JPH0718662B2 - Ceramic firing box - Google Patents
Ceramic firing boxInfo
- Publication number
- JPH0718662B2 JPH0718662B2 JP63139825A JP13982588A JPH0718662B2 JP H0718662 B2 JPH0718662 B2 JP H0718662B2 JP 63139825 A JP63139825 A JP 63139825A JP 13982588 A JP13982588 A JP 13982588A JP H0718662 B2 JPH0718662 B2 JP H0718662B2
- Authority
- JP
- Japan
- Prior art keywords
- melting point
- ceramic
- low
- box
- molded body
- 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 - Fee Related
Links
- 239000000919 ceramic Substances 0.000 title claims description 55
- 238000010304 firing Methods 0.000 title description 29
- 238000002844 melting Methods 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 31
- 230000008018 melting Effects 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 21
- 229910010293 ceramic material Inorganic materials 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 description 33
- 230000008020 evaporation Effects 0.000 description 29
- 239000011230 binding agent Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
Landscapes
- Furnace Charging Or Discharging (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、Pb,B,Biなどの低融点蒸発物を含むセラミッ
ク組成物にバインダーを混合して成形した後、焼成工程
において、このセラミック成形体を収納して焼成するた
めのセラミックス焼成用匣に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention relates to a ceramic composition containing a low-melting point evaporant such as Pb, B, and Bi mixed with a binder, which is then molded in a firing step. The present invention relates to a ceramic firing box for accommodating and firing a molded body.
セラミック焼結体の製造にあたっては、まず各原料粉を
所定割合となるように秤量して混合した後、これを仮焼
し、この仮焼粉を粉砕して細かな粉砕粉を得る。つい
で、この粉砕粉にポリビニルアルコール（PVA）を系や
ポリビニルブチラール（PVB）系などの成形用バインダ
ーや焼結助剤などを混合し、この混合粉を加圧成形その
他の適宜成形手段によって成形した後、この粉体のセラ
ミック成形体（生成形体）を焼成用匣に納め、焼成工程
を通じて焼き上げると共に上記バインダーを熱分解して
蒸発除去させている。In the production of the ceramic sintered body, first, the respective raw material powders are weighed and mixed so as to have a predetermined ratio, then calcined, and the calcined powder is pulverized to obtain fine pulverized powder. Next, polyvinyl alcohol (PVA) -based or polyvinyl butyral (PVB) -based molding binders, sintering aids, etc. were mixed with this pulverized powder, and the mixed powder was molded by pressure molding or other appropriate molding means. After that, the powdery ceramic molded body (green molded body) is placed in a firing box, baked during the firing process, and the binder is thermally decomposed and evaporated.
このように、セラミック成形体の焼成工程においては、
成形用のバインダーを熱分解して大気中などへ蒸発除去
させる必要があるため、一般には、受け皿状などの開放
構造の焼成用匣が用いられている。Thus, in the firing process of the ceramic molded body,
Since it is necessary to thermally decompose the binder for molding and remove it by evaporating it into the atmosphere or the like, an open-structure firing box such as a saucer is generally used.
