JPS6367705A - Manufacture of magnetic iron powder - Google Patents
Manufacture of magnetic iron powderInfo
- Publication number
- JPS6367705A JPS6367705A JP61212119A JP21211986A JPS6367705A JP S6367705 A JPS6367705 A JP S6367705A JP 61212119 A JP61212119 A JP 61212119A JP 21211986 A JP21211986 A JP 21211986A JP S6367705 A JPS6367705 A JP S6367705A
- Authority
- JP
- Japan
- Prior art keywords
- iron powder
- aluminum
- magnetic iron
- magnetic
- atomic ratio
- 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.)
- Pending
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 229910052598 goethite Inorganic materials 0.000 claims abstract description 37
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 claims abstract description 37
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims abstract description 19
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims abstract description 5
- TWWDDFFHABKNMQ-UHFFFAOYSA-N oxosilicon;hydrate Chemical compound O.[Si]=O TWWDDFFHABKNMQ-UHFFFAOYSA-N 0.000 claims description 13
- WMWXXXSCZVGQAR-UHFFFAOYSA-N dialuminum;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3] WMWXXXSCZVGQAR-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 43
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 21
- 229910052782 aluminium Inorganic materials 0.000 abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- 239000001257 hydrogen Substances 0.000 abstract description 15
- 239000003973 paint Substances 0.000 abstract description 14
- 229910052759 nickel Inorganic materials 0.000 abstract description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract description 7
- 230000005415 magnetization Effects 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011019 hematite Substances 0.000 abstract description 3
- 229910052595 hematite Inorganic materials 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 abstract 3
- 229920006395 saturated elastomer Polymers 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 21
- 235000013980 iron oxide Nutrition 0.000 description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 19
- 238000000151 deposition Methods 0.000 description 16
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 14
- 230000008021 deposition Effects 0.000 description 12
- 229910052698 phosphorus Inorganic materials 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 230000002776 aggregation Effects 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 5
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 235000019353 potassium silicate Nutrition 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910001388 sodium aluminate Inorganic materials 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000005372 silanol group Chemical group 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- 229940007718 zinc hydroxide Drugs 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
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 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
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 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
- 229940024545 aluminum hydroxide Drugs 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 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
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- -1 sodium hydroxide Chemical class 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（イ）産業上の利用分野
本発明は高密度磁気記録媒体用磁性鉄粉の製造方法に関
するものであり、詳しくは針状又は紡錘状のゲータイト
或いはその脱水物であるヘマタイト（以下、酸化鉄と略
称する。）の表面への燐酸アルミニウムの被着処理、更
に燐酸アルミニウムの被着処理と組合わせて酸化珪素水
和物、酸化アルミニウム水和物及び水酸化ニッケルから
選ばれる１種以上の化合物を被着処理後、水素気流中で
還元することを特徴とする磁性鉄粉の製造方法に関する
ものである。Detailed Description of the Invention (a) Field of Industrial Application The present invention relates to a method for producing magnetic iron powder for high-density magnetic recording media, and specifically, acicular or spindle-shaped goethite or its dehydrate. Aluminum phosphate deposition treatment on the surface of hematite (hereinafter abbreviated as iron oxide), and in combination with aluminum phosphate deposition treatment, selected from silicon oxide hydrate, aluminum oxide hydrate, and nickel hydroxide. The present invention relates to a method for producing magnetic iron powder, which comprises reducing one or more compounds in a hydrogen stream after deposition treatment.
（ロ）従来の技術
従来、磁気記録媒体用磁性鉄粉は、針状又は紡錘状の酸
化鉄の形状を保持した磁性鉄粉を得るために、酸化鉄表
面に酸化珪素水和物及び／又は酸化アルミニウム永和物
の被着処理、更に酸化珪素水和物及び／又は酸化アルミ
ニウム永和物の被着処理と組合わせて水酸化亜鉛、水酸
化ニッケル及び水酸化コバルト等を被着処理後、水素気
流中で還元することにより製造されている。(B) Conventional technology Conventionally, magnetic iron powder for magnetic recording media has been prepared by adding silicon oxide hydrate and/or After the deposition treatment of aluminum oxide permanent, and further the deposition treatment of zinc hydroxide, nickel hydroxide, cobalt hydroxide, etc. in combination with the deposition treatment of silicon oxide hydrate and/or aluminum oxide permanent, hydrogen gas flow is applied. It is produced by reduction in
（ハ）発明が解決しようとする問題点
酸化鉄表面への酸化珪素水和物及び／又は酸化アルミニ
ウム永和物の被着処理、更に酸化珪素水和物及び／又は
酸化アルミニウム永和物の被若処理と組合わせて水酸化
亜鉛、水酸化ニッケル及び水酸化コバルト等の被着処理
を行っても、酸化鉄粒子の形状を保持し、凝集が少なく
且つ塗料分散性の良い磁性鉄粉を得ることは困難であっ
た。(c) Problems to be solved by the invention Treatment for depositing silicon oxide hydrate and/or aluminum oxide permanent on the surface of iron oxide, and further treatment for depositing silicon oxide hydrate and/or aluminum oxide permanent. Even if adhesion treatment with zinc hydroxide, nickel hydroxide, cobalt hydroxide, etc. is performed in combination with It was difficult.
