JPH0352424B2 - - Google Patents
Info
- Publication number
- JPH0352424B2 JPH0352424B2 JP60140210A JP14021085A JPH0352424B2 JP H0352424 B2 JPH0352424 B2 JP H0352424B2 JP 60140210 A JP60140210 A JP 60140210A JP 14021085 A JP14021085 A JP 14021085A JP H0352424 B2 JPH0352424 B2 JP H0352424B2
- Authority
- JP
- Japan
- Prior art keywords
- density
- ferrite
- shaped
- present
- powder
- 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 26
- 239000000843 powder Substances 0.000 claims description 18
- 229910052596 spinel Inorganic materials 0.000 claims description 11
- 239000011029 spinel Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910006540 α-FeOOH Inorganic materials 0.000 description 2
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- -1 MnCO 3 Chemical class 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 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
- 150000002739 metals Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は電子工業用磁性材料の製造に利用され
る高密度フエライト焼結体の製造法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing a high-density sintered ferrite body used in producing magnetic materials for the electronic industry.
従来、フエライト用原料粉体としてはFe2O3，
MnCO3，Mn3O4，NiO，ZnO等の金属酸化物や
金属炭酸塩、さらには各金属の硫酸塩水溶液をア
ルカリで中和沈殿させた共沈原料粉末等があり、
これらを用いてフエライト焼結体を作成してい
た。
Conventionally, raw material powder for ferrite has been Fe 2 O 3 ,
There are metal oxides and metal carbonates such as MnCO 3 , Mn 3 O 4 , NiO, and ZnO, as well as coprecipitation raw material powders made by neutralizing and precipitating sulfate solutions of various metals with alkali.
These were used to create sintered ferrite bodies.
しかしこれらの原料を用いた場合、通常の焼成
雰囲気を制御した焼成法では、理論密度の95〜97
％のものしか得ることができないため、ホツトプ
レス焼結が、熱間静水圧プレス（HIP）焼結法等
を採用して高密度フエライト焼結体を製造してい
る。しかしこれらの方法はその工程上製品のコス
トが高くならざるを得ないという欠点があつた。
However, when these raw materials are used, the theoretical density of 95 to 97
%, hot press sintering, hot isostatic pressing (HIP) sintering, etc. are used to manufacture high-density ferrite sintered bodies. However, these methods have the disadvantage that the cost of the product inevitably increases due to the process.
〔発明の目的〕
本発明の目的は低価格で、高密度フエライト焼
結体を提供することにある。[Object of the Invention] An object of the present invention is to provide a high-density sintered ferrite body at low cost.
本発明は粒子形状が盤状のスピネルフエライト
粉末を主成分とする原料フエライト粉末を加圧成
形し、焼成することを特徴とする高密度フエライ
ト焼結体の製造法に関するものである。
The present invention relates to a method for producing a high-density sintered ferrite body, which is characterized in that a raw material ferrite powder whose main component is spinel ferrite powder with a plate-like particle shape is pressure-molded and fired.
本発明において原料の粒子形状が盤状のスピネ
ルフエライト粉末は、例えば粒子形状が盤状のγ
−Fe2O3とマンガン、亜鉛、ニツケル等の水酸化
物または酸化物との混合物を700℃以下、好まし
くは550〜700℃の温度で熱処理して焼結させる方
法で製造することができる。粒子形状が盤状のγ
−Fe2O3は、塩化第二鉄の如き第二鉄塩と水酸化
ナトリウムの如きアルカリとを、水の存在下にエ
タノールアミンの如きオキシアルキルアミンを第
二鉄塩に対して30〜80倍モル添加して、反応させ
て水酸化第二鉄のスラリを得、スラリを水熱処理
して盤状のα−FeOOHを得、盤状のα−
FeOOH粉末を加熱脱水して盤状のα−Fe2O3粉
末とし、これを水素の如き還元性ガスで還元して
盤状のFe3O4粉末とし、次いで再酸化することに
よつて得ることができる。 In the present invention, the raw material spinel ferrite powder with a plate-like particle shape is, for example, γ having a plate-like particle shape.