ところが、セラミック組成物には、Pb,B,BBiなどの低融
点蒸発物を含むものが多くある。例えば、Pbを含むセラ
ミック組成物には、圧電体セラミックスとして、 PbZrO3−PbTiO3 Pb（Sn1/2Sb1/2）O3−PbZrO3−PbTiO3 Pb（Mn1/3Nb2/3）O3−PbZrO3−PbTiO3 などがあり、コンデンサなどに用いられる複合ペロブス
カイト誘電体セラミックスとして、 Pb（Fe1/2Nb1/2）O3−Pb（Mg1/3Nb2/3）O3 Pb（Fe2/3Ｗ1/3）O3−Pb（Fe1/2Nb1/2）O3 Pb（Mg1/2Ｗ1/2）O3−PbTiO3 などがある。また、Ｂを含むセラミック組成物には、低
温焼結多層基板に用いられている Al2O3−CaO−SiO2−MgO−B2O3 BaO−SiO2−Al2O3−CaO−B2O3 などがある。However, many ceramic compositions contain low-melting point vaporized substances such as Pb, B, and BBi. For example, in a ceramic composition containing Pb, as a piezoelectric ceramic, PbZrO 3 -PbTiO 3 Pb (Sn 1/2 Sb 1/2 ) O 3 -PbZrO 3 -PbTiO 3 Pb (Mn 1/3 Nb 2/3 ) O 3 -PbZrO 3 -PbTiO 3 etc., and as composite perovskite dielectric ceramics used for capacitors, Pb (Fe 1/2 Nb 1/2 ) O 3 -Pb (Mg 1/3 Nb 2/3 ) O 3 Pb (Fe 2/3 W 1/3 ) O 3 -Pb (Fe 1/2 Nb 1/2) O 3 Pb (Mg 1/2 W 1/2) O 3 -PbTiO 3 or the like. Further, the ceramic composition containing B includes Al 2 O 3 —CaO—SiO 2 —MgO—B 2 O 3 BaO—SiO 2 —Al 2 O 3 —CaO—B, which is used for a low temperature sintered multilayer substrate. 2 O 3 etc.
このような低融点蒸発物を組成に含むセラミック成形体
を開放構造の焼成用匣に収納して焼成した場合、バイン
ダーばかりでなく低融点組成物も大気中などへ蒸発して
しまい、セラミック焼結体の組成が調合時のものからず
れ、物理的特性や電気的特性にバラツキを生じるという
問題があった。When a ceramic compact containing such a low-melting point evaporant in its composition is stored in an open-structure firing box and fired, not only the binder but also the low-melting point composition evaporates into the atmosphere, etc. There is a problem that the composition of the body deviates from that at the time of preparation, and the physical characteristics and the electrical characteristics vary.
このため、Pb,B,Biなどの低融点蒸発物を組成に含むセ
ラミック成形体の焼成用としては、一般に、第４図に示
すようなほぼ密閉された構造の擦り合わせ匣12が用いら
れている。そして、このの擦り合わせ匣12内にセラミッ
ク成形体１と共にこのセラミック成形体１に含まれる低
融点蒸発物の粉末13を入れてき、低融点蒸発物の粉末13
を蒸発させることによってセラミック成形体１を低融点
蒸発物の飽和雰囲気中に置き、これによってセラミック
成形体１からの低融点蒸発物の蒸発を抑制している。し
かしながら、この密閉構造の擦り合わせ匣12を用いる
と、酸素不足によってバインダーが熱分解しにくく、し
かも蒸発したバインダーを外部へ排出できにくく、完全
にバインダーを除去することができないという問題があ
った。Therefore, for firing a ceramic molded body containing a low-melting point vaporized substance such as Pb, B, Bi, etc., generally, a rubbing box 12 having a substantially sealed structure as shown in FIG. 4 is used. There is. Then, the powder 13 of the low melting point vapor contained in the ceramic molded body 1 and the powder 13 of the low melting point vapor are put into the rubbing box 12 together with the ceramic molded body 1.
The ceramic molded body 1 is placed in a saturated atmosphere of the low-melting-point evaporated material by evaporating, and thereby evaporation of the low-melting-point evaporated material from the ceramic molded body 1 is suppressed. However, when the rubbing box 12 having the closed structure is used, there is a problem that the binder is less likely to be thermally decomposed due to lack of oxygen, and the evaporated binder is difficult to be discharged to the outside, so that the binder cannot be completely removed.