この原因としては、次の理由が挙げられる。This may be due to the following reasons.
第１に、酸化鉄表面に酸化珪素水和物を被着処理すると
、酸化珪素水和物の活性なシラノール基（Ｓｉ−ＯＨ）
によって酸化鉄粒子が凝集し易く、従って磁性鉄粉も凝
集しており塗料分散性が悪い。First, when silicon oxide hydrate is deposited on the surface of iron oxide, active silanol groups (Si-OH) of silicon oxide hydrate are formed.
The iron oxide particles tend to aggregate, and therefore the magnetic iron powder also aggregates, resulting in poor paint dispersibility.
又、酸化鉄の凝集防止のため表面処理量を少なくしたり
、シラノール基生成の少ない珪素化合物を使用すると磁
性鉄粉の形状保持性は不充分で磁気特性が悪化する。Furthermore, if the amount of surface treatment is reduced to prevent agglomeration of iron oxide, or if a silicon compound with less silanol group formation is used, the shape retention of the magnetic iron powder will be insufficient and the magnetic properties will deteriorate.
第２に、酸化鉄表面に酸化アルミラム水和物を被着処理
すると、酸化アルミラム水和物はシラノール基はど活性
な水酸基を有していないので酸化鉄の凝集は少ないが、
酸化珪素水和物に比し酸化アルミニウム水和物の粒子径
が大きく表面被覆性が弱いため、形状保持性が不充分で
良好な磁気特性を持つ磁性鉄粉は得られない。Second, when aluminum oxide hydrate is deposited on the surface of iron oxide, aluminum oxide hydrate does not have silanol groups or active hydroxyl groups, so iron oxide aggregation is small;
Compared to silicon oxide hydrate, aluminum oxide hydrate has a larger particle size and weaker surface coverage, so shape retention is insufficient and magnetic iron powder with good magnetic properties cannot be obtained.
又、酸化鉄の還元時における生成磁性鉄粉の焼結防止及
び磁気特性制御のために、酸化珪素水和物及び／又は酸
化アルミニウム水和物の被着処理と組合わせて水酸化ニ
ッケル、水酸化亜鉛、水酸化コバルト及び水酸化クロム
等の被着処理を行うと、酸化珪素水和物及び／又は酸化
アルミニウム永和物の被着処理の場合と同様に、処理量
を増加すると磁性鉄粉の飽和磁化が低下すると共に磁性
鉄粉の凝集が起こり塗料分散性が悪化する。In addition, in order to prevent sintering and control the magnetic properties of the magnetic iron powder produced during the reduction of iron oxide, nickel hydroxide, water, etc. When depositing zinc oxide, cobalt hydroxide, chromium hydroxide, etc., as in the case of depositing silicon oxide hydrate and/or permanent aluminum oxide, increasing the amount of treatment increases the amount of magnetic iron powder. As saturation magnetization decreases, agglomeration of magnetic iron powder occurs, resulting in poor paint dispersibility.
（ニ）問題点を解決するための手段
本発明者らは、上記問題点を解決すべく種々の表面処理
方法について鋭意検討した結果、針状又は紡錘状の酸化
鉄表面を酸化珪素と同一結晶形態である燐酸アルミニウ
ムで被着処理後還元すると、凝集が少なく且つ塗料分散
性の良好な磁性鉄粉が得られることを見出し本発明を完
成したものである。(d) Means for Solving the Problems As a result of intensive study on various surface treatment methods to solve the above problems, the inventors found that the needle-shaped or spindle-shaped iron oxide surface was made of the same crystal as silicon oxide. The inventors completed the present invention by discovering that magnetic iron powder with less agglomeration and good paint dispersibility can be obtained by reduction after deposition treatment with aluminum phosphate, which is a form of aluminum phosphate.
即ち、本発明は針状又は紡錘状の酸化鉄表面への燐酸ア
ルミニウムの被着処理、更に燐酸アルミニウムの被着処
理と組合わせて酸化珪素水和物、酸化アルミニウム水和
物及び水酸化ニッケルから選ばれる１種以上の化合物を
被着処理後、水素気流中で還元することを特徴とする磁
性鉄粉の製造方法に関するものである。That is, the present invention involves applying aluminum phosphate to a needle-like or spindle-like surface of iron oxide, and furthermore, combining the process with applying aluminum phosphate to form a coating from silicon oxide hydrate, aluminum oxide hydrate, and nickel hydroxide. The present invention relates to a method for producing magnetic iron powder, which comprises reducing one or more selected compounds in a hydrogen stream after a deposition treatment.
本発明は酸化鉄表面を燐酸アルミニウムで被着処理する
際に、必要に応じ酸化アルミニウム水和物を被着しても
差し支えない。In the present invention, when the iron oxide surface is coated with aluminum phosphate, aluminum oxide hydrate may be coated if necessary.
