JP4532971B2 - Magnesia sintered body with excellent durability - Google Patents
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本発明は、耐久性にすぐれたマグネシア焼結体に関する。なお、本発明でいう耐久性とは、耐熱衝撃抵抗性や耐食性だけでなく、加熱・冷却の繰り返しによる変形や粒子離脱に対する安定性を意味する。 The present invention relates to a magnesia sintered body excellent in durability. The durability as used in the present invention means not only thermal shock resistance and corrosion resistance, but also stability against deformation and particle detachment due to repeated heating and cooling.
マグネシア焼結体は耐熱温度が高く、代表的な塩基性材料で、古くから金属溶解用るつぼなどに使用されている。
最近、磁気記録媒体のニーズが高まり、磁気テープはオーディオ分野などに広く使用されているが、従来の磁気テープは、強磁性粉末をバインダーに分散させて塗布する方法が用いられていたが、最近の高密度記録のニーズに対応して、Ｃｏ−Ｎｉ合金などの金属磁性材料をポリエステルフィルム、ポリイミドフィルムなどの非磁性支持体上に蒸着、スパッタリング、イオンプレーティング等の方法により金属薄膜を形成した金属薄膜型磁気記録媒体が使われるようになってきた。これらの方法の中で磁性薄膜製造に適した方法として、マグネシア製蒸発源用るつぼに磁性金属を入れて、この磁性金属に電子ビームを照射して磁性金属を溶解させて蒸着する方法が広く採用されている。しかしながら、蒸着時にはスプラッシュと呼ばれる現象が見られるが、このスプラッシュとは、るつぼから脱粒した粒子が溶解した磁性金属に混入し、その粒子に電子ビームがあたって粒子が飛び出し、支持体にピンホールを開けてしまい、このピンホールが磁性記録媒体の特性劣化を引き起こす問題がある。
The magnesia sintered body has a high heat-resistant temperature and is a typical basic material, and has been used for crucibles for melting metals for a long time.
Recently, there has been a growing need for magnetic recording media, and magnetic tapes are widely used in the audio field and the like, but conventional magnetic tapes have been used by dispersing ferromagnetic powder in a binder and applying it recently. In response to the needs of high-density recording, metal magnetic materials such as Co-Ni alloys were deposited on non-magnetic supports such as polyester films and polyimide films by sputtering, ion plating, and other methods. Metal thin film type magnetic recording media have come to be used. Among these methods, as a method suitable for the production of magnetic thin films, a method of depositing a magnetic metal in a magnesia crucible for evaporation source and irradiating the magnetic metal with an electron beam to dissolve the magnetic metal and depositing is widely adopted. Has been. However, a phenomenon called splash is observed at the time of vapor deposition, but this splash is a mixture of particles that have been shed from the crucible and dissolved in the magnetic metal. There is a problem that this pinhole causes deterioration of characteristics of the magnetic recording medium.
この問題を解決する方法として、特許文献１にマグネシア純度を向上させる方法が開示されているが、ただ単にマグネシア純度の向上だけではスプラッシュを低減することはできない。また、特許文献２には不純物酸化物の含有率を０．５重量％以下にすることが開示されているものの十分に満足できるものではない。 As a method for solving this problem, Patent Document 1 discloses a method for improving magnesia purity, but it is not possible to reduce splash by simply improving magnesia purity. Further, although Patent Document 2 discloses that the content of impurity oxide is 0.5% by weight or less, it is not fully satisfactory.
さらに、磁性記録媒体の生産性向上を目的として、連続長時間の成膜や大きい成膜速度を確保するために電子ビーム強度を高めることがなされているが、電子ビーム強度を高めるほどスプラッシュが起こりやすくなることから、スプラッシュの発生が起こらない蒸着源用るつぼが求められている。また、加熱・冷却により、るつぼの体積変化によりクラックが発生し、耐久性に劣る問題もある。
本発明の目的は、耐久性が高く、スプラッシュを発生しないマグネシア焼結体を提供する点にある。 An object of the present invention is to provide a magnesia sintered body that has high durability and does not generate splash.