従来にあっては、上述の如くPb,B,Biなどの低融点蒸発
物を組成に含むセラミック成形体を焼成する工程におい
ては、開放構造の焼成用匣を用いるとバインダーの除去
性に優れるが、低融点蒸発物の蒸発によってセラミック
焼結体の組成にバラツキが生じ、また密閉構造の焼成用
匣を用いると低融点蒸発物の蒸発を抑制できるもののバ
インダーの除去を完全に行えないという問題があった。Conventionally, as described above, in the step of firing a ceramic compact containing Pb, B, Bi, or another low-melting point evaporant in its composition, if an open-structure firing box is used, the binder removal property is excellent. However, the composition of the ceramic sintered body varies due to the evaporation of the low-melting point evaporation material, and the use of a closed-type firing box can suppress the evaporation of the low-melting point evaporation material but cannot completely remove the binder. there were.
したがって、本発明は低融点蒸発物の蒸発を抑制しなが
らセラミック成形体中からバインダーを完全に除去する
ことができるようにすることを目的とする。Therefore, it is an object of the present invention to completely remove the binder from the ceramic molded body while suppressing the evaporation of the low melting point evaporated material.
本発明のセラミックス焼成用匣は、低融点蒸発物を組成
の一部に含んだセラミック成形体を納めるための収納空
間を高融点材料によって形成された匣体の内部に形成
し、この匣体の少なくとも一部分に前記収納空間と匣体
外部とを通気させるための多孔質部を設け、前記収納空
間の内面ないし多孔質部内部に前記低融点蒸発物ないい
し前記低融点蒸発物を含んだセラミック材料を付着させ
ることにより、前記多孔質部の少なくとも大部分を塞い
だことを特徴としている。The ceramic firing case of the present invention forms a storage space for accommodating a ceramic molded body containing a low-melting point evaporated material in a part of its composition inside a box body formed of a high-melting point material, and At least a part is provided with a porous portion for ventilating the storage space and the outside of the box, and a ceramic material containing the low melting point vapor or the low melting point vapor on the inner surface of the storage space or inside the porous portion. Is adhered to block at least most of the porous portion.
本発明にあっては、叙述の如くセラミック成形体を収納
する匣体の少なくとも一部に多孔質を設け、この多孔質
部の少なくとも大部分を低融点蒸発物ないし低融点蒸発
物を含んだ低融点蒸発物材料で塞いでいるので、セラミ
ック成形体を焼成させるため収納空間内の温度を上昇さ
せ、その温度が当該低融点蒸発物の融点温度近くまで達
すると、収納空間内面ないし多孔質部内に付着させた低
融点蒸発物が蒸発して収納空間内に充満され、収納空間
内は過飽和状態となって低融点蒸発物のセラミック成形
体からの蒸発を抑制することができる。このとき、収納
空間内の温度を上昇させるにつれて、多孔質部を塞いで
いた低融点蒸発物も蒸発し、蒸発後には多孔質部が開口
され、匣体外部からの酸素の供給及び匣体外部への熱分
解されたバインダーのガスの排出を促すことができる。In the present invention, as described above, at least a part of the box for housing the ceramic molded body is provided with a porous material, and at least most of the porous part has a low melting point vapor or a low melting point vaporizing material containing Since it is blocked with the melting point evaporating material, the temperature in the storage space is raised to fire the ceramic molded body, and when the temperature reaches close to the melting point temperature of the low melting point evaporating material, the inside surface of the storage space or the porous portion is The attached low-melting point evaporation material evaporates and fills the storage space, and the storage space is in a supersaturated state, so that evaporation of the low-melting point evaporation material from the ceramic molded body can be suppressed. At this time, as the temperature in the storage space rises, the low-melting point evaporation material that has blocked the porous portion also evaporates, the porous portion is opened after evaporation, and the supply of oxygen from the outside of the housing and the outside of the housing It is possible to promote discharge of the gas of the thermally decomposed binder to the.
