JPS6122604A - Magnetic metal powder and manufacture thereof - Google Patents
Magnetic metal powder and manufacture thereofInfo
- Publication number
- JPS6122604A JPS6122604A JP59142790A JP14279084A JPS6122604A JP S6122604 A JPS6122604 A JP S6122604A JP 59142790 A JP59142790 A JP 59142790A JP 14279084 A JP14279084 A JP 14279084A JP S6122604 A JPS6122604 A JP S6122604A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic metal
- iron
- metal powder
- magnetic
- zno
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 28
- 239000002184 metal Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 33
- 150000003752 zinc compounds Chemical class 0.000 claims abstract description 21
- 229910052909 inorganic silicate Inorganic materials 0.000 claims abstract description 19
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 claims abstract description 18
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 4
- 239000011701 zinc Substances 0.000 claims abstract description 4
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 238000000151 deposition Methods 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 6
- 150000002505 iron Chemical class 0.000 abstract description 5
- 229910052681 coesite Inorganic materials 0.000 abstract description 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 229910052682 stishovite Inorganic materials 0.000 abstract description 3
- 229910052905 tridymite Inorganic materials 0.000 abstract description 3
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 229910052718 tin Inorganic materials 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 9
- 239000000725 suspension Substances 0.000 description 9
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 6
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 150000003377 silicon compounds Chemical class 0.000 description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 3
- 229960001763 zinc sulfate Drugs 0.000 description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- -1 alkaline earth metal salts Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910006540 α-FeOOH Inorganic materials 0.000 description 1
- 229910003153 β-FeOOH Inorganic materials 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Powder Metallurgy (AREA)
- Magnetic Record Carriers (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、磁性金属粉末に係シ、さらに詳しくは、配向
特性に優れた磁気記録材料用の磁性鉄粉およびその製造
法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to magnetic metal powder, and more particularly to magnetic iron powder for use in magnetic recording materials with excellent orientation properties and a method for producing the same.
高記録密度用磁性材料として、磁性鉄粉が注目されてお
シ、この磁性鉄粉は通常、オキシ水酸化鉄を出発原料と
し、これにオキシ水酸化鉄結晶の針状性を保持するため
の化合物を被着させ、炉別、脱水後、還元して製造する
。Magnetic iron powder is attracting attention as a magnetic material for high recording density.This magnetic iron powder usually uses iron oxyhydroxide as a starting material, and this is supplemented with iron oxyhydroxide crystals that retain their acicular properties. It is manufactured by depositing a compound, separating it in a furnace, dehydrating it, and reducing it.
オキシ水酸化鉄結晶の針状性保持のために被着する化合
物の成分、量および被着の均一性は、還元処理時に起る
鉄粒子間の焼結性に影響し、最終゛製品の分散性、配向
性および磁気特性が大きく左右される。The composition, amount, and uniformity of deposition of the compound deposited to maintain the acicular nature of iron oxyhydroxide crystals affect the sinterability between iron particles that occurs during reduction treatment, and the dispersion of the final product. properties, orientation, and magnetic properties are greatly affected.
オキシ水酸化鉄に被着する耐熱性の金属酸化物となる化
合物として一般に珪酸塩が多く用いられているが、さら
に、還元時の焼結性、磁性鉄粉の分散性、配向性を改良
することを目的として、珪酸塩に、Ｍ化合物（特開昭５
８−７７５０５号公報、特公昭５７−２９５２３号公報
）、カルシウム塩（特開昭５８−４２７０４号公報等）
、アルカリ土類金属塩等を添加する方法が提案されてい
る。また、珪酸塩に代えてアルミニウム塩を用いる方法
（特開昭５２−１３４８５８号公報）も提案されている
。Silicates are commonly used as compounds that form heat-resistant metal oxides that adhere to iron oxyhydroxide, but they also improve the sinterability during reduction, the dispersibility, and orientation of magnetic iron powder. For this purpose, M compound (Unexamined Japanese Patent Publication No.
8-77505, Japanese Patent Publication No. 57-29523), calcium salts (Japanese Patent Publication No. 58-42704, etc.)
, a method of adding alkaline earth metal salts, etc. has been proposed. Furthermore, a method using an aluminum salt in place of a silicate (Japanese Patent Application Laid-open No. 134858/1983) has also been proposed.