酸化鉄表面への燐酸アルミニウムの被着処理方法として
は、■酸化鉄の分散液に燐酸アルミニウムコロイド溶液
を添加する方法、■酸化鉄の分散液に塩基性塩化アルミ
ニウム水溶液と重燐酸アルミニウム水溶液を添加する方
法、■酸化鉄の分散液にアルミン酸ナトリウム水溶液と
、１；！ｆ酸水溶液とを添加する方法、■酸化鉄の分散
液にアルミニウム塩水溶液と燐酸塩水溶液を添加する方
法等を挙げることができる。Methods for adhering aluminum phosphate to iron oxide surfaces include: ■ adding an aluminum phosphate colloidal solution to an iron oxide dispersion; ■ adding a basic aluminum chloride aqueous solution and an aluminum biphosphate aqueous solution to an iron oxide dispersion. How to do this, ■ add sodium aluminate aqueous solution to iron oxide dispersion, 1;! (2) A method in which an aqueous solution of an aluminum salt and an aqueous phosphate solution are added to an iron oxide dispersion.
この場合、アルミニウムと燐の被着量を変化させること
により酸化鉄表面に燐酸アルミニウム単独、更に必要に
応じ燐酸アルミニウム及び酸化アルミニウム水和物を被
着することもできる。In this case, by changing the amounts of aluminum and phosphorus deposited, it is possible to deposit aluminum phosphate alone or, if necessary, aluminum phosphate and aluminum oxide hydrate on the iron oxide surface.
アルミニウム及び燐の被着量は、Ａｌ／Ｆｅ原子比が０
．５〜１０％、Ｐ／Ｆｅ原子比が０．５〜１０％の範囲
が好ましい。The amount of deposited aluminum and phosphorus is such that the Al/Fe atomic ratio is 0.
．． The P/Fe atomic ratio is preferably in the range of 5 to 10%, and the P/Fe atomic ratio is in the range of 0.5 to 10%.
へｌ／Ｆｅ原子比及びＰ／Ｆｅ原子比が０．５％未満で
は磁性鉄粉の形状保持性が不充分で、ＡＡ／Ｆｅ原子比
及びＰ／Ｆｅ原子比が１０％を越えると磁性鉄粉の飽和
磁化が低下する。When the Hel/Fe atomic ratio and P/Fe atomic ratio are less than 0.5%, the shape retention of the magnetic iron powder is insufficient, and when the AA/Fe atomic ratio and P/Fe atomic ratio exceed 10%, the magnetic iron powder The saturation magnetization of the powder decreases.
上記酸化鉄表面への燐酸アルミニウムの被着処理と組合
わせて、必要に応じ酸化珪素水和物、酸化アルミニウム
水和物及び水酸化ニッケルから選ばれる１種以上の化合
物で酸化鉄表面の被着処理を行っても良い。In combination with the above-mentioned coating treatment of aluminum phosphate on the iron oxide surface, coating the iron oxide surface with one or more compounds selected from silicon oxide hydrate, aluminum oxide hydrate, and nickel hydroxide as necessary. Processing may be performed.
酸化珪素水和物の被着源としては、水ガラス、ケイ酸ソ
ーダ及びコロイダルシリカ等が挙げられる。Examples of the deposition source of silicon oxide hydrate include water glass, sodium silicate, and colloidal silica.
珪素の被着量は、Ｓｉ／Ｆｅ原子比が０．５〜６％の範
囲が好ましい。The amount of silicon deposited is preferably in the range of a Si/Fe atomic ratio of 0.5 to 6%.
Ｓｉ／Ｆｅ原子比が０．５％未満では添加効果がなく、
６％を越えると形状保持性は向上するが磁性鉄粉の凝集
が甚だしく、塗料分散性が悪化する。When the Si/Fe atomic ratio is less than 0.5%, there is no addition effect;
When it exceeds 6%, shape retention improves, but agglomeration of magnetic iron powder becomes severe and paint dispersibility deteriorates.
又、水酸化アルミニウム水和物の被着源としては、塩化
アルミニウム、塩基性塩化アルミニウム、アルミン酸ナ
トリウム等が挙げられる。Further, examples of the deposition source of aluminum hydroxide hydrate include aluminum chloride, basic aluminum chloride, sodium aluminate, and the like.
アルミニウムの被着量は、燐酸アルミニウムの被着にお
けるアルミニウムとの合計量が上記ｉ／Ｆｅ原子比０．
５〜１０％の範囲を満足すれば良い。The amount of aluminum deposited is such that the total amount of aluminum and aluminum in the deposition of aluminum phosphate is the above i/Fe atomic ratio of 0.
It is sufficient to satisfy the range of 5 to 10%.
水酸化ニッケルの被着源としては、塩化ニッケル及び硝
酸ニッケル等が挙げられる。Examples of the deposition source of nickel hydroxide include nickel chloride and nickel nitrate.
ニッケルの被着量は、Ｎｉ／Ｆｅ原子比が０．３〜１０
％の範囲が好ましい。この範囲では、表面処理酸化鉄の
水素気流中における還元時にニッケルが還元助剤となり
、磁性鉄粉の飽和磁化が高くなる。The amount of nickel deposited is such that the Ni/Fe atomic ratio is 0.3 to 10.
A range of % is preferred. In this range, nickel serves as a reduction aid during reduction of the surface-treated iron oxide in a hydrogen stream, and the saturation magnetization of the magnetic iron powder becomes high.