以下、本発明の実施例を添付図に基づいて詳述する。 Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
第１図に示すように、匣体３はセラミック成形体１を載
置するため板状のセッター５と多孔質の上蓋体６とから
構成されている。セッター５は緻密な高融点のアルミナ
焼結体によって平板状に形成されている。上蓋体６は、
アルミナを基材とするセラミックス多孔質体により形成
されていて全体が多孔質部４となっており、その空孔は
上蓋体６の内面から外面に連通していて通気性を有して
おり、しかもこ空孔率は20％〜80％（体積比）となって
いる。また、上蓋体６の下面には凹所８が設けられてお
り、セッター５の上に上蓋体６を載置すると、上蓋体６
とセッター５との間には、下面をセッター５によって塞
がれ、上面及び側周面を多孔質の上蓋体６によって囲ま
れた収納空間２が形成される。As shown in FIG. 1, the box 3 is composed of a plate-shaped setter 5 and a porous upper lid 6 for mounting the ceramic molded body 1. The setter 5 is formed in a flat plate shape by a dense high melting point alumina sintered body. The upper lid 6 is
It is formed of a ceramics porous body having alumina as a base material, and has a porous portion 4 as a whole, and the pores thereof communicate from the inner surface to the outer surface of the upper lid body 6 and have air permeability, Moreover, the porosity is 20% to 80% (volume ratio). Further, a recess 8 is provided on the lower surface of the upper lid body 6. When the upper lid body 6 is placed on the setter 5, the upper lid body 6 is placed.
A storage space 2 is formed between the setter 5 and the setter 5, and the lower surface is closed by the setter 5 and the upper surface and the side peripheral surface are surrounded by the porous upper lid 6.
この多孔質体で形成された上蓋体６は、焼成しようとす
るセラミック成形体１の調合原料のスラリー中に予め浸
漬して付着したスラリーを乾燥させてあり、従って上蓋
体６の表面及び多孔質部４内部（空孔内）には、低融点
蒸発物を組成として含むセラミック材料が付着させられ
ている。The upper lid 6 formed of this porous body is obtained by previously immersing it in the slurry of the raw material for forming the ceramic molded body 1 to be fired and drying the attached slurry. A ceramic material containing a low-melting point vaporized substance as a composition is attached to the inside of the portion 4 (inside the pores).
しかして、Pb,B,Biなどの低融点蒸発物を組成に含むセ
ラミック材料にポリビニルアルコールやポリビニルブチ
ラールなどのバインダーを混合した後、所定形状に成形
されたセラミック成形体１を焼成する工程にいては、ま
ずセッター５の上にセラミック成形体１を積み重ねて、
あるいは並べて載置し、このセラミック成形体１を覆う
ようにしてセッター５の上に上蓋体６を被せる。さら
に、このセラミック成形体１を収納した匣体３を第２図
に示すような受け匣７内に入れ、これを第３図に示すよ
うに複数段に積み重ねる。ここで、受け匣７は、ムライ
ト質のセラミックスによって形成されており、周縁部４
辺の上面には比較的大きな切り欠き９が設けられてお
り、切り欠き９を通して自由に通気するようになってい
る。そして、受け匣７を用いて多孔質の上蓋体６に荷重
がかからないように積み重ねられた匣体３は、焼成炉中
に入れられ、加熱される。焼成炉中で徐々温度を上昇さ
せて焼成工程を進行させると、まず上蓋体６に付着させ
られているセラミック材料の低融点蒸発物が蒸発し、こ
低融点蒸発物の蒸気ガスは空気よりも重いので、収納空
間２内に沈降し、これによって収納空間２内で低融点蒸
発物の蒸気ガスが過飽和状態になり、セラミック成形体
１からの低融点蒸発物の蒸発が抑制され、低融点蒸発物
の蒸発によってセラミック焼結体の組成に変動を生じる
のを防止することができるのである。一方、上蓋体６の
低融点蒸発物が蒸発すると、蒸発した後には多孔質部４
の空孔が開口されるで、収納空間２内に酸素（空気）が
供給され、バインダーが燃焼させられて熱分解し、燃焼
した後のガスは多孔質部４から外部へ排出され、切り欠
き９を通って大気へ放出される。したがって、バインダ
ーを完全に燃焼させて除去することができ、かつ速やか
にバインダーを燃焼させることができるので高速の焼成
も可能なる。上蓋体６空孔率は、上記のごとく20％〜80
％としているが、これは空孔率が20％以下であると、焼
成物によっては、バインダーの燃焼が不完全になる場合
があり、また空孔率が80％以上であると、低融点蒸発物
の蒸発量抑制効果が不完全になることがあるためであ
る。In the process of firing the ceramic molded body 1 having a predetermined shape after mixing a binder such as polyvinyl alcohol or polyvinyl butyral with a ceramic material containing Pb, B, Bi or other low melting point evaporated material in the composition. First, stack the ceramic molded body 1 on the setter 5,