- It can be produced by a method in which a mixture of Fe 2 O 3 and a hydroxide or oxide of manganese, zinc, nickel, etc. is heat treated and sintered at a temperature of 700°C or lower, preferably 550 to 700°C. γ with a plate-like particle shape
-Fe 2 O 3 is obtained by combining a ferric salt such as ferric chloride with an alkali such as sodium hydroxide, and adding an oxyalkylamine such as ethanolamine in the presence of water to a concentration of 30 to 80% relative to the ferric salt. Double the molar amount was added, reacted to obtain a slurry of ferric hydroxide, hydrothermally treated the slurry to obtain a plate-shaped α-FeOOH, and a plate-shaped α-FeOOH.
Obtained by heating and dehydrating FeOOH powder to obtain plate-shaped α-Fe 2 O 3 powder, reducing this with a reducing gas such as hydrogen to obtain plate-shaped Fe 3 O 4 powder, and then reoxidizing it. be able to.
本発明において高密度フエライト焼結体は、例
えば原料フエライト粉末に、通常のセラミツクス
の製法と同様にポリビニルアルコールの如きバイ
ンダーを加えて成形体とした後、500℃程度まで
は空気中で、次いで窒素の如き不活性ガス雰囲気
下に1300〜1400℃程度まで昇温して焼成すること
によつて製造することができる。 In the present invention, the high-density ferrite sintered body is produced by adding a binder such as polyvinyl alcohol to the raw material ferrite powder in the same manner as in ordinary ceramic manufacturing methods to form a molded body, and then heating it in air up to about 500°C and then heating it in nitrogen. It can be produced by firing at a temperature of about 1,300 to 1,400° C. in an inert gas atmosphere.
本発明においては主原料として盤状のスピネル
フエライトを少なくとも60重量％以上、好ましく
は約80重量％以上含むものを用いると高密度変化
に対する顕著な効果が認められる。また各種特性
を改良するため盤状のスピネルフエライト粉末に
添加物を加えてもよい。添加物は20重量％以下の
量で加えても、本発明の高密度焼結体作成の効果
が失われないことが認められる。一方本発明にお
いて主成分として用いられる盤状のスピネルフエ
ライトの原料粉末は、仮焼等の熱処理を行つても
よいが、その際、仮焼温度が高くなりすぎて、盤
状性がそこなわれると、本発明の効果は失われ
る。また、熱処理により盤状性をそこなわなくて
も、α−Fe2O3の析出があつたりして、単一のス
ピネル相から他の相が出たものを用いたのでは高
密度の焼結体は得られない。よつて本発明の目的
とする効果を得るには、主成分の原料粉末は盤状
でありかつスピネル相であることが必要である。 In the present invention, when a material containing at least 60% by weight or more, preferably about 80% by weight or more of disk-shaped spinel ferrite is used as the main raw material, a remarkable effect on high density changes is observed. Additionally, additives may be added to the disk-shaped spinel ferrite powder in order to improve various properties. It is recognized that even if the additive is added in an amount of 20% by weight or less, the effect of producing a high-density sintered body of the present invention is not lost. On the other hand, the disc-shaped raw material powder of spinel ferrite used as the main component in the present invention may be subjected to heat treatment such as calcination, but in that case, the calcination temperature becomes too high and the disc-shaped property is impaired. Then, the effect of the present invention is lost. In addition, even if heat treatment does not impair the platy properties, α-Fe 2 O 3 may precipitate, and if a single spinel phase with other phases is used, high-density sintering may occur. No body is obtained. Therefore, in order to obtain the desired effect of the present invention, it is necessary that the raw material powder as the main component has a disc shape and a spinel phase.
以下本発明を実施例について詳細に説明する。 Hereinafter, the present invention will be described in detail with reference to examples.
実施例 １
粒径0.1μm、盤状比3.2、比表面積27m2／ｇの53
モル％Fe2O3、28モル％MoO、19モル％ZnOの組
成を有する盤状のMn−Znフエライト粉末に、濃
度５％のPVA（ポリビニルアルコール）溶液を15
重量％添加して造粒し、成形圧力1t／cm2で10mmφ
×５mmの成形体ペレツトを作成した。Example 1 53 with a particle size of 0.1 μm, a platelet ratio of 3.2, and a specific surface area of 27 m 2 /g.
A PVA (polyvinyl alcohol) solution with a concentration of 5% was added to a disc-shaped Mn-Zn ferrite powder having a composition of mol% Fe 2 O 3 , 28 mol% MoO, and 19 mol% ZnO.