本発明は、前記のような現状を鑑みて鋭意研究を重ねてきた結果、マグネシア含有量だけでなく、ＣａＯ及びＳｉＯ２含有量、不純物量、かさ密度、結晶粒径をある特定の範囲内に制御することにより、スプラッシュの発生がなく、耐久性にすぐれたマグネシア焼結体を見出した。また同時に、スプラッシュの発生は結晶粒界強度が非常に大きな影響を及ぼしており、スプラッシュに対する抵抗性とサンドブラストテストによる摩耗体積とに非常に密接な関係があることも見出した。 In the present invention, as a result of intensive research in view of the current situation as described above, not only the magnesia content but also the CaO and SiO 2 content, the impurity content, the bulk density, and the crystal grain size are within a specific range. By controlling, the inventors have found a magnesia sintered body that is free from splash and has excellent durability. At the same time, it was also found that the occurrence of splash has a great influence on the grain boundary strength, and there is a very close relationship between the resistance to splash and the wear volume by the sandblast test.
即ち、本発明は、（ａ）マグネシアを９５重量％以上含有し、（ｂ）ＣａＯ及びＳｉＯ２を各々０．５〜２重量％含有し、（ｃ）不純物が１重量％以下であり、（ｄ）かさ密度が２．６ｇ／ｃｍ３以上であり、（ｅ）結晶粒径の累積分布曲線の５０％径が７０〜１５０μｍ、８０％径が２００〜３００μｍであることを特徴とするマグネシア焼結体に関する。 That is, the present invention comprises (a) 95% by weight or more of magnesia, (b) 0.5 to 2% by weight of CaO and SiO 2 , (c) 1% by weight or less of impurities, d) Magnesia firing characterized in that the bulk density is 2.6 g / cm 3 or more, and (e) the 50% diameter of the cumulative distribution curve of the crystal grain size is 70 to 150 μm, and the 80% diameter is 200 to 300 μm. Concerning union.
以下に本発明の耐久性にすぐれたマグネシア焼結体が充足すべき各要件について詳細に記載する。 Each requirement to be satisfied by the magnesia sintered body excellent in durability of the present invention will be described in detail below.
（ａ）マグネシアを９５重量％以上含有する点。
本発明においては、マグネシアを９５重量％以上、好ましくは９７重量％以上含有することが必要である。マグネシア含有量が９５重量％未満の場合は、不純物量が増加し、溶融した磁性金属中に溶けだし、表面に浮遊し、スプラッシュの原因となる。また、ガラス相や第２相が多く含有するので、耐熱性や耐食性の低下の原因となるので好ましくない。
(A) The point which contains magnesia 95weight% or more.
In the present invention, it is necessary to contain magnesia at 95% by weight or more, preferably 97% by weight or more. When the content of magnesia is less than 95% by weight, the amount of impurities increases, starts to dissolve in the molten magnetic metal, floats on the surface, and causes splash. Moreover, since it contains many glass phases and 2nd phases, it becomes a cause of the fall of heat resistance and corrosion resistance, and is unpreferable.
（ｂ）ＣａＯ及びＳｉＯ２を各々０．５〜２重量％含有する点。
本発明においてはＣａＯ及びＳｉＯ２を各々０．５〜２重量％含有することが必要で、とくにＣａＯを０．７〜１．５重量％、ＳｉＯ２を０．５〜１．２重量％含有することが好ましい。
ＣａＯ及びＳｉＯ２が共存し、各々の含有量が本願発明の範囲内とすることで焼結性の向上だけでなく、結晶粒界強度を大きくすることができ、その結果、耐熱性や耐食性の向上に寄与するだけでなく、粒子離脱が発生しにくくなり、スプラッシュの発生を抑制することができる。ＣａＯ及びＳｉＯ２が各々０．５重量％未満の場合は、焼結性の低下や結晶粒界強度の低下をきたすので好ましくなく、２重量％を超える場合にはその他の不純物と結晶粒界にガラス相や第２相を形成して、耐熱性や耐食性の低下だけでなく、溶融した磁性金属中に溶けて浮遊し、スプラッシュが発生しやすくなるので好ましくない。
(B) CaO and that it contains a SiO 2 respectively 0.5-2 wt%.