Ｎｉ／Ｆｅ原子比が０．３％未満では効果がなく、１０
％を越えると磁性鉄粉の磁気特性が悪化する。There is no effect when the Ni/Fe atomic ratio is less than 0.3%, and 10
%, the magnetic properties of the magnetic iron powder deteriorate.
本発明に使用される針状又は紡錘状酸化鉄には特に限定
はないが、例えば炭酸アンモニウム等の炭酸アルカリ及
び水酸化ナトリウム等の水酸化アルカリ水溶液に第一鉄
塩水溶液を添加し、酸素含有ガスを吹き込み製造したゲ
ーサイト、更には脱水を行ったヘマタイト等が使用され
る。The needle-shaped or spindle-shaped iron oxide used in the present invention is not particularly limited, but for example, a ferrous salt aqueous solution is added to an aqueous solution of an alkali carbonate such as ammonium carbonate and an alkali hydroxide such as sodium hydroxide, and an oxygen-containing Goethite produced by blowing gas, and hematite produced by dehydration are used.
又、表面処理を行った針状又は紡錘状酸化鉄の還元は、
水素気流中３００〜５００℃で容易に還元を行うことが
でき、針状又は紡錘状磁性鉄粉を製造することができる
。In addition, the reduction of surface-treated acicular or spindle-shaped iron oxides is as follows:
Reduction can be easily carried out at 300 to 500°C in a hydrogen stream, and acicular or spindle-shaped magnetic iron powder can be produced.
（ホ）発明の効果
本発明により得られる磁性鉄粉は次の特徴を有している
。(e) Effects of the invention The magnetic iron powder obtained by the invention has the following characteristics.
第一に、磁性鉄粉は酸化鉄の形状を保持し、優れた磁気
特性を示す。First, magnetic iron powder retains the shape of iron oxide and exhibits excellent magnetic properties.
第二に、磁性鉄粉は凝集が少なく、塗料への分散性が非
常に良い。Second, magnetic iron powder has little agglomeration and has very good dispersibility in paints.
第三に、水酸化ニッケルを被着処理すると、磁性鉄粉は
更に飽和磁化が向上する。Thirdly, by applying nickel hydroxide, the saturation magnetization of the magnetic iron powder is further improved.
（へ）実施例
次に実施例を挙げて本発明を説明するが、本発明はこれ
らに限定されるものではない。(f) Examples The present invention will now be described with reference to Examples, but the present invention is not limited thereto.
実施例１
平均長軸径０．３０μｍ、軸比１５及び比表面積１０６
ｎｒ／ｇの針状ゲーサイト１００ｇを２１の水にｐＨ１
１で分散する。Example 1 Average long axis diameter 0.30 μm, axial ratio 15 and specific surface area 106
100 g of acicular goethite of nr/g was added to water of 21 pH 1.
Distributed by 1.
この分散液に、０．２モル／ｌの燐酸アルミニウムコロ
イド溶液１８０ｍ１を添加し攪拌しながら徐々にｐＨ９
とした。To this dispersion, 180 ml of a 0.2 mol/l aluminum phosphate colloid solution was added and the pH was gradually adjusted to 9 with stirring.
And so.
このゲーサイトを水洗口過後、乾燥し表面処理ゲーサイ
トを得た。This goethite was rinsed with water and then dried to obtain a surface-treated goethite.
アルミニウム及び燐の被着量は、Ａｌ／Ｐｅ原子比２．
３％及びＰ／Ｆｅ原子比２．１％であった。The amount of deposited aluminum and phosphorus is determined by the Al/Pe atomic ratio of 2.
3% and the P/Fe atomic ratio was 2.1%.
この処理ゲーサイトを水素気流中４００℃で還元し磁性
鉄粉を得た。This treated goethite was reduced at 400° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は
保持力（Ｈｅ） １５１００ｅ 、飽和磁化（σｓ）１
２２ｅｍｕ／ｇ 、角形比（ＳＱ） ０．５１３ 、比
表面積（ＳＳＡ）５６ｎｆ／ｇであった。The magnetic properties of the obtained magnetic iron powder are coercive force (He) 15100e and saturation magnetization (σs) 1
22 emu/g, squareness ratio (SQ) 0.513, and specific surface area (SSA) 56 nf/g.
この磁性鉄粉を以下の処方で塗料化した。This magnetic iron powder was made into a paint using the following formulation.
磁性鉄粉 ６０部塩化ビニル
、酢酸ビニル共重合体 ９部〔積水化学側製：エス
レフクＣ〕
ポリウレタン〔成田薬品ｎ５ ： Ｅ５５１１ ６部界
面活性剤〔レシチン〕 ２部トルエン
４０部メチルエチルケトン
４０部メチルイソブチルケトン
４０部上記混合物をサンドミルで６時間分散して得
られた塗料を、ポリエステルフィルム上に乾燥塗膜厚３
．０μｍになるように塗布し磁場配向後、乾燥し磁気テ
ープを得た。得られたテープの磁気特性を表１に示す。Magnetic iron powder 60 parts Vinyl chloride, vinyl acetate copolymer 9 parts [Sekisui Chemical: S-Refuku C] Polyurethane [Narita Yakuhin N5: E5511 6 parts Surfactant [lecithin] 2 parts Toluene
40 parts methyl ethyl ketone
40 parts methyl isobutyl ketone
Disperse 40 parts of the above mixture in a sand mill for 6 hours and apply the resulting paint to a polyester film with a dry coating thickness of 3.