Alternatively, they are placed side by side, and the upper lid 6 is covered on the setter 5 so as to cover the ceramic molded body 1. Further, the box body 3 accommodating the ceramic molded body 1 is put into a receiving box 7 as shown in FIG. 2 and stacked in a plurality of stages as shown in FIG. Here, the receiving case 7 is made of mullite ceramics, and the peripheral portion 4
A relatively large notch 9 is provided on the upper surface of the side, and the ventilation is freely performed through the notch 9. Then, the box bodies 3 stacked by using the receiving box 7 so as not to apply a load to the porous upper lid body 6 are put into a firing furnace and heated. When the temperature is gradually raised in the firing furnace to advance the firing process, first, the low melting point evaporation material of the ceramic material attached to the upper lid 6 is evaporated, and the vapor gas of the low melting point evaporation gas is more than air. Since it is heavy, it settles in the storage space 2, whereby the vapor gas of the low-melting point vapor is supersaturated in the storage space 2 and the evaporation of the low-melting point vapor from the ceramic molded body 1 is suppressed, and the low-melting point vaporization is suppressed. It is possible to prevent the composition of the ceramic sintered body from fluctuating due to evaporation of the substance. On the other hand, when the low-melting point evaporation material of the upper lid body 6 evaporates, after the evaporation, the porous portion 4
Oxygen (air) is supplied into the storage space 2 by the opening of the holes, the binder is burned and thermally decomposed, and the burned gas is discharged from the porous portion 4 to the outside, and the notch is formed. It is released to the atmosphere through 9. Therefore, the binder can be completely burned and removed, and the binder can be quickly burned, so that high-speed firing is also possible. The upper cover 6 porosity is 20% to 80% as described above.
%, But if the porosity is 20% or less, the burning of the binder may be incomplete depending on the fired product, and if the porosity is 80% or more, the low melting point evaporation occurs. This is because the effect of suppressing the evaporation amount of the substance may be incomplete.
なお、上記実施例では、全体が多孔質部となった上蓋体
を用いたが、多孔質部は上蓋体の一部に設けられていて
も良い。また、下側のセッターの全体もしくは一部に多
孔質部を設けることも可能である。上蓋体及びセッター
の形状も図示のようなものに限定されず、セッターの上
面に凹所を設け、上蓋体を板状にしても差し支えない。In addition, in the above-described embodiment, the upper lid body having the entire porous portion is used, but the porous portion may be provided in a part of the upper lid body. Further, it is also possible to provide a porous portion on the whole or a part of the lower setter. The shapes of the upper lid and the setter are not limited to those shown in the drawings, and a recess may be provided on the upper surface of the setter so that the upper lid may have a plate shape.
