JPH0624150B2 - β-alumina tube firing method - Google Patents
β-alumina tube firing methodInfo
- Publication number
- JPH0624150B2 JPH0624150B2 JP2213254A JP21325490A JPH0624150B2 JP H0624150 B2 JPH0624150 B2 JP H0624150B2 JP 2213254 A JP2213254 A JP 2213254A JP 21325490 A JP21325490 A JP 21325490A JP H0624150 B2 JPH0624150 B2 JP H0624150B2
- Authority
- JP
- Japan
- Prior art keywords
- alumina tube
- firing
- alumina
- tube
- metal foil
- 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 48
- 238000010304 firing Methods 0.000 title claims description 35
- 238000000034 method Methods 0.000 title claims description 9
- 230000001681 protective effect Effects 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 239000011888 foil Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- 239000000395 magnesium oxide Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007784 solid electrolyte Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- Compositions Of Oxide Ceramics (AREA)
- Secondary Cells (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は焼成時における歩留り率を大幅に改善すること
ができるβ−アルミナ管の焼成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 β-alumina tube firing method capable of significantly improving the yield rate during firing.
（従来の技術） 一端が閉じられ、他端が開口した有底筒状体のβ−アル
ミナ管は、ナトリウム−硫黄電池の固体電解質管や熱電
変換装置のナトリウムイオン伝導用固体電解質管、SOＸ
センサー用固体電解質管等に広く用いられており、その
焼成方法として自重による変形を極力防止できるようβ
−アルミナ管素地をその底部が上になるよう焼台治具上
に前記開口をもって倒立させて焼成用保護管内で焼成す
る方法が提案されている。(Prior Art) A β-alumina tube having a bottomed tubular body with one end closed and the other end opened includes a solid electrolyte tube for a sodium-sulfur battery, a solid electrolyte tube for sodium ion conduction in a thermoelectric conversion device, and SO X.
It is widely used for solid electrolyte tubes for sensors, etc., and as a firing method, it is possible to prevent deformation due to its own weight as much as possible
A method has been proposed in which the alumina tube base material is inverted on the baking table jig with the opening so that the bottom of the alumina tube material is upside, and then baked in the baking protection tube.
ところが、従来の方法においては焼成用保護管の直角度
不良や、β−アルミナ管を載置する焼台治具の寸法精度
不良等によって更にはβ−アルミナ管の焼成収縮が大き
い事もあって焼成時にβ−アルミナ管と焼成用保護管内
表面とが接触する場合があり、これが原因で保護管内部
のマグネシア成分等がβ−アルミナ管表面上で反応して
生成物を生じβ−アルミナ結晶の異常成長が起こり、そ
の結果マグネシア成分付着部分でのβ−アルミナの機械
的強度が低下し、かつイオン導電特性にも異常をきたす
という問題があり、また外観不良を発生させるという問
題もあった。更には、β−アルミナ管の焼成収縮の際に
焼成用保護管と接触しβ−アルミナ管表面に傷がつくと
いう問題点が発生しており、また、上記のような寸法精
度不良等がない場合であってもハンドリング中における
衝撃や、焼成中のガス熱流に伴う保護管の揺れ等によっ
てβ−アルミナ管と保護管とが接触する場合があり、同
様の問題点が発生していた。However, in the conventional method, the firing shrinkage of the β-alumina tube may be further large due to a defect in the squareness of the firing protection tube, a poor dimensional accuracy of the firing table jig on which the β-alumina tube is placed, and the like. When firing, the β-alumina tube may come into contact with the inner surface of the protective tube for firing, which causes magnesia components inside the protective tube to react on the surface of the β-alumina tube to produce a product of β-alumina crystals. Abnormal growth occurs, and as a result, the mechanical strength of β-alumina in the magnesia component-attached portion is lowered, and the ionic conductivity characteristics are also abnormal, and there is a problem in that the appearance is poor. Further, there is a problem that the surface of the β-alumina tube is scratched by coming into contact with the protective tube for firing during the shrinkage of the β-alumina tube, and there is no dimensional accuracy defect as described above. Even in such cases, the β-alumina tube and the protective tube may come into contact with each other due to impact during handling, shaking of the protective tube due to gas heat flow during firing, and the like, and similar problems occur.
（発明が解決しようとする課題） 本発明は上記のような従来の問題点を解決して、焼成用
保護管のマグネシア成分等がβ−アルミナ管表面上で反
応して生成物を生じること及びβ−アルミナ管表面にお
けるスリ傷の発生を確実に防止し、機械的強度の低下、
イオン導電特性の異常、外観不良等を発生させることな
く極めて高い歩留りを達成することができるβ−アルミ
ナ管の焼成方法を提供することを目的として完成された
ものである。(Problems to be Solved by the Invention) The present invention solves the conventional problems as described above, in which a magnesia component or the like of a protective tube for firing reacts on the β-alumina tube surface to produce a product, and Surely prevent the occurrence of scratches on the surface of β-alumina tube and reduce the mechanical strength,
The present invention has been completed for the purpose of providing a method for firing β-alumina tubes that can achieve an extremely high yield without causing abnormalities in ionic conductivity characteristics, appearance defects, and the like.
