JPH0735293B2 - Method for manufacturing beta-alumina sintered body - Google Patents
Method for manufacturing beta-alumina sintered bodyInfo
- Publication number
- JPH0735293B2 JPH0735293B2 JP1312860A JP31286089A JPH0735293B2 JP H0735293 B2 JPH0735293 B2 JP H0735293B2 JP 1312860 A JP1312860 A JP 1312860A JP 31286089 A JP31286089 A JP 31286089A JP H0735293 B2 JPH0735293 B2 JP H0735293B2
- Authority
- JP
- Japan
- Prior art keywords
- beta
- alumina
- sintered body
- calcination
- 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
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 title claims description 52
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 238000000034 method Methods 0.000 title claims description 12
- 239000000843 powder Substances 0.000 claims description 29
- 238000001354 calcination Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 18
- 238000004513 sizing Methods 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 9
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000010304 firing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000007547 defect Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000002159 abnormal effect Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 description 1
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- RPMPQTVHEJVLCR-UHFFFAOYSA-N pentaaluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3] RPMPQTVHEJVLCR-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/39—Accumulators not provided for in groups H01M10/05-H01M10/34 working at high temperature
- H01M10/3909—Sodium-sulfur cells
- H01M10/3918—Sodium-sulfur cells characterised by the electrolyte
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Secondary Cells (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明はベータアルミナ焼結体の製造方法に係り、更に
詳しくは、仮焼前の原料調合・粉砕、乾燥粉末及び／ま
たは仮焼後の粉末の粒度を解砕整粒して均一化すること
によって、ベータアルミナ焼結体の特性を安定化させ、
且つ作業効率を向上化させたベータアルミナ焼結体の製
造方法に関する。Description: TECHNICAL FIELD The present invention relates to a method for producing a beta-alumina sintered body, and more specifically, to prepare and pulverize raw materials before calcination, dry powder and / or after calcination. By crushing and sizing the particle size of the powder to make it uniform, the characteristics of the beta-alumina sintered body are stabilized,
The present invention also relates to a method for producing a beta-alumina sintered body with improved work efficiency.
［従来の技術］ ベータアルミナは、Naイオンのイオン伝導率が極めて高
いため、ナトリウム−硫黄電池の隔膜など、固体電解質
としての用途が注目されている。[Prior Art] Beta-alumina has a very high ionic conductivity of Na ions, and therefore, its application as a solid electrolyte such as a diaphragm of a sodium-sulfur battery is drawing attention.
ベータアルミナ焼結体の製造は、従来は、例えば、第３
図に示すような工程で行なわれており、アルミナ、ナト
リウム塩等の主原料およびリチウム、マグネシウム、ジ
ルコニウム等の添加物を出発原料とし、湿式混合・粉
砕、乾燥後、仮焼し、得られたベータアルミナ仮焼粉末
を粉砕処理して、その後スラリー調整し、造粒、成形、
焼成することにより得ていた。The production of a beta-alumina sintered body has hitherto been carried out by, for example, the third method.
The process is as shown in the figure, and the main raw materials such as alumina and sodium salts and the additives such as lithium, magnesium and zirconium are used as starting raw materials, wet-mixed and pulverized, dried, and then calcined to obtain. The beta-alumina calcined powder is pulverized, then slurry is adjusted, granulated, molded,
It was obtained by firing.
［発明が解決しようとする課題］ しかしながら、上記した従来の方法によれば、混合物の
凝集状態が不均一なため仮焼後に著しい集塊を形成する
と共に、粒径、組成等の仮焼状態が不均一であり、異常
粒の成長等により焼結体の欠陥の原因となっていた。ま
た、ベータアルミナ仮焼粉末を粉砕処理する際に、集塊
の性状の差によって被粉砕物に差が生じていた。[Problems to be Solved by the Invention] However, according to the above-mentioned conventional method, since the aggregated state of the mixture is non-uniform, remarkable agglomerates are formed after calcination, and the calcination state such as particle size and composition is It was non-uniform and caused defects in the sintered body due to abnormal grain growth and the like. In addition, when the beta-alumina calcined powder was pulverized, a difference occurred in the pulverized objects due to the difference in the properties of the agglomerates.