上記実施例では、匣体に予めセラミック成形体の調合原
料を付着させておいたが、セラミック成形体調合原料に
含まれる低融点蒸発物だけを焼成工程の前に予め匣体に
付着させておいても良い。但し、セラミック成形体の製
造にあたっては、そのの調合原料が用意されているか
ら、これを利用するのが便利であう。In the above-mentioned example, the compounding raw material of the ceramic molded body was previously attached to the box, but only the low melting point evaporation material contained in the ceramic molded body compounding raw material was previously attached to the box before the firing step. You may stay. However, in the production of the ceramic molded body, it is convenient to use the prepared raw material because it is prepared.
また、もっとも、PbやＢ等の低融点蒸発物は空気よりも
重いので、収納空間内の上部に付着させるのが効果的で
ある。また、上記実施例においては、初めは多孔質部は
この低融点蒸発物等によって塞がれているが、焼成工程
において匣体の温度が上昇するにつれて低融点蒸発物の
蒸発量が多くなり、低融点蒸発物蒸発に伴って多孔質部
の通気率も大きくなり、低融点蒸発物の蒸発量とバラン
スしながら通気率が大きくなってゆき、また低融点蒸発
物が蒸発した後に多孔質部が開口されるので、これは好
ましい実施態様である。更に、多孔質部に付着させるこ
とによって付着力が大きくなり、低融点蒸発物の剥離な
どが生じにくい。In addition, since the low melting point vaporized substances such as Pb and B are heavier than air, it is effective to attach them to the upper part of the storage space. Further, in the above example, the porous portion is initially blocked by this low-melting point evaporated material, etc., but the evaporation amount of the low-melting point evaporated material increases as the temperature of the box increases in the firing step, The air permeability of the porous part increases with the evaporation of the low-melting point evaporated material, and the air permeability increases while balancing the evaporation amount of the low-melting point evaporated material. This is the preferred embodiment as it is open. Further, the adhesion to the porous portion increases the adhesion, so that the low melting point evaporated material is less likely to peel off.
なお、匣体は繰りり返し使用されるので、低融点蒸発物
等のセラミック材料が焼成工程によって消耗した場合に
は、再び匣体をスラリーに浸漬乾燥させてセラミック材
料を匣体に付着させるものである。Since the box is used repeatedly, when the ceramic material such as low melting point evaporation material is consumed by the firing process, the box is again immersed in the slurry and dried to adhere the ceramic material to the box. Is.
又、多孔質部からバインダーが排出され易い状態、つま
り通気部が残るようにしてもよく、更に、匣体内部と外
部をつなぐ通気部は低融点蒸発物が外部に排出されにく
い構造、つまり蛇行状としておくほうが好ましい。Also, the binder may be easily discharged from the porous part, that is, the ventilation part may be left, and the ventilation part that connects the inside and the outside of the box is a structure in which the low melting point vapor is difficult to be discharged to the outside, that is, meandering. It is preferable to keep the shape.
（実施例１） 80wt％Pb（Mg1/3Nb2/3）O3−15wt％Pb（Ｚ1/3Nb2/3）O3
−5wt％PbTiO3組成を有する複合ペロブスカイト誘電体
材料によりセラミック成形体を形成した。この低融点蒸
発物Pbを組成に含むセラミック成形体を、第１図に示し
たようなアルミナ焼結体のセッッターとアルミナを基材
とする多孔質の上蓋体からなる匣体内に納めた。この上
蓋体には、予め上記組成のスラリーに浸漬乾燥させてセ
ラミック成形体と同組成セラミック材料を付着させてお
いた。これを第３図のようにムライト質の受け匣内に入
れ、焼成炉中で焼成温度1000℃に設定して高速で昇降温
させて焼成した。この結果、キュリー点は室温付近（25
℃）にあって組成から推定される値からのずれが小さ
く、焼成による組成の変動の小さいことが裏付けられ
た。また、比誘電率εが20000の良好な誘電体が得られ
た。Example 1 80 wt% Pb (Mg 1/3 Nb 2/3 ) O 3 −15 wt% Pb (Z 1/3 Nb 2/3 ) O 3
Thereby forming a ceramic molding of a composite perovskite dielectric material having a -5wt% PbTiO 3 composition. The ceramic molded body containing the low-melting point evaporated material Pb in its composition was placed in a box body composed of a setter of an alumina sintered body as shown in FIG. 1 and a porous upper lid body based on alumina. A ceramic material having the same composition as that of the ceramic compact was previously attached to the upper lid by dipping and drying in a slurry having the above composition. As shown in FIG. 3, this was placed in a mullite-like container, and the firing temperature was set at 1000 ° C. in a firing furnace to raise and lower the temperature at a high speed for firing. As a result, the Curie point is around room temperature (25
C.), the deviation from the value estimated from the composition was small, which confirmed that the composition variation due to firing was small. Also, a good dielectric having a relative permittivity ε of 20000 was obtained.
