JPH0214874A - Production of alumina ceramic - Google Patents
Production of alumina ceramicInfo
- Publication number
- JPH0214874A JPH0214874A JP1131495A JP13149589A JPH0214874A JP H0214874 A JPH0214874 A JP H0214874A JP 1131495 A JP1131495 A JP 1131495A JP 13149589 A JP13149589 A JP 13149589A JP H0214874 A JPH0214874 A JP H0214874A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- mgo
- zro2
- compound
- firing
- 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.)
- Granted
Links
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 34
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 8
- 150000003755 zirconium compounds Chemical class 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- -1 aluminum compound Chemical class 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 18
- 238000010304 firing Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000003980 solgel method Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052593 corundum Inorganic materials 0.000 abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 9
- 238000001354 calcination Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract 2
- 150000001399 aluminium compounds Chemical class 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000000395 magnesium oxide Substances 0.000 description 24
- 239000002245 particle Substances 0.000 description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical group [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 150000001339 alkali metal compounds Chemical class 0.000 description 4
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- WNZPMZDPEDYPKZ-UHFFFAOYSA-M [OH-].[O--].[Y+3] Chemical compound [OH-].[O--].[Y+3] WNZPMZDPEDYPKZ-UHFFFAOYSA-M 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
本発明は新規な組成のアルミナ磁器の製造方法に関する
ものであり、特に螢光体等の焼成用容器として、また透
光性に優れた性質を有する改良されたアルミナ磁器の製
造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing alumina porcelain with a novel composition, and in particular, to an improved alumina porcelain that has excellent translucency and can be used as a container for firing phosphors, etc. Relating to a manufacturing method.
アルミナ磁器は機械的強度及び耐蝕性が大きく、更に透
光性を有する等の優れた素材であるので、各種用途に使
用されている。Alumina porcelain is an excellent material that has high mechanical strength and corrosion resistance, and also has translucency, so it is used for various purposes.
螢光体製造の分野においても原料を焼成する際の容器（
ルツボ）としてアルミナ磁器が使用されている。ところ
で、螢光体は一般に母体構成原料、付活剤構成原料及び
融剤を混合し、これを焼成することによって製造される
。In the field of phosphor manufacturing, containers (
Alumina porcelain is used as a crucible. Incidentally, a phosphor is generally manufactured by mixing a base material, an activator material, and a flux, and firing the mixture.
ここで、融剤としては一般に原料全体の約２゜〜８０重
量％のアルカリ金属化合物及び／又はアルカリ土類金属
化合物が用いられる。この様な螢光体製造において、ア
ルミナ磁器ルツボを繰り返し使用すると、殆どの場合数
回で割れてしまう。Here, as a fluxing agent, an alkali metal compound and/or alkaline earth metal compound is generally used in an amount of about 2 to 80% by weight of the total raw materials. When an alumina porcelain crucible is used repeatedly in the production of such a phosphor, it almost always breaks after a few times.
その原因としては、ルツボ内壁部のアルミナ（α−Ａｔ
□０．）が螢光体原料の融剤中のアルカリ金属及び／又
はアルカリ土類金属と反応してβ−ＡＩＩＯ，に変化し
てルツボ外壁部のアルミナとは相の異なるものとなり、
その結果熱膨張係数に差が生じ、従って高温焼成及び冷
却の繰り返しにおいて歪を生じるためと考えられる。The cause of this is that the alumina (α-At
□0. ) reacts with the alkali metal and/or alkaline earth metal in the flux of the phosphor raw material and changes into β-AIIO, which has a different phase from the alumina on the outer wall of the crucible,
As a result, a difference occurs in the coefficient of thermal expansion, which is thought to cause distortion during repeated high-temperature firing and cooling.
これを防止するために、従来Ａｌ２Ｏ３に微量のＭｇＯ
、Ｔｉｅ、、ＣａＯあるいはＬａ２’ｓ 、 Ｙ２Ｏ３
、Ｅｒ２０ａ等の希土類元素酸化物を単独であるいは混
合して添加することが行われていたが、この様な従来の
添加剤を含むアルミナルツボを用いた場合でも、上記の
如きアルカリ金属化合物及び／又はアルカリ土類金属化
合物を大量に含む原料を焼成する螢光体製造においては
、破損する迄の繰り返し使用回数は依然として少ない。To prevent this, conventionally a trace amount of MgO was added to Al2O3.