特公昭４７−２９７０６号公報および特開昭５６−７３
４０８号公報には、オキシ水酸化鉄等に直接亜鉛化合物
等を被着させ、還元によシ、磁性鉄粉表面に耐酸化性に
鉄−亜鉛合金層を形成する提案がある。Japanese Patent Publication No. 47-29706 and Japanese Patent Publication No. 56-73
No. 408 proposes that a zinc compound or the like is directly deposited on iron oxyhydroxide or the like to prevent reduction and form an oxidation-resistant iron-zinc alloy layer on the surface of magnetic iron powder.
オキシ水酸化鉄に珪酸塩を主体とする化合物を直接被着
する方法においては、オキシ水酸化鉄結晶の形状保持性
に優れるものの、磁性鉄粉の微粒子化に伴いこれらの方
法で製造された磁性鉄粉は、テープ化後の配向特性が低
下する。Although the methods of directly depositing silicate-based compounds on iron oxyhydroxide have excellent shape retention properties of iron oxyhydroxide crystals, the magnetic iron powder produced by these methods Iron powder has poor orientation properties after being made into a tape.
本発明は、分散性、配向性すなわち、磁気記録媒体とし
ての配向特性が改良された磁性金属粉末およびその製造
方法を提供することを、その目的とする。An object of the present invention is to provide a magnetic metal powder with improved dispersibility and orientation, that is, orientation characteristics as a magnetic recording medium, and a method for producing the same.
本発明は、磁性金属のコアと、外表面にＺｎＯの存在す
る５ｉ０２のシェルとからなる磁性金属粉末である。The present invention is a magnetic metal powder consisting of a magnetic metal core and a 5i02 shell with ZnO on the outer surface.
本発明において、シェルの５ｉｎ２： ＺｎＯのモル比
は１：０．１〜１：０．７、好ましくは、１：０．２５
〜１：０．５５である。さらに好ましくは、シェルの外
表面の５ｉ０２ ： ＺｎＯのモル比が１：１である。In the present invention, the molar ratio of 5in2:ZnO in the shell is 1:0.1 to 1:0.7, preferably 1:0.25.
~1:0.55. More preferably, the molar ratio of 5i02:ZnO on the outer surface of the shell is 1:1.
本発明において磁性金属は、金属鉄およびＦｅ −Ｃｏ
、 Ｆｅ−Ｎｉ、 Ｆｅ−Ｚｎ等の磁性合金鉄であれば
いづれでもよい。In the present invention, magnetic metals include metallic iron and Fe-Co
, Fe-Ni, Fe-Zn, or any other magnetic alloy iron may be used.
本発明の磁性金属粉末は、オキシ水酸化鉄の表面に無機
珪酸塩を被着し、ついで亜鉛化合物または無機珪酸塩と
亜鉛化合物との混合物を被着した後、炉別して加熱脱水
し、還元することにょシ製造する。The magnetic metal powder of the present invention is produced by depositing an inorganic silicate on the surface of iron oxyhydroxide, then depositing a zinc compound or a mixture of an inorganic silicate and a zinc compound, and then separating the powder in a furnace, heating and dehydrating it, and reducing it. Manufacture in particular.
本発明において、オキシ水酸化鉄は、鉄塩の単独または
Ｎｉ、Ｃｏ、 Ｃｒ、 Ｚｎ、 ５ｎ１Ａｔ等の鉄以外
の金属の塩類を添加し丸鉄塩の水溶液を酸化して得られ
る含水酸化第２鉄であり、針状性に優れたものであれば
ａ Ｆｅ００Ｈｓ β−ＦｅＯＯＨおよびｒ −Ｆｅ
ＯＯＨのいづれでもよい。通常は、α−ＦｅＯＯＨが針
状性に優れるので好ましく使用される。In the present invention, iron oxyhydroxide is a hydrous oxidized iron salt obtained by oxidizing an aqueous solution of round iron salt by adding iron salt alone or salts of metals other than iron such as Ni, Co, Cr, Zn, and 5n1At. If it is iron and has excellent acicularity, a Fe00Hs β-FeOOH and r -Fe
Either OOH is acceptable. Usually, α-FeOOH is preferably used because it has excellent acicular properties.
無機珪酸塩は、水可溶性のものであればよく、安価で入
手の容易な水硝子が使用される。また、亜鉛化合物も水
可溶性のものであればよく、硫酸亜鉛、硝酸亜鉛等の無
機亜鉛類が好ましく使用される。The inorganic silicate may be any water-soluble one, and water glass, which is inexpensive and easily available, is used. Further, the zinc compound may also be water-soluble, and inorganic zinc compounds such as zinc sulfate and zinc nitrate are preferably used.
