JPH0438807A - Manufacture of strontium-ferrite magnet high in residual magnetic flux density and coercive force - Google Patents
Manufacture of strontium-ferrite magnet high in residual magnetic flux density and coercive forceInfo
- Publication number
- JPH0438807A JPH0438807A JP2145344A JP14534490A JPH0438807A JP H0438807 A JPH0438807 A JP H0438807A JP 2145344 A JP2145344 A JP 2145344A JP 14534490 A JP14534490 A JP 14534490A JP H0438807 A JPH0438807 A JP H0438807A
- Authority
- JP
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- Prior art keywords
- powder
- ratio
- sio2
- mixture
- calcined
- 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.)
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Links
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 230000004907 flux Effects 0.000 title description 11
- 239000000843 powder Substances 0.000 claims abstract description 82
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 238000010298 pulverizing process Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims abstract description 10
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000010304 firing Methods 0.000 claims description 15
- 229910052712 strontium Inorganic materials 0.000 claims description 14
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052681 coesite Inorganic materials 0.000 abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 9
- 239000000377 silicon dioxide Substances 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 abstract description 9
- 238000005245 sintering Methods 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 3
- 239000000292 calcium oxide Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 20
- 235000013339 cereals Nutrition 0.000 description 16
- 239000002245 particle Substances 0.000 description 12
- 239000008188 pellet Substances 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 241000255789 Bombyx mori Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 241000985694 Polypodiopsida Species 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
Landscapes
- Hard Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明はストロンチウムフェライト磁石の製造方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION <Industrial Field of Application> The present invention relates to a method for manufacturing a strontium ferrite magnet.
〈従来の技術〉
従来モータ等の回転機器の励磁は巻線型の［１石で行っ
ていたが省エネルギーの立場から永久磁石を使用するこ
とが多くなってきた０回転機器の励磁用永久磁石として
は電機子に流れる過大な電流によって大きな反磁界が磁
石に作用するので保磁力（ｉＨｃ）の高い材料が望まれ
、ストロンチウムフェライト磁石がよく用いられている
。<Conventional technology> Conventionally, excitation of rotating equipment such as motors was performed using a single wire-wound magnet, but permanent magnets are increasingly being used from the standpoint of energy conservation. Since a large demagnetizing field acts on the magnet due to the excessive current flowing through the armature, a material with a high coercive force (iHc) is desired, and strontium ferrite magnets are often used.
しかしながらこの種のストロンチウムフェライト磁石の
磁気特性は残Ｗ［東密度（Ｂｒ）が４０００ Ｇ以上の
場合は保磁力（ｉＨｃ）が４００００ｅ未満であり、逆
に１ｌｌｃが４０００ Ｏｅ以上の場合は［ｌｒが４０
０００未満のものが多（、Ｂｒおよび１ｌｌｃ共に４０
００を趙えるものを得ることは掻めで困難であった。However, the magnetic properties of this type of strontium ferrite magnet are such that the coercive force (iHc) is less than 40,000e when the residual W density (Br) is 4000 G or more, and conversely, when the 1llc is 4000 Oe or more, the [lr] 40
Many are less than 000 (both Br and 1llc are 40
It was extremely difficult to find anything that could beat 00.
保磁力を改善するには単磁区結晶粒子の存在率を高くす
ればよく、そのため本焼成の前段階である仮焼組織で結
晶粒度のバラツキを小さく、かつ微細粒子を構成してお
くことが重要と考えられる。To improve the coercive force, it is sufficient to increase the abundance of single-domain crystal grains, so it is important to minimize the variation in crystal grain size and form fine grains in the calcined structure, which is the stage before the main firing. it is conceivable that.
ところが従来、仮焼温度は１３００℃程度としてできる
だけ結晶粒を粗大化し、単結晶に近いものを得るように
心がけられていたので、仮焼温度が高（、仮焼体の結晶
粒度のバラツキは異常に大きいものとなっていた。However, in the past, the calcination temperature was set at around 1300°C to make the crystal grains as coarse as possible and to obtain something close to a single crystal. It had become a big thing.
一方ストロンチウムフェライト磁石を製造する場合にＳ
ｒＯとＦｅオ０．のモル数の比ｎを、幾分ＳｒＯ過剰に
する（ｎ＜６）方がよいことが経験的に知られており、
特開昭４９−７２６９５号公報にも開示されている。On the other hand, when manufacturing strontium ferrite magnets, S
rO and FeO0. It is empirically known that it is better to make the ratio n of the number of moles of SrO somewhat excessive (n<6),
It is also disclosed in Japanese Unexamined Patent Publication No. 49-72695.