．． It was applied to a thickness of 0 μm, oriented in a magnetic field, and dried to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
実施例２
実施例１のゲーサイト１００ｇを２１の水にｐＨ３で分
散する。Example 2 100 g of goethite from Example 1 is dispersed in 21 water at pH 3.
この分散液に、０．２モル／１の塩化アルミニウム水溶
液１５０ｍｊ！及び、０．２モル／１の燐酸ナトリウム
水溶液１５０ｍ１を添加し攪拌しながら徐々にｐＨ１ｏ
とし、更に０．２モル／ｌの水ガラス水溶液１８０ｍｊ
２を添加し攪拌した後徐々にｐＨ９とした。Add 150 mj of a 0.2 mol/1 aluminum chloride aqueous solution to this dispersion! Then, 150 ml of 0.2 mol/1 sodium phosphate aqueous solution was added and the pH was gradually adjusted to 1o while stirring.
and further 180 mj of 0.2 mol/l water glass aqueous solution
2 was added and stirred, and the pH was gradually adjusted to 9.
このゲーサイトを水洗口過後、乾燥し処理ゲーサイトを
得た。This goethite was rinsed with water and then dried to obtain treated goethite.
アルミニウム、燐及び珪素の被着量はＡ１／Ｆｅ原子比
１．９％、Ｐ／Ｆｅ原子比１．２％及びＳｉ／Ｆｅ原子
比２．５％であった。The deposited amounts of aluminum, phosphorus, and silicon were A1/Fe atomic ratio 1.9%, P/Fe atomic ratio 1.2%, and Si/Fe atomic ratio 2.5%.
この処理ゲーサイトを水素気流中４００℃で還元し磁性
鉄粉を得た。This treated goethite was reduced at 400° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は、
Ｈｃ １５４００ｅ 、 （ＦＳ １２６ ｅｍｕ／ｇ
、 ＳＱ Ｏ，５２０、ＳＳＡ９ｍ１ｇ
であった。The magnetic properties of the obtained magnetic iron powder are as follows: Hc 15400e, (FS 126 emu/g
, SQO, 520, SSA 9ml/g.
この磁性鉄粉を実施例１と同じ処方で塗料化し磁気テー
プを得た。得られたテープの磁気特性を表１に示す。This magnetic iron powder was made into a paint using the same recipe as in Example 1 to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
実施例３
実施例１の針状ゲーサイト１００ｇを２１の水にｐＨ３
で分散する。Example 3 100 g of acicular goethite from Example 1 was added to 21 water at pH 3.
Disperse with.
この分散液に、０．２モル／ｌの塩基性塩化アルミニウ
ム水溶液６５ｍ１．０．２モル／ｌの重燐酸アルミニウ
ム水溶液６５ｍｊ２及び０．２モル／ｌの塩化ニッケル
水溶液２５０ａ＋ｊ！を添加し攪拌しながら徐々にｐＨ
９とした。To this dispersion were added 65ml of a 0.2 mol/l basic aluminum chloride aqueous solution, 65ml of a 0.2 mol/l aluminum biphosphate aqueous solution and 250ml of a 0.2 mol/l nickel chloride aqueous solution! and gradually adjust the pH while stirring.
It was set as 9.
このゲーサイトを水洗口過後、乾燥し表面処理ゲーサイ
トを得た。This goethite was rinsed with water and then dried to obtain a surface-treated goethite.
アルミニウム、燐及びニッケルの被着量は、Ａｌ／Ｆｅ
原子比２．５％、Ｐ／Ｆｅ原子比１．６％及び：Ｈ／Ｆ
ｅ原子比４．０％であった。The amount of aluminum, phosphorus and nickel deposited is Al/Fe
Atomic ratio 2.5%, P/Fe atomic ratio 1.6% and :H/F
The e atomic ratio was 4.0%.
この処理ゲーサイトを水素気流中４００℃でＭ元し磁性
鉄粉を得た。This treated goethite was subjected to M at 400° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は
１１ｃ １５０５０ｅ 、 ｔｙｓ １２８ ｅｍｕ／
ｇ 、 ＳＱ Ｏ，５１２、ＳＳＡ３４ｍ／ｇであった
。The magnetic properties of the obtained magnetic iron powder are 11c 15050e, tys 128 emu/
g, SQ O, 512, and SSA 34 m/g.
この磁性鉄粉を実施例１と同じ処方で塗料化し磁気テー
プを得た。得られたテープの磁気特性を表１に示す。This magnetic iron powder was made into a paint using the same recipe as in Example 1 to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
実施例４
実施例１の針状ゲーサイｈ１００ｇを２！の水にｐＨ３
で分散する。Example 4 100g of the needle-shaped gesai h of Example 1 was added to 2! pH 3 in water
Disperse with.