In the present invention, it is necessary to contain 0.5 to 2% by weight of CaO and SiO 2 respectively, especially 0.7 to 1.5% by weight of CaO and 0.5 to 1.2% by weight of SiO 2. It is preferable to do.
CaO and SiO 2 coexist, and by making each content within the scope of the present invention, not only the sinterability can be improved, but also the grain boundary strength can be increased. As a result, the heat resistance and corrosion resistance can be increased. In addition to contributing to the improvement, particle separation is less likely to occur and the occurrence of splash can be suppressed. When CaO and SiO 2 are each less than 0.5% by weight, it is not preferable because they cause a decrease in sinterability and a decrease in grain boundary strength. A glass phase or a second phase is formed, which not only lowers heat resistance and corrosion resistance, but also dissolves and floats in the molten magnetic metal, and splash is likely to occur.
（ｃ）不純物が１重量％以下である点。
不純物が１重量％以下、好ましくは０．８重量％以下であることが必要である。本発明での不純物とはマグネシア、ＣａＯ及びＳｉＯ２以外の成分を言うが、不純物が１重量％を超える場合には結晶粒界にガラス相や第２相を多く形成し、耐熱性や耐食性の低下だけでなく、溶融した磁性金属中に溶けて浮遊し、スプラッシュが発生しやすくなるので好ましくない。
(C) The impurity is 1% by weight or less.
It is necessary that the impurities be 1% by weight or less, preferably 0.8% by weight or less. The impurities in the present invention refer to components other than magnesia, CaO and SiO 2 , but when the impurities exceed 1% by weight, many glass phases and second phases are formed at the grain boundaries, and heat resistance and corrosion resistance are improved. This is not preferable because it is not only lowered, but also melts and floats in the molten magnetic metal and splash is likely to occur.
（ｄ）かさ密度が２．６ｇ／ｃｍ３以上である点。
本発明においては、かさ密度は２．６ｇ／ｃｍ３以上、好ましくは２．６５ｇ／ｃｍ３以上が必要である。かさ密度が２．６ｇ／ｃｍ３未満の場合は、焼結体に気孔が多く形成され、強度低下をきたすので好ましくない。なお、本発明では緻密には焼結させていないので、上限は２．８ｇ／ｃｍ３程度である。
(D) The bulk density is 2.6 g / cm 3 or more.
In the present invention, the bulk density is 2.6 g / cm 3 or more, preferably 2.65 g / cm 3 or more. When the bulk density is less than 2.6 g / cm 3 , many pores are formed in the sintered body and the strength is lowered, which is not preferable. In the present invention, since the sintering is not performed densely, the upper limit is about 2.8 g / cm 3 .
（ｅ）結晶粒径の累積分布曲線の５０％径が７０〜１５０μｍ、８０％径が２００〜３００μｍである点。
本発明においては結晶粒径の累積分布曲線（結晶粒径の累積分布曲線とは、測定した結晶粒径をある幅の粒径に区分し、その区分した粒径以上または粒径以下の結晶粒子量の総和の全粒子量に対する割合で示すことを言う。）の５０％径が７０〜１５０μｍ、８０％径が２００〜３００μｍ、好ましくは５０％径が８０〜１２０μｍ、８０％径が２１０〜２５０μｍであることが必要である。５０％径が７０μｍ未満の場合は、粒子離脱が起こりやすくなって、スプラッシュが発生しやすくなる。一方、１５０μｍを越える場合には焼結体強度が低くなるので好ましくない。８０％径が２００μｍ未満の場合は結晶粒径分布がシャープになり、結晶粒子の詰まりが悪くなり、結晶粒子の結合力が低下するので好ましくなく、３００μｍを越える場合には、逆に結晶粒径分布が広くなりすぎて焼結体組織の不均一性が低下して、スプラッシュの発生が起こりやすくなるので好ましくない。
(E) The 50% diameter of the cumulative distribution curve of crystal grain size is 70 to 150 μm, and the 80% diameter is 200 to 300 μm.
