JPH09268075A - Ceramic material and production of the same - Google Patents

Ceramic material and production of the same

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Publication number
JPH09268075A
JPH09268075A JP8079973A JP7997396A JPH09268075A JP H09268075 A JPH09268075 A JP H09268075A JP 8079973 A JP8079973 A JP 8079973A JP 7997396 A JP7997396 A JP 7997396A JP H09268075 A JPH09268075 A JP H09268075A
Authority
JP
Japan
Prior art keywords
ceramic
nitrate
metal compound
metal compounds
ceramics
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.)
Withdrawn
Application number
JP8079973A
Other languages
Japanese (ja)
Inventor
Yoichi Oya
洋一 大矢
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sony Corp
Original Assignee
Sony Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sony Corp filed Critical Sony Corp
Priority to JP8079973A priority Critical patent/JPH09268075A/en
Publication of JPH09268075A publication Critical patent/JPH09268075A/en
Withdrawn legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To obtain a ceramic material consisting of particles having fine particle sizes by constituting with a baked material obtained by mixing metal compounds with a specific compound and baking, and sufficiently performing a reaction by a baking of one time. SOLUTION: This ceramic material is constituted by a baked material obtained by mixing metal compounds e.g. as a metal oxide and/or a carbonic acid salt (e.g.; Y2 O3 , BaCO3 and CuO) with a nitric acid salt, preferably ammonium nitrate, and burning. As a result, a mean particle size of the ceramic (e.g.; 1-2-3YBCO ceramic material) particles constituting the baked material is 0.1-0.9μ. The nitric acid salt is preferably used in larger number of mols than that of the metal compounds. That is, since the metal compounds are converted into nitric acid salts having high reactivities and then baked, reactions among the metal compounds during the baking are accelerated.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は電子材料、磁性材料
等として多用されているセラミックス及びその製造方法
に関する。詳しくは、セラミックスを構成する金属を含
有する金属化合物と硝酸塩を混合させた後に焼成するこ
とにより、1回の焼成で十分に反応が起こるようにし、
微細な粒径のセラミックス粒子よりなる焼成体として製
造されるセラミックス及びその製造方法に係わるもので
ある。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to ceramics frequently used as electronic materials, magnetic materials, etc., and a method for manufacturing the same. Specifically, by mixing a metal compound containing a metal constituting a ceramic and a nitrate, and then baking the mixture, a reaction can be sufficiently performed by one-time baking,
The present invention relates to a ceramic produced as a fired body made of fine ceramic particles and a method for producing the same.

【0002】[0002]

【従来の技術】セラミックスは、電子部品に使用される
セラミック基板として、その他の電子材料として、さら
には磁性材料等としても多用されており、中でも酸化物
セラミックスは一般的な材料として多用されている。
2. Description of the Related Art Ceramics are widely used as a ceramic substrate used for electronic parts, other electronic materials, and also as a magnetic material. Among them, oxide ceramics are commonly used as a general material. .

【0003】このような酸化物セラミックスは、通常以
下のような工程を経て製造される。すなわち、図3に示
されるように、セラミックスを構成する金属を含有する
金属化合物である金属酸化物或いは炭酸塩の秤量101
を行い、これらの混合102を行い、これを成形103
した後、焼成104を行う。この工程中、焼成104工
程において酸化物間の反応が起こっている。しかしなが
ら、これらの反応性が鈍いことから反応速度は非常に遅
く、未反応物質が混在して得るべきセラミックスが得ら
れない可能性が高い。そこで、実際にセラミックスを製
造する場合には、焼成104の後、粉砕105を行い、
再度混合102,成形103,焼成104を行い、これ
を2〜3回繰り返すようにしている。
Such oxide ceramics are usually manufactured through the following steps. That is, as shown in FIG. 3, the amount 101 of metal oxide or carbonate which is a metal compound containing a metal constituting ceramics is weighed.
Then, these are mixed 102, and this is molded 103
After that, firing 104 is performed. During this process, a reaction between oxides occurs in the baking 104 process. However, since their reactivity is low, the reaction rate is very slow, and there is a high possibility that a ceramic to be obtained with unreacted substances mixed cannot be obtained. Therefore, when actually manufacturing ceramics, after firing 104, crushing 105 is performed,
Mixing 102, molding 103, and firing 104 are performed again, and this is repeated 2-3 times.