このため、粉砕後、粗大気孔などの焼結体の欠陥の原因
となる凝集体が残留し、これを取り除くため長時間の粉
砕を行なう必要があり作業時間も長くなる等の作業性に
も問題があった。For this reason, after pulverization, aggregates that cause defects in the sintered body such as coarse air holes remain, and it is necessary to perform pulverization for a long time to remove this, which causes a problem in workability such as a long working time. was there.
［課題を解決するための手段］ そこで、本発明者等は上記従来のベータアルミナ焼結体
の製造方法における問題を解決し、ベータアルミナ焼結
体の特性の安定化と向上を図ることのできる製造方法を
開発するため、種々検討を重ねた結果、本発明を完成し
た。[Means for Solving the Problems] Therefore, the present inventors can solve the problems in the conventional method for producing a beta-alumina sintered body, and stabilize and improve the characteristics of the beta-alumina sintered body. As a result of various studies to develop a manufacturing method, the present invention has been completed.
即ち、本発明によれば、ベータアルミナ原料粉末を調合
・粉砕、乾燥、仮焼し、得られたベータアルミナ仮焼粉
末を粉砕した後、スラリー調整、造粒、成形、焼成する
ベータアルミナ焼結体の製造方法において、原料粉末を
調合・粉砕、乾燥した後、仮焼する前または仮焼後に、
解砕し、1000μｍ以下の粒子に整粒することを特徴とす
るベータアルミナ焼結体の製造方法が提供される。That is, according to the present invention, beta-alumina sintering in which the beta-alumina raw material powder is prepared, pulverized, dried, and calcined, and the obtained beta-alumina calcined powder is pulverized, followed by slurry adjustment, granulation, molding and firing. In the method for producing a body, after mixing, pulverizing and drying the raw material powder, before or after calcination,
Provided is a method for producing a beta-alumina sintered body, which comprises crushing and sizing into particles of 1000 μm or less.
また、ベータアルミナ原料粉末を調合・粉砕、乾燥、仮
焼し、得られたベータアルミナ仮焼粉末を粉砕した後、
スラリー調整、造粒、成形、焼成するベータアルミナ焼
結体の製造方法において、原料粉末を調合・粉砕、乾燥
した後、仮焼する前および仮焼後にそれぞれ解砕し、50
00μｍ以下の粒子に整粒することを特徴とするベータア
ルミナ焼結体の製造方法が提供される。In addition, after mixing and pulverizing the beta-alumina raw material powder, drying and calcination, and pulverizing the obtained beta-alumina calcination powder,
In the method for producing a beta-alumina sintered body in which slurry adjustment, granulation, molding and firing are performed, raw material powders are mixed and pulverized, dried, and then crushed before and after calcination, respectively, and 50
Provided is a method for producing a beta-alumina sintered body, which comprises sizing particles to a size of 00 μm or less.
［作用］ 本発明においては、ベータアルミナ焼結体を製造するに
当り、ベータアルミナ用の出発原料の湿式混合・粉砕、
乾燥後、仮焼する際に、予めその乾燥物を解砕して、10
00μｍ以下の整粒工程を組入れて構成する。また、仮焼
したベータアルミナ仮焼粉末を粉砕・スラリー調整・造
粒処理する前に、予め解砕し、1000μｍ以下の整粒操作
工程を前記仮焼前の乾燥・解砕・整粒工程を行なうこと
なく組入れて構成する。[Operation] In the present invention, when the beta-alumina sintered body is manufactured, the starting raw material for the beta-alumina is wet-mixed and ground,
After calcination after drying, crush the dried product in advance and
It is configured by incorporating a sizing process of 00 μm or less. In addition, the calcined beta-alumina calcined powder is crushed in advance before being crushed, adjusted in slurry and granulated, and the sieving operation step of 1000 μm or less is performed by the drying, crushing and sizing step before the calcination. Configure by incorporating without doing.
また、仮焼前及び後の双方で解砕整粒する工程を実施し
てもよく、この場合は整粒粒度を5000μｍ以下で行なえ
ばよい。A step of crushing and sizing may be carried out both before and after the calcination, and in this case, the sizing particle size may be 5000 μm or less.
