a conventional magnetoplan produced by heating and firing and crushing. The bite-type ferrite particle powder is a mixture of coarse particles and ultrafine particles, which is a so-called wide particle size distribution.When such magnetic powder is used as a magnetic material for magnetic cards, the square ratio Only a magnetic card with a low and a poor surface was obtained.
他方、最近、用途によっては保磁力の小さい磁気カード
も要求されており、この要求を満たす磁気カードの磁性
材料に、従来から保磁力低減下の為にTi、Co、Zn等の金
属元素が含有しているマグネトプランバイト型フェライ
ト粒子粉末が使用されている。この場合、保磁力低減下
の為のTi、Co、Zn等が含有されていることにより、必然
的に保磁力の低下は認められるものの同時に角型比も低
下するという欠点が生じ、高記録密度の磁気カードとは
言う難いものとなってしまうのである。On the other hand, recently, magnetic cards with low coercive force have been required for some applications, and the magnetic materials of magnetic cards that satisfy this requirement have traditionally contained metallic elements such as Ti, Co, and Zn to reduce coercive force. Magnetoplumbite type ferrite particle powder is used. In this case, since Ti, Co, Zn, etc. are contained to reduce the coercive force, the coercive force is inevitably reduced, but at the same time, the squareness ratio is also reduced, resulting in a high recording density. It is difficult to say that it is a magnetic card.
本発明者らは、マグネトプランバイト型フェライト粒子
粉末を高記録密度の磁気カード用の磁性材料として用い
るに当たり、適当な保磁力である500〜3000Oeの範囲の
保磁力を得ると同時に、表面性が優れ、且つ角型比の高
い磁気カードを得るために、粒度分布が狭く、表面性に
悪影響を与えない適度の粒子サイズを有し、且つ配向性
が優れているマグネトプランバイト型フェライト粒子粉
末を探究して来た。この探究過程において、適度の粒子
サイズを得る方法及び各種添加剤の作用効果について検
討を重ねた結果、Al2O3、SiO2とBaCl2又は／及びBi2O3
の組合わせたものの所定量を焼成前のフェライト組成に
添加することにより高記録密度の磁気カード用磁性材料
として好適な粒度分布が狭く、適度の粒子サイズを有
し、配向性が優れているマグネトプランバイト型フェラ
イト粒子粉末が得られることを見出し、本発明を完成す
るに至ったのである。The inventors of the present invention, when using the magnetoplumbite type ferrite particle powder as a magnetic material for a magnetic card having a high recording density, obtain a coercive force in the range of 500 to 3000 Oe, which is an appropriate coercive force, and at the same time have a surface property. In order to obtain an excellent magnetic card with a high squareness ratio, a magnetoplumbite-type ferrite particle powder having a narrow particle size distribution, an appropriate particle size that does not adversely affect the surface property, and excellent orientation is obtained. I've been searching. In this exploration process, as a result of repeated studies on the method of obtaining an appropriate particle size and the effect of various additives, Al 2 O 3 , SiO 2 and BaCl 2 or / and Bi 2 O 3
By adding a predetermined amount of the combination of the above to the ferrite composition before firing, a magnetic material suitable for a magnetic material for a high recording density magnetic card has a narrow particle size distribution, an appropriate particle size, and an excellent orientation. The present inventors have completed the present invention by finding that a plumbite type ferrite particle powder can be obtained.