In the present invention, the cumulative distribution curve of crystal grain size (the cumulative distribution curve of crystal grain size is a crystal grain having a measured crystal grain size divided into a certain width and having a grain size greater than or less than the grain size. 50% diameter is 70 to 150 μm, 80% diameter is 200 to 300 μm, preferably 50% diameter is 80 to 120 μm, and 80% diameter is 210 to 250 μm. It is necessary to be. When the 50% diameter is less than 70 μm, particle detachment is likely to occur, and splash is likely to occur. On the other hand, when the thickness exceeds 150 μm, the strength of the sintered body is lowered, which is not preferable. If the 80% diameter is less than 200 μm, the crystal grain size distribution becomes sharp and the clogging of the crystal grains worsens, and the bonding force of the crystal grains decreases, which is not preferred. Since the distribution becomes too wide, the non-uniformity of the sintered body structure is lowered, and the occurrence of splash is likely to occur.
本発明においては結晶粒径及び累積分布曲線は下記の方法により測定する。
焼結体を真空中で十分に脱気し、その状態で樹脂を流し込んで、焼結体を樹脂中に埋め、固める。樹脂に埋め込んで固めた焼結体をラップ研磨し、鏡面にまで仕上げる。仕上げた焼結体を顕微鏡で１視野に結晶粒子が１００個以上観察できる倍率で観察し、写真撮影する。写真から画像解析により１個１個の結晶の面積を測定し、その値から等価円直径に換算し、換算した等価円直径に形状係数として１．７を乗じた値を結晶粒径とする。５００個、好ましくは１０００個の結晶粒径を上記方法により測定し、累積分布を取って、５０％粒径及び８０％粒径を求める。
In the present invention, the crystal grain size and the cumulative distribution curve are measured by the following methods.
The sintered body is sufficiently deaerated in a vacuum, and a resin is poured in that state, and the sintered body is embedded in the resin and hardened. The sintered body embedded in resin and hardened is lapped and finished to a mirror surface. The finished sintered body is observed with a microscope at a magnification at which 100 or more crystal particles can be observed in one field of view, and photographed. The area of each crystal is measured from the photograph by image analysis, converted to an equivalent circle diameter from the value, and a value obtained by multiplying the converted equivalent circle diameter by 1.7 as a shape factor is defined as a crystal grain size. The crystal grain size of 500, preferably 1000, is measured by the above method, and the cumulative distribution is taken to determine the 50% grain size and 80% grain size.
本発明の耐久性にすぐれたマグネシア焼結体は種々の方法で作製できるが、その一例を以下に示す。
マグネシア原料粉体は電融粉体を各粒度に粉砕された粉体を用い、純度は９９重量％以上、好ましくは９９．５重量％以上の粉体を用いる。ＣａＯ及びＳｉＯ２としては平均粒子径が５０μｍ以下で、ＣａＯ及びＳｉＯ２の純度が９９％重量以上の粉体を用いるが、酸化物だけでなく、炭酸塩、水酸化物の形態あるいはＣａＯとＳｉＯ２化合物の形態で用いることができる。目的とする結晶粒径となるように各粒度の粉体を混合し、さらに、所定の組成となるようにＣａＯ及びＳｉＯ２を添加混合し、水もしくは有機溶剤等の溶媒とバインダー（セルロース、ＰＶＡ等）の成形助剤を添加して成形用粉体とする。成形はプレス成形、スタンピング成形等の成形法により所望の形状に成形する。また、鋳込成形法を用いる場合は目的となる結晶粒径となるように各粒度のマグネシア粉体と所定の組成となるようにＣａＯ及びＳｉＯ２を配合し、溶媒、界面活性剤及びバインダーを添加してボールミルでスラリーを作製し、石膏型等の型を用いて上方鋳込成形、充填鋳込成形、振動鋳込成形等の方法により成形する。
得られた成形体を１４５０〜１７００℃、好ましくは１５００〜１６５０℃焼成により焼結体を得る。
Although the magnesia sintered compact excellent in durability of the present invention can be produced by various methods, an example thereof is shown below.