このように、ベータアルミナ用の原料調合・乾燥粉末ま
たは、およびベータアルミナ仮焼粉末の解砕整粒操作を
行なうことにより、仮焼後の集塊の生成を抑制すること
ができるので、仮焼後の粉砕操作が容易になると共に、
仮焼物の組成が均質化するため、異常粒成長等による焼
結体の欠陥が少なくなる。更に、仮焼粉末の粒度が均一
化し、粉砕時間の短縮化を図りうるとともに、粗大気孔
等の焼結体の欠陥を少なくすることができる。In this way, by performing the crushing and sizing operation of the raw material preparation / dry powder for beta-alumina or the calcined powder of beta-alumina, it is possible to suppress the formation of agglomerates after calcination. Later crushing operation becomes easy,
Since the composition of the calcined product is homogenized, defects in the sintered body due to abnormal grain growth are reduced. Furthermore, the particle size of the calcined powder can be made uniform, the crushing time can be shortened, and defects in the sintered body such as coarse air holes can be reduced.
本発明において、ベータアルミナとはβ−アルミナ（Na
2O・11Al2O3）、β″−アルミナ（Na2O・5Al2O3）、β
−アルミナ、β´−アルミナを含むものである。In the present invention, beta-alumina means β-alumina (Na
2 O · 11Al 2 O 3 ), β ″ -alumina (Na 2 O / 5Al 2 O 3 ), β
-Alumina and β'-alumina are included.
［実施例］ 以下、本発明を実施例に基きさらに詳細に説明するが、
本発明はこれら実施例に限られるものではない。[Examples] Hereinafter, the present invention will be described in more detail with reference to Examples.
The present invention is not limited to these examples.
［ベータアルミナ焼結体の製造］ 第１図は、本発明のベータアルミナ焼結体の製造方法の
工程図である。[Manufacture of Beta-Alumina Sintered Body] FIG. 1 is a process diagram of a method for manufacturing a beta-alumina sintered body of the present invention.
ベータアルミナの主原料として、Al2O3，Na2O，添加物
としてMgO,Li2O，ZrO2等の所定量を計量し、これをボー
ル・ミル中で湿式混合で、１時間、混合・粉砕する。次
に上記のスラリーをステンレスパットに入れ、熱風乾燥
機により110℃で16時間乾燥した。次にこの乾燥物をロ
ールクラッシャーで解砕し、振動ふるい機によって粒度
1000〜5000μｍまたは1000μｍ以下に整粒した。Al 2 O 3 , Na 2 O as the main raw material of beta-alumina, and MgO, Li 2 O, ZrO 2 etc. as prescribed additives were weighed in a predetermined amount and mixed in a ball mill by wet mixing for 1 hour. ·Smash. Next, the above slurry was put into a stainless steel pad and dried at 110 ° C. for 16 hours by a hot air dryer. Next, this dried product was crushed with a roll crusher and the particle size was measured with a vibration sieving machine.
The particle size was adjusted to 1000 to 5000 μm or 1000 μm or less.
次に、上記整粒した粒子をアルミナ磁器ルツボに入れ、
電気炉により1250℃で６時間、加熱して仮焼を行なっ
た。仮焼物はＸ線回析法による結晶組成分析により結晶
相の定量を行ない、α−Al2O3残留率を次式により算出
した。Next, put the sized particles in an alumina porcelain crucible,
Calcination was performed by heating in an electric furnace at 1250 ° C. for 6 hours. The calcined product was subjected to X-ray diffraction analysis for crystal composition analysis to quantify the crystal phase, and the α-Al 2 O 3 residual rate was calculated by the following formula.
但し、Ｉβはβ−Al2O3（100）のピーク強度、Ｉβ″は
β″−Al2O3（103）のピーク強度、Ｉαはα−Al2O3（1
01）のピーク強度を表わす。 However, Iβ is the peak intensity of β-Al 2 O 3 (100), Iβ ″ is the peak intensity of β ″ -Al 2 O 3 (103), and Iα is the α-Al 2 O 3 (1
It represents the peak intensity of 01).