【0004】[0004]

【発明が解決しようとする課題】しかしながら、このよ
うに何度も焼成を繰り返すと、粒子成長が進行し、微細
な粒径の粒子よりなるセラミックスを得ることが困難と
なり、特性の良好なセラミックスを得ることが難しい。
なお、粉砕工程は非常に煩雑な作業であり、生産性を損
なう要因になっている。
However, if firing is repeated many times in this way, particle growth proceeds, making it difficult to obtain ceramics composed of particles having a fine particle diameter, and ceramics having good characteristics are obtained. Hard to get.
The crushing process is a very complicated work, which is a factor that impairs productivity.

【0005】また、このような酸化物セラミックス、特
に複雑な分子構造を有する高温酸化物超電導材料等にお
いては、微量の添加物によりその特性が大きく左右され
ることから、添加物の均一な分散が望まれている。しか
しながら、上述のような製造方法においては、酸化物の
反応性が非常に鈍いことから、酸化物の金属部分を微量
の添加物に置換し、添加物を均一に分散させることは非
常に難しい。
Further, in such oxide ceramics, especially high temperature oxide superconducting materials having a complicated molecular structure, the characteristics are greatly influenced by a small amount of the additive, so that the additive is uniformly dispersed. Is desired. However, in the above-described manufacturing method, since the reactivity of the oxide is extremely low, it is very difficult to replace the metal portion of the oxide with a trace amount of the additive and disperse the additive uniformly.

【0006】そこで本発明は、従来の実情に鑑みて提案
されたものであり、焼成工程を何度も繰り返すことなく
反応が十分に行われ、微量の添加物が均一に分散され、
微細な粒径のセラミックス粒子よりなり、良好な特性を
有するセラミックス及びその製造方法を提供することを
目的とする。
Therefore, the present invention has been proposed in view of the conventional circumstances, and the reaction is sufficiently performed without repeating the firing step many times, and a trace amount of the additive is uniformly dispersed,
It is an object of the present invention to provide a ceramic having fine characteristics and comprising ceramic particles having a fine particle diameter, and a method for producing the same.

【0007】[0007]

【課題を解決するための手段】上述の課題を解決するた
めに本発明のセラミックスは、金属酸化物或いは炭酸塩
といった金属化合物と硝酸塩を混合させた後に焼成して
得られた焼成体よりなり、当該焼成体を構成するセラミ
ックス粒子の平均粒径が0.1μm〜0.9μmである
ことを特徴とするものである。
In order to solve the above problems, the ceramics of the present invention comprises a fired body obtained by mixing a metal compound such as a metal oxide or a carbonate with a nitrate and then firing the mixture. The average particle diameter of the ceramic particles constituting the fired body is 0.1 μm to 0.9 μm.

【0008】また、本発明のセラミックスの製造方法
は、金属酸化物或いは炭酸塩といった金属化合物と硝酸
塩を混合させて、金属化合物を硝酸塩に置換した後、こ
れらを焼成することを特徴とするものである。
The method for producing ceramics of the present invention is characterized by mixing a metal compound such as a metal oxide or a carbonate with a nitrate, substituting the metal compound with a nitrate, and then firing these. is there.

【0009】なお、このようにしてセラミックスを製造
する場合には、硝酸塩として硝酸アンモニウムを使用す
ることが好ましい。硝酸塩としては、他のものも使用可
能であり、硝酸も使用可能である。
When producing ceramics in this way, it is preferable to use ammonium nitrate as the nitrate. Other nitrates can be used, and nitric acid can also be used.