この分散液に、０．２モル／Ｉ！の塩化アルミニウム水
溶液１６５ｍ＋２．０．２モル／１の燐酸ナトリウム水
溶液１６５ｍｆｆ及び０．２モル／ｌの塩化ニッケル水
溶液１７０ｍ１！を添加し攪拌しながら徐々にｐＨ１０
とし、更に０．２モル／ｌの水ガラス水溶液１８０ｎ＋
ｊ！を添加し攪拌した後徐々にｐＨ９とした。This dispersion contains 0.2 mol/I! 165 m of aqueous aluminum chloride solution + 165 mff of 2.0.2 mol/l aqueous sodium phosphate solution and 170 m1 of 0.2 mol/l nickel chloride aqueous solution! and gradually raise the pH to 10 while stirring.
and further 0.2 mol/l water glass aqueous solution 180n+
j! After stirring, the pH was gradually adjusted to 9.
このゲーサイトを水洗口過後、乾燥し表面処理ゲーサイ
トを得た。This goethite was rinsed with water and then dried to obtain a surface-treated goethite.
アルミニウム、燐、珪素及びニッケルの被着量は、Ａｊ
２／Ｆｅ原子比２．０％、Ｐ／Ｆｅ原子比１．２％、Ｓ
ｉ／Ｆｅ原子比２．２％及びＮ＋／Ｆｅ原子比２．７％
であった。The amount of aluminum, phosphorus, silicon and nickel deposited is Aj
2/Fe atomic ratio 2.0%, P/Fe atomic ratio 1.2%, S
i/Fe atomic ratio 2.2% and N+/Fe atomic ratio 2.7%
Met.
この処理ゲーサイトを水素気流中４２０℃で還元し磁性
鉄粉を得た。This treated goethite was reduced at 420° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は
１１ｃ １５１００ｅ 、 ａｓ １３４ ｅｍｕ／ｇ
、 ＳＱ Ｏ，５１８，５ＳＡ５９ ｒｄ ／ｇであ
った。The magnetic properties of the obtained magnetic iron powder are 11c 15100e, as 134 emu/g
, SQO,518,5SA59rd/g.
この磁性鉄粉を実施例１と同じ処方で塗料化し磁気テー
プを得た。得られたテープの磁気特性を表１に示す。This magnetic iron powder was made into a paint using the same recipe as in Example 1 to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
実施例５
平均長軸径０．１５μｍ、軸比６、比表面積９７ｍ／ｇ
の紡錘状ゲーサイト１００ｇを２βの水にｐＨ３で分散
する。Example 5 Average major axis diameter 0.15 μm, axial ratio 6, specific surface area 97 m/g
100 g of spindle-shaped goethite is dispersed in 2β water at pH 3.
この分散液に、０．２モル／ｐの塩基性塩化アルミニウ
ム水溶液１１５＋ｎＡ’、０．２モル／ｊｌ！の重リン
酸アルミニウム水溶液１１５ｍ！！及び０．２モル／ｌ
の塩化ニッケル水溶液１４０ｍＡを添加し攪拌しながら
徐々にｐＨ９とした。To this dispersion was added a 0.2 mol/p basic aluminum chloride aqueous solution 115+nA', 0.2 mol/jl! 115m of aluminum biphosphate aqueous solution! ! and 0.2 mol/l
140 mA of an aqueous nickel chloride solution was added thereto, and the pH was gradually adjusted to 9 with stirring.
このゲーサイトを水洗口過後、乾燥し処理ゲーサイトを
得た。This goethite was rinsed with water and then dried to obtain treated goethite.
アルミニウム、燐及びニッケルの被着量は、ｉ／Ｆｅ原
子比４．３％、Ｐ／Ｆｅ原子比３．７％及びＮ＋／’Ｆ
ｅ原子比２．２％であった。The deposited amounts of aluminum, phosphorus, and nickel were: i/Fe atomic ratio 4.3%, P/Fe atomic ratio 3.7%, and N+/'F.
The e atomic ratio was 2.2%.
この処理ゲーサイトを水素気流中３９０°Ｃで還元し磁
性鉄粉を得た。This treated goethite was reduced at 390°C in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は、
ｔｉｃ １４８００ｅ 、 ａｓ １３５ ｅｍｕ／ｇ
、 ＳＱ Ｏ，４９５、ＳＳＡ３６ｍ／ｇ
であった。The magnetic properties of the obtained magnetic iron powder are as follows: tic 14800e, as 135 emu/g
, SQ O, 495, and SSA 36 m/g.
この磁性鉄粉を実施例１と同じ処方で塗料化し磁気テー
プを得た。得られたテープの磁気特性を表１に示す。This magnetic iron powder was made into a paint using the same recipe as in Example 1 to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
比較例１
実施例１と同じゲーサイ）１００ｇを２２の水にｐＨ３
で分散する。Comparative Example 1 100 g of the same game machine as in Example 1 was added to 22 water at pH 3.
Disperse with.
この分散液に、０．２モル／１の塩化ニッケル水溶液１
３０ｍｊ！を添加し攪拌しながらｐＨ１１とし、更に０
．２モル／ｌの水ガラス水溶液４３５ｍ／を添加し攪拌
した後、徐々にｐＨ９とした。To this dispersion, add 1 part of a 0.2 mol/1 nickel chloride aqueous solution.
30mj! was added and adjusted to pH 11 with stirring, and further adjusted to 0.
．． After adding 435 m/l of a 2 mol/l water glass aqueous solution and stirring, the pH was gradually adjusted to 9.