次で、仮焼物を必要に応じ、ロールクラッシャーで解砕
し、振動ふるい機によって粒度1000〜5000μｍまたは10
00μｍ以下に整粒し、マイクロトラック粒度測定装置に
よって粒子径の分布測定を行なった。次いで、ボール・
ミルで30時間湿式粉砕したものにポリビニルアルコール
水溶液を加えてスラリーを調製した。Next, if necessary, the calcined product is crushed with a roll crusher and the particle size is 1000 to 5000 μm or 10 with a vibrating screener.
The particle size was adjusted to 00 μm or less, and the particle size distribution was measured with a Microtrac particle size analyzer. Then the ball
A polyvinyl alcohol aqueous solution was added to a wet-milled product for 30 hours to prepare a slurry.
次に、このスラリーをスプレードライヤーによって造粒
・乾燥して顆粒を調製し、該顆粒を静水圧プレス機を使
用して、成形圧力2.0ton/cm2で加圧し、30×60×60mmの
形状の成形体を作製した。次で、この成形体を白金ルツ
ボに入れ、電気焼成炉により1620℃で30分間焼成し焼結
体を得た。この焼結体について下記の各試験を行なっ
た。Next, this slurry is granulated and dried by a spray dryer to prepare granules, and the granules are pressed at a molding pressure of 2.0 ton / cm 2 using a hydrostatic press to give a shape of 30 × 60 × 60 mm. A molded body of was produced. Next, this molded body was put into a platinum crucible and sintered in an electric firing furnace at 1620 ° C. for 30 minutes to obtain a sintered body. The following tests were conducted on this sintered body.
・曲げ強度測定： JIS Z−R1601に準拠した４点曲げ強度測定し、後記比較
例３のβ−アルミナ焼結体強度を100として相対比で表
わした。Bending strength measurement: Four-point bending strength was measured according to JIS Z-R1601, and the relative strength was expressed with the strength of β-alumina sintered body of Comparative Example 3 described below as 100.
・欠陥径測定： 第２図に示すように焼結体Ａの斜線部分を切断して試験
片を得て、その切断面を鏡面研磨し、研磨した部分１を
光学顕微鏡で微構造組織の観察をし、気孔クラック等の
最大径を測定した。Defect diameter measurement: As shown in FIG. 2, the oblique line portion of the sintered body A was cut to obtain a test piece, the cut surface was mirror-polished, and the polished portion 1 was observed with an optical microscope for a microstructure structure. Then, the maximum diameter of pore cracks and the like was measured.
・最大結晶粒径測定： 第２図の鏡面研磨部１を更に熱濃リン酸でエッチング
し、その部分を光学顕微鏡で観察して結晶粒子径を測定
し、その中の最大のものを最大結晶粒径とした。・ Measurement of maximum crystal grain size: The mirror-polished part 1 in FIG. 2 was further etched with hot concentrated phosphoric acid, and the part was observed with an optical microscope to measure the crystal grain size. The particle size was used.
上記の方法によって、ベータアルミナ焼結体を作製し、
上記測定方法によって各測定を行なった。下記の実施例
１〜16および比較例１〜７の測定結果を表−１及び表−
２に示した。By the above method, a beta alumina sintered body is produced,
Each measurement was performed by the above measuring method. The measurement results of the following Examples 1 to 16 and Comparative Examples 1 to 7 are shown in Table-1 and Table-
Shown in 2.
（実施例１〜６） 前記ベータアルミナ焼結体の製造において、ベータアル
ミナ用原料の仮焼前でのみ、解砕し、粒度を1000μｍ以
下に整粒して焼結体を得た。そのときの製造条件等と焼
結体特性の測定結果を表−１に示した。(Examples 1 to 6) In the production of the beta-alumina sintered body, the raw material for beta-alumina was crushed only and the particle size was adjusted to 1000 µm or less to obtain a sintered body. Table 1 shows the manufacturing conditions and the measurement results of the characteristics of the sintered body at that time.
（比較例１〜３） 前記ベータアルミナ焼結体の製造において、ベータアル
ミナ用原料の仮焼前で、解砕、粒度の整粒をしないで従
来法と同様にして焼結体を得た。実施例１と同様に、そ
の結果等を表−１に示した。(Comparative Examples 1 to 3) In the production of the beta-alumina sintered body, before the calcination of the beta-alumina raw material, a sintered body was obtained in the same manner as in the conventional method without crushing and grain size regulation. The results and the like are shown in Table 1 in the same manner as in Example 1.