（比較例１） 匣体にセラミック材料を付着させず、上記実施例１と同
じ条件で、同じ組成のセラミック成形体を焼成した。こ
の結果、キュリー点は45℃だけ高温側にずれ、組成変動
（Pbの一部の蒸発）の大きいことを示した。また、比誘
電率εも9000に低下した。(Comparative Example 1) A ceramic compact having the same composition was fired under the same conditions as in Example 1 above without adhering the ceramic material to the box. As a result, it was shown that the Curie point was shifted to the high temperature side by 45 ℃, and the compositional variation (partial evaporation of Pb) was large. Further, the relative permittivity ε also decreased to 9,000.
（実施例２） BaO−SiO2−Al2O3−CaO−B2O3の組成（低融点蒸発物は
Ｂ）を有する多層基板材料によって板状のセラミック成
形体を形成した。これを実施例１と同様にして焼成し
た。但し、上蓋体には上記多層基板材料と同じ組成のス
ラリーに浸漬乾燥させておいた。この結果、焼成された
セラミック多層基板の反り変形は１％以内であった。(Example 2) Composition of BaO-SiO 2 -Al 2 O 3 -CaO-B 2 O 3 ( low-melting evaporation was B) to form a plate-shaped ceramic molded bodies by the multilayer substrate material having a. This was fired in the same manner as in Example 1. However, the upper lid was immersed and dried in a slurry having the same composition as the above-mentioned multilayer substrate material. As a result, the warped deformation of the fired ceramic multilayer substrate was within 1%.
（比較例２） 上蓋体をスラリー浸漬せず、上記実施例２と同じセラミ
ック成形体を実施例２と同じ条件で焼成した。この結
果、焼成されたセラミック多層基板の反り変形は５％で
あった。Comparative Example 2 The same ceramic compact as in Example 2 was fired under the same conditions as in Example 2 without immersing the upper lid in the slurry. As a result, the warped deformation of the fired ceramic multilayer substrate was 5%.
本発明によれば、あらかじめ多孔質部に低融点物質を付
着させて多孔質部を塞いでおくことにより収納空間内を
ほぼ密閉させておき、収容空間温度を上昇させるととも
に低融点蒸発物を収納空間内に充満させてセラミック成
形体から低融点蒸発物の蒸発を防ぎ、セラミック焼結体
の組成のバラツキを小さくすることができる。また、そ
後多孔質部を開口し、この開口から収納空間内の酸素供
給や燃焼されたガスの放出を促し、セラミック成形体か
らバインダーを確実に除去することができる。従って、
本発明のセラミックス焼成用匣を用いることにより、セ
ラミック成形体に含まれている低融点蒸発物の蒸発を防
止しながら、バインダーを確実に除去することが可能と
なるものであり、セラミック成形体の焼成工程と脱バイ
ンダー工程とを同時に行うことができるものである。According to the present invention, the low melting point substance is attached to the porous part in advance to close the inside of the storage space to close the storage space, thereby raising the temperature of the storage space and storing the low melting point evaporated material. It is possible to prevent the evaporation of the low-melting point evaporation material from the ceramic molded body by filling the space and reduce the variation in the composition of the ceramic sintered body. Further, after that, the porous portion is opened, oxygen supply in the storage space and release of burned gas are promoted from this opening, and the binder can be reliably removed from the ceramic molded body. Therefore,
By using the ceramic firing box of the present invention, it is possible to reliably remove the binder while preventing evaporation of the low-melting point evaporated material contained in the ceramic molded body. The baking step and the binder removal step can be performed simultaneously.