しかし過剰ＳｒＯは結晶粒の成長を促進させるため、単
磁区結晶粒子の存在率を高めることができず、磁気特性
は満足いくものではなかった。However, excess SrO promotes the growth of crystal grains, making it impossible to increase the abundance of single-domain crystal grains, resulting in unsatisfactory magnetic properties.
また、ストロンチウムフェライト磁石は焼成温度を高め
るにつれて焼成密度の向上と結晶粒の成長により残留磁
束密度は向上するが保磁力は著しく低下する。そこで粒
成長抑制添加物を多く含有させれば保磁力は４０００
Ｏｅ以上に高めることはできるが、この場合には非磁性
組成の増加、結晶配向度の低下等により、残留磁束密度
が低下する。In addition, as the firing temperature of strontium ferrite magnets increases, the residual magnetic flux density improves due to the improvement in the firing density and the growth of crystal grains, but the coercive force significantly decreases. Therefore, if a large amount of grain growth inhibiting additives is included, the coercive force will increase to 4000.
Although it is possible to increase the magnetic flux density to more than Oe, in this case, the residual magnetic flux density decreases due to an increase in the non-magnetic composition, a decrease in the degree of crystal orientation, etc.
また、ストロンチウムフェライト磁石の焼結体の磁気特
性は仮焼組織に概ね依存する。従って仮焼組織で結晶粒
度のバラツキが小さく、かつ微細粒子を構成することに
よって焼成後の結晶組織を微細化し単磁区粒子の存在率
を高め、保磁力を改善できる。一方、仮焼ｍ繊で六角板
状の粗大結晶組織を発達させることによって、磁場成形
時の結晶配向性を高め、焼成後の残ｌｉ！７磁束密度を
改善できる。しかしながら保磁力の改善と磁束密度の改
善の両者を同時に満足させることは従来技術では困難で
あった。Further, the magnetic properties of a sintered body of a strontium ferrite magnet generally depend on the calcined structure. Therefore, by forming the calcined structure with small variations in crystal grain size and fine grains, the crystal structure after sintering can be made finer, the abundance of single-domain grains can be increased, and the coercive force can be improved. On the other hand, by developing a hexagonal plate-like coarse crystal structure in the calcined m-fiber, the crystal orientation during magnetic field forming is improved, and the remaining li after firing is improved. 7. Magnetic flux density can be improved. However, it has been difficult with conventional techniques to simultaneously satisfy both the improvement of coercive force and the improvement of magnetic flux density.
〈発明が解決しようとする！１１３１＞また、本発明者
らは先に特願平１−３１５３４８号にて原料の酸化鉄と
炭酸ストロンチウムの組成比および仮焼前の５ｉＯｚ添
加量の規制、および仮焼温度、焼成温度の規制等により
Ｂｒ≧４０００（Ｇ）、１１１ｃ≧４０００ （Ｏｅ）
の磁電特性が得られることを示したが、本発明の目的は
更に優れた磁気特性、即ちＢｒ≧４１００（Ｃ；）、Ｉ
Ｈｃ≧４０００ （Ｏｅ）を有するストロンチウムフェ
ライト磁石の製造方法を提供することである。<Invention tries to solve! 1131> In addition, the present inventors previously disclosed in Japanese Patent Application No. 1-315348 the composition ratio of iron oxide and strontium carbonate as raw materials, the amount of 5iOz added before calcination, and the regulation of calcination temperature and firing temperature. etc., Br≧4000 (G), 111c≧4000 (Oe)
However, the object of the present invention is to obtain even better magnetic properties, namely, Br≧4100(C;), I
An object of the present invention is to provide a method for manufacturing a strontium ferrite magnet having Hc≧4000 (Oe).