（課題を解決するための手段） 上記の課題を解決するためになされた本発明に係るβ−
アルミナ管の焼成方法は、一端が底部により閉じられ、
他端が開口とされた有底筒状のβ−アルミナ管素地の底
部側を該β−アルミナ管素地の軸方向ストレート部長さ
の少なくとも４％以上の長さに亘り白金族元素からなる
金属箔により覆って焼台治具上に前記開口をもって倒立
させるとともに該焼台治具上に焼成用保護管を前記β−
アルミナ管素地との間に所要の空隙をあけて施蓋して倒
立するβ−アルミナ管素地と焼成用保護管との直接接触
を防止しつつ焼成することを特徴とするものである。(Means for Solving the Problems) β-according to the present invention made to solve the above problems
The firing method for alumina tubes is that one end is closed by the bottom,
A metal foil made of a platinum group element extending from the bottom side of a bottomed tubular β-alumina tube base material having an opening at the other end to a length of at least 4% or more of the axial straight portion length of the β-alumina tube base material. And invert it on the baking table jig with the opening, and at the same time, the baking protection tube is placed on the baking table jig with the β-
The firing is performed while preventing a direct contact between the β-alumina tube base body and the protective tube for firing which are upside down by providing a required gap with the alumina tube base body.
以下、本発明を図面を参考にしながら詳細に説明する
と、β−アルミナ管素地(1)は一端が閉じられて底部(2)
が形成されているとともに、他端が開口(3)に形成され
た有底筒状のものであり、該β−アルミナ管素地(1)は
前記開口(3)を焼台治具(4)に嵌合させて倒立させて底部
(2)が上になった状態としてあり、また、この焼台治具
(4)には前記β−アルミナ管素地(1)との間に所要の空隙
を残して焼成用保護管(5)が施蓋され、該β−アルミナ
管素地(1)が焼成用保護管(5)で覆われた状態で例えばガ
ス窯中において約1620℃程度で焼成される。この際該β
−アルミナ管素地は16〜22％焼成収縮する。焼成用保護
管(5)は例えばマグネシアとα−アルミナの混合物等か
らなるスピネル質セラミック質で、β−アルミナ管素地
(1)と焼成用保護管(5)との空隙は２〜８mm程度としてお
く。焼成の際にβ−アルミナ管素地(1)よりNa2O蒸気が
揮発するため該空隙を８mmより大きくするとNa2Oの揮発
量が増大し、β−アルミナ管素地(1)が大幅な組成変化
をきたすため８mm以下とすることが好ましい。また２mm
より少ないと窯詰作業が困難となり、また金属箔(6)と
焼成用保護管(5)とが接触し易くなり、２mm以上にする
ことが好ましい。また、倒立するβ−アルミナ管素地
(1)のうち底部(2)により閉じられている上側の所要長さ
の部分は白金族元素からなる金属箔(6)で覆ってあり、
焼台治具(4)上で倒立するβ−アルミナ管素地(1)が焼成
用保護管(5)と直接接触することなく焼成が行なわれよ
う構成されている。金属箔(6)としては白金、ロジウ
ム、パラジウム等の白金族元素金属の単体またはそれら
の合金が用いられ、０．１mm以下の厚みのキャップ状
（図示参照）あるいは筒状のものが使用される。０．１
mmより厚い場合には金属箔(6)の自重が焼成の際のβ−
アルミナ管素地(1)の収縮に悪影響を及ぼし、また偏荷
重の際には変形したβ−アルミナを発生し易く、寸法精
度の高いβ−アルミナ管を高歩留で得られなくなる。な
お、金属箔(6)の重量はβ−アルミナ管素地(1)の単位荷
重断面積当たり15ｇ／cm2以下とすることが好ましい。
また金属箔(6)を必要以上に厚くすることは当然金属箔
(6)のコストが高くなり経済的でないから、金属箔(6)は
0.01〜０．１mmの厚みとするのが実用的である。また、
この金属箔(6)はβ−アルミナ管素地(1)が焼成用保護管
(5)と接触する可能性の最も高い部所、即ち、底部(2)の
近傍の所要長さに亘る部分に装着されるものであるが、
その長さはβ−アルミナ管素地(1)の軸方向ストレート
部長さの少なくとも４％以上の長さに亘って覆うものと
する。その理由は４％より少ない場合には焼成中に金属
箔(6)が接触抵抗によりズレ上ってβ−アルミナ管(1)が
焼成用保護管(5)に直接接触するおそれがあるからであ
る。Hereinafter, the present invention will be described in detail with reference to the drawings.The β-alumina tube body (1) has one end closed and a bottom part (2).