即ち、本発明は、フィッシャーサブシーブサイザー法に
よる平均粒径が0.2〜0.7μｍで且つ配向度が0.92以上で
ある磁気カード用マグネトプランバイト型フェライト粒
子粉末及びバリウム又は／及びストロンチウムの化合物
と酸化鉄との混合物を焼成、粉砕する工程から成るモル
比Fe2O3/MO（M:Ba又は／及びSr）＝5.6〜6.1の組成を有
した磁気カード用マグネトプランバイト型フェライト粒
子粉末の製造法において、バリウム又は／及びストロン
チウムの化合物と酸化鉄との混合物に酸化鉄（Fe2O3換
算）に対して0.05〜3.00重量％のAl2O3、0.10〜3.00重
量％のSiO2と0.95〜25.00重量％のBaCl2又は／及び0.25
〜1.55重量％のBi2O3を添加混合した後、800〜1100℃の
温度範囲で焼成し、次いで粉砕してフィッシャーサブシ
ーブサイザー法による平均粒径が0.2〜0.7μｍで且つ配
向度（Br/4πIs）が0.92以上であるマグネトプランバイ
ト型フェライト粒子粉末を得ることを特徴とする磁気カ
ード用マグネトプランバイト型フェライト粒子粉末の製
造法である。That is, the present invention relates to a magnetoplumbite-type ferrite particle powder for a magnetic card having an average particle size of 0.2 to 0.7 μm and an orientation degree of 0.92 or more according to the Fisher subsieve sizer method, and a compound of barium or / and strontium and iron oxide. A process for producing a magnetoplumbite-type ferrite particle powder for a magnetic card having a composition of a molar ratio Fe 2 O 3 / MO (M: Ba or / and Sr) = 5.6 to 6.1, which comprises the steps of firing and pulverizing a mixture with In a mixture of a barium or / and strontium compound and iron oxide, 0.05 to 3.00 wt% of Al 2 O 3 , 0.10 to 3.00 wt% of SiO 2 and 0.95 to iron oxide (Fe 2 O 3 conversion) are added. 25.00 wt% BaCl 2 and / or 0.25
~ 1.55% by weight of Bi 2 O 3 was added and mixed, followed by firing in the temperature range of 800 to 1100 ° C, and then crushing to obtain an average particle size of 0.2 to 0.7 µm by the Fisher subsieve sizer method and an orientation degree (Br / 4πIs) is 0.92 or more to obtain a magnetoplumbite type ferrite particle powder, which is a method for producing a magnetoplumbite type ferrite particle powder for a magnetic card.
先ず、本発明に係る磁気カード用マグネトプランバイト
型フェライト粒子粉末は、フィッシャーサブシーブサイ
ザー法による平均粒径が0.2〜0.7μｍで且つ配向度（Br
/4πIs）が0.92以上のフェライト粒子粉末からなり、そ
の配向度の大きさに応じてこれを用いた磁気カードの角
型比も向上し、また、粒度分布が狭く、適度の粒子サイ
ズを有している為、表面性の優れた高記録密度の磁気カ
ード用の磁性材料として好適である。First, the magnetoplumbite-type ferrite particle powder for magnetic cards according to the present invention has an average particle size of 0.2 to 0.7 μm and an orientation degree (Br
/ 4πIs) is 0.92 or more, and the squareness ratio of the magnetic card using this is improved according to the degree of orientation, and the particle size distribution is narrow and the particle size is moderate. Therefore, it is suitable as a magnetic material for a high recording density magnetic card having excellent surface properties.
次に、本発明実施にあたっての諸条件について説明す
る。Next, various conditions for carrying out the present invention will be described.
本発明におけるマグネトプランバイト型フェライト粒子
粉末の組成は、Fe2O3/MO（M:Ba又は／及びSr）のモル比
を5.6〜6.1の範囲にする必要がある。この範囲外では磁
気特性、殊に飽和磁化が極端に低くなり磁気カード用の
磁性粉末として実用上望ましくない。The composition of the magnetoplumbite type ferrite particle powder in the present invention needs to have a molar ratio of Fe 2 O 3 / MO (M: Ba or / and Sr) in the range of 5.6 to 6.1. Outside this range, the magnetic properties, especially the saturation magnetization, become extremely low, which is not practically desirable as magnetic powder for magnetic cards.
平均粒径は、フィッシャーサブシーブサイザー法による
測定で0.2〜0.7μｍの範囲の大きさにする必要がある。
0.2μｍ以下の場合、角型比の低い磁気カードとなり、
0.7μｍ以上の場合には表面性の悪い塗膜を有した磁気
カードが得られ、高記録密度の磁気カード用には適さな
いものとなる。The average particle size needs to be in the range of 0.2 to 0.7 μm as measured by the Fisher subsieve sizer method.