As the magnesia raw material powder, a powder obtained by pulverizing electrofused powder to each particle size is used, and a powder having a purity of 99% by weight or more, preferably 99.5% by weight or more is used. As CaO and SiO 2 , a powder having an average particle diameter of 50 μm or less and a purity of 99% by weight or more of CaO and SiO 2 is used. However, not only oxides but also carbonates, hydroxides, or CaO and SiO 2 are used. It can be used in the form of two compounds. Powders of various particle sizes are mixed so as to have a target crystal grain size, and CaO and SiO 2 are added and mixed so as to have a predetermined composition, and a solvent such as water or an organic solvent and a binder (cellulose, PVA). Etc.) is added to form a molding powder. The molding is performed in a desired shape by a molding method such as press molding or stamping molding. In addition, when using the casting method, magnesia powder of each particle size and CaO and SiO 2 are blended so as to have a predetermined composition so as to obtain a target crystal particle size, and a solvent, a surfactant and a binder are added. It is added and a slurry is produced by a ball mill, and then molded by a method such as upward casting, filling casting, vibration casting, etc. using a mold such as a plaster mold.
The obtained molded body is sintered at 1450 to 1700 ° C., preferably 1500 to 1650 ° C., to obtain a sintered body.
本発明の耐久性マグネシア焼結体は前述の実施例、比較例にかかる表１からも明らかなように、耐久性が高く、スプラッシュを発生しない。その性質を利用して金属溶解用、ノズル等の金属鋳造用やセッター、台板などの焼成用道具類としてすぐれた特性を発揮するだけでなく、金属蒸着用るつぼとしても有用である。 The durable magnesia sintered body of the present invention has high durability and does not generate splash, as is apparent from Table 1 according to the above-described Examples and Comparative Examples. Utilizing these properties, it not only exhibits excellent properties for metal melting, metal casting such as nozzles, and firing tools such as setters and base plates, but it is also useful as a crucible for metal deposition.
以下に実施例および比較例を挙げて、本発明を説明するが、本発明はこれにより何ら限定されるものでない。 Hereinafter, the present invention will be described with reference to examples and comparative examples, but the present invention is not limited thereto.
表１に示す配合重量比で、純度９９．５％の電融マグネシア原料の各粒度の粉体を混合したものをマグネシア原料粉体として用いた。この粉体に平均粒子径１０μｍでＣａＯ純度が９９．５重量％の炭酸カルシウム粉体及び平均粒子径が１０μｍでＳｉＯ２純度が９９．５重量％のケイ石を混合し、水及びバインダーを添加してプレス成形し、燃焼し、１００×１００×１５ｍｍの試料を得た。得られた焼結体特性を表２に示す。
得られた試料のスプラッシュに対する抵抗性を評価するため、サンドブラストによる摩耗特性を評価した。評価方法はブラストノズルと試料が８０゜となるように試料をブラストノズルから５０ｍｍの位置に置き、ブラスト粉体として３６メッシュの電融アルミナ粉体を１ｋｇ／分供給し、ブラストノズルへのエアー供給圧力を１．５ｋｇｆ／ｃｍ２とし、３０秒間ブラストテストし、下式よりブラスト摩耗体積を算出した。
In order to evaluate the resistance of the obtained sample to splash, the wear characteristics by sandblasting were evaluated. In the evaluation method, the sample is placed at a position 50 mm from the blast nozzle so that the sample is 80 ° and the blast nozzle is supplied with 1 kg / min of 36 mesh fused alumina powder as blast powder, and air is supplied to the blast nozzle. The pressure was set to 1.5 kgf / cm 2 , a blast test was performed for 30 seconds, and the blast wear volume was calculated from the following formula.
