JPH0419169B2 - - Google Patents
Info
- Publication number
- JPH0419169B2 JPH0419169B2 JP56207356A JP20735681A JPH0419169B2 JP H0419169 B2 JPH0419169 B2 JP H0419169B2 JP 56207356 A JP56207356 A JP 56207356A JP 20735681 A JP20735681 A JP 20735681A JP H0419169 B2 JPH0419169 B2 JP H0419169B2
- Authority
- JP
- Japan
- Prior art keywords
- ferrite
- temperature
- suspension
- precipitate
- ions
- 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 - Lifetime
Links
- 229910000859 α-Fe Inorganic materials 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910001427 strontium ion Inorganic materials 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- 230000005294 ferromagnetic effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 239000000725 suspension Substances 0.000 description 12
- 230000005291 magnetic effect Effects 0.000 description 8
- 239000002244 precipitate Substances 0.000 description 7
- 229960004887 ferric hydroxide Drugs 0.000 description 4
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 4
- 229910003514 Sr(OH) Inorganic materials 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 235000014413 iron hydroxide Nutrition 0.000 description 3
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Compounds Of Iron (AREA)
- Hard Magnetic Materials (AREA)
Description
【発明の詳細な説明】
本発明は、高密度磁気記憶用及び優れた異方性
のSrフエライトの焼結体用の原料であるSrフエ
ライト粉末の製造に関するものであつて、詳しく
はSrFe12O19の結晶構造を有した分散性の良好な
微細な板状の強磁性単結晶粒子より成る沈澱の製
造法である。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to the production of Sr ferrite powder, which is a raw material for high-density magnetic storage and for sintered bodies of Sr ferrite with excellent anisotropy . This is a method for producing a precipitate consisting of fine plate-shaped ferromagnetic single crystal grains with good dispersibility and a crystal structure of 19 .
周知の通り、SrフエライトはSrCO3とFe2O3又
は水酸化鉄（）との混合物を高温に於て熱分解
することにより製造されている。 As is well known, Sr ferrite is produced by thermally decomposing a mixture of SrCO 3 and Fe 2 O 3 or iron hydroxide () at high temperatures.
この場合、混合物の種類によつて多少異るが、
Srフエライトは約800℃で生成し始め、焼成温度
が上るにつれてSrフエライト生成が促進される。 In this case, although it varies somewhat depending on the type of mixture,
Sr ferrite begins to form at about 800°C, and as the firing temperature increases, Sr ferrite formation is accelerated.
上記の熱分解法で生成したSrフエライト粒子
は粒子間が焼結された状態となり易く、各Srフ
エライト粒子の（001）面を同一方向に配向する
ことは困難である。 The Sr ferrite particles produced by the above thermal decomposition method tend to be in a sintered state between particles, and it is difficult to orient the (001) planes of each Sr ferrite particle in the same direction.
現在、磁気記憶用材に要求される性能は、より
大きなHcを有した高密度な磁気記録能であり、
また、複雑な形状の異方性焼結体には、磁場プレ
スの操作なしに、加圧のみで配高し易い微細な
Srフエライト粒子が要求されている。 Currently, the performance required for magnetic storage materials is high-density magnetic recording ability with a larger Hc.
In addition, for complex-shaped anisotropic sintered bodies, fine particles can be easily placed using only pressure without the need for magnetic field press operation.
Sr ferrite particles are required.
本発明は、かかる要求に適した、Srフエライ
ト粒子１ケ１ケが実質的にバラバラの状態である
強磁性沈澱の製造法に関するものである。以下本
発明の詳細について述べる。 The present invention relates to a method for producing a ferromagnetic precipitate in which each Sr ferrite particle is substantially dispersed, and is suitable for meeting such requirements. The details of the present invention will be described below.
第２鉄塩の酸性水溶液にNaOHを添加すると
酸性又はアルカリ性の水酸化第２鉄のけんだく液
が得られる。酸性けんだく液を加熱すると水酸化
第２鉄は90℃以上の温度でα−Fe2O3に変化す
る。一方アルカリ性けんだく液を90℃以上の温度
で加熱すると、水酸化第２鉄はα−FeO（OH）
又はα−Fe2O3に変化する。α−Fe2O3の生成比
はけんだく液の温度や過剰NaOH濃度によつて
左右される。Srの硝酸塩や塩化物とNaOHの水
溶液を混合するSrイオンが水酸化物として沈澱
してくる。α−Fe2O3とSrフエライトの結晶格子
の骨組みは似ており、本発明者はα−Fe2O3生成
時にSrイオンが共存しこれが沈澱するならばSr
フエライトが生成する筈であると考えた。Srイ
オンが沈澱する度合はPHと水溶液の温度によつて
左右される。そこで、本発明者は、数多くの実験
の結果、Srイオン１原子にFe（）は８原子以
下、出発けんだく液のPHは12又はそれ以上の場合
に水酸化第２鉄は、250℃でSrフエライトに変化
し始め、反応温度が高くなるにつれてその生成比
が増し300℃では殆どすべての水酸化鉄がSrフエ
ライトに変化することを発見し、本発明に到達し
た。 When NaOH is added to an acidic aqueous solution of a ferric salt, an acidic or alkaline suspension of ferric hydroxide is obtained. When an acidic suspension is heated, ferric hydroxide changes to α-Fe 2 O 3 at a temperature of 90°C or higher. On the other hand, when an alkaline suspension is heated to a temperature of 90℃ or higher, ferric hydroxide turns into α-FeO(OH).
