JP3540515B2 - Method for producing β ″ -alumina - Google Patents

Method for producing β ″ -alumina Download PDF

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Publication number
JP3540515B2
JP3540515B2 JP21452596A JP21452596A JP3540515B2 JP 3540515 B2 JP3540515 B2 JP 3540515B2 JP 21452596 A JP21452596 A JP 21452596A JP 21452596 A JP21452596 A JP 21452596A JP 3540515 B2 JP3540515 B2 JP 3540515B2
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JP
Japan
Prior art keywords
alumina
powder
producing
stoichiometric ratio
present
Prior art date
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Expired - Fee Related
Application number
JP21452596A
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Japanese (ja)
Other versions
JPH1059714A (en
Inventor
和洋 長谷崎
政智 鎌田
光 本村
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.)
Mitsubishi Heavy Industries Ltd
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Mitsubishi Heavy Industries Ltd
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Publication date
Application filed by Mitsubishi Heavy Industries Ltd filed Critical Mitsubishi Heavy Industries Ltd
Priority to JP21452596A priority Critical patent/JP3540515B2/en
Publication of JPH1059714A publication Critical patent/JPH1059714A/en
Application granted granted Critical
Publication of JP3540515B2 publication Critical patent/JP3540515B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Compositions Of Oxide Ceramics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Secondary Cells (AREA)

Description

【0001】
【発明の属する技術分野】
本発明はAMTEC(アルカリ金属熱電変換)材料、Na−S又はNa−Cl二次電池材料として使用されるβ″−アルミナの製造方法に関する。
【0002】
【従来の技術】
従来のβ″−アルミナの製造方法を図2によって説明する。
β″−アルミナはNa2 CO3 及びAl2 3 を出発原料11にする。Na2 Oが蒸発するのを考慮に入れて所定の化学量論比でエタノール中で20時間混合12させる。混合12後、さらに800〜1000℃で大気中1時間加熱し有機物質を蒸発させ予備焼成13する。その後乳鉢で荒粉砕、成形14し、最後に1600℃で加熱15することにより、所定の化学量論比のβ″−アルミナを得ている。
【0003】
【発明が解決しようとする課題】
従来の方法では、高温で合成するためにNaなどが蒸発し化学量論比からずれて所定の性能を発揮できない問題点があった。本発明はこのような問題点を解消しうるβ″−アルミナの製造方法を提供しようとするものである。
【0004】
【課題を解決するための手段】
本発明は合金製造にしばしば採用されるメカニカルアロイング法を採用することによって、従来法の問題点を解消したものであって、Na2 O粉体とAl2 3 粉体を化学量論比になるように配合し、該配合物を不活性雰囲気下で硬質ボールによりNa2 O粉体とAl2 3 粉体との反応が始まるまで十分粉砕し反応させ、得られた粉砕物を大気雰囲気下、500〜800℃で所定時間加熱することを特徴とするβ″−アルミナの製造方法である。
【0005】
(作用)
メカニカルアロイングは粉体成分を機械的に混合、粉砕して粉体成分を反応させる方法であるため、炭酸化合物などを必要とせず、β″−アルミナの構成成分を化学量論比に混合することで反応化できる。そのため、低温加熱で結晶化できるのでNaなどが蒸発し化学量論比からずれることがない。
【0006】
【実施例】
本発明の一実施例を図1によって説明する。Na2 OとAl2 3 酸化物粉体をそれぞれ化学量論比で1:5.33になるように秤量01する。この秤量したものをステンレスポットに入れ、粉砕用のジルコニアボールを原料の重量の50倍入れ、蓋をして窒素雰囲気に置換して100時間粉砕02させる。得られた粉を800℃で3時間大気中で加熱結晶化03し、β″−アルミナを得る。
【0007】
図3に、上記方法で得られた材料のx線回折図を示す。この図から得られた物質がβ″−アルミナであることが判明した。
【0008】
【発明の効果】
本発明方法により、化学量論比から外れることなくβ″−アルミナが得られ、その工業的効果は顕著なものがある。
【図面の簡単な説明】
【図1】本発明の実施態様の工程図。
【図2】従来のβ″−アルミナの製造方法の一態様の工程図。
【図3】本発明の実施例で得られたβ″−アルミナのx線回折図。
[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing β ″ -alumina used as an AMTEC (alkali metal thermoelectric conversion) material, Na—S or Na—Cl secondary battery material.
[0002]
[Prior art]
A conventional method for producing β ″ -alumina will be described with reference to FIG.
β ″ -alumina is Na 2 CO 3 and Al 2 O 3 as starting materials 11. Mixing 12 in ethanol at a predetermined stoichiometric ratio in ethanol for 20 hours taking into account the evaporation of Na 2 O. After 12, the organic material is further heated in the air at 800 to 1000 ° C. for 1 hour to evaporate the organic substance and preliminarily baked 13. Thereafter, it is roughly pulverized in a mortar, molded 14, and finally heated at 1600 ° C. 15 to obtain a predetermined stoichiometric amount. A stoichiometric β ″ -alumina is obtained.
[0003]
[Problems to be solved by the invention]
In the conventional method, there is a problem in that Na or the like evaporates due to synthesis at a high temperature, deviates from the stoichiometric ratio, and a predetermined performance cannot be exhibited. An object of the present invention is to provide a method for producing β ″ -alumina which can solve such problems.
[0004]
[Means for Solving the Problems]
The present invention has solved the problems of the conventional method by adopting a mechanical alloying method often employed in alloy production, wherein Na 2 O powder and Al 2 O 3 powder are stoichiometrically mixed. And pulverize the mixture sufficiently in an inert atmosphere with a hard ball until the reaction between the Na 2 O powder and the Al 2 O 3 powder starts to react. A process for producing β ″ -alumina, comprising heating at 500 to 800 ° C. for a predetermined time in an atmosphere.
[0005]
(Action)
Mechanical alloying is a method in which powder components are mechanically mixed and pulverized to react the powder components. Therefore, a carbonic acid compound is not required, and the components of β ″ -alumina are mixed in a stoichiometric ratio. Therefore, it can be crystallized by heating at a low temperature, so that Na or the like does not evaporate and does not deviate from the stoichiometric ratio.
[0006]
【Example】
One embodiment of the present invention will be described with reference to FIG. Na 2 O and Al 2 O 3 oxide powder are each weighed 01 so as to have a stoichiometric ratio of 1: 5.33. The weighed material is placed in a stainless steel pot, and zirconia balls for grinding are placed 50 times the weight of the raw material. The lid is replaced with a nitrogen atmosphere, and crushed 02 for 100 hours. The obtained powder is crystallized by heating at 800 ° C. for 3 hours in the air to obtain β ″ -alumina.
[0007]
FIG. 3 shows an x-ray diffraction diagram of the material obtained by the above method. From this figure, it was found that the substance obtained was β ″ -alumina.
[0008]
【The invention's effect】
According to the method of the present invention, β ″ -alumina can be obtained without deviating from the stoichiometric ratio, and its industrial effect is remarkable.
[Brief description of the drawings]
FIG. 1 is a process diagram of an embodiment of the present invention.
FIG. 2 is a process chart of one embodiment of a conventional method for producing β ″ -alumina.
FIG. 3 is an x-ray diffraction diagram of β ″ -alumina obtained in an example of the present invention.