第１図は本発明の一実施例を示す断面図、第２図は同上
の焼成用匣を納めるための受け匣を示す斜視図、第３図
は同上の焼成用匣を受け匣に納めて積み重ねた状態を示
す断面図、４図は従来例の擦り合わせ匣を示す断面図で
ある。 １……セラミック成形体 ２……収納空間 ３……匣体 ４……多孔質部FIG. 1 is a sectional view showing an embodiment of the present invention, FIG. 2 is a perspective view showing a receiving box for accommodating the same firing box, and FIG. 3 is a receiving box for receiving the same firing box in the same. FIG. 4 is a cross-sectional view showing a stacked state and FIG. 4 is a cross-sectional view showing a conventional rubbing box. 1 ... Ceramic molded body 2 ... Storage space 3 ... Box 4 ... Porous part
Claims (1)
ック成形体を納めるための収納空間を高融点材料によっ
て形成された匣体の内部に形成し、この匣体の少なくと
も一部分に前記収納空間と匣体外部とを通気させるため
の多孔質部を設け、前記収納空間の内面ないし多孔質部
内部に前記低融点蒸発物ないし前記低融点蒸発物を含ん
だセラミック材料を付着させることにより、前記多孔質
部の少なくとも大部分を塞いだことを特徴とするセラミ
ックス焼成用匣。1. A storage space for accommodating a ceramic molded body containing a low-melting point vaporized substance as a part of its composition is formed inside a box made of a high-melting material, and at least a part of the box is formed. By providing a porous portion for ventilating the storage space and the outside of the box, by adhering the low melting point vapor or the ceramic material containing the low melting point vapor to the inner surface of the storage space or the inside of the porous portion. A ceramic sagger for burning ceramics, characterized in that at least most of the porous portion is closed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63139825A JPH0718662B2 (en) | 1988-06-07 | 1988-06-07 | Ceramic firing box |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63139825A JPH0718662B2 (en) | 1988-06-07 | 1988-06-07 | Ceramic firing box |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01310293A JPH01310293A (en) | 1989-12-14 |
| JPH0718662B2 true JPH0718662B2 (en) | 1995-03-06 |
Family
ID=15254352
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63139825A Expired - Fee Related JPH0718662B2 (en) | 1988-06-07 | 1988-06-07 | Ceramic firing box |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0718662B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2535514Y2 (en) * | 1991-10-21 | 1997-05-14 | 日本碍子株式会社 | Sagger mounting plate |
| JP4959950B2 (en) * | 2005-03-29 | 2012-06-27 | 京セラ株式会社 | Sintered body and wiring board |
| JP4841506B2 (en) * | 2007-06-11 | 2011-12-21 | 東邦チタニウム株式会社 | Method for producing metal oxide |
| JP6035682B2 (en) * | 2013-04-19 | 2016-11-30 | 岩崎電気株式会社 | Manufacturing method of arc tube for ceramic metal halide lamp |
| JP7459478B2 (en) * | 2018-10-26 | 2024-04-02 | 住友金属鉱山株式会社 | Sagger and sagger packing, and method for producing lithium metal composite oxide |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5922149B2 (en) * | 1980-11-17 | 1984-05-24 | 株式会社明電舎 | Ceramic firing containers containing lead |
-
1988
- 1988-06-07 JP JP63139825A patent/JPH0718662B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01310293A (en) | 1989-12-14 |
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