Or it changes to α-Fe 2 O 3 . The production ratio of α-Fe 2 O 3 depends on the temperature of the suspension and the excess NaOH concentration. When Sr nitrate or chloride is mixed with an aqueous solution of NaOH, Sr ions will precipitate as hydroxide. The crystal lattice frameworks of α-Fe 2 O 3 and Sr ferrite are similar, and the present inventor believes that if Sr ions coexist and precipitate during α-Fe 2 O 3 formation, Sr
I thought that ferrite should be generated. The degree to which Sr ions precipitate depends on the pH and the temperature of the aqueous solution. Therefore, as a result of numerous experiments, the present inventor found that when Fe() is 8 atoms or less per 1 atom of Sr ion and the pH of the starting suspension is 12 or more, ferric hydroxide can be heated at 250℃. The present invention was achieved by discovering that iron hydroxide begins to change to Sr ferrite, and as the reaction temperature increases, the production ratio increases and at 300°C, almost all iron hydroxide changes to Sr ferrite.
即ち、本発明は、Srイオン１原子に対して８
原子以下の鉄（）イオンを含むPH12又はそれ以
上の溶液をCO2の非存在下に調製するとともに
250〜320℃に加熱することにより、該溶液中に
SrFe12O19の結晶構造を有する強磁性板状微結晶
子を生ぜしめることを特徴とするSrフエライト
の製造法である。 That is, in the present invention, 8
A solution containing subatomic iron() ions with a pH of 12 or higher is prepared in the absence of CO 2 and
into the solution by heating to 250-320°C.
This is a method for producing Sr ferrite characterized by producing ferromagnetic plate-like microcrystallites having a crystal structure of SrFe 12 O 19 .
次に、本発明の実施条件について述べる。 Next, conditions for implementing the present invention will be described.
Srイオン１原子に対してFe（）が８を超える
場合には、Srフエライトの生成に好適ないかな
る水熱合成条件下でも、α−Fe2O3の副生が避け
られない。また、けんだく液の温度を320℃以上
にしてもSrフエライトの生成に及ぼす効果は少
く、従つて経済性の点で好しくない。また、前記
出発けんだく液の調製は、CO2の混入による
SrCO3の生成を避けるために、CO2の非存在下で
行なう必要があり、具体的には後出実施例に示し
ている通り、CO2を含まないN2雰囲気中で行な
えばよい。この様にして得られたSrフエライト
は、１〜2μｍの板状粒子より成り立ち、10KOe
に於ける磁気測定によれば、反応条件により、磁
化の強さＭ値は40〜50emu／ｇ、Hcは900〜
150Oeの範囲の磁性を有している。 When Fe() exceeds 8 per 1 atom of Sr ion, the by-product of α-Fe 2 O 3 is unavoidable under any hydrothermal synthesis conditions suitable for producing Sr ferrite. Further, even if the temperature of the suspension is set to 320° C. or higher, the effect on the formation of Sr ferrite is small, and therefore it is not favorable from an economic point of view. In addition, the preparation of the starting suspension may be due to the incorporation of CO2 .
In order to avoid the generation of SrCO 3 , it is necessary to carry out the process in the absence of CO 2 , and specifically, as shown in the Examples below, it may be carried out in an N 2 atmosphere that does not contain CO 2 . The Sr ferrite obtained in this way is composed of plate-like particles of 1 to 2 μm, and has a diameter of 10 KOe.
According to magnetic measurements in
It has magnetism in the range of 150Oe.