オキシ水酸化鉄に、無機珪酸塩、ついで亜鉛化合物また
は無機珪酸塩と亜鉛化合物との混合物を被着させる方法
には、特に制限はないが、以下の方法によシ行うことが
できる。There are no particular restrictions on the method for depositing the inorganic silicate and then the zinc compound or the mixture of the inorganic silicate and zinc compound on the iron oxyhydroxide, but the following method can be used.
ヘキサメタリン酸ナトリウム等の分散剤の水溶液に、オ
キシ水酸化鉄を添加して分散させてスラリーとし、該ス
ラリーに無機珪酸塩を添加することによシ、無機珪酸塩
の一部がオキシ水酸化鉄表面に被着する。ついで、該ス
ラリーに亜鉛化合物の水溶液を添加し、酸を加えて中和
することによシ、オキシ水酸化鉄に被着、した無機珪酸
壇上に、亜鉛化合物と無機珪酸塩との混合物が被着する
。By adding iron oxyhydroxide to an aqueous solution of a dispersing agent such as sodium hexametaphosphate and dispersing it to form a slurry, and adding an inorganic silicate to the slurry, a part of the inorganic silicate becomes iron oxyhydroxide. Adheres to the surface. Next, an aqueous solution of a zinc compound is added to the slurry, and acid is added to neutralize the slurry, so that the mixture of the zinc compound and the inorganic silicate is coated on the iron oxyhydroxide. wear it.
亜鉛化合物水溶液の添加時機を調整することによ勺、第
２段階として被着する亜鉛化合物と無機珪酸塩の混合比
を変えることができ、また、実質的に無機珪酸壇上に水
酸化亜鉛の単独を被着することができる。By adjusting the timing of addition of the zinc compound aqueous solution, it is possible to change the mixing ratio of the zinc compound and inorganic silicate deposited in the second step, and it is also possible to substantially change the mixing ratio of the zinc compound and inorganic silicate to be deposited on the inorganic silicate plate. can be coated.
無機珪酸塩および亜鉛化合物または無機珪酸塩と亜鉛化
合物との混合物を被着したオキシ水酸化鉄を戸別した後
常法によシ、たとえば空気中５００〜−−７〜００℃の
温度で加熱脱水することによシ、オキシ水酸化鉄の脱水
によシ生成する針状の酸化鉄のコアと、ｚｎＯまたはＺ
ｎＯとＳｉＯ□との混合酸化物の被膜を有する５ｔＯ２
のシェルが形成される。この粉末を常法によシ、たとえ
ば４００℃以上の温度で水素ガスを用いて還元すること
により、磁性金属をコアとし、ＺｎＯまたはＺｎＯと５
ｉ０２との混合酸化物の被膜を有するＳ ｉ ０２をシ
ェルとする磁性金属粉末゛を製造することができる。After the iron oxyhydroxide coated with an inorganic silicate and a zinc compound or a mixture of an inorganic silicate and a zinc compound is removed from house to house, it is dehydrated by heating in air at a temperature of 500 to 7 to 00°C, for example. By doing so, the acicular iron oxide core produced by dehydration of iron oxyhydroxide and ZnO or Z
5tO2 with a mixed oxide film of nO and SiO□
shell is formed. By reducing this powder using a conventional method, for example, using hydrogen gas at a temperature of 400°C or higher, ZnO or ZnO and 5
It is possible to produce a magnetic metal powder having a shell of S i 02 having a coating of a mixed oxide with i 02 .
本発明の磁性金属粉末は、そのシェルの外表面にＺｎＯ
が存在することによシ、該粉末を用いた磁気記録媒体た
とえば磁気テープの配向特性である残留飽和磁束密度（
Ｂｒ）および角形比（Ｒｓ）の向上に寄与する。すなわ
ち、表面に存在するＺｎＯが何等かの形で磁性金属粉末
の分散性および配向性に作用するものと推定される。し
たがって、シェル全体として、５ｉ０２ ： ＺｎＯの
モル比が、１：０．１〜１：０．７、好ましくは１：０
．２５〜１：０．５５のＺｎＯを含有する必要があシ、
そのＺｎＯは、シェルの外表面側に偏シ、外表面にＺｎ
Ｏが存在する必要がある。The magnetic metal powder of the present invention has ZnO on the outer surface of its shell.