【0010】また、上記のようにしてセラミックスを製
造する場合には、金属化合物とこの金属化合物のモル数
以上のモル数の硝酸塩を混合することが好ましい。硝酸
塩の量が金属化合物のモル数よりも少ないと、硝酸塩と
金属化合物間の反応が十分でなく、未置換の金属化合物
が残存し、混合,焼成時の金属化合物間の反応速度を速
める効果が薄れる。
Further, in the case of producing ceramics as described above, it is preferable to mix a metal compound and a nitrate in a mole number equal to or greater than the mole number of the metal compound. When the amount of nitrate is less than the number of moles of the metal compound, the reaction between the nitrate and the metal compound is not sufficient and the unsubstituted metal compound remains, which has the effect of accelerating the reaction rate between the metal compounds during mixing and firing. Fades.

【0011】本発明のセラミックスの製造方法において
は、金属化合物と硝酸塩を混合させた後、これらを焼成
するため、金属化合物は反応性の高い硝酸塩に置換され
た後に焼成されることとなり、焼成時の金属化合物間の
反応が促進され、1回の焼成で反応が十分に行われる。
また、金属化合物と硝酸塩の混合時に、微量の添加物を
添加すれば、金属化合物の金属部分がイオンの状態とな
りやすくなっていることから、この金属部分は添加物に
よりたやすく置換され、添加物が均一に分散される。
In the method for producing ceramics of the present invention, since the metal compound and the nitrate are mixed and then fired, the metal compound is replaced with the highly reactive nitrate, and then fired. The reaction between the above metal compounds is promoted, and the reaction is sufficiently performed by firing once.
Also, when a trace amount of an additive is added during mixing of the metal compound and the nitrate, the metal portion of the metal compound is likely to be in an ionic state, so this metal portion is easily replaced by the additive, Are evenly dispersed.

【0012】そして、このような製造方法により製造さ
れる本発明のセラミックスにおいては、セラミックス粒
子の平均粒径が0.1μm〜0.9μmと微細なものと
なり、良好な特性を有するものとなる。
In the ceramic of the present invention manufactured by such a manufacturing method, the average particle diameter of the ceramic particles is as fine as 0.1 μm to 0.9 μm, and good characteristics are obtained.

【0013】[0013]

【実施例】以下、本発明を適用した具体的な実施例につ
いて実験結果に基づいて説明する。ここでは、本発明を
適用したセラミックスの製造方法により1−2−3YB
COセラミックスを製造し、このセラミックスの特性を
調査した。なお、比較のために、従来のセラミックスの
製造方法により1−2−3YBCOセラミックスを製造
し、このセラミックスの特性を調査した。
DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, specific embodiments to which the present invention is applied will be described based on experimental results. Here, 1-2-3YB is produced by the method for producing ceramics according to the present invention.
A CO ceramic was manufactured and the characteristics of this ceramic were investigated. For comparison, a 1-2-3YBCO ceramic was manufactured by a conventional ceramic manufacturing method, and the characteristics of this ceramic were investigated.

【0014】先ず、本発明を適用したセラミックスの製
造方法によりセラミックスを製造した。すなわち、初め
に図1に示すように秤量1を行った。具体的には金属化
合物としてY23 を112.91g、BaCO3 を3
94.62g、CuOを238.65g秤量し、これら
酸化物及び炭酸塩と6モル以上に相当する重量の硝酸ア
ンモニウムを秤量した。
First, ceramics were manufactured by the method for manufacturing ceramics according to the present invention. That is, first, weighing 1 was performed as shown in FIG. Specifically, 112.91 g of Y 2 O 3 and 3 of BaCO 3 were used as metal compounds.
94.62 g of CuO and 238.65 g of CuO were weighed, and these oxides and carbonates and ammonium nitrate in a weight corresponding to 6 mol or more were weighed.