If it is less than 0.2 μm, it becomes a magnetic card with a low squareness ratio.
When it is 0.7 μm or more, a magnetic card having a coating film with poor surface property is obtained, which is not suitable for a magnetic card having a high recording density.
配向度（Br/4πIs）は、マグネトプランバイト型フェラ
イト粒子粉末110g EVA（エチレン−酢酸ビニル共重合樹
脂）（三井ポリケミカル（株）製）15g及びステアリン
酸亜鉛0.5gを混合した後、80℃に加熱して混練し、次い
で、冷却固化した後、粉砕し、更に、該粉砕物を所定の
金型に投入し加熱溶解して10000Oeの磁場を印可した
後、冷却固化して得た成形測定試料を15KOeの磁場で測
定し、0.92以上とする必要がある。0.92以下の配向度を
有したフェライト粒子粉末を磁気カードの磁性材料とし
て使用した場合、角型比の低い磁気カードが得られ好ま
しくない。The degree of orientation (Br / 4πIs) was calculated by mixing magnetoplumbite type ferrite particle powder 110g EVA (ethylene-vinyl acetate copolymer resin) (manufactured by Mitsui Polychemical Co., Ltd.) 15g and zinc stearate 0.5g at 80 ° C. After heating and kneading, cooling and solidifying, and then crushing, further, the crushed product is put into a predetermined mold, heated and melted, and a magnetic field of 10,000 Oe is applied, followed by cooling and solidifying to obtain a molding measurement. It is necessary to measure the sample with a magnetic field of 15 KOe and to set it to 0.92 or more. When ferrite particle powder having an orientation degree of 0.92 or less is used as a magnetic material for a magnetic card, a magnetic card having a low squareness ratio is obtained, which is not preferable.
本発明に於ける酸化鉄原料としてはα−Fe2O3、γ−Fe2
O3あるいはFe3O4等のいずれもが使用できる。また、バ
リウム、ストロンチウムの原料としてはBaCO3、SrCO3が
使用できるが、加熱してBaO、SrOとなるBa化合物、Sr化
合物も使用できる。Examples of the iron oxide raw material in the present invention include α-Fe 2 O 3 and γ-Fe 2
Either O 3 or Fe 3 O 4 can be used. In addition, although BaCO 3 and SrCO 3 can be used as raw materials for barium and strontium, Ba compounds and Sr compounds that become BaO and SrO by heating can also be used.
次に、本発明に於ける添加剤について説明する。本発明
に於けるAl2O3は、酸化アルミニウム、水酸化アルミニ
ウム等のアルミニウム化合物が使用できる。その添加量
としては、酸化鉄（Fe2O3換算）に対してAl2O3換算で0.
05〜3.00重量％の間で有効である。0.05重量％以下では
本発明の目的とする効果は得られず、また、3.00重量％
以上添加した場合、生成物フェライトの飽和磁化が低下
し、且つ配向度の低い微粒子のフェライト粒子となり好
ましくない。Next, the additive in the present invention will be described. Aluminum compounds such as aluminum oxide and aluminum hydroxide can be used as Al 2 O 3 in the present invention. The amount added is 0 in terms of Al 2 O 3 with respect to iron oxide (as Fe 2 O 3 ).
Effective between 05 and 3.00% by weight. If it is less than 0.05% by weight, the desired effect of the present invention cannot be obtained.
When added in the above amount, the saturation magnetization of the product ferrite is lowered and the ferrite particles are fine particles having a low degree of orientation, which is not preferable.
本発明に於けるSiO2の添加量としては、酸化鉄（Fe2O3
換算）に対して0.10〜3.00重量％の間で有効である。0.
10重量％以下では、その添加効果が少なく、また焼成時
結晶の異常発生が見られ粒子サイズの大きいフェライト
粒子となる。また、3.00重量％以上の場合、生成物フェ
ライトの飽和磁化が低下し、しかも配向度の低いフェラ
イト粒子となり好ましくない。尚、SiO2としては二酸化
ケイ素、水ガラス等が使用できる。The amount of SiO 2 added in the present invention is iron oxide (Fe 2 O 3
(Converted) is effective between 0.10 and 3.00% by weight. 0.