＜３１題を解決するための手段〉
即ち、本発明は、酸化鉄と炭酸ストロンチウムを混合し
、造粒・仮焼した後、該仮焼物を粉砕し、しかる後磁場
中成形して得られる成形体を焼成してストロンチウムフ
ェライト磁石を製造する方法において、炭酸ストロンチ
ウム１モルに対しＦｅｚｅｓを５．３〜５．９モルおよ
び５１０．をＸモ）Ｉ／、ただし、Ｐｅ、Ｏ，のモル数
と（１−ｘ）モルの比が６となる組成比で混合し、１０
００〜１２５０’Ｃの温度で仮焼した後、咳仮焼物を粉
砕して得る微粉末（以下Ａ粉末と呼ぶ）と、５ｉＯｔを
含まない上記組成比の原料を１２００〜１３００℃の温
度で仮焼した後、該仮焼物をむ）砕して得る微粉末（以
下Ｂ粉末と叶ぶ）をＢ粉末に対するＡ粉末の混合比率（
重量比）が５０〜７５％の範囲で混合し、次いで該混合
粉に更に重量比で最終的にＳｉｎｇが０．４０〜０．７
０％、ＣａＯが０．３５〜０．４９％かつＣａｂ／５ｉ
ｆｔ比が０．５〜１．２５となるように添加した後、磁
場中成形し、しかる後焼成することを特徴とする残留磁
束密度および保磁力の高いストロンチウムフェライト磁
石の製造方法である。<Means for Solving Problem 31> That is, the present invention provides a molded product obtained by mixing iron oxide and strontium carbonate, granulating and calcining, pulverizing the calcined product, and then molding in a magnetic field. In a method for manufacturing a strontium ferrite magnet by firing a body, 5.3 to 5.9 mol of Fezes and 510. Xmo)I/, where the ratio of the number of moles of Pe, O, and (1-x) mole is 6, and 10
After calcining at a temperature of 00 to 1250'C, a fine powder obtained by crushing the cough calcined material (hereinafter referred to as powder A) and a raw material with the above composition ratio that does not contain 5iOt are calcined at a temperature of 1200 to 1300'C. After firing, the calcined material is crushed to produce a fine powder (hereinafter referred to as B powder), which is mixed at a mixing ratio of A powder to B powder (
Then, the mixed powder is further mixed with a final weight ratio of 0.40 to 0.7.
0%, CaO 0.35-0.49% and Cab/5i
This is a method for producing a strontium ferrite magnet with high residual magnetic flux density and coercive force, which is characterized by adding strontium ferrite magnets such that the ft ratio becomes 0.5 to 1.25, forming the magnets in a magnetic field, and then firing them.
く作 用〉
本発明では、上記の微粉砕したＡ粉末とＢ粉末とを混合
することによって、成形前の粒度分布を平均粒径が比較
的小さい（ｄ−０，２〜０．４ｎ）部分と大きな部分（
ｄ−０，９〜１．１ｍ）の“２山タイプの粒度分布を構
成する。このような粒度構成は成形時の金型内へのスラ
リーの最密充填が可能となり、その結果、成形密度の高
い成形体が得られる。加えて磁場成形で粗大粒子の磁化
容５軸への配向性が改善される。これら成形体は以後の
焼成工程の結晶粒成長の段階で微粒子は周囲の粒子に蚕
食され、比較的均一な結晶＆１１織が得られ焼結密度の
向上と結晶配向度も高くなる。Effect> In the present invention, by mixing the above-mentioned finely pulverized powder A and powder B, the particle size distribution before molding is divided into a portion where the average particle size is relatively small (d-0.2 to 0.4n). and a large portion (
d-0.9~1.1m) constitutes a two-peak type particle size distribution.Such a particle size structure enables the closest packing of the slurry into the mold during molding, and as a result, the molding density In addition, the magnetic field forming improves the orientation of the coarse particles to the five axes of magnetization.These compacts are produced by forming fine particles into the surrounding particles during the crystal grain growth stage of the subsequent firing process. It is eroded by silkworms, and a relatively uniform crystalline &11 weave is obtained, resulting in improved sintered density and a high degree of crystal orientation.
従って、当然Ａ粉末のみを原料とした場合には［１ｒが
低く、一方Ｂ粉末のみを原料とした場合には１ｆ−１ｃ
が低い材料しか得られないが、本発明のようにＡおよび
Ｂ粉末を混合することによって高８ｒ、高ｉＨｃの材料
を得ることができる。Therefore, naturally, when only powder A is used as a raw material, [1r is low, while when only powder B is used as a raw material, 1f-1c
However, by mixing A and B powders as in the present invention, a material with high 8r and high iHc can be obtained.
次に本発明の限定理由を個々に述べる。ｎ値が５．３未
満ではＳｒＯが過剰になりすぎるためＡ粉末としてはＳ
ｉ島の仮焼前添加量が多くなり、仮焼組織が微細になり
すぎる。一方、Ｓｉｎｇを添加しないＢ粉末としては、
ｎ値が５．３未満ではフェライト化反応が促進され仮焼
後の結晶粒が粗大化し、粒度のバラツキも大きくなりＡ
粉末との混合において幅広い粒度分布となり目標とする
磁気特性が得られないので好ましくない、ｎ値が５．９
を超えるとＡ粉末においては、５ｉＯ１の仮焼前添加量
が少なくなるため仮焼組織が比較的大きくなりＢ粉末と
の混合において所期の粒度分布（２山タイプ）を達成し
得ないので好ましくない、ＢＦＡ末としてはｎ（ｌが５
９を趙えるとＡ粉末と粒度分布がほとんど変わらないた
め、所期の粒度分布を構成し得ないので好ましくない、
従って本発明におけるΔ粉末およびＢ粉末としては、炭
酸ストロンチウム１モルに対してＦｅｚＯｘを５．３〜
５．９モルの組成比にし、かつＡ粉末としては５ｉ０．
をＸモル、ただしＦｅ１Ｏ＝のモル数と（１−ｘ）モル
の比が６となる組成比に限定した。Next, the reasons for the limitations of the present invention will be described individually. If the n value is less than 5.3, SrO is too excessive, so SrO is used as powder A.