Is formed, and the other end is in the shape of a cylinder with a bottom formed in the opening (3), the β-alumina tube substrate (1) is the baking jig (4) the opening (3) To the bottom
(2) is in the upside state
A protective tube for firing (5) is capped on (4) leaving a required gap between the β-alumina tube substrate (1) and the β-alumina tube substrate (1). In the state covered with (5), for example, it is fired at about 1620 ° C. in a gas kiln. At this time, the β
-Alumina tube substrate shrinks by 16-22%. The protective tube (5) for firing is, for example, a spinel ceramic material composed of a mixture of magnesia and α-alumina, and a β-alumina tube base material.
The gap between (1) and the protective tube for firing (5) is about 2 to 8 mm. Since Na 2 O vapor volatilizes from the β-alumina tube matrix (1) during firing, increasing the gap to more than 8 mm increases the amount of Na 2 O volatilized, and the β-alumina tube matrix (1) has a large composition. In order to cause a change, the thickness is preferably 8 mm or less. 2mm again
If the amount is smaller, the kiln packing operation becomes difficult, and the metal foil (6) and the protective tube for firing (5) easily come into contact with each other. Also, the inverted β-alumina tube substrate
The portion of the required length on the upper side that is closed by the bottom portion (2) of (1) is covered with a metal foil (6) made of a platinum group element,
The β-alumina tube base material (1) which is inverted on the baking table jig (4) is configured to be baked without directly contacting the baking protection tube (5). As the metal foil (6), a simple substance of a platinum group element metal such as platinum, rhodium, palladium or an alloy thereof is used, and a cap-shaped (see the figure) or cylindrical shape having a thickness of 0.1 mm or less is used. . 0.1
When the thickness is larger than mm, the weight of the metal foil (6) is β-
This adversely affects the contraction of the alumina tube base material (1), and deformed β-alumina is likely to be generated at the time of an unbalanced load, so that a β-alumina tube having high dimensional accuracy cannot be obtained with a high yield. The weight of the metal foil (6) is preferably 15 g / cm 2 or less per unit load cross-sectional area of the β-alumina tube substrate (1).
Also, it is natural to make the metal foil (6) thicker than necessary.
Since the cost of (6) is high and it is not economical, the metal foil (6)
It is practical that the thickness is 0.01 to 0.1 mm. Also,
This metal foil (6) is a β-alumina tube substrate (1) protective tube for firing.
(5) is most likely to come into contact with the part, that is, the part that is attached to the part over the required length in the vicinity of the bottom part (2),
Its length shall cover at least 4% or more of the length of the axial straight portion of the β-alumina tube body (1). The reason is that if it is less than 4%, the metal foil (6) may shift due to contact resistance during firing and the β-alumina tube (1) may come into direct contact with the firing protection tube (5). is there.
このように、本発明においては焼台治具(4)上で倒立さ
せたβ−アルミナ管素地(1)のうち焼成時において上側
となる底部(2)側の該β−アルミナ管素地(1)の軸方向ス
トレート部長さの少なくとも４％以上の長さに亘る部分
に装着した金属箔(6)によって該β−アルミナ管素地(1)
が焼成用保護管(5)の内面に直接接触することを確実に
防止しつつ焼成するようにしたので、たとえ倒立させた
β−アルミナ管素地(1)が傾斜したとしても、従来のよ
うに焼成されたβ−アルミナ管表面にマグネシア成分等
の反応生成物が生じることがなく外観不良を発生させる
ことがない。Thus, in the present invention, of the β-alumina tube substrate (1) inverted on the baking table jig (4), the β-alumina tube substrate (1) on the bottom (2) side which is the upper side during firing (1) ) The β-alumina tube base material (1) is provided with a metal foil (6) attached to a portion extending over at least 4% of the length of the axial straight portion.
Since the firing is performed while surely preventing direct contact with the inner surface of the firing protection tube (5), even if the inverted β-alumina tube substrate (1) is inclined, it is as in the conventional case. No reaction product such as magnesia component is generated on the surface of the baked β-alumina tube, and no defective appearance occurs.