Add % by weight and granulate it to 10mmφ at a molding pressure of 1t/ cm2 .
A molded pellet having a size of 5 mm was prepared.
なお比較のため盤状γ−Fe2O3とMnCO3，
ZnOを用いたもの、粒状のα−Fe2O3とMnCO3，
ZnOを用いたものを、同じ組成比になるように配
合しボールミル混合した。乾燥後各一部はそのま
まで造粒した後成形し、残りのものは800〜1000
℃で空気中にて仮焼し、再度、ボールミルにて粉
砕、混合し、乾燥後造粒を行ない上記と同一条件
下で成形体を作成した。 For comparison, plate-like γ-Fe 2 O 3 and MnCO 3 ,
Those using ZnO, granular α-Fe 2 O 3 and MnCO 3 ,
Those using ZnO were blended to have the same composition ratio and mixed in a ball mill. After drying, part of each part is granulated and molded as it is, and the remaining part is 800~1000 granules.
The mixture was calcined in air at ℃, pulverized again in a ball mill, mixed, dried, and then granulated to produce a molded body under the same conditions as above.
これら実施例１の成形体および比較のための成
形体を、500℃までは空気中で加熱昇温を行ない
バインダーを燃焼させた後、500℃からはN2中で
1300℃まで昇温し、この温度にて３時間焼成し、
同N2中で冷却して各試料を取り出した。 The molded bodies of Example 1 and the comparative molded bodies were heated in air up to 500°C to burn the binder, and then heated in N 2 from 500°C.
Raise the temperature to 1300℃ and bake at this temperature for 3 hours,
Each sample was taken out after cooling in the same N 2 atmosphere.
得られた焼結体の密度を測定した結果、本発明
の盤状のスピネルフエライト粉末を用いた焼結体
ではその密度は理論密度の99.5％であり、他の原
料、例えば盤状γ−Fe2O3、とMnCO3，ZnOを
用いて仮焼しなかつたものではその密度は95.6
％、仮焼したものでは97.5％、また粒状α−
Fe2O3，MnCO3，ZnOを用い、仮焼しなかつた
ものではその密度は96％、仮焼したものでは97％
と低い値であつた。 As a result of measuring the density of the obtained sintered body, the density of the sintered body using the disc-shaped spinel ferrite powder of the present invention was 99.5% of the theoretical density, and the density of the sintered body using the disc-shaped spinel ferrite powder of the present invention was 99.5% of the theoretical density. 2 O 3 , MnCO 3 , and ZnO that were not calcined had a density of 95.6.
%, calcined 97.5%, and granular α-
Using Fe 2 O 3 , MnCO 3 , and ZnO, the density is 96% when not calcined and 97% when calcined.
It was a low value.
盤状のスピネルフエライト粉末を用いると容易
に高密度の各種Mn−Znフエライトが得られる。
このフエライトを磁気ヘツドに加工して磁気ヘツ
ドにした場合重要な特性である耐摩耗性が優れて
いた。
By using disk-shaped spinel ferrite powder, various high-density Mn-Zn ferrites can be easily obtained.
When this ferrite was processed into a magnetic head, it had excellent wear resistance, which is an important property.
Claims (1)
主成分とする原料フエライト粉末を加圧成形し、
焼成することを特徴とする高密度フエライト焼結
体の製造法。1 Pressure molding raw material ferrite powder whose main component is spinel ferrite powder with a plate-like particle shape,
A method for producing a high-density ferrite sintered body, which is characterized by firing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60140210A JPS623070A (en) | 1985-06-28 | 1985-06-28 | Manufacture of high density ferrite sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60140210A JPS623070A (en) | 1985-06-28 | 1985-06-28 | Manufacture of high density ferrite sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS623070A JPS623070A (en) | 1987-01-09 |
| JPH0352424B2 true JPH0352424B2 (en) | 1991-08-09 |
Family
ID=15263477
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60140210A Granted JPS623070A (en) | 1985-06-28 | 1985-06-28 | Manufacture of high density ferrite sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS623070A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0347743A (en) * | 1989-04-18 | 1991-02-28 | Bridgestone Corp | Method and apparatus for winding band-like member |
-
1985
- 1985-06-28 JP JP60140210A patent/JPS623070A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS623070A (en) | 1987-01-09 |
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