The amount of i-island added before calcination increases, and the calcination structure becomes too fine. On the other hand, as powder B without adding Sing,
If the n value is less than 5.3, the ferritization reaction will be accelerated, the crystal grains will become coarse after calcination, and the variation in grain size will become large.A
When mixed with powder, the particle size distribution becomes wide and the target magnetic properties cannot be obtained, which is undesirable, and the n value is 5.9.
If it exceeds 5iO1, the amount of 5iO1 added before calcination in powder A becomes smaller, so the calcination structure becomes relatively large, making it impossible to achieve the desired particle size distribution (two-peak type) when mixed with powder B, which is preferable. No, the BFA powder is n (l is 5
9, the particle size distribution is almost the same as that of powder A, so it is not possible to form the desired particle size distribution, which is not preferable.
Therefore, the Δ powder and B powder in the present invention contain 5.3 to 5.3 to 1 mole of FezOx per mole of strontium carbonate.
The composition ratio is 5.9 mol, and the A powder is 5i0.
was limited to X moles, however, the composition ratio was such that the ratio of the number of moles of Fe1O= to (1-x) moles was 6.
仮焼温度に関しては、Ａ粉末においては１０００’Ｃ未
満ではストロンチウムフェライトの反応が十分でな（，
１２５０℃を超えると仮焼組織が比較的大きく粒度のバ
ラツキも大きくなり、５ｉＪＯ前添加効果が小さくなる
ためＡ粉末の仮焼塩度は１０００〜１２５０℃とした。Regarding the calcination temperature, the reaction of strontium ferrite is not sufficient at less than 1000'C for A powder (,
If the temperature exceeds 1250°C, the calcined structure becomes relatively large and the variation in particle size becomes large, and the effect of adding 5iJO beforehand becomes small, so the calcined salinity of powder A was set at 1000 to 1250°C.
一方Ｂ粉末において１２００”Ｃ未満では所期の粒度分
布（２山タイプ）を達成し得ないので好ましくない、
１３００℃を趙えると仮焼後の結晶粒の粗大化が起こり
、ＡおよびＢ粉末の混合により好ましい粒度分布が得ら
れない、従ってＢ粉末の仮焼塩度は１２００〜１３００
℃とした。On the other hand, if the B powder is less than 1200"C, it is not preferable because the desired particle size distribution (two-peak type) cannot be achieved.
If the temperature is heated to 1300°C, the crystal grains will become coarse after calcination, and a preferable particle size distribution cannot be obtained by mixing A and B powders. Therefore, the calcination salinity of B powder is 1200 to 1300.
℃.
次に添加物に関して述べる。Next, let's talk about additives.
従来からＳｉｎ、の添加効果としては結晶粒の粗大化を
抑制し、保磁力の高い磁石が得られることが知られてい
るが、本発明によると最終的添加量が０．４０％未満で
は保磁力が低くなり、０．７０％を趙えると残留磁束密
度が低くなり好ましくないので、０、４０〜０．７０％
とした。It has been known that the effect of adding Sin is to suppress coarsening of crystal grains and obtain a magnet with high coercive force, but according to the present invention, if the final amount added is less than 0.40%, the coercive force The magnetic force becomes low, and if it exceeds 0.70%, the residual magnetic flux density will become low, which is not preferable, so 0.40 to 0.70%.
And so.
一方ＣａＯはフェライト化反応を促進し、結晶粒の粗大
化および高密度化する作用のあることが知られているが
、本発明においては０．３５％未満では保磁力は高くな
るが残留磁束密度は低い、一方、０．４９％を趙えると
焼結性が促進され、結晶粒の粗大化が起こり保磁力が低
下するので好ましくない。On the other hand, it is known that CaO promotes the ferrite reaction and has the effect of coarsening and increasing the density of crystal grains, but in the present invention, if it is less than 0.35%, the coercive force increases, but the residual magnetic flux density On the other hand, if it exceeds 0.49%, sinterability is promoted, crystal grains become coarser, and the coercive force decreases, which is not preferable.