When it is 10% by weight or less, the effect of addition is small, and abnormal occurrence of crystals is observed during firing, resulting in ferrite particles having a large particle size. On the other hand, when the content is 3.00% by weight or more, the saturation magnetization of the product ferrite is lowered, and further, ferrite particles having a low degree of orientation are obtained, which is not preferable. As SiO 2 , silicon dioxide, water glass or the like can be used.
本発明に於けるBaCl2の添加量としては、酸化鉄（Fe2O3
換算）に対して0.95〜25.00重量％の間で有効である。
0.95重量％以下の場合は、粒子間の焼結が部分的に発生
し単一粒子化が困難となる。他方、25.00重量％以上の
場合、本発明の目的とする効果は得られるが、経済的で
なく必要以上に添加する意味がない。The amount of BaCl 2 added in the present invention is iron oxide (Fe 2 O 3
(Converted) is effective between 0.95 and 25.00% by weight.
If it is 0.95% by weight or less, sintering between particles partially occurs and it becomes difficult to form a single particle. On the other hand, when the content is 25.00% by weight or more, the effect aimed at by the present invention can be obtained, but it is not economical and it is meaningless to add more than necessary.
本発明に於けるBi2O3の添加量としては、酸化鉄（Fe2O3
換算）に対して0.25〜1.55重量％である。0.25重量％以
下である場合には、本発明の目的を達成することができ
ない。1.55重量％以上の場合、飽和磁化が低下し、また
経済的でない。The amount of Bi 2 O 3 added in the present invention is iron oxide (Fe 2 O 3
(Converted) to 0.25 to 1.55% by weight. When it is 0.25% by weight or less, the object of the present invention cannot be achieved. When it is more than 1.55% by weight, the saturation magnetization is lowered and it is not economical.
以上、本発明の目的とする磁気カード用マグネトプラン
バイト型フェライト粒子粉末、即ち、粒子分布が狭く、
適度の粒子サイズを有し、配向性が優れているフェライ
ト粒子粉末を得ることを考慮した場合、酸化鉄（Fe2O3
換算）に対して0.05〜3.00重量％のAl2O3、0.10〜3.00
重量％のSiO2、0.95〜25.00重量％のBaCl2及び0.25〜1.
55重量％のBi2O3が好ましい。As described above, the magnetoplumbite-type ferrite particle powder for a magnetic card, which is the object of the present invention, that is, the particle distribution is narrow,
Considering obtaining ferrite particle powders with moderate particle size and excellent orientation, iron oxide (Fe 2 O 3
(Converted) 0.05 to 3.00% by weight of Al 2 O 3 , 0.10 to 3.00
Wt% SiO 2 , 0.95 to 25.00 wt% BaCl 2 and 0.25 to 1.
55% by weight of Bi 2 O 3 is preferred.
尚、本発明に於ける各添加剤を添加する時期は、焼成工
程の直前が適当である。即ち、原料配合工程、焼成工
程、粉砕工程の各工程において、焼成工程の直前の工程
である原料配合の時点に添加することができる。Incidentally, it is appropriate to add each additive in the present invention immediately before the firing step. That is, in each of the raw material blending step, the firing step, and the crushing step, it can be added at the time of raw material blending, which is the step immediately before the firing step.
本発明に於ける焼成温度範囲は、800〜1100℃の間であ
れば差支えない。800℃以下の場合、フェライト化反応
を十分に生起させることが出来ない。1100℃以上の温度
の場合には、粒子の粗大化及び粒子間相互の焼結が生起
するので好ましくない。The firing temperature range in the present invention may be between 800 and 1100 ° C. If the temperature is 800 ° C or lower, the ferritic reaction cannot be sufficiently generated. A temperature of 1100 ° C. or higher is not preferable because coarsening of particles and mutual sintering of particles occur.