Claims (1)

Na2 O粉体とAl2 3 粉体を化学量論比になるように配合し、該配合物を不活性雰囲気下で硬質ボールによりNa2 O粉体とAl2 3 粉体との反応が始まるまで十分粉砕し反応させ、得られた粉砕物を大気雰囲気下、500〜800℃で所定時間加熱することを特徴とするβ″−アルミナの製造方法。Na 2 O powder and Al 2 O 3 powder are blended so as to have a stoichiometric ratio, and the blend is mixed with Na 2 O powder and Al 2 O 3 powder by a hard ball under an inert atmosphere. A process for producing β ″ -alumina, which comprises sufficiently pulverizing and reacting until the reaction starts, and heating the obtained pulverized material at 500 to 800 ° C. for a predetermined time in an air atmosphere.
JP21452596A 1996-08-14 1996-08-14 Method for producing β ″ -alumina Expired - Fee Related JP3540515B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP21452596A JP3540515B2 (en) 1996-08-14 1996-08-14 Method for producing β ″ -alumina

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP21452596A JP3540515B2 (en) 1996-08-14 1996-08-14 Method for producing β ″ -alumina

Publications (2)

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JPH1059714A JPH1059714A (en) 1998-03-03
JP3540515B2 true JP3540515B2 (en) 2004-07-07

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101213481B1 (en) 2010-12-06 2012-12-20 삼성에스디아이 주식회사 Beta alumina solid electrolyte and manufacturing method thereof

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