, Tie, , CaO or La2's, Y2O3
, Er20a, and other rare earth element oxides have been added singly or in combination, but even when using an alumina crucible containing such conventional additives, the above-mentioned alkali metal compounds and/or Alternatively, in the production of phosphors in which raw materials containing large amounts of alkaline earth metal compounds are fired, the number of repeated uses before breakage is still small.
そこで、本発明者は、螢光体製造の如き大量のアルカリ
金属化合物及び／又はアルカリ土類金属化合物との接触
下での高温焼成においても十分な機械的強度及び耐蝕性
をもち、多数回の繰り返し使用に耐えるアルミナ磁器を
製造すべ（種々検討の結果、特定の２種の添加剤を特定
割合で特定量混合することにより目的が達成されること
を見出した。Therefore, the present inventor has developed a method that has sufficient mechanical strength and corrosion resistance even in high-temperature firing in contact with large amounts of alkali metal compounds and/or alkaline earth metal compounds, such as in the production of phosphors, and that can be used multiple times. To produce alumina porcelain that can withstand repeated use.As a result of various studies, it was discovered that this objective could be achieved by mixing two specific types of additives in specific amounts in specific proportions.
即ち、本発明は、ＭｇＯ粉末、−焼成によりＭｇＯに変
化し得るマグネシウム化合物、ＺｒＯ７粉末、焼成によ
りＺｒＯ□に変化し得るジルコニウム化合物、ＭｇＯ・
ＺｒＯ２焼結体粉末、Ａｌ２Ｏ３粉末、焼成によりＡｌ
２Ｏ．に変化し得るアルミニウム化合物の中からアルミ
ニウム化合物、マグネシウム化合物及びジルコニウム化
合物を選択し、マグネシウム化合物及びジルコニウム化
合物の重量比がＭｇＯ及びＺｒＯ□換算で２＝８〜７：
３であり、且つその合計量がＡｌ２Ｏ．に対し０．１〜
０．６５重量％である量を秤量し、これらを混合し、焼
成することを特徴とするアルミナ磁器の製造方法である
。That is, the present invention provides MgO powder, a magnesium compound that can be converted to MgO by firing, a ZrO7 powder, a zirconium compound that can be converted to ZrO□ by firing, and MgO.
ZrO2 sintered body powder, Al2O3 powder, Al by firing
2O. An aluminum compound, a magnesium compound, and a zirconium compound are selected from aluminum compounds that can be changed into
3, and the total amount is Al2O. 0.1~
This method of producing alumina porcelain is characterized by weighing out 0.65% by weight, mixing them, and firing them.
本発明のアルミナ磁器の製造方法は、常法に従いＭｇＯ
粉末及びＺｒＯ２粉末をＡｌｌ０Ｉ粉末と混合して分散
せしめ、これを成形後焼成することによって実施される
。ＭｇＯ粉末及びＺｒＯｚ粉末はそれぞれ単、独の粉末
としてＡｌｔａｓ粉末に添加してもよいし。The method for manufacturing alumina porcelain of the present invention is carried out using MgO
This is carried out by mixing and dispersing the powder and ZrO2 powder with the AllIOI powder, molding the mixture, and then firing it. The MgO powder and the ZrOz powder may be added to the Altas powder as separate powders.
また予めＭｇＯ粉末とＺｒＯ□粉末とを適宜の割合で混
合し、焼結し、その後粉砕した焼結体粉末をＡＩＪｎ粉
末に添加してもよい、 Ａ１．Ｏ，粉末は一般に０．１
〜５μの平均粒径のものが使用され、ＭｇＯ粉末は平均
粒径０．５〜２μのものが、ＺｒＯｉ粉末は平均粒径０
．４〜３μのものが、またＭｇ０４ｒＯ□焼結体粉末は
平均粒径０．５〜３μのものが使用される。尚、Ａ１１
ａｓ 、ＭｇＯ及びＺｒＯｚの代わりに、焼成によりこ
れらに変化し得るもの、たとえばＡ１． Ｍｇ及びＺｒ
の硫酸塩、硫化物又は塩化物等を用いることもできる。Alternatively, MgO powder and ZrO□ powder may be mixed in an appropriate ratio in advance, sintered, and then pulverized sintered body powder may be added to the AIJn powder. A1. O, powder is generally 0.1
An average particle size of ~5μ is used, MgO powder has an average particle size of 0.5 to 2μ, and ZrOi powder has an average particle size of 0.