尚、上記焼成温度の場合、焼成後の粉砕は例えばアトマ
イザー、アトライター等の通常の粉砕機を使用して比較
的緩和な条件で行うことができ、特別な粉砕機や強力な
粉砕は必要でない。In the case of the above-mentioned firing temperature, the pulverization after firing can be carried out under a relatively mild condition by using an ordinary pulverizer such as an atomizer or an attritor, and no special pulverizer or strong pulverization is required. .
次に、実施例並びに比較例により本発明を説明する。 Next, the present invention will be described with reference to Examples and Comparative Examples.
尚、実施例、比較例に於ける平均粒子はフィッシャーサ
ブシーブサイザー法により測定したものであり、生成物
の構造解析にはＸ線を用いた。The average particles in Examples and Comparative Examples were measured by the Fisher subsieve sizer method, and X-ray was used for structural analysis of the products.
マグネトプランバイト型フェライト粒子粉末の保磁力及
び配向度は、マグネトプランバイト型フェライト粒子粉
末110g EVA（エチレン−酢酸ビニル共重合樹脂）（三井
ポリケミカル（株）製）15g及びステアリン酸亜鉛0.5g
を混合した後、80℃に加熱して混練し、次いで冷却固化
した後、粉砕し、更に該粉砕物を所定の金型に投入し加
熱溶融して10000Oeの磁場を印加した後、冷却固して得
た成形測定試料を直流BHトレーサー（（株）横河電機
製）を使用し、測定磁場15KOeで測定した。また磁性塗
膜シートの磁気特性はV.S.M.で外部磁場10KOeの下で測
定した値である。The coercive force and degree of orientation of the magnetoplumbite-type ferrite particle powder are as follows: 110g EVA (ethylene-vinyl acetate copolymer resin) (manufactured by Mitsui Polychemicals Co., Ltd.) and 0.5g zinc stearate.
, And then kneaded by heating to 80 ° C., then cooled and solidified, and then crushed, and then the crushed product is put into a predetermined mold, heated and melted, and a magnetic field of 10,000 Oe is applied, followed by cooling and solidification. The obtained molded measurement sample was measured using a DC BH tracer (manufactured by Yokogawa Electric Co., Ltd.) with a measurement magnetic field of 15 KOe. The magnetic properties of the magnetic coating film sheet are values measured by VSM under an external magnetic field of 10 KOe.
実施例１ Fe2O3/BaOのモル比が5.9になるように、酸化鉄（α−Fe
2O3）粉末1150gと炭酸バリウム245gとを混合するに際し
て、Al2O3 2.0g（Fe2O3に対して0.18重量％に相当）、S
iO2 3.5g（Fe2O3に対して0.30重量％に相当）及びBaCl2
・2H2O 51.0g（Fe2O3に対してBaCl2換算で4.00重量％に
相当）とを複合添加し、充分混合させた後、該混合物を
1080℃で２時間焼成した。次いでこの焼成物を粉砕機で
粉砕した後、水洗し、水可溶物を除去した。得られた粒
子はＸ線分析の結果、マグネトプランバイト型バリウム
フェライト粒子であり、組成分析の結果、Fe2O3/BaO＝
5.98であった。Example 1 Iron oxide (α-Fe) was used so that the molar ratio of Fe 2 O 3 / BaO was 5.9.
2 O 3 ) powder 1150 g and barium carbonate 245 g are mixed, Al 2 O 3 2.0 g (equivalent to 0.18 wt% with respect to Fe 2 O 3 ), S
iO 2 3.5g (equivalent to 0.30% by weight with respect to Fe 2 O 3 ) and BaCl 2
・ 2H 2 O 51.0 g (corresponding to 4.00 wt% in terms of BaCl 2 with respect to Fe 2 O 3 ) was added in a composite manner and mixed sufficiently, and then the mixture was mixed.
It was baked at 1080 ° C for 2 hours. Next, this fired product was crushed with a crusher and then washed with water to remove water-soluble substances. The obtained particles were magnetoplumbite type barium ferrite particles as a result of X-ray analysis, and Fe 2 O 3 / BaO =
It was 5.98.