【0015】次に図1中に示すように混合2を行った。
すなわち、上記各酸化物及び炭酸塩と硝酸アンモニウム
を乳鉢内にて5〜10分程度混合した。この際、上記各
酸化物及び炭酸塩の酸素は遊離し、酸化物及び炭酸塩は
硝酸塩に置換されることとなる。この際、水も生成され
るため、混合物はペースト状となる。また、硝酸アンモ
ニウムが十分に添加されていることから、酸化物及び炭
酸塩の全体が硝酸塩に置換されることとなる。
Mixing 2 was then carried out as shown in FIG.
That is, the above oxides and carbonates and ammonium nitrate were mixed in a mortar for about 5 to 10 minutes. At this time, oxygen of each of the oxides and carbonates is released, and the oxides and carbonates are replaced with nitrates. At this time, since water is also generated, the mixture becomes a paste. Further, since ammonium nitrate is sufficiently added, the entire oxides and carbonates are replaced with nitrates.

【0016】なお、このとき、微量の添加物を添加すれ
ば、酸化物及び炭酸塩の金属部分がイオンの状態になり
易くなっていることから、この金属部分は添加物により
たやすく置換され、添加物を均一に分散することが可能
である。
At this time, if a trace amount of an additive is added, the metal portion of the oxide and carbonate is likely to be in an ionic state, so that the metal portion is easily replaced by the additive, It is possible to disperse the additives uniformly.

【0017】さらに、図1中に示すように加熱3を行っ
た。具体的には、上記混合物を温度150〜200℃程
度のホットプレート上で加熱し、余分な硝酸アンモニウ
ムを除去した。
Further, heating 3 was performed as shown in FIG. Specifically, the above mixture was heated on a hot plate at a temperature of about 150 to 200 ° C. to remove excess ammonium nitrate.

【0018】続いて、図1中に示すように、成形4を行
った。具体的には凝集粒子をほぐした後、油圧プレス等
により100〜200kg/mm2 程度の圧力をかけ、
所望の形状に成形した。
Subsequently, as shown in FIG. 1, molding 4 was performed. Specifically, after loosening the aggregated particles, a pressure of about 100 to 200 kg / mm 2 is applied by a hydraulic press or the like,
It was molded into the desired shape.

【0019】そして最後に、図1中に示すように焼成5
を行った。すなわち、空気中において焼成温度を900
〜1000℃とし、3時間の焼成を行って、セラミック
スを得た。
Finally, as shown in FIG. 1, firing 5
Was done. That is, the firing temperature in air is 900
The temperature was set to ˜1000 ° C., and firing was performed for 3 hours to obtain ceramics.

【0020】そして、このセラミックスの特性としてセ
ラミックス粒子の粒径を金属顕微鏡により調査したとこ
ろ、0.1〜0.3μmの粒径を有していた。また、こ
のセラミックスに対してX線回折を行ってみたところ、
Ba2 CuO3 等の未反応物も検出されず、結晶構造も
斜方晶系をなしていた。なお、このX線回折のチャート
を図2に示す。図2中ピークの上或いは横の文字は反射
の指数である。
When the particle diameter of the ceramic particles was examined by a metallographic microscope as a characteristic of this ceramic, it had a particle diameter of 0.1 to 0.3 μm. Also, when I tried X-ray diffraction on this ceramic,
Unreacted materials such as Ba 2 CuO 3 were not detected, and the crystal structure was orthorhombic. The X-ray diffraction chart is shown in FIG. The letters above or beside the peak in FIG. 2 are the indices of reflection.