（比較例4,5） 実施例１と同様にして、ベータアルミナ用原料の仮焼前
で、解砕して粒度の整粒をした。但し、整粒を1000〜50
00μｍの範囲で行なった。その結果を表−１に示した。(Comparative Examples 4 and 5) In the same manner as in Example 1, the raw material for beta-alumina was crushed and the particle size was adjusted before calcination. However, sizing should be 1000 to 50
It was performed in the range of 00 μm. The results are shown in Table-1.
（実施例７〜８） 前記ベータアルミナ焼結体の製造において、仮焼前の解
砕、整粒は行なわず、ベータアルミナの仮焼粉末を解砕
し、粒度1000μｍ以下に整粒して、焼結体を得た。その
結果を表−１に示した。(Examples 7 to 8) In the production of the beta-alumina sintered body, the calcination powder before calcination was not crushed, but the calcinated powder of beta-alumina was crushed and the particle size was controlled to 1000 μm or less, A sintered body was obtained. The results are shown in Table-1.
（比較例６） 実施例７において、ベータアルミナの仮焼粉末を、解砕
し、粒度1000〜5000μｍで整粒して焼結体を得た。その
結果を表−１に示した。(Comparative Example 6) In Example 7, the calcined powder of beta-alumina was crushed and sized to a particle size of 1000 to 5000 µm to obtain a sintered body. The results are shown in Table-1.
（実施例９〜16） 前記ベータアルミナ焼結体の製造において、仮焼前およ
び仮焼後の双方で共に解砕し、粒度を5000μｍ以下に整
粒しして、焼結体を得た。その結果を表−２に示した。 (Examples 9 to 16) In the production of the beta-alumina sintered body, both before and after calcination were crushed and the particle size was adjusted to 5000 µm or less to obtain a sintered body. The results are shown in Table-2.
（比較例７） 仮焼前および仮焼後に、共に解砕し、粒度を5000μｍ以
上に整粒した以外は実施例９と同様にして焼結体を得
た。その結果を表−２に示した。(Comparative Example 7) A sintered body was obtained in the same manner as in Example 9 except that the powder was crushed both before and after calcination and the particle size was adjusted to 5000 µm or more. The results are shown in Table-2.
なお、表中の判定の欄の◎は最適を、○は適を、△は適
用可能を、×は不敵を表わしている。In the table, ⊚ indicates the optimum, ∘ indicates appropriate, Δ indicates applicable, and x indicates invincible.
上記の結果より、仮焼前または仮焼後のいずれか一方
で、解砕し、粒度1000μｍ以下に整粒したものでは、判
定欄から分かるように、良い結果が得られた。特に、仮
焼前および仮焼後の双方共に解砕整粒したものでは、粒
度が1000μｍ以下のものは勿論、ベータアルミナ原料粉
末の仮焼前後のいずれかまたは双方での整粒粒度が1000
〜5000μｍの範囲であれば、例えば、実施例９〜10に見
られるように良い結果が得られることが分る。 From the above results, good results were obtained, as can be seen from the judgment column, in the case of crushing and sizing to a particle size of 1000 μm or less either before or after calcination. In particular, in the case of crushed and sized particles both before and after calcination, the particle size is 1000 μm or less, and the sized particle size before and after calcination of the beta-alumina raw material powder is 1000 or less.
It can be seen that in the range of up to 5000 μm, good results can be obtained, for example, as seen in Examples 9 to 10.
［発明の効果］ 以上説明したように、本発明のベータアルミナ粉末の製
造方法によれば、仮焼後の集塊の生成を抑制することが
できるので、仮焼後の粉砕操作が容易になるとともに、
仮焼物の組成が均質化するため、異常粒成長等の焼結体
の欠陥が少なくなる。更に、仮焼粉末の粒度が均一化
し、粉砕時間の短縮化を図りうると共に粗大気孔等の焼
結体の欠陥を少なくすることができる。[Effects of the Invention] As described above, according to the method for producing beta-alumina powder of the present invention, it is possible to suppress the formation of agglomerates after calcination, so that the pulverization operation after calcination becomes easy. With
Since the composition of the calcined product is homogenized, defects in the sintered body such as abnormal grain growth are reduced. Furthermore, the particle size of the calcined powder can be made uniform, the crushing time can be shortened, and defects in the sintered body such as coarse air holes can be reduced.