得られたマグネトプランバイト型バリウムフェライト粒
子粉末の平均粒径はフィッシャーサブシーブサイザー法
により測定した結果、0.55μｍであり、電子顕微鏡観察
の結果、粒度分布の狭いものであった。また、磁気測定
の結果、保磁力IHcは2480Oe、配向度（Br/4πIs）は0.9
40であった。The average particle size of the obtained magnetoplumbite-type barium ferrite particle powder was 0.55 μm as a result of measurement by the Fisher subsieve sizer method, and as a result of electron microscope observation, the particle size distribution was narrow. As a result of magnetic measurement, the coercive force I Hc is 2480 Oe and the degree of orientation (Br / 4πIs) is 0.9.
It was 40.
続いて、上記のマグネトプランバイト型フェライト粒子
粉末を用いて、下記に示した通りの組成に配合し、ボー
ルミルにより８時間混合分散させ磁性塗料を得た。Subsequently, the above-mentioned magnetoplumbite-type ferrite particle powder was blended into the composition shown below and mixed and dispersed by a ball mill for 8 hours to obtain a magnetic coating material.
マグネトプランバイト型バリウム フェライト粒子粉末 100.0重量％ 塩化ビニル酢酸ビニル共重合体： 25.5重量％ ブタジエンアクリロニトリルゴム（5:1） トルエン 83.3重量％ メチルエチルケトン 138.0重量％ メチルイソブチルケトン 46.0重量％ レシチン 4.0重量％ リン酸エステル 4.0重量％ 得られた磁性塗料を20μｍのポリエチレンテレフタレー
トのフィルム上に厚さ４μｍに塗布して磁場配向処理
後、乾燥して磁性塗料膜シートを作成した。得られた磁
性塗膜シートの磁気特性を測定した結果、保磁力IHc:24
60Oe、角型比は0.91であり、表面性の優れたものであっ
た。Magnetoplumbite type barium ferrite powder 100.0% by weight Vinyl chloride vinyl acetate copolymer: 25.5% by weight Butadiene acrylonitrile rubber (5: 1) Toluene 83.3% by weight Methyl ethyl ketone 138.0% by weight Methyl isobutyl ketone 46.0% by weight Lecithin 4.0% by weight phosphoric acid Ester 4.0% by weight The obtained magnetic paint was applied on a 20 μm polyethylene terephthalate film to a thickness of 4 μm, subjected to a magnetic field orientation treatment, and dried to prepare a magnetic paint film sheet. As a result of measuring the magnetic properties of the obtained magnetic coating film sheet, coercive force I Hc: 24
The surface ratio was 60 Oe and the squareness ratio was 0.91, and the surface properties were excellent.
実施例２〜９、比較例１〜6; 酸化鉄原料の種類、Ba若しくはSr化合物の種類及び量、
添加剤の種類及び量、及び焼成温度を種々変化させた以
外は、実施例１と同様にしてマグネトプランバイト型バ
リウムフェライト粒子粉末、マグネトプランバイト型ス
トロンチウムフェライト粒子粉末又はマグネトプランバ
イト型バリウム−ストロンチウム複合フェライト粒子粉
末を得た。Examples 2-9, Comparative Examples 1-6; type of iron oxide raw material, type and amount of Ba or Sr compound,
Magnetoplumbite-type barium ferrite particle powder, magnetoplumbite-type strontium ferrite particle powder or magnetoplumbite-type barium-strontium was prepared in the same manner as in Example 1 except that the type and amount of the additive and the firing temperature were variously changed. A composite ferrite particle powder was obtained.
実施例２〜９で得られたマグネトプランバイト型フェラ
イト粒子粉末は、電子顕微鏡観察の結果、いずれも粒度
分布幅の狭いものであり、適度の粒子サイズを有し、且
つ配向度（Br/4πIs）の高いものであった。The magnetoplumbite-type ferrite particle powders obtained in Examples 2 to 9 were all observed by electron microscopy and had a narrow particle size distribution width, an appropriate particle size, and an orientation degree (Br / 4πIs). ) Was high.