Due to the presence of powder, the residual saturation magnetic flux density (
Br) and squareness ratio (Rs). That is, it is presumed that ZnO present on the surface affects the dispersibility and orientation of the magnetic metal powder in some way. Therefore, in the shell as a whole, the molar ratio of 5i02:ZnO is 1:0.1 to 1:0.7, preferably 1:0.
．． It is necessary to contain ZnO of 25 to 1:0.55,
The ZnO is concentrated on the outer surface of the shell, and the ZnO is on the outer surface.
O must exist.
以下に１本発明を実施例により、さらに具体的に説明す
る。ただし、本発明の範囲は、下記実施例によシ何等限
定されるものではない。The present invention will be explained in more detail below with reference to Examples. However, the scope of the present invention is not limited in any way by the following examples.
実施例１
０．３ｆ／を濃度のへキサメタリン酸ナトリウム水溶液
に、高アルカリ領域で合成したＮｉ １．５ ａｔｍ％
／Ｆｅを含有するα−オキシ水酸化鉄結晶を添加し、１
５ ｆ／を濃度の懸濁液２ｔを調製した。該懸濁液に水
硝子２号の２．６ｗｔ％水溶液２５９艷を添加攪拌した
。分析の結果、ｓｉｏ□に換算して、４．Ｏｗｔ％／Ｆ
ｅの珪素化合物がα−オキシ水酸化鉄結晶に被着してい
た。Example 1 Ni 1.5 atm% synthesized in a high alkaline region in a sodium hexametaphosphate aqueous solution with a concentration of 0.3 f/
/Fe-containing α-iron oxyhydroxide crystals are added, and 1
2 t suspensions were prepared with a concentration of 5 f/. To the suspension was added 259 g of a 2.6 wt % aqueous solution of Mizu Glass No. 2 and stirred. As a result of the analysis, converted to sio□, 4. Owt%/F
The silicon compound of e was deposited on the α-iron oxyhydroxide crystal.
得られた懸濁液に、０．８４モル／を濃度の硫酸亜鉛水
溶液１０−を徐々に添加し、ついでＩＮ硫酸水溶液を添
加して中和した後、１０時間熟成した。To the obtained suspension, an aqueous solution of zinc sulfate 10-10% having a concentration of 0.84 mol/mole was gradually added, then an aqueous IN sulfuric acid solution was added to neutralize the suspension, and the suspension was aged for 10 hours.
この水懸濁液から濾過してα−オキシ水酸化鉄結晶を回
収し、水洗・乾燥後、６７５℃の温度に加熱して脱水し
、ついで、水素気流中において４００℃の温度で還元し
、ＺｎＯとＳｉＯ２との混合酸化物で被覆されたＳｉＯ
２シエルを有する磁性金属粉末を得た。α-Iron oxyhydroxide crystals are collected from this aqueous suspension by filtration, washed with water, dried, heated to a temperature of 675°C to dehydrate, and then reduced in a hydrogen stream at a temperature of 400°C. SiO coated with mixed oxide of ZnO and SiO2
A magnetic metal powder having 2 shells was obtained.
得られた磁性金属粉末のＺｎＯおよびＳｌＯ□の分析結
果、ＢＥＴ法で測定した比表面積および粉末磁気特性を
第１表中に示す。Table 1 shows the analysis results of ZnO and SlO□ of the obtained magnetic metal powder, the specific surface area measured by the BET method, and the powder magnetic properties.
実施例２
０．３ｆ／を濃度のへキサメタリン酸ナトリウム水溶液
に、弱アルカリ領域で合成し六Ｎｆ １．５ ａｔｍ％
／Ｆｅを含むα−オキシ水酸化鉄結晶を添加し、１５ｆ
／を濃度の懸濁液２ｔを調製した。該懸濁液に水硝子２
号のｓ、７ｖｔｒｔｓ水溶液５６９−を添加攪拌した。Example 2 Synthesizing in a weakly alkaline region in a sodium hexametaphosphate aqueous solution with a concentration of 0.3f/6Nf 1.5 atm%
/Fe-containing α-iron oxyhydroxide crystals are added,
2 t of suspension with a concentration of / was prepared. Add 2 ml of water glass to the suspension.
No. s, 7vtrts aqueous solution 569- was added and stirred.