以下、本発明を実施例により更に具体的に説明
する。 EXAMPLES Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例 １
0.075mol SrCl2、0.45mol FeCl3と6mol過剰
NaOHを含むアルカリ性けんだく液500mlをN2中
でCO2が混入しない様に作製した。この赤褐色け
んだく液（PH12）をオートクレーブ内で加熱し、
300℃の温度で5hr保持してから室温で取出した。
反応後けんだく液のPHは12.4となり液中には茶色
強磁性沈澱が生じていた。Ｘ−線分折によれば沈
澱物は、平均厚さ600−700〓のSrFe12O19板状粒
子と微量のSr（OH）2の無水物より成立つていた。
3M HC104で処理することによつてSr水酸化物を
溶解後充分水洗し、100℃の温度で空気中で乾燥
粉末材料とした。最高磁場10KOeで磁気を測定
した結果Ｍは41emu／ｇでありHcは1.26KOeで
あつた。Example 1 0.075mol SrCl 2 , 0.45mol FeCl 3 and 6mol excess
500 ml of an alkaline suspension containing NaOH was prepared in N 2 to avoid contamination with CO 2 . This reddish-brown suspension liquid (PH12) is heated in an autoclave,
It was kept at a temperature of 300°C for 5 hours and then taken out at room temperature.
After the reaction, the pH of the suspension was 12.4, and a brown ferromagnetic precipitate had formed in the solution. According to X-ray spectroscopy, the precipitate consisted of SrFe 12 O 19 plate-like particles with an average thickness of 600-700 mm and a small amount of anhydrous Sr(OH) 2 .
After dissolving the Sr hydroxide by treatment with 3M HC104 , the material was thoroughly washed with water and dried in air at a temperature of 100° C. to form a powder material. As a result of measuring magnetism at the highest magnetic field of 10 KOe, M was 41 emu/g and Hc was 1.26 KOe.
実施例 ２
0.11mol Sr（OH）2、0.45mol Fe（NO3）3と
0.3mol NaOHを含むアルカリ性褐色けんだく液
500mlをN2雰囲気中で作製した。このけんだく液
をオートクレーブを用いて300℃の温度で5hr保持
してから、室温に冷した。沈澱している強磁性物
SrFe12O19を濾別し、3M HC104で数回共存する
Sr（OH）2分を溶解除去してから、水洗し、100℃
の温度で空気中で乾燥させた。最高磁場10KOe
に於ける磁気測定の結果Ｍは44emu／ｇ、Hcは
1.0KOeであつた。Example 2 0.11mol Sr(OH) 2 , 0.45mol Fe(NO 3 ) 3 and
Alkaline brown suspension containing 0.3mol NaOH
500ml was made in N2 atmosphere. This suspension was maintained at a temperature of 300°C for 5 hours using an autoclave, and then cooled to room temperature. Precipitated ferromagnetic material
Filter out SrFe 12 O 19 and coexist with 3M HC10 4 several times
Dissolve and remove Sr(OH) for 2 minutes, then wash with water and heat to 100°C.
dried in air at a temperature of . Maximum magnetic field 10KOe
The result of magnetic measurement at M was 44emu/g, and Hc was
It was 1.0KOe.
Claims (1)
（）イオンを含むPH12又はそれ以上の溶液を
CO2の非存在下に調製するとともに250〜320℃に
加熱することにより、該溶液中にSrFe12O19の結
晶構造を有する強磁性板状微結晶粒子を生ぜしめ
ることを特徴とするSrフエライトの製造法。1. A solution with a pH of 12 or higher containing 8 or less iron () ions per 1 atom of Sr ions.
An Sr ferrite characterized by producing ferromagnetic plate-like microcrystalline particles having a crystal structure of SrFe 12 O 19 in the solution by preparing it in the absence of CO 2 and heating it to 250 to 320°C. manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20735681A JPS58110432A (en) | 1981-12-21 | 1981-12-21 | Manufacture of sr ferrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20735681A JPS58110432A (en) | 1981-12-21 | 1981-12-21 | Manufacture of sr ferrite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58110432A JPS58110432A (en) | 1983-07-01 |
| JPH0419169B2 true JPH0419169B2 (en) | 1992-03-30 |
Family
ID=16538369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20735681A Granted JPS58110432A (en) | 1981-12-21 | 1981-12-21 | Manufacture of sr ferrite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58110432A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2586846Y2 (en) * | 1992-04-22 | 1998-12-14 | 株式会社シマノ | fishing rod |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107032776A (en) * | 2016-11-22 | 2017-08-11 | 武汉理工大学 | Single-phase multiferroic M types strontium ferrite ceramics and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4923676A (en) * | 1972-06-22 | 1974-03-02 | ||
| JPS55154321A (en) * | 1979-05-21 | 1980-12-01 | Hitachi Metals Ltd | Manufacture of magnetic oxide particle |
-
1981
- 1981-12-21 JP JP20735681A patent/JPS58110432A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4923676A (en) * | 1972-06-22 | 1974-03-02 | ||
| JPS55154321A (en) * | 1979-05-21 | 1980-12-01 | Hitachi Metals Ltd | Manufacture of magnetic oxide particle |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2586846Y2 (en) * | 1992-04-22 | 1998-12-14 | 株式会社シマノ | fishing rod |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58110432A (en) | 1983-07-01 |
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