また、得られたマグネトプランバイト型フェライト粒子
を用いて、実施例１と同様にして磁性塗膜シートを作製
した。得られた磁性塗膜シートはいずれも角型比が高
く、しかも表面性の優れたものであった。Further, a magnetic coating film sheet was produced in the same manner as in Example 1 by using the obtained magnetoplumbite type ferrite particles. The obtained magnetic coating film sheets all had a high squareness ratio and excellent surface properties.
比較例１、３、５及び６で得られたマグネトプランバイ
ト型バリウムフェライト粒子粉末は、適度の粒子サイズ
を有するものの粒度分布が広く、配向度の低いものであ
った。また、比較例２及び４で得られたマグネトプラン
バイト型バリウムフェライト粒子粉末は、角型比の高い
磁気カードに適したものではあるが、粒子サイズが大き
い為に表面性の悪い塗膜となり、結果的に高記録密度の
磁気カード用磁性材料としては適さないものであった。The magnetoplumbite-type barium ferrite particle powders obtained in Comparative Examples 1, 3, 5 and 6 had a moderate particle size, but had a wide particle size distribution and a low degree of orientation. Further, the magnetoplumbite type barium ferrite particle powders obtained in Comparative Examples 2 and 4 are suitable for a magnetic card having a high squareness ratio, but since the particle size is large, they become a coating film having poor surface properties, As a result, it was not suitable as a magnetic material for high recording density magnetic cards.
この時の主要製造条件及び諸特性を表１に示す。Table 1 shows the main manufacturing conditions and various characteristics at this time.
〔効果〕 本発明に係る磁気カード用マグネトプランバイト型フェ
ライト粒子粉末は、前述実施例に示した通り、粒度分布
がより狭く、適度の粒子サイズを有し、且つ配向度（Br
/4πIs）が大きいので、これを用いてなる磁気カードも
所望の保磁力を有し、且つ角型比が高く、しかも表面性
の優れた高記録密度のものとなる。 [Effect] The magnetoplumbite-type ferrite particle powder for magnetic cards according to the present invention has a narrower particle size distribution, an appropriate particle size, and an orientation degree (Br
Since / 4πIs) is large, a magnetic card using this also has a desired coercive force, a high squareness ratio, and a high recording density with excellent surface properties.
また、本発明方法によれば、Fe2O3/MO（M:Ba又は／及び
Sr）モル比5.6〜6.1の組成からなるバリウム又は／及び
ストロンチウムの化合物と酸化鉄との混合物にAl2O3、S
iO2とBaCl2又は／及びBi2O3とを添加する系において、
粒度分布がより狭く、フィッシャーサブシーブサイザー
法による平均粒径が0.2〜0.7μｍを有し、配向度（Br/4
πIs）が0.92以上の磁気カード用マグネトプランバイト
型フェライト粒子粉末が得られる。Further, according to the method of the present invention, Fe 2 O 3 / MO (M: Ba or / and
Sr) a mixture of barium and / or strontium compounds having a molar ratio of 5.6 to 6.1 and iron oxide in a mixture of Al 2 O 3 and S
In a system in which iO 2 and BaCl 2 or / and Bi 2 O 3 are added,
The particle size distribution is narrower, the average particle size according to the Fisher subsieve sizer method is 0.2 to 0.7 μm, and the degree of orientation (Br / 4
Magnetoplumbite type ferrite particle powder for magnetic cards with πIs) of 0.92 or more is obtained.
更に、保磁力低減下の為に用いられるTi、Co、Zn等を添
加しても角型比を低下させることなく保磁力を制御する
ことができる。Furthermore, the coercive force can be controlled without lowering the squareness ratio even if Ti, Co, Zn or the like used for reducing the coercive force is added.