従ってＣａＯは０．３５〜０．４９％とした。Therefore, CaO was set at 0.35 to 0.49%.
次にＣａｂ／５ｉｆｔ比は０．５未満では保磁力は高く
なるが残Ｖｌｊｍ束密度が低くなり好ましくない。Next, if the Cab/5ift ratio is less than 0.5, the coercive force becomes high, but the residual Vljm flux density becomes low, which is not preferable.
方、１．２５を趙えると結晶粒の粗大化が起こり、保磁
力が著しく低下するので好ましくない、従ってＣａｂ／
５ｉｆｔ比は０．５〜１．２５とした。On the other hand, if the value exceeds 1.25, the crystal grains will become coarser and the coercive force will drop significantly, which is undesirable.
The 5ift ratio was set to 0.5 to 1.25.
次に上記したＢ粉末と混合するＡ粉末の混合比率は重量
比で５０％未満では保磁力（ｉＨｃ）が４０００ （Ｏ
ｅ）未満となり７５％を超えると残留磁束密度（Ｂｒ）
が４１００（Ｇ）未満となる。従ってＢ粉末と混合する
Ａ粉末の比率を重量で５０〜７５％の範囲に限定した。Next, if the mixing ratio of powder A and powder B is less than 50% by weight, the coercive force (iHc) will be 4000 (O
If it becomes less than e) and exceeds 75%, the residual magnetic flux density (Br)
becomes less than 4100 (G). Therefore, the ratio of powder A to be mixed with powder B was limited to a range of 50 to 75% by weight.
なお仮焼物の粉砕は粗粉砕、微粉砕と行われるが粗粉砕
はアトマイザ−などで１〜３ｎ程虞に粉砕し、微粉砕で
はアトライター、振動ボールミルなどでｄ＝０．７〜０
．９１程度に粉砕することが望ましい。The pulverization of the calcined product is carried out as coarse pulverization and fine pulverization. Coarse pulverization is performed by using an atomizer, etc., to about 1 to 3 nm, and fine pulverization is performed by using an attritor, vibrating ball mill, etc. to d = 0.7 to 0.
．． It is desirable to crush the powder to about 91%.
また磁場中成形は磁場が強い程良く、５ｋＯｅ以上が好
適であり、成形圧力は５００〜１５００ｋｇ、／ｃ４程
度が好適である。In addition, the stronger the magnetic field is, the better the molding in a magnetic field is, preferably 5 kOe or more, and the molding pressure is preferably about 500 to 1500 kg, /c4.
焼成温度に関しては］２４０〜＋２６０’ｃが好適であ
る。Regarding the firing temperature, 240 to +260'C is suitable.
以下、実施例によって本発明の詳細な説明する。Hereinafter, the present invention will be explained in detail with reference to Examples.
〈実施例〉
実施例１
炭酸ストロンチウム１モルに対してＰｅ２Ｏ３を５６５
モルの割合で秤量した暮木紹成の原ｔ１にＳｉＯ２を０
．０５８モルの割合で添加後、ヘノノニルミキサーで混
合した。混合粉をペレント状にして１０５０℃の温度で
仮焼した。また、Ｓｉｎｇを含まない上記基本組成比の
原事］の混合粉をペレット状にして１２２０゛Ｃの温度
で仮焼した。これら仮焼ベレットをそれぞれアトマイザ
−を用いて粗、中粉砕した（この時前者をＡ粉末、後者
をＢ粉末と呼ぶことにするン、中粉砕したＢＦＡ末中に
混合するＡ粉末を重量比で０％（Ｂ粉末のみ）、２５％
、３３％、５０％、６７％、７５％および１００％（Ａ
粉末のみ）の割合で混合し、次いでアトライターにて第
１表に示す添加物を添加し４０％スラリー状で混合、微
粉砕を施した。微粉砕後の平均（ｄ）を０．８ｎとした
後、スラリーを遠心分Ｈ機にかけ（４０％→６０％スラ
リー）７ｋＯｅの磁界中でＩｔ／ｃｄの圧力下で成形し
た。<Example> Example 1 565% of Pe2O3 per mole of strontium carbonate
0 SiO2 was added to Kuraki Shonari's original t1 weighed in molar proportions.
．． After addition, the mixture was mixed using a henononyl mixer. The mixed powder was made into a pellet and calcined at a temperature of 1050°C. Further, the mixed powder of the above basic composition ratio containing no Sing was made into pellets and calcined at a temperature of 1220°C. These calcined pellets were coarsely and medium-pulverized using an atomizer (at this time, the former will be referred to as A powder and the latter as B powder). 0% (B powder only), 25%
, 33%, 50%, 67%, 75% and 100% (A
Then, the additives shown in Table 1 were added using an attritor, mixed in the form of a 40% slurry, and pulverized. After the average (d) after pulverization was set to 0.8 n, the slurry was subjected to a centrifugal H machine (40% → 60% slurry) and molded under a pressure of It/cd in a magnetic field of 7 kOe.