このゲーサイトを水洗口過後、乾燥し処理ゲーサイトを
得た。This goethite was rinsed with water and then dried to obtain treated goethite.
珪素及びニッケルの被着量は、Ｓｉ／Ｆｅ原子比５゜４
％及びＮｉ／Ｆｅ原子比２．１％であった。The amount of silicon and nickel deposited is a Si/Fe atomic ratio of 5°4.
% and the Ni/Fe atomic ratio was 2.1%.
この処理ゲーサイトを水素気流中４２０℃で還元し磁性
鉄粉を得た。This treated goethite was reduced at 420° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は、
Ｈｃ １４６００ｅ 、ａｓ １２７ ｅｍｕ／ｇ 、
ＳＱ Ｏ，５０５，５ＳＡ５７ｒＪ／ｇ
であった。The magnetic properties of the obtained magnetic iron powder are Hc 14600e, as 127 emu/g,
SQO,505,5SA57rJ/g.
この磁性鉄粉を実施例１と同じ処方で塗料化し磁気テー
プを得た。得られたテープの磁気特性を表１に示す。This magnetic iron powder was made into a paint using the same recipe as in Example 1 to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
比較例２
実施例１と同じゲーサイ）１００ｇを２１１の水にｐＨ
１１で分散する。Comparative Example 2 100g of the same game machine as in Example 1 was added to water with a pH of 211.
Dispersed by 11.
この分散液に、０．２モル／ｌのアルミン酸ナトリウム
水溶液４００ｍｆを添加し撹拌した後、徐々にｐＨ９と
した。To this dispersion, 400 mf of a 0.2 mol/l aqueous sodium aluminate solution was added and stirred, and then the pH was gradually adjusted to 9.
このゲーサイトを水洗口過後、乾燥し処理ゲーサイトを
得た。This goethite was rinsed with water and then dried to obtain treated goethite.
アルミニウムの被着量は、Ａｌ／Ｆｅ原子比５．７％で
あった。The amount of aluminum deposited was an Al/Fe atomic ratio of 5.7%.
この処理ゲーサイトを水素気流中４００℃で還元し磁性
鉄粉を得た。This treated goethite was reduced at 400° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は、
Ｈｃ １２５００ｅ 、 ａｓ １０３ ｅｍｕ／ｇ
ＳＳＱ Ｏ，４８３、ＳＳ＾５１ｎ？／ｇ
であり、磁性鉄粉は形状が崩れ磁気特性は不充分なもの
である。The magnetic properties of the obtained magnetic iron powder are: Hc 12500e, as 103 emu/g
SSQ O,483, SS^51n? /g, the magnetic iron powder loses its shape and has insufficient magnetic properties.
比較例３
実施例１と同じゲーサイｌ−１００ｇを２１の水にｐＨ
１１で分散する。Comparative Example 3 100 g of the same Gesai l as in Example 1 was added to water with a pH of 21.
Dispersed by 11.
この分散液に、０．２モル／ｌのアルミン酸ナトリウム
水溶液１７０ＩＩ１１及び０．２モル／ｌの水ガラス水
溶液３００ｍ１を添加し攪拌した後、徐々にｐＨ９とし
た。To this dispersion, 0.2 mol/l sodium aluminate aqueous solution 170II11 and 0.2 mol/l water glass aqueous solution 300 ml were added and stirred, and then the pH was gradually adjusted to 9.
このゲーサイトを水洗口過後、乾燥し処理ゲーサイトを
得た。This goethite was rinsed with water and then dried to obtain treated goethite.
アルミニウム及び珪素の被着量は、Ａｌｌ／Ｆｅ原子比
２．３％及びＳｉ／Ｆｅ原子比３，８％であった。The amounts of aluminum and silicon deposited were an All/Fe atomic ratio of 2.3% and a Si/Fe atomic ratio of 3.8%.
この処理ゲーサイトを水素気流中４００℃で還元し磁性
鉄粉を得た。This treated goethite was reduced at 400° C. in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は、
ｔｉｃ １４４００ｅ 、 ａｓ １２１ ｅｍｕ／ｇ
ＸＳＱ Ｏ，４９０，５ＳＡ５８ ｔｒｉ ／ｇ
であった。The magnetic properties of the obtained magnetic iron powder are as follows: tic 14400e, as 121 emu/g
XSQ O, 490, 5SA58 tri/g.
この磁性鉄粉を実施例１と同じ処方で塗料化し磁気テー
プを得た。得られたテープの磁気特性を表１に示す。This magnetic iron powder was made into a paint using the same recipe as in Example 1 to obtain a magnetic tape. Table 1 shows the magnetic properties of the obtained tape.
比較例４
実施例５の紡錘状ゲーサイト２００ｇを２１！の水にｐ
Ｈ３で分散する。Comparative Example 4 200g of the spindle-shaped goethite of Example 5 was added to 21! p in the water of
Disperse in H3.
この分散液に０．２モル／ｌの塩化ニッケル水溶ＦＥ１
５５ｍｌを添加し攪拌しながらｐＨ１１とし、更に０．
２モル／Ｉｌのアルミン酸ソーダ４４０ｍ１を添加し攪
拌した後、徐々にｐＨ９とした。In this dispersion, 0.2 mol/l of nickel chloride aqueous solution FE1 was added.