分析の結果、５１０２に換算して７．２ｗｔ％／Ｆｅの
珪素化合物がα−オキシ水酸化鉄結晶に被着していた。As a result of the analysis, a silicon compound of 7.2 wt %/Fe in terms of 5102 was adhered to the α-iron oxyhydroxide crystal.
この懸濁液に、０．８４モル／を濃度の硫酸亜鉛水溶液
１０１ｄを徐々に添加し、ついでＩＮ硫酸水溶液を用い
て中和した後、１０時間熟成した。To this suspension, 101d of an aqueous zinc sulfate solution having a concentration of 0.84 mol/m was gradually added, and then neutralized using an IN aqueous sulfuric acid solution, and then aged for 10 hours.
得られた懸濁液から珪素化合物および亜鉛化合物の被着
したα−オキシ水酸化鉄結晶を炉別し、水洗乾燥した後
、大気中６２５℃の温度に加熱して脱水した。ついで水
素気液中３８０℃の温度で還元し、ＺｎＯと５ｉｎ２と
の混合酸化物で被覆されたＳｉＯ□シェルを有する磁性
鉄粉を得た。The α-iron oxyhydroxide crystals coated with the silicon compound and the zinc compound were separated from the resulting suspension, washed with water and dried, and then heated to a temperature of 625° C. in the atmosphere for dehydration. Then, it was reduced in hydrogen gas and liquid at a temperature of 380° C. to obtain magnetic iron powder having a SiO□ shell coated with a mixed oxide of ZnO and 5in2.
得られた磁性鉄粉の諸粉末特性を第１表中に示す。Various powder properties of the obtained magnetic iron powder are shown in Table 1.
実施例３ 実施例２と同一の条件で処理し磁性鉄粉を得た。Example 3 A magnetic iron powder was obtained by processing under the same conditions as in Example 2.
得られた磁性鉄粉の諸粉末特性を第１表中に示す。Various powder properties of the obtained magnetic iron powder are shown in Table 1.
比較例１．２および３
実施例１．２、および３において、亜鉛化合物の添加を
行なわない以外には、同一の条件で処理し、Ｓｈｏ□の
みのシェルを有する磁性粉末を得た。Comparative Examples 1.2 and 3 Examples 1.2 and 3 were treated under the same conditions except that no zinc compound was added, and magnetic powders having only Sho□ shells were obtained.
得られた磁性粉末の諸粉末特性を第１表中に示す。Various powder characteristics of the obtained magnetic powder are shown in Table 1.
試験例
実施例および試験例で得られた磁性鉄粉のテープ化配向
試験を行った。Test Examples A tape orientation test was conducted on the magnetic iron powder obtained in Examples and Test Examples.
磁性鉄粉、分散剤（デイオミン・市販品）、バインダー
（塩化ビニル−酢酸ビニル共重合体）および溶剤（トル
エンおよびシクロヘキサノンの混合溶媒）を１００ｍ１
のステンレス製ボールミルで混合混練して塗料化した。100ml of magnetic iron powder, dispersant (Diomine, commercially available), binder (vinyl chloride-vinyl acetate copolymer), and solvent (mixed solvent of toluene and cyclohexanone)
The mixture was mixed and kneaded in a stainless steel ball mill to form a paint.
得られた磁性塗料を４８００ガウスの磁場をかけてプラ
スチックテープに５μｍの厚さに塗布し、磁気テープを
作成した。The obtained magnetic paint was applied to a plastic tape to a thickness of 5 μm while applying a magnetic field of 4800 Gauss to prepare a magnetic tape.
得られた磁気テープの配向特性を第１表中に示〔発明の
効果〕
本発明の磁性金属粉末は、前記第１表中に示す如く、テ
ープ化配向特性である残留飽和磁束密度二Ｂｒおよび角
形比：Ｒ８が、従来法（比較例参照）に比べ高い値とな
る。すなわち、分散性および配向性の優れた磁性金属粉
末であシ、この磁性金属粉末を用いることによシ、高記
録密度の磁気記録媒体の製造を可能とするものである。The orientation characteristics of the obtained magnetic tape are shown in Table 1. [Effects of the Invention] As shown in Table 1, the magnetic metal powder of the present invention has a residual saturation magnetic flux density of 2Br and 2Br, which are the orientation characteristics of the tape. Squareness ratio: R8 has a higher value than that of the conventional method (see comparative example). That is, the magnetic metal powder has excellent dispersibility and orientation, and by using this magnetic metal powder, it is possible to manufacture a magnetic recording medium with high recording density.