【0021】また、比較のために各酸化物及び炭酸塩を
上記のように秤量した後、これら酸化物及び炭酸塩のみ
を上記のようにして混合し、これらを上記のようにして
成形、焼成してセラミックスを製造した。ただし、ここ
では、1回の焼成時間を20時間とし、焼成後、粉砕し
て再度混合、成形、粉砕を行うようにし、これを3回繰
り返してセラミックスを製造した。
For comparison, the respective oxides and carbonates were weighed as described above, then only these oxides and carbonates were mixed as described above, and these were molded and fired as described above. To produce ceramics. However, here, one firing time was set to 20 hours, and after firing, pulverization was performed to perform mixing, molding, and pulverization again, and this was repeated three times to produce ceramics.

【0022】そして、このセラミックスの特性としてセ
ラミックス粒子の粒径を金属顕微鏡により調査したとこ
ろ、1〜3μmの粒径を有していた。また、このセラミ
ックスに対してX線回折を行ってみたところ、Ba2
uO3 等の未反応物が検出された。
When the particle size of the ceramic particles was examined with a metallographic microscope as a characteristic of this ceramic, it had a particle size of 1 to 3 μm. Moreover, when X-ray diffraction was performed on this ceramic, it was found that Ba 2 C
Unreacted substances such as uO 3 were detected.

【0023】この結果から、本発明のセラミックスの製
造方法のように、金属化合物と硝酸塩を混合させた後、
これらを焼成するようにすれば、金属化合物は反応性の
高い硝酸塩に置換された後に焼成されることとなり、焼
成時の金属化合物間の反応が促進され、1回の焼成で反
応が十分に行われることが確認された。
From these results, after mixing the metal compound and the nitrate as in the method for producing a ceramic of the present invention,
If these are fired, the metal compound is fired after being replaced with a highly reactive nitrate, and the reaction between the metal compounds at the time of firing is promoted, and the reaction can be performed sufficiently by one firing. It was confirmed that

【0024】そして、このような製造方法により製造さ
れる本発明のセラミックスにおいては、セラミックス粒
子の平均粒径が0.1μm〜0.9μmの範囲内の微細
なものとなり、良好な特性を有するものとなることが確
認された。
In the ceramic of the present invention manufactured by such a manufacturing method, the average particle diameter of the ceramic particles is fine within the range of 0.1 μm to 0.9 μm, and has good characteristics. It was confirmed that

【0025】なお、本発明のセラミックスの製造方法に
おいては、焼成を繰り返す必要がないことから、煩雑な
粉砕工程を行う必要もなく、生産性が向上する。しか
も、金属化合物と硝酸塩を混合する工程は通常の製造工
程に組み込むことが可能であり、余計な製造工程を増や
すことがなく、生産性を損なうこともない。
In the method for producing ceramics of the present invention, since it is not necessary to repeat firing, it is not necessary to perform a complicated pulverizing step and productivity is improved. In addition, the step of mixing the metal compound and the nitrate can be incorporated into a normal manufacturing process, which does not increase the number of unnecessary manufacturing processes and does not impair the productivity.

【0026】[0026]

【発明の効果】以上の説明からも明らかなように、本発
明のセラミックスの製造方法においては、金属化合物と
硝酸塩を混合させた後、これらを焼成するため、金属化
合物は反応性の高い硝酸塩に置換された後に焼成される
こととなり、焼成時の金属化合物間の反応が促進され、
1回の焼成で反応が十分に行われ、生産性が向上する。
As is apparent from the above description, in the method for producing ceramics of the present invention, the metal compound and the nitrate are mixed and then baked, so that the metal compound is converted into a highly reactive nitrate. It will be fired after being substituted, the reaction between the metal compounds during firing is promoted,
The reaction is sufficiently carried out by one firing, and the productivity is improved.