．． Mg04rO□ sintered powder has an average particle size of 0.5 to 3μ. Furthermore, A11
as , MgO and ZrOz, those which can be converted into these by calcination, such as A1. Mg and Zr
It is also possible to use sulfates, sulfides, chlorides, and the like.
本発明のアルミナ磁器の製造方法においては、原料であ
るＭｇＯ粉末、ＺｒＯ□粉末及びＭｇＯ・ＺｒＯ□焼結
体粉末の平均粒径はＡｌ２Ｏ．の平均粒径の０．５〜２
倍であることが好ましく、これによりＡｌａＯｓ中への
添加剤の分散の均一性が高められ、焼結密度等の諸特性
の向上に役立つ。In the method for producing alumina porcelain of the present invention, the average particle diameter of the raw materials MgO powder, ZrO□ powder, and MgO.ZrO□ sintered body powder is Al2O. 0.5 to 2 of the average particle size of
It is preferable that the amount is twice as high as that of the sintered material, thereby increasing the uniformity of dispersion of the additive into the AlaOs, which is useful for improving various properties such as sintered density.
また、これら原料の粒度分布はできるだけシャープであ
ることが磁器の耐久性向上に役立つので好ましい。均一
な粒度をもつ原料の製造にはゾルゲル法と称される新し
い方法を用いることが好ましい。ゾルゲル法とは、例え
ば金属のアルコキシドを調製し、これを加水分解して解
膠することによりゾルを形成し、これをゲル化する方法
である。ここで、ゲル化の際にゾルを非水溶媒中にオリ
フィスから滴下させ、これを乾燥せしめることにより粒
度分布の良好なゲルを得ることができる。例えば、アル
ミナのゲルを得るためには、アルミニウムイソプロポキ
シドを加水分解し、塩酸を添加して解膠し、このゾルを
オリフィスからヘキサン中に滴下し、撹拌し、乾燥する
。得られるゲルの粒度は撹拌速度によりコントロールで
きる。同様にＭｇＯ及びＺｒＯ□についてもゾルゲル法
により所望の均一な粒径のものを得ることができる。Further, it is preferable that the particle size distribution of these raw materials be as sharp as possible, since this will help improve the durability of the porcelain. Preferably, a new method called sol-gel method is used to produce raw materials with uniform particle size. The sol-gel method is a method in which, for example, a metal alkoxide is prepared, hydrolyzed and peptized to form a sol, and the sol is turned into a gel. Here, during gelation, a gel with a good particle size distribution can be obtained by dropping the sol into a nonaqueous solvent from an orifice and drying it. For example, to obtain an alumina gel, aluminum isopropoxide is hydrolyzed, hydrochloric acid is added to peptize the sol, and the sol is dropped into hexane through an orifice, stirred, and dried. The particle size of the resulting gel can be controlled by the stirring speed. Similarly, MgO and ZrO□ can also be obtained with desired uniform particle diameters by the sol-gel method.
以上の如き本発明の製造方法によって得られたアルミナ
磁器は、大結晶粒子を含まず、密度が高く、アルカリ金
属化合物及びアルカリ土類金属化合物に対する耐蝕性が
良好であり、螢光体製造用ルツボとして使用した場合に
も従来のルツボに比較して極めて多数回の使用に耐える
。The alumina porcelain obtained by the production method of the present invention as described above does not contain large crystal grains, has high density, has good corrosion resistance against alkali metal compounds and alkaline earth metal compounds, and is suitable for use in crucibles for producing phosphors. Even when used as a crucible, it can withstand much more use than conventional crucibles.