本発明は、分散性、配向性の改良された磁性金属粉末お
よびその製造方法を提供するものであシ、その産業的意
義は極めて大きい。The present invention provides a magnetic metal powder with improved dispersibility and orientation, and a method for producing the same, and has extremely great industrial significance.
Claims (6)
ｉＯ＿２のシェルとからなる磁性金属粉末(1) S with magnetic metal core and ZnO on the outer surface
Magnetic metal powder consisting of iO_2 shell
ある特許請求の範囲第（１）項記載の磁性金属粉末(2) Magnetic metal powder according to claim (1), wherein the magnetic metal is iron or a magnetic alloy mainly composed of iron.
０．７である特許請求の範囲第（１）項記載の磁性金属
粉末(3) ZnO/SiO_2 molar ratio in the shell is 0.1~
0.7 magnetic metal powder according to claim (1)
いで、該無機珪酸塩上に、亜鉛化合物または、亜鉛化合
物と無機珪酸塩との混合物を被着した後、加熱脱水し、
さらに還元ガス中において加熱還元することを特徴とす
る磁性金属粉末の製造方法(4) depositing an inorganic silicate on the surface of iron oxyhydroxide, then depositing a zinc compound or a mixture of a zinc compound and an inorganic silicate on the inorganic silicate, followed by heating and dehydration;
A method for producing magnetic metal powder characterized by further heating and reducing the powder in a reducing gas.
求の範囲第（４）項記載の磁性金属粉末の製造方法(5) The method for producing magnetic metal powder according to claim (4), wherein the inorganic silicate is a water-soluble salt of silicic acid.
の範囲第（４）項記載の磁性金属粉末の製造方法(6) The method for producing magnetic metal powder according to claim (4), wherein the zinc compound is a water-soluble salt of zinc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59142790A JPS6122604A (en) | 1984-07-10 | 1984-07-10 | Magnetic metal powder and manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59142790A JPS6122604A (en) | 1984-07-10 | 1984-07-10 | Magnetic metal powder and manufacture thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6122604A true JPS6122604A (en) | 1986-01-31 |
Family
ID=15323666
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59142790A Pending JPS6122604A (en) | 1984-07-10 | 1984-07-10 | Magnetic metal powder and manufacture thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6122604A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59143601A (en) * | 1983-02-04 | 1984-08-17 | 田之内 寅雄 | Method and device for detecting position of retreat and stoppage of tool rest in veneer lathe |
| JPS59150703A (en) * | 1983-02-17 | 1984-08-29 | 田之内 寅雄 | Outer-circumference drive method and device having axial core fixing function of material wood in veneer lathe |
| JPS59204502A (en) * | 1983-05-06 | 1984-11-19 | 田之内 寅雄 | Outer-circumference drive with axial fixing function of material wood in veneer lathe |
| US5124207A (en) * | 1989-04-20 | 1992-06-23 | Toda Kogyo Corp. | Magnetic iron oxide particles |
| CN111360269A (en) * | 2020-04-03 | 2020-07-03 | 南京环达新材料有限公司 | Multi-stage nanostructure reinforced laminated nickel-based composite material and preparation method thereof |
-
1984
- 1984-07-10 JP JP59142790A patent/JPS6122604A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59143601A (en) * | 1983-02-04 | 1984-08-17 | 田之内 寅雄 | Method and device for detecting position of retreat and stoppage of tool rest in veneer lathe |
| JPS6111765B2 (en) * | 1983-02-04 | 1986-04-04 | Tanochi Torao | |
| JPS59150703A (en) * | 1983-02-17 | 1984-08-29 | 田之内 寅雄 | Outer-circumference drive method and device having axial core fixing function of material wood in veneer lathe |
| JPS6111766B2 (en) * | 1983-02-17 | 1986-04-04 | Torao Tanochi | |
| JPS59204502A (en) * | 1983-05-06 | 1984-11-19 | 田之内 寅雄 | Outer-circumference drive with axial fixing function of material wood in veneer lathe |
| JPS6111767B2 (en) * | 1983-05-06 | 1986-04-04 | Torao Tanochi | |
| US5124207A (en) * | 1989-04-20 | 1992-06-23 | Toda Kogyo Corp. | Magnetic iron oxide particles |
| CN111360269A (en) * | 2020-04-03 | 2020-07-03 | 南京环达新材料有限公司 | Multi-stage nanostructure reinforced laminated nickel-based composite material and preparation method thereof |
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