【0027】なお、本発明のセラミックスの製造方法に
おいては、焼成を繰り返す必要がないことから、煩雑な
粉砕工程を行う必要もなく、生産性が向上する。しか
も、金属化合物と硝酸塩を混合する工程は通常の製造工
程に組み込むことが可能であり、余計な製造工程を増や
すことがなく、生産性を損なうこともない。
In the ceramics manufacturing method of the present invention, since it is not necessary to repeat firing, it is not necessary to perform a complicated crushing step, and the productivity is improved. In addition, the step of mixing the metal compound and the nitrate can be incorporated into a normal manufacturing process, which does not increase the number of unnecessary manufacturing processes and does not impair the productivity.

【0028】また、本発明のセラミックスの製造方法に
おいて、金属化合物と硝酸塩の混合時に、微量の添加物
を添加すれば、金属化合物の金属部分がイオンの状態と
なりやすくなっていることから、この金属部分は添加物
によりたやすく置換され、添加物が均一に分散され、製
造されるセラミックスの特性の調整が容易に行われる。
Further, in the method for producing a ceramic of the present invention, if a small amount of an additive is added when the metal compound and the nitrate are mixed, the metal portion of the metal compound is likely to be in an ionic state. The portion is easily replaced by the additive, the additive is uniformly dispersed, and the characteristics of the ceramics produced are easily adjusted.

【0029】そして、このような製造方法により製造さ
れる本発明のセラミックスにおいては、セラミックス粒
子の平均粒径が0.1μm〜0.9μmと微細なものと
なり、良好な特性を有するものとなる。
In the ceramic of the present invention manufactured by such a manufacturing method, the average particle diameter of the ceramic particles is as fine as 0.1 μm to 0.9 μm, and good characteristics are obtained.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明を適用したセラミックスの製造方法の工
程を示すチャートである。
FIG. 1 is a chart showing steps of a method for producing ceramics to which the present invention is applied.

【図2】本発明を適用したセラミックスのX線回折の結
果を示すチャートである。
FIG. 2 is a chart showing the results of X-ray diffraction of ceramics to which the present invention is applied.

【図3】従来のセラミックスの製造方法の工程を示すチ
ャートである。
FIG. 3 is a chart showing the steps of a conventional ceramic manufacturing method.

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 金属化合物と硝酸塩を混合させた後に焼
成して得られた焼成体よりなり、当該焼成体を構成する
セラミックス粒子の平均粒径が0.1μm〜0.9μm
であることを特徴とするセラミックス。
1. A fired body obtained by mixing a metal compound and a nitrate and firing the mixture. The average particle size of ceramic particles constituting the fired body is 0.1 μm to 0.9 μm.
Ceramics characterized by being
【請求項2】 金属化合物と硝酸塩を混合させた後、こ
れらを焼成することを特徴とするセラミックスの製造方
法。
2. A method for producing ceramics, which comprises mixing a metal compound and a nitrate and then firing these.
【請求項3】 硝酸塩が硝酸アンモニウムであることを
特徴とする請求項2記載のセラミックスの製造方法。
3. The method for producing ceramics according to claim 2, wherein the nitrate is ammonium nitrate.
【請求項4】 金属化合物とこの金属化合物のモル数以
上のモル数の硝酸塩を混合することを特徴とする請求項
2記載のセラミックスの製造方法。
4. The method for producing ceramics according to claim 2, wherein the metal compound is mixed with a nitrate in a mole number equal to or more than the mole number of the metal compound.
JP8079973A 1996-04-02 1996-04-02 Ceramic material and production of the same Withdrawn JPH09268075A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8079973A JPH09268075A (en) 1996-04-02 1996-04-02 Ceramic material and production of the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP8079973A JPH09268075A (en) 1996-04-02 1996-04-02 Ceramic material and production of the same

Publications (1)

Publication Number Publication Date
JPH09268075A true JPH09268075A (en) 1997-10-14

Family

ID=13705277

Family Applications (1)

Application Number Title Priority Date Filing Date
JP8079973A Withdrawn JPH09268075A (en) 1996-04-02 1996-04-02 Ceramic material and production of the same

Country Status (1)

Country Link
JP (1) JPH09268075A (en)

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