本発明のもう一つの局面は、ＭｇＯ及びｚｒＯｘを重量
比２：８〜７：３にて含み、その合計量がＡｌ２Ｏ３に
対し０．１〜０．６５重量％であるＡ１２０ｉ、ＭｇＯ
及びＺｒＯ２からなる混合物を水素雰囲気中で焼成する
ことを特徴とする透光性アルミナ磁器の製造方法である
。このように水素雰囲気中で焼成を行なうと透光性焼成
焼結体が得られ、これはアルカリ金属蒸気にもおかされ
ないためナトリウムランプ等のアルカリ金属蒸気放電灯
の発光管として使用可能である。Another aspect of the invention is an A120i, MgO containing MgO and zrOx in a weight ratio of 2:8 to 7:3, the total amount of which is 0.1 to 0.65% by weight relative to Al2O3.
and ZrO2 is fired in a hydrogen atmosphere. By performing firing in a hydrogen atmosphere in this manner, a translucent fired sintered body is obtained, which is not affected by alkali metal vapor and can therefore be used as an arc tube for an alkali metal vapor discharge lamp such as a sodium lamp.
以下、実施例により本発明を説明する。The present invention will be explained below with reference to Examples.
実施例１
平均粒子径０．３μの純度９９．８％のα−Ａ１２０ｍ
、ならびに平均粒子径０．５μのＭｇＯ１ＺｒＯ□及び
ＭｇＯ・ＺｒＯ□焼結体をそれぞれの添加量を変化させ
、十分に分散混合しスプレードライヤーで乾燥後、ラバ
ープレス（１５００ｋｇ／ ｃｍ”）で内径５０ｍｍ、
高さ５０ｍｍの円筒形に成形し、１６５０℃で２時間焼
結してアルミナ磁器ルツボを製造した。Example 1 α-A120m with an average particle size of 0.3μ and a purity of 99.8%
, and MgO1ZrO□ and MgO・ZrO□ sintered bodies with an average particle size of 0.5 μ were varied in their respective addition amounts, sufficiently dispersed and mixed, dried with a spray dryer, and then dried with a rubber press (1500 kg/cm”) to an inner diameter of 50 mm. ,
It was molded into a cylindrical shape with a height of 50 mm and sintered at 1650° C. for 2 hours to produce an alumina porcelain crucible.
このルツボ中にて螢光体の焼成を行うために、螢光体の
母体構成原料二酸化イツトリウム（平均粒径３μ）、付
活剤原料：酸化ユーロピウム、融剤；炭酸ナトリウム及
び炭酸カリウムを従来の組成比にて調合し、十分混合し
たものを装入した。In order to fire the phosphor in this crucible, yttrium dioxide (average particle size 3 μm), the base material of the phosphor, europium oxide, an activator material, and sodium carbonate and potassium carbonate as a flux were used in the conventional manner. The mixture was prepared according to the composition ratio, and the mixture was thoroughly mixed and charged.
これを１１００℃の温度で２時間焼成した。この焼成を
ルツボが割れる迄繰り返し行った。This was baked at a temperature of 1100° C. for 2 hours. This firing process was repeated until the crucible cracked.
ルツボの各組成における焼結密度と繰り返し使用回数と
を表−１に示す。Table 1 shows the sintered density and number of repeated uses for each composition of the crucible.
Ａｌ２Ｏ３に対するＭｇＯ＋ＺｒＯ２の添加量が０，３
重量％である場合のＭｇＯ／ ＺｒＯ□（重量比）と繰
り返し使用回数（回）との関係を図示すると第１図のよ
うになる。また、ＭｇＯ／ＺｒＯ□の重量比が５０１５
０である場合のＡｌ２Ｏ３に対するＭｇＯ＋ＺｒＯ２の
添加量（重量％）と繰り返し使用回数（回）との関係を
図示すると第２図のようになる。第１図から明らかなよ
うに、顕著な効果の達成されるＭｇＯ／ＺｒＯ□（重量
比）の範囲は２：８〜７：３である。The amount of MgO+ZrO2 added to Al2O3 is 0.3
The relationship between MgO/ZrO□ (weight ratio) and the number of times of repeated use (times) in terms of weight % is shown in FIG. In addition, the weight ratio of MgO/ZrO□ is 5015
The relationship between the amount of MgO+ZrO2 added to Al2O3 (weight %) and the number of times of repeated use (times) in the case of 0 is shown in FIG. As is clear from FIG. 1, the range of MgO/ZrO□ (weight ratio) in which significant effects are achieved is from 2:8 to 7:3.