成形体は自然乾燥した後、１２５２℃１１２６０’Ｃの
温度で１時間の焼成を施した。得られた焼結体の磁気特
性を第１表に示した。After the molded body was air-dried, it was fired at a temperature of 1252°C (11260'C) for 1 hour. The magnetic properties of the obtained sintered body are shown in Table 1.
第１表からＢ粉末に混合するＡ粉末の割合と磁気特性（
Ｂｒ、 １ｌｌｃ）の関係を求め第１図に示した。From Table 1, the ratio of A powder mixed with B powder and the magnetic properties (
Br, 1llc) was determined and shown in Figure 1.
Ｂ「はＡＦＩＪ末の混合比率が増すにつれて僅かに減少
し、７５％を超えると著しく減少する。一方ｔ）ｌｃは
Ａ粉末の混合比率が２５％を超えると著しく増加し、５
０％以上になると緩やかに増加する。第１図から明らか
なようにＢ粉末と混合するＡ粉末の比率を重曹比で５０
〜７５％の時Ｂ「≧４１００（Ｇ）、 １１１Ｃ≧４０
００ （Ｏｅ）を同時に満足する。B' decreases slightly as the mixing ratio of AFIJ powder increases, and decreases significantly when the mixing ratio of AFIJ powder exceeds 75%.On the other hand, t)lc increases significantly when the mixing ratio of A powder exceeds 25%, and 5
When it reaches 0% or more, it increases gradually. As is clear from Figure 1, the ratio of powder A to be mixed with powder B is 50 in terms of baking soda ratio.
When ~75% B "≧4100 (G), 111C≧40
00 (Oe).
実施例２
実施例１で用いたＡ粉末とＢ粉末を重量比でそれぞれ５
０％ずつ混合し、次いでアトライターにて第２表に示す
添加物を添加し、微粉砕後は実施例１と同様に処理して
焼成後の磁気特性を調べた。Example 2 The weight ratio of powder A and powder B used in Example 1 was 5 each.
Then, the additives shown in Table 2 were added using an attritor, and after pulverization, the mixture was treated in the same manner as in Example 1, and the magnetic properties after firing were examined.
その結果を第２表に示す。The results are shown in Table 2.
第２表から明らかなようにＢ粉末中に混合するＡ粉末の
割合が本発明の範囲においてもＣａｂ／５ｉｆｔ比が０
．５未満、或いは１．２５を超えると目標特性は得られ
ない。As is clear from Table 2, even when the proportion of A powder mixed in B powder is within the range of the present invention, the Cab/5ift ratio is 0.
．． If it is less than 5 or more than 1.25, the target characteristics cannot be obtained.
実施例３
炭酸ストロンチウム１モルに対しＦｅｒｎｓを５．２０
．５．３０．５．４０．５．５０．５．６５．５．８０
．５．９０および５９５モルの割合で秤量した基本組成
の原料に５ｉＯｚをＸモル、ただしＦｅｚｅｓのモル数
と（１−χ）モルの比が６となるようにＳｉｎ、を添加
した。即ちｎ値の小さい順に５ｉｆｔを０．１３３モル
、Ｏ，］ １１７モル０．１００モル、０．０８３モル
、０．０５８モル、０．０３３モル、０．０１７モルお
よび０．００８モル添加し、ヘンシェルミキサで混合し
た。Example 3 5.20 Ferns per mole of strontium carbonate
．． 5.30.5.40.5.50.5.65.5.80
．． X moles of 5iOz were added to raw materials having a basic composition weighed at a ratio of 5.90 and 595 moles, but Sin was added so that the ratio of the number of moles of Fezes to (1-χ) moles was 6. That is, 0.133 mol of 5ift, 0.100 mol, 0.083 mol, 0.058 mol, 0.033 mol, 0.017 mol and 0.008 mol of 5ift were added in descending order of n value, Mixed in a Henschel mixer.