（実施例） 内径30mm、長さ240 mm、厚さ１．６mmのナトリウム−硫
黄電池に用いる有底筒状のβ−アルミナ管となるβ−ア
ルミナ管素地の底部に厚さ0.03mm、ストレート部長さ30
mmのキャップ状の白金箔を被せて500 本の焼成を従来と
同じ焼成条件で行なったところ、外観不良となるものは
１本も発生しなかった。これに対して、白金箔を用いず
に焼成した場合は約80％（500 本中400 本）のものが表
面上に接触による痕跡がある外観不良となっており、本
発明の優れた効果が確認できた。(Example) An inner diameter of 30 mm, a length of 240 mm, and a thickness of 1.6 mm. A bottomed cylindrical β-alumina tube used for a sodium-sulfur battery. 30
When 500 pieces of cap-shaped platinum foil were covered and 500 pieces were baked under the same baking conditions as in the conventional case, none of them had a poor appearance. On the other hand, when fired without using platinum foil, about 80% (400 out of 500) had a poor appearance due to contact marks on the surface, and the excellent effect of the present invention It could be confirmed.
（発明の効果） 以上の説明からも明らかなように、本発明においては、
β−アルミナ管の表面に焼成用保護管との接触による反
応生成物の発生による痕跡のない優れた外観を有する製
品を高い歩留り率で得ることができるもので、ガス窯焼
成時におけるガス燃焼の熱流に伴う焼成用保護管の揺れ
が若干あっても或いは焼成用保護管や焼台治具に寸法誤
差があっても充分対処できるうえに使用する白金族元素
からなる金属箔は繰り返し何度も使用できるのでコスト
上も有利な利点もある。(Effects of the Invention) As is apparent from the above description, in the present invention,
A product with an excellent appearance without traces due to the generation of reaction products on the surface of the β-alumina tube due to contact with the protective tube for firing can be obtained at a high yield rate. Even if there is some shaking of the firing protection tube due to the heat flow or there is a dimensional error in the firing protection tube or the baking table jig, the metal foil made of the platinum group element used can be repeatedly used. Since it can be used, there is an advantage in terms of cost.
従って、本発明は従来の問題点を一掃したβ−アルミナ
管の焼成方法として、産業の発展に寄与するところは極
めて大である。Therefore, the present invention is extremely useful as a method for firing β-alumina tubes that eliminates the conventional problems and contributes to industrial development.
第１図は焼台治具にβ−アルミナ管素地を倒立させて焼
成用保護管の施蓋した本発明方法の実施状態を示す一部
切欠正面図である。 (1)：β−アルミナ管素地、(2)：底部、 (3)：開口、(4)：焼台治具、(5)：焼成用保護管、 (6)：白金族元素からなる金属箔。FIG. 1 is a partially cutaway front view showing an embodiment of the method of the present invention in which a β-alumina tube base material is inverted on a baking table jig and a firing protection tube is covered. (1): β-alumina tube base, (2): bottom, (3): opening, (4): baking jig, (5): protective tube for firing, (6): metal consisting of platinum group element Foil.
Claims (1)
された有底筒状のβ−アルミナ管素地の底部側を該β−
アルミナ管素地の軸方向ストレート部長さの少なくとも
４％以上の長さに亘り白金族元素からなる金属箔により
覆って焼台治具上に前記開口をもって倒立させるととも
に該焼台治具上に焼成用保護管を前記β−アルミナ管素
地との間に所要の空隙をあけて施蓋して倒立するβ−ア
ルミナ管素地と焼成用保護管との直接接触を防止しつつ
焼成することを特徴とするβ−アルミナ管の焼成方法。1. A bottomed tubular β-alumina tube base material having one end closed by a bottom portion and the other end being opened by the bottom portion.
Alumina tube base material is covered with a metal foil made of a platinum group element for at least 4% or more of the length in the axial direction of the straight part, and is inverted with the opening on the baking table jig and baked on the baking table jig. It is characterized in that the protective tube is fired while preventing direct contact between the β-alumina tube base body and the protective tube for firing which are upside down by covering the β-alumina tube base body with a required gap opened. Method of firing β-alumina tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2213254A JPH0624150B2 (en) | 1990-08-10 | 1990-08-10 | β-alumina tube firing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2213254A JPH0624150B2 (en) | 1990-08-10 | 1990-08-10 | β-alumina tube firing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0494064A JPH0494064A (en) | 1992-03-26 |
| JPH0624150B2 true JPH0624150B2 (en) | 1994-03-30 |
Family
ID=16636056
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2213254A Expired - Lifetime JPH0624150B2 (en) | 1990-08-10 | 1990-08-10 | β-alumina tube firing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0624150B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0832862B1 (en) * | 1996-09-30 | 2002-11-20 | Kyocera Corporation | Heat- and corrosion-resisting protection tube |
| US6227127B1 (en) | 1998-04-28 | 2001-05-08 | Kyocera Corporation | Furnace material, heat resisting protection tube and protective member using the same sintered material |
| JP4749009B2 (en) * | 2005-03-17 | 2011-08-17 | 岩崎電気株式会社 | Reflector manufacturing method |
-
1990
- 1990-08-10 JP JP2213254A patent/JPH0624150B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0494064A (en) | 1992-03-26 |
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