Claims (1)
(A) containing 95% by weight or more of magnesia, (b) containing 0.5 to 2% by weight of CaO and SiO 2 , (c) 1% by weight or less of impurities, and (d) a bulk density of 2 0.6 g / cm 3 or more, and (e) a magnesia sintered body characterized in that the 50% diameter of the cumulative distribution curve of crystal grain size is 70 to 150 μm and the 80% diameter is 200 to 300 μm.
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| JP2004124787A JP4532971B2 (en) | 2004-04-20 | 2004-04-20 | Magnesia sintered body with excellent durability |
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| JP4532971B2 true JP4532971B2 (en) | 2010-08-25 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4721947B2 (en) * | 2006-04-19 | 2011-07-13 | 株式会社ニッカトー | Corrosion-resistant magnesia sintered body, heat treatment member comprising the same, and method for producing the sintered body |
| JP2008133146A (en) * | 2006-11-27 | 2008-06-12 | Noritake Co Ltd | Support for firing solid electrolyte body, method for producing solid electrolyte body, and method for production of the support |
| KR100814855B1 (en) | 2007-02-21 | 2008-03-20 | 삼성에스디아이 주식회사 | Sintered magnesium oxide, and plasma display panel prepared therefrom |
| KR100839423B1 (en) | 2007-02-21 | 2008-06-19 | 삼성에스디아이 주식회사 | Sintered magnesium oxide, and plasma display panel prepared therefrom |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59190218A (en) * | 1983-04-12 | 1984-10-29 | Ube Kagaku Kogyo Kk | High-density magnesia clinker and its preparation |
| JPS6183654A (en) * | 1984-09-27 | 1986-04-28 | 新日本化学工業株式会社 | Magnesia clinker and manufacture |
| JPS61132557A (en) * | 1984-11-29 | 1986-06-20 | 新日本化学工業株式会社 | Magnesia sintered body |
| JPH01270564A (en) * | 1988-04-18 | 1989-10-27 | Kurosaki Refract Co Ltd | Dense magnesia carbon brick |
| JPH03250504A (en) * | 1990-02-28 | 1991-11-08 | Shin Nippon Kagaku Kogyo Co Ltd | High temperature electric insulating filler and sheath heater filled therewith |
| JPH0867552A (en) * | 1994-06-22 | 1996-03-12 | Mitsubishi Materials Corp | Magnesia-titania refractory and its production |
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2004
- 2004-04-20 JP JP2004124787A patent/JP4532971B2/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59190218A (en) * | 1983-04-12 | 1984-10-29 | Ube Kagaku Kogyo Kk | High-density magnesia clinker and its preparation |
| JPS6183654A (en) * | 1984-09-27 | 1986-04-28 | 新日本化学工業株式会社 | Magnesia clinker and manufacture |
| JPS61132557A (en) * | 1984-11-29 | 1986-06-20 | 新日本化学工業株式会社 | Magnesia sintered body |
| JPH01270564A (en) * | 1988-04-18 | 1989-10-27 | Kurosaki Refract Co Ltd | Dense magnesia carbon brick |
| JPH03250504A (en) * | 1990-02-28 | 1991-11-08 | Shin Nippon Kagaku Kogyo Co Ltd | High temperature electric insulating filler and sheath heater filled therewith |
| JPH0867552A (en) * | 1994-06-22 | 1996-03-12 | Mitsubishi Materials Corp | Magnesia-titania refractory and its production |
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| JP2005306652A (en) | 2005-11-04 |
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