これらのｒ昆合粉をペレット状にして１０５０℃の温度
で仮焼した。この時ＳｉＪを添加しない基本組成の原＃
−１混合む）をペレット状にして１２２０’Ｃの温度で
仮焼した。これらの仮焼ベレットをそれぞれアトライタ
ーを用いて粗、中粉砕した。この時５ｉＯ１添加材をＡ
粉末、５ｉＯＨを添加しない材料をＢｔｊｌ末と呼ぶこ
とにする。These r-kongo flours were made into pellets and calcined at a temperature of 1050°C. At this time, the basic composition without adding SiJ #
-1 mixture) was made into pellets and calcined at a temperature of 1220'C. These calcined pellets were respectively coarsely and medium-pulverized using an attritor. At this time, add 5iO1 additive to A
The powder and the material to which 5iOH is not added will be referred to as Btjl powder.
中粉砕した同し組成のＢ粉末中にＡ粉末を重量比でそれ
ぞれ５０％の割合で混合し、次いでアトライターで第３
表に示す添加物を添加し、＠粉砕後は実施例１と同様に
処理して焼成後の磁気特性を洲べた。その結果を第３表
に示す。Powder A was mixed in a medium-pulverized powder B with the same composition at a weight ratio of 50%, and then mixed with a third powder using an attritor.
The additives shown in the table were added, and after pulverization, the material was treated in the same manner as in Example 1 to examine the magnetic properties after firing. The results are shown in Table 3.
第３表に示したようにｎ値が５．３０未満でも、或いは
ｎ値が５．９を趙えてもＢｒ≧４１００ ・（Ｇ ）、
１）Ｉｃ≧４０００ （Ｏｅ）を同時に満足する条件は
得られない。As shown in Table 3, even if the n value is less than 5.30 or even if the n value exceeds 5.9, Br≧4100 (G),
1) A condition that simultaneously satisfies Ic≧4000 (Oe) cannot be obtained.
実施例４
炭酸ストロンチウム１モルに対してＦｅ、０１を５．７
０モルの割合で秤量した基本組成の原料にＳｉｎ。Example 4 5.7 Fe, 01 per mole of strontium carbonate
Sin to the raw materials of the basic composition weighed at a ratio of 0 moles.
４０．０５０モルの割合で添加した後、ヘンシェルミキ
サーで混合した。混合粉をペレット状にして９７０℃１
１０００°ｃ、１１５０℃、１２００℃および１２５３
℃の各々の温度で仮焼した。この時Ｓｉｎｇを含まない
上記組成比の原料の混合粉をペレット状にして１■７０
’Ｃ，１２００℃１１２５０℃，，１３００℃および１
３２０’Ｃの各々の温度で仮焼した。これら仮焼粉をア
トマイザ−を用いて粗、中粉砕した。この時Ｓ１０．を
添加した仮焼粉の粉砕品をＡ粉末と吋び、Ｓ１０！を含
まない仮焼粉の粉砕品をＢ粉末と呼ぶことにする。５ｍ
類のＡ粉末と５ｆｌ類のＢ粉末を組み合わせ、それぞれ
重量比で５０％ずつ混合し、次いでアトライターにて第
４表に示す添加物を添加し、微粉砕後は実施例１と同様
に処理して焼成後の磁気特性を洲べた。その結果を第４
表に示す、いずれも最終添加量のＳｉｎ、は０．５８８
％、ＣＢＯ／Ｓ：Ｏｅ比は０．７である−る−
第４表に示したように仮焼温度がｔｏｏｏ℃未満、或い
は１２５０℃を趙えるＡ粉末と１２００℃未満、或いは
ｌ３００℃を趙えるＢ粉末を混合した混合粉では目標特
性を得ることができないことが判る。After adding at a ratio of 40.050 mol, they were mixed in a Henschel mixer. Make the mixed powder into pellets and heat to 970℃1
1000°C, 1150°C, 1200°C and 1253
Calcining was performed at each temperature of ℃. At this time, the mixed powder of the raw materials with the above composition ratio that does not contain Sing is made into pellets and 1.70
'C, 1200℃11250℃, 1300℃ and 1
Each sample was calcined at a temperature of 320'C. These calcined powders were coarsely and medium-pulverized using an atomizer. At this time S10. The pulverized calcined powder added with S10 is referred to as A powder. The pulverized product of calcined powder that does not contain B powder will be referred to as B powder. 5m
A powder of type A and a powder of type B of 5fl were combined and mixed at a weight ratio of 50%, then the additives shown in Table 4 were added using an attritor, and after pulverization, the same treatment as in Example 1 was carried out. The magnetic properties after firing were investigated. The result is the fourth
The Sin of the final addition amount shown in the table is 0.588.
%, and the CBO/S:Oe ratio is 0.7. It can be seen that the target properties cannot be obtained with the mixed powder containing the B powder.