第１図は本発明のベータアルミナ粉末および焼結体の製
造方法の一実施例の工程図、第２図は焼成体試験片の斜
視図、第３図は従来のベータアルミナ粉末および焼結体
の製造方法の工程図である。 １……鏡面研磨部、Ａ……焼結体FIG. 1 is a process diagram of an embodiment of a method for producing beta-alumina powder and a sintered body of the present invention, FIG. 2 is a perspective view of a test piece for a fired body, and FIG. 3 is a conventional beta-alumina powder and a sintered body. FIG. 6 is a process drawing of the manufacturing method of FIG. 1 ... Mirror polished part, A ... Sintered body
Claims (2)
燥、仮焼し、得られたベータアルミナ仮焼粉末を粉砕し
た後、スラリー調整、造粒、成形、焼成するベータアル
ミナ焼結体の製造方法において、原料粉末を調合・粉
砕、乾燥した後、仮焼する前または仮焼後に、解砕し、
1000μｍ以下の粒子に整粒することを特徴とするベータ
アルミナ焼結体の製造方法。1. Production of a beta-alumina sintered body in which beta-alumina raw material powder is prepared, pulverized, dried and calcined, and the resulting beta-alumina calcined powder is pulverized, followed by slurry adjustment, granulation, molding and firing. In the method, after mixing, pulverizing and drying the raw material powder, before calcination or after calcination, crush,
A method for producing a beta-alumina sintered body, which comprises sizing particles to a size of 1000 μm or less.
燥、仮焼し、得られたベータアルミナ仮焼粉末を粉砕し
た後、スラリー調整、造粒、成形、焼成するベータアル
ミナ焼結体の製造方法において、原料粉末を調合・粉
砕、乾燥した後、仮焼する前および仮焼後にそれぞれ解
砕し、5000μｍ以下の粒子に整粒することを特徴とする
ベータアルミナ焼結体の製造方法。2. Production of a beta-alumina sintered body in which a beta-alumina raw material powder is prepared, pulverized, dried and calcined, and the resulting beta-alumina calcined powder is pulverized, followed by slurry adjustment, granulation, molding and firing. A method for producing a beta-alumina sintered body, characterized in that, in the method, raw material powders are prepared, pulverized, dried, and then crushed before calcination and after calcination, respectively, and sized to particles of 5000 μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1312860A JPH0735293B2 (en) | 1989-12-01 | 1989-12-01 | Method for manufacturing beta-alumina sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1312860A JPH0735293B2 (en) | 1989-12-01 | 1989-12-01 | Method for manufacturing beta-alumina sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03174352A JPH03174352A (en) | 1991-07-29 |
| JPH0735293B2 true JPH0735293B2 (en) | 1995-04-19 |
Family
ID=18034311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1312860A Expired - Lifetime JPH0735293B2 (en) | 1989-12-01 | 1989-12-01 | Method for manufacturing beta-alumina sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0735293B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102529089B1 (en) | 2022-06-24 | 2023-05-08 | (주)코미코 | Materials For Plasma Spray Comprising Y-O-F Composition, Manufacturing Method Thereof, And Plasma Spay Coating Using The Same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1387608A (en) * | 1971-10-29 | 1975-03-19 | Gen Electric | Making high purity sodium aluminate and use thereof in making sintered beta-alumina bodies |
| JPS60251172A (en) * | 1984-05-24 | 1985-12-11 | 日本特殊陶業株式会社 | Beta-alumina ceramic |
-
1989
- 1989-12-01 JP JP1312860A patent/JPH0735293B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102529089B1 (en) | 2022-06-24 | 2023-05-08 | (주)코미코 | Materials For Plasma Spray Comprising Y-O-F Composition, Manufacturing Method Thereof, And Plasma Spay Coating Using The Same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03174352A (en) | 1991-07-29 |
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