Add 55 ml and adjust the pH to 11 while stirring, and further adjust to 0.
After adding 440 ml of 2 mol/Il sodium aluminate and stirring, the pH was gradually adjusted to 9.
このゲーサイトを水洗口過後、乾燥し処理ゲーサイトを
得た。This goethite was rinsed with water and then dried to obtain treated goethite.
アルミニウム及びニッケルの？＆ −ｆ ｆｆｉは、Ａ
ｌｌ／Ｆｅ原子比５．５％及びＮｉ／Ｆｅ原子比２．５
％であった。Of aluminum and nickel? & -f ffi is A
ll/Fe atomic ratio 5.5% and Ni/Fe atomic ratio 2.5
%Met.
この処理ゲーサイトを水素気流中３９０°Ｃで還元し磁
性鉄粉を得た。This treated goethite was reduced at 390°C in a hydrogen stream to obtain magnetic iron powder.
得られた磁性鉄粉の磁気特性は、
１１ｃ １２３００ｅ 、 ａｓ １１８ ｅｍｕ／ｇ
、 ＳＱ Ｏ，４７５，５ＳＡ５５イ／ｇ
であり、磁性鉄粉は形状が崩れ磁気特性は不充分なもの
である。The magnetic properties of the obtained magnetic iron powder are: 11c 12300e, as 118 emu/g
, SQ O, 475,5SA55 i/g, and the magnetic iron powder loses its shape and has insufficient magnetic properties.
以下余白Margin below
Claims (1)
るヘマタイトの表面に燐酸アルミニウムを被着処理後、
還元することを特徴とする磁性鉄粉の製造方法。 ２、針状又は紡錘状のゲータイト或いはその脱水物であ
るヘマタイトの表面への燐酸アルミニウムの被着処理と
組合わせて酸化珪素水和物、酸化アルミニウム水和物及
び水酸化ニッケルから選ばれる１種以上の化合物を被着
処理後、還元することを特徴とする磁性鉄粉の製造方法
。[Claims] 1. After applying aluminum phosphate to the surface of acicular or spindle-shaped goethite or its dehydrated hematite,
A method for producing magnetic iron powder characterized by reduction. 2. One type selected from silicon oxide hydrate, aluminum oxide hydrate, and nickel hydroxide in combination with a coating treatment of aluminum phosphate on the surface of acicular or spindle-shaped goethite or its dehydrated hematite. A method for producing magnetic iron powder, which comprises reducing the above-mentioned compound after being deposited thereon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61212119A JPS6367705A (en) | 1986-09-09 | 1986-09-09 | Manufacture of magnetic iron powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61212119A JPS6367705A (en) | 1986-09-09 | 1986-09-09 | Manufacture of magnetic iron powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6367705A true JPS6367705A (en) | 1988-03-26 |
Family
ID=16617193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61212119A Pending JPS6367705A (en) | 1986-09-09 | 1986-09-09 | Manufacture of magnetic iron powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6367705A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5443617A (en) * | 1993-10-06 | 1995-08-22 | Kawasaki Teitoku Co., Ltd. | Powdery raw material composition for a permanent magnet |
| US5453137A (en) * | 1994-03-30 | 1995-09-26 | Kawasaki Teitoku Co., Ltd. | Material for a permanent magnet |
| US5478409A (en) * | 1994-01-12 | 1995-12-26 | Kawasaki Teitoku Co., Ltd. | Method of producing sintered-or bond-rare earth element-iron-boron magnets |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5613411A (en) * | 1979-07-16 | 1981-02-09 | Kawasaki Steel Corp | Manufacture of magnetic powder of metallic iron |
-
1986
- 1986-09-09 JP JP61212119A patent/JPS6367705A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5613411A (en) * | 1979-07-16 | 1981-02-09 | Kawasaki Steel Corp | Manufacture of magnetic powder of metallic iron |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5443617A (en) * | 1993-10-06 | 1995-08-22 | Kawasaki Teitoku Co., Ltd. | Powdery raw material composition for a permanent magnet |
| US5562782A (en) * | 1993-10-06 | 1996-10-08 | Kawasaki Teitoku Co., Ltd. | Method for producing magnetically anisotropic permanent magnet |
| US5580400A (en) * | 1993-10-06 | 1996-12-03 | Kawasaki Teitoku Co., Ltd. | Magnetically anisotropic permanent magnet |
| US5478409A (en) * | 1994-01-12 | 1995-12-26 | Kawasaki Teitoku Co., Ltd. | Method of producing sintered-or bond-rare earth element-iron-boron magnets |
| US5453137A (en) * | 1994-03-30 | 1995-09-26 | Kawasaki Teitoku Co., Ltd. | Material for a permanent magnet |
| US5569333A (en) * | 1994-03-30 | 1996-10-29 | Kawasaki Teitoku Co., Ltd. | Process for producing a material for a permanent magnet |
| US5569336A (en) * | 1994-03-30 | 1996-10-29 | Kawasaki Teitoku Co., Ltd. | Bonded permanent magnet |
| US5569335A (en) * | 1994-03-30 | 1996-10-29 | Kawasaki Teitoku Co., Ltd. | Sintered permanent magnet |
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