図１は、実施例１で得られたマグネトプランバイト型バ
リウムフェライト粒子の粒子構造を示す電子顕微鏡写真
（×5,000）であり、図２は比較例１で得られたマグネ
トプランバイト型バリウムフェライト粒子の粒子構造を
示す電子顕微鏡写真（×5,000）である。1 is an electron micrograph (× 5,000) showing the particle structure of the magnetoplumbite-type barium ferrite particles obtained in Example 1, and FIG. 2 is the magnetoplumbite-type barium ferrite particles obtained in Comparative Example 1. 2 is an electron micrograph (× 5,000) showing the particle structure of
Claims (2)
平均粒径が0.2〜0.7μｍで且つ配向度（Br/4πIs）が0.
92以上であることを特徴とする磁気カード用マグネトプ
ランバイト型フェライト粒子粉末。1. A Fischer subsieve sizer method has an average particle size of 0.2 to 0.7 μm and an orientation degree (Br / 4πIs) of 0.1.
A magnetoplumbite-type ferrite particle powder for magnetic cards, which is 92 or more.
物と酸化鉄との混合物を焼成、粉砕する工程から成るモ
ル比Fe2O3/MO（M:Ba又は／及びSr）＝5.6〜6.1の組成を
有した磁気カード用マグネトプランバイト型フェライト
粒子粉末の製造法において、バリウム又は／及びストロ
ンチウムの化合物と酸化鉄との混合物に、酸化鉄（Fe2O
3換算）に対して0.05〜3.00重量％のAl2O3、0.10〜3.00
重量％のSiO2と0.95〜25.00重量％のBaCl2又は／及び0.
25〜1.55重量％のBi2O3を添加混合した後、800〜1100℃
の温度範囲で焼成し、次いで粉砕してフィッシャーサブ
シーブサイザー法による平均粒径が0.2〜0.7μｍで且つ
配向度（Br/4πIs）が0.92以上であるマグネトプランバ
イト型フェライト粒子粉末を得ることを特徴とする磁気
カード用マグネトプランバイト型フェライト粒子粉末の
製造法。2. A composition having a molar ratio of Fe 2 O 3 / MO (M: Ba or / and Sr) = 5.6 to 6.1, which comprises a step of firing and pulverizing a mixture of a barium or / and strontium compound and iron oxide. In the method for producing a magnetoplumbite-type ferrite particle powder for a magnetic card, the mixture of a barium or / and strontium compound and iron oxide is mixed with iron oxide (Fe 2 O
3 basis) relative to 0.05 to 3.00 wt% of Al 2 O 3, 0.10~3.00
Wt% SiO 2 and 0.95 to 25.00 wt% BaCl 2 and / or 0.
25 to 1.55 was added and mixed by weight% of Bi 2 O 3, 800~1100 ℃
Firing in the temperature range of, and then pulverizing to obtain a magnetoplumbite-type ferrite particle powder having an average particle size of 0.2 to 0.7 μm and an orientation degree (Br / 4πIs) of 0.92 or more by the Fischer subsieve sizer method. A method for producing a magnetoplumbite-type ferrite particle powder for a characteristic magnetic card.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62017621A JPH07106910B2 (en) | 1987-01-27 | 1987-01-27 | Magnetoplumbite-type ferrite particle powder for magnetic card and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62017621A JPH07106910B2 (en) | 1987-01-27 | 1987-01-27 | Magnetoplumbite-type ferrite particle powder for magnetic card and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63185825A JPS63185825A (en) | 1988-08-01 |
| JPH07106910B2 true JPH07106910B2 (en) | 1995-11-15 |
Family
ID=11948941
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62017621A Expired - Fee Related JPH07106910B2 (en) | 1987-01-27 | 1987-01-27 | Magnetoplumbite-type ferrite particle powder for magnetic card and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07106910B2 (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5526605B2 (en) | 2008-05-27 | 2014-06-18 | 株式会社島津製作所 | Impact test equipment |
-
1987
- 1987-01-27 JP JP62017621A patent/JPH07106910B2/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5526605B2 (en) | 2008-05-27 | 2014-06-18 | 株式会社島津製作所 | Impact test equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63185825A (en) | 1988-08-01 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |