JPH07165460A - Production of formed magnesia - Google Patents

Production of formed magnesia

Info

Publication number
JPH07165460A
JPH07165460A JP5119875A JP11987593A JPH07165460A JP H07165460 A JPH07165460 A JP H07165460A JP 5119875 A JP5119875 A JP 5119875A JP 11987593 A JP11987593 A JP 11987593A JP H07165460 A JPH07165460 A JP H07165460A
Authority
JP
Japan
Prior art keywords
magnesia
powder
mixed
molding
organic solvent
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.)
Pending
Application number
JP5119875A
Other languages
Japanese (ja)
Inventor
Takeo Nakagawa
威雄 中川
Seizo Takahashi
清造 高橋
Kozo Hirozawa
耕造 広沢
Osamu Asagami
修 浅上
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.)
KOUNOSHIMA KAGAKU KOGYO KK
Konoshima Chemical Co Ltd
Original Assignee
KOUNOSHIMA KAGAKU KOGYO KK
Konoshima Chemical Co Ltd
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 KOUNOSHIMA KAGAKU KOGYO KK, Konoshima Chemical Co Ltd filed Critical KOUNOSHIMA KAGAKU KOGYO KK
Priority to JP5119875A priority Critical patent/JPH07165460A/en
Publication of JPH07165460A publication Critical patent/JPH07165460A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To produce a defect-free homogeneous formed article of magnesia by extrusion molding. CONSTITUTION:Magnesia powder is mixed with a sintering assistant and a deflocculating agent in wet state and dried. The obtained powder is mixed with a forming binder dissolved in an organic solvent and liquid paraffin and the mixture is extrusion-molded.

Description

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

【0001】[0001]

【産業上の利用分野】本発明は、押出成形法によるマグ
ネシア成形体の製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a magnesia compact by an extrusion molding method.

【0002】[0002]

【従来技術及びその問題点】高純度マグネシア焼結体
は、酸化雰囲気中での耐熱性に優れると共に、酸化鉛や
アルカリに対する耐食性に優れるため、PZT等の電子
セラミック材料やβ−アルミナなどの焼成用容器、ある
いは熱電対用保護管等の用途がある。従来、このような
用途に使用される容器は、鋳込み成形によって作られて
いる。この鋳込み成形では、成形体にクラックが発生す
るのを防ぐため、バインダーを添加しているが、バイン
ダーが溶媒に溶けて溶媒の粘度を上げるため、鋳込み速
度が遅くなり、成形時間が長くなる問題があった。ま
た、鋳込み成形では、成形体を一個ずつしか作成できな
いため、量産化には適していない。これに対し、押出成
形法は、連続製造が可能なため、大量生産に適している
方法として実用されているが、従来の方法では成形体中
に欠陥が残るため、欠陥がない均質な成形体を得ること
が困難であった。
2. Description of the Related Art High-purity magnesia sintered bodies have excellent heat resistance in an oxidizing atmosphere and excellent corrosion resistance to lead oxide and alkali, so that they can be used for firing electronic ceramic materials such as PZT and β-alumina. There are applications such as containers for thermocouples and protective tubes for thermocouples. Conventionally, containers used for such applications are made by casting. In this cast molding, a binder is added in order to prevent cracks from occurring in the molded body, but since the binder dissolves in the solvent and increases the viscosity of the solvent, the casting speed becomes slow and the molding time becomes long. was there. In addition, the cast molding is not suitable for mass production because only one molded body can be produced. On the other hand, the extrusion molding method has been practically used as a method suitable for mass production because continuous production is possible, but in the conventional method, defects remain in the molded body, so that a uniform molded body without defects is formed. Was difficult to obtain.

【0003】[0003]

【発明の目的】本発明の目的は、前記問題点を解決し、
押出成形法によって、欠陥がない均質な成形体を製造す
ることができる方法を提供するものである。
The object of the present invention is to solve the above problems,
It is intended to provide a method capable of producing a defect-free homogeneous molded body by an extrusion molding method.

【0004】[0004]

【問題点を解決するための手段】本発明は、マグネシア
粉末、焼結助剤及び解膠剤を湿式混合した後、乾燥して
得られた粉末に、有機溶媒に溶解した成形用バインダ
ー、及び流動パラフィンを添加、混合した後、押出成形
することを特徴とするマグネシア成形体の製造方法に関
するものである。
According to the present invention, a powder obtained by wet-mixing a magnesia powder, a sintering aid and a deflocculant, and then drying the powder, and a molding binder dissolved in an organic solvent, and The present invention relates to a method for producing a magnesia molded body, which comprises adding and mixing liquid paraffin, and then extruding.

【0005】本発明においては、まずマグネシア粉末、
焼結助剤及び解膠剤を湿式混合した後、乾燥して混合粉
末を得る。マグネシア粉末としては、BET比表面積が
5〜170m2/g(比表面積径0.01〜0.2μ
m)、純度99.9%以上の高純度超微粉単結晶酸化マ
グネシウムが好ましい。このような高純度超微粉単結晶
酸化マグネシウムは、特公平2−289号公報に開示さ
れた方法、即ちマグネシウム蒸気と酸素含有ガスを乱流
拡散状態で酸化させる方法により合成することができ
る。BET比表面積が170m2/gを超えた酸化マグネ
シウムを製造することも可能であり、本発明にも有用で
あるが、製造コストがきわめて高くなること、通常の粉
末の取扱いが困難になることなどから現状では実用性が
低い。また、比表面積が5m2/g未満となると、粉末の
焼結活性が低下し、密度の高い焼結体が得られないので
好ましくない。焼結助剤としては、ZrO2、Y23
が用いられる。
In the present invention, first, magnesia powder,
The sintering aid and the deflocculant are wet mixed and then dried to obtain a mixed powder. The magnesia powder has a BET specific surface area of 5 to 170 m 2 / g (specific surface area diameter of 0.01 to 0.2 μm).
m), high-purity ultrafine single crystal magnesium oxide having a purity of 99.9% or more is preferable. Such high-purity ultrafine single crystal magnesium oxide can be synthesized by the method disclosed in Japanese Examined Patent Publication No. 2-289, that is, a method of oxidizing magnesium vapor and an oxygen-containing gas in a turbulent diffusion state. It is possible to produce magnesium oxide having a BET specific surface area of more than 170 m 2 / g, and it is also useful in the present invention, but the production cost is extremely high, and it is difficult to handle ordinary powders. Therefore, the practicality is low at present. On the other hand, if the specific surface area is less than 5 m 2 / g, the sintering activity of the powder is lowered, and a sintered body having a high density cannot be obtained, which is not preferable. ZrO 2 , Y 2 O 3 or the like is used as the sintering aid.

【0006】マグネシア粉末に対する添加割合は、マグ
ネシア粉末100重量部に対して、焼結助剤0.05〜
0.5重量部、解膠剤0.5〜5重量部が好ましい。湿
式混合は、マグネシア粉末、焼結助剤及び解膠剤にアル
コール、トルエン等の有機溶媒を加えて、ボールミル等
により行う。次いで、乾燥して溶媒を除去し、粉砕して
適当な顆粒に整粒して混合粉末を得る。
The addition ratio of the sintering aid to the magnesia powder is 0.05 to 100 parts by weight of the magnesia powder.
0.5 part by weight and a deflocculant 0.5 to 5 parts by weight are preferred. The wet mixing is performed by adding an organic solvent such as alcohol or toluene to the magnesia powder, the sintering aid and the deflocculant, and using a ball mill or the like. Then, the solvent is removed by drying, and the mixture is crushed and sized into appropriate granules to obtain a mixed powder.

【0007】得られた混合粉末に、アルコール、トルエ
ン等の有機溶媒に溶解した成形用バインダー、及び流動
パラフィンを添加し、混合する。成形用バインダーとし
ては、特に制限はなく、有機溶媒に可溶なバインダーが
用いられる。成形用バインダーの添加割合は、マグネシ
ア100重量部に対して、0.1〜5重量部、特に0.
3〜2重量部が好ましい。有機溶媒及び流動パラフィン
の添加量及び割合は、均質な成形体が得られるように適
宜選択すればよいが、通常、マグネシア100重量部に
対して、有機溶媒5〜20重量部、流動パラフィン5〜
20重量部の範囲で用いられる。特に、流動パラフィン
を添加することにより、成形過程の粉末の流動性が向上
する。次いで得られた混合物を押出成形し、乾燥して溶
媒を除去し、さらに脱バインダーした後、焼結する。焼
結は、酸化性雰囲気下、例えば空気中で1500〜18
00℃の温度で行われる。
A molding binder dissolved in an organic solvent such as alcohol or toluene and liquid paraffin are added to the obtained mixed powder and mixed. The molding binder is not particularly limited, and a binder soluble in an organic solvent is used. The addition ratio of the molding binder is 0.1 to 5 parts by weight, especially 0.1% by weight, relative to 100 parts by weight of magnesia.
3 to 2 parts by weight is preferable. The addition amount and ratio of the organic solvent and the liquid paraffin may be appropriately selected so that a homogeneous molded body can be obtained. Usually, 5 to 20 parts by weight of the organic solvent and 5 to 5 parts of the liquid paraffin are added to 100 parts by weight of magnesia.
Used in the range of 20 parts by weight. In particular, the addition of liquid paraffin improves the fluidity of the powder during the molding process. The resulting mixture is then extruded, dried to remove the solvent, debindered and then sintered. Sintering is performed in an oxidizing atmosphere, for example, in air at 1500 to 18
It is carried out at a temperature of 00 ° C.

【0008】[0008]

【実施例】以下に実施例を示し、本発明をさらに具体的
に説明する。 実施例1〜4及び比較例1 トルエン300gに、高純度超微粉単結晶酸化マグネシ
ウム(比表面積径0.2μm)400g、焼結助剤0.
4g及び解膠剤8gを添加し、7時間ボールミル混合を
行った後、乾燥して溶媒を除去し、粉砕して混合粉末を
得た。得られた混合粉末に、成形用バインダー(バイン
ドセラムSA541(樹脂分40%);三井東圧化学
(株)製)、トルエン及び流動パラフィンを表1に記載
の割合で添加し、混合した。次いで得られた混合物を、
押出速度5mm/min、押出比6.3で、外径10
φ、内径6φのパイプ形状に押出成形した。得られた成
形体を乾燥して溶媒を除去した後、空気中で0.5℃/
minの速度で昇温しながら、脱バインダーし、続けて
1600℃以上の温度で焼結した。乾燥後の成形体の密
度及び焼結体の密度を測定した結果を表2に示す。
EXAMPLES The present invention will be described more concretely with reference to the following examples. Examples 1 to 4 and Comparative Example 1 To 300 g of toluene, 400 g of high-purity ultrafine single-crystal magnesium oxide (specific surface area diameter 0.2 μm), sintering aid 0.
After adding 4 g and a deflocculant 8 g and performing ball mill mixing for 7 hours, it dried and the solvent was removed and it grind | pulverized and the mixed powder was obtained. A molding binder (Bind Serum SA541 (resin content 40%); manufactured by Mitsui Toatsu Chemicals, Inc.), toluene and liquid paraffin were added to the obtained mixed powder in the proportions shown in Table 1 and mixed. The resulting mixture is then
Extrusion speed 5 mm / min, extrusion ratio 6.3, outer diameter 10
It was extruded into a pipe shape with φ and an inner diameter of 6φ. The obtained molded product is dried to remove the solvent, and then in air at 0.5 ° C /
The binder was removed while the temperature was raised at a rate of min, followed by sintering at a temperature of 1600 ° C. or higher. The results of measuring the density of the molded body and the density of the sintered body after drying are shown in Table 2.

【0009】[0009]

【表1】 [Table 1]

【0010】[0010]

【表2】 [Table 2]

【0011】[0011]

【発明の効果】本発明の製造方法によれば、押出成形法
によって、欠陥がない均質な成形体を大量に生産するこ
とができる。
According to the manufacturing method of the present invention, it is possible to produce a large amount of defect-free and homogeneous moldings by the extrusion molding method.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 マグネシア粉末、焼結助剤及び解膠剤を
湿式混合した後、乾燥して得られた粉末に、有機溶媒に
溶解した成形用バインダー、及び流動パラフィンを添
加、混合した後、押出成形することを特徴とするマグネ
シア成形体の製造方法。
1. A magnesia powder, a sintering aid, and a deflocculant are wet-mixed and then dried, and a molding binder and liquid paraffin dissolved in an organic solvent are added to and mixed with the powder. A method for producing a magnesia molded body, which comprises performing extrusion molding.
JP5119875A 1993-05-21 1993-05-21 Production of formed magnesia Pending JPH07165460A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5119875A JPH07165460A (en) 1993-05-21 1993-05-21 Production of formed magnesia

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5119875A JPH07165460A (en) 1993-05-21 1993-05-21 Production of formed magnesia

Publications (1)

Publication Number Publication Date
JPH07165460A true JPH07165460A (en) 1995-06-27

Family

ID=14772412

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5119875A Pending JPH07165460A (en) 1993-05-21 1993-05-21 Production of formed magnesia

Country Status (1)

Country Link
JP (1) JPH07165460A (en)

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