〈発明の効果〉
本発明によって、Ｂｒが４１００（Ｇ）以上で、かつ１
１ｃが４０００ （Ｏｅ）以上を兼ね備えた、特にカー
モーター用磁石として好適な高Ｂｒ、高１１１ｃのスト
ロンチウムフェライト磁石を容品に得ることができ、省
エネルギー等の点でその及ぼす効果は大きい。<Effects of the Invention> According to the present invention, Br is 4100 (G) or more and 1
A high Br, high 111c strontium ferrite magnet, which has 1c of 4000 (Oe) or more and is particularly suitable as a magnet for a car motor, can be obtained in a package, and has great effects in terms of energy saving and the like.
第１図は仮焼条件の異なる仮焼粉の混合比率と焼成後の
磁気特性（Ｂｒ、 １Ｈｃ）の関係を示した図であるFigure 1 shows the relationship between the mixing ratio of calcined powder under different calcining conditions and the magnetic properties (Br, 1Hc) after firing.
Claims (1)
た後、該仮焼物を粉砕し、しかる後磁場中成形して得ら
れる成形体を焼成してストロンチウムフェライト磁石を
製造する方法において、炭酸ストロンチウム１モルに対
しＦｅ＿２Ｏ＿３を５．３〜５．９モルおよびＳｉＯ＿
２をｘモル、ただし、Ｆｅ＿２Ｏ＿３のモル数と（１−
ｘ）モルの比が６となる組成比で混合し、１０００〜１
２５０℃の温度で仮焼した後、該仮焼物を粉砕して得る
微粉末（以下Ａ粉末と呼ぶ）と、ＳｉＯ＿２を含まない
上記組成比の原料を１２００〜１３００℃の温度で仮焼
した後、該仮焼物を粉砕して得る微粉末（以下Ｂ粉末と
呼ぶ）をＢ粉末に対するＡ粉末の混合比率（重量比）が
５０〜７５％の範囲で混合し、次いで該混合粉に更に重
量比で最終的にＳｉＯ＿２が０．４０〜０．７０％、Ｃ
ａＯが０．３５〜０．４９％かつＣａＯ／ＳｉＯ＿２比
が０．５〜１．２５となるように添加した後、磁場中成
形し、しかる後焼成することを特徴とする残留磁束密度
および保磁力の高いストロンチウムフェライト磁石の製
造方法。In the method of manufacturing a strontium ferrite magnet by mixing iron oxide and strontium carbonate, granulating and calcining the mixture, pulverizing the calcined product, and then firing the molded product obtained by molding in a magnetic field, the strontium carbonate 5.3 to 5.9 mol of Fe_2O_3 and SiO_
2 to x moles, where the number of moles of Fe_2O_3 and (1-
x) Mix at a composition ratio where the molar ratio is 6, 1000 to 1
After calcining at a temperature of 250°C, a fine powder obtained by crushing the calcined product (hereinafter referred to as A powder) and a raw material having the above composition ratio that does not contain SiO_2 are calcined at a temperature of 1200 to 1300°C. , a fine powder obtained by pulverizing the calcined product (hereinafter referred to as B powder) is mixed at a mixing ratio (weight ratio) of A powder to B powder in the range of 50 to 75%, and then the mixed powder is further mixed with a weight ratio of A powder to B powder. Finally, SiO_2 is 0.40-0.70%, C
After adding so that aO is 0.35 to 0.49% and CaO/SiO_2 ratio is 0.5 to 1.25, it is molded in a magnetic field and then fired. A method for manufacturing strontium ferrite magnets with high magnetic force.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2145344A JPH0438807A (en) | 1990-06-05 | 1990-06-05 | Manufacture of strontium-ferrite magnet high in residual magnetic flux density and coercive force |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2145344A JPH0438807A (en) | 1990-06-05 | 1990-06-05 | Manufacture of strontium-ferrite magnet high in residual magnetic flux density and coercive force |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0438807A true JPH0438807A (en) | 1992-02-10 |
Family
ID=15383014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2145344A Pending JPH0438807A (en) | 1990-06-05 | 1990-06-05 | Manufacture of strontium-ferrite magnet high in residual magnetic flux density and coercive force |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0438807A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07249510A (en) * | 1994-03-09 | 1995-09-26 | Tdk Corp | Oxide permanent magnet and its manufacture |
| KR20020016254A (en) * | 2000-08-25 | 2002-03-04 | 신현준 | A method for manufacturing ferrite permant magnet |
-
1990
- 1990-06-05 JP JP2145344A patent/JPH0438807A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07249510A (en) * | 1994-03-09 | 1995-09-26 | Tdk Corp | Oxide permanent magnet and its manufacture |
| KR20020016254A (en) * | 2000-08-25 | 2002-03-04 | 신현준 | A method for manufacturing ferrite permant magnet |
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