また、第２図から明らかなように、顕著な効果の達成さ
れるＡｌ２Ｏ．に対するＭｇＯ＋ ＺｒＯ□の添加量（
重量％）は０．１〜０．６５である。Moreover, as is clear from FIG. 2, Al2O. Amount of MgO + ZrO□ added to (
weight%) is 0.1 to 0.65.
実施例２
市販のアルミニウムイソプロポキシド番こ水を加えて加
水分解した後、塩酸を０．２モル添加して７０℃で７日
間かけて解膠を行い、これを無水ヘキサン中に０．１ｍ
ｍ径のオリフィスより滴下し、強力に撹拌することによ
り平均粒子径０．３μの透明なアルミナを得た。同様に
してマグネシウムとジルコニウムのインプロポキシドか
らそれぞれゾルを調製し、ゲル化させた。それぞれ０．
３μ及び０．５μの平均粒子径を有する透明体であった
。Example 2 Commercially available aluminum isopropoxide was hydrolyzed by adding diluted water, then peptized by adding 0.2 mol of hydrochloric acid at 70°C for 7 days, and 0.1 mol of this was added to anhydrous hexane.
Transparent alumina with an average particle size of 0.3 μm was obtained by dropping the solution through an orifice with a diameter of m and stirring vigorously. Sols of magnesium and zirconium impropoxide were prepared in the same manner and gelatinized. 0 each.
They were transparent bodies with average particle diameters of 3μ and 0.5μ.
上記アルミナに対しそれぞれ０．１５重重量の上記酸化
マグネシウム及び酸化ジルコニウムを添加し、乾燥後、
実施例１におけると同様な成形体とし、１３００℃で焼
成して透明な焼結体（ルツボ）を得た。この時の焼結密
度は３．９６であった。0.15 weight of each of the above magnesium oxide and zirconium oxide was added to the above alumina, and after drying,
A molded body similar to that in Example 1 was prepared and fired at 1300° C. to obtain a transparent sintered body (crucible). The sintered density at this time was 3.96.
このルツボを使用して実施例１と同様な螢光体焼成繰り
返しテストを行ったところ、３５回をすぎても何ら変化
がなかった。When this crucible was used to perform a repeated phosphor firing test similar to that in Example 1, no change was observed even after 35 times.
第１図は本発明の製造方法によって得たアルミナ磁器に
おけるＭｇＯ／ ＺｒＯａ （重量比）と繰り返し使用
回数（回）との関係を示すグラフである。
第２図は本発明の製造方法によって得たアルミナ磁器に
おけるＡｌ２Ｏ３に対するＭｇＯ＋ ＺｒＯ□の添加量
（重量％）と繰り返し使用回数（回）との関係を示すグ
ラフである。
第
図
Ｍ９０／ＺｒＯ２ｆｔ’ｇ＞ｃ）
第
図FIG. 1 is a graph showing the relationship between MgO/ZrOa (weight ratio) and the number of repeated uses (times) in alumina porcelain obtained by the manufacturing method of the present invention. FIG. 2 is a graph showing the relationship between the amount of MgO+ZrO□ added to Al2O3 (wt%) and the number of times of repeated use (times) in alumina porcelain obtained by the manufacturing method of the present invention. Fig. M90/ZrO2ft'g>c) Fig.
Claims (4)
ネシウム化合物、ＺｒＯ＿２粉末、焼成によりＺｒＯ＿
２に変化し得るジルコニウム化合物、ＭｇＯ・ＺｒＯ＿
２焼結体粉末、Ａｌ＿２Ｏ＿３粉末、焼成によりＡｌ＿
２Ｏ＿３に変化し得るアルミニウム化合物の中からアル
ミニウム化合物、マグネシウム化合物及びジルコニウム
化合物を選択し、マグネシウム化合物及びジルコニウム
化合物の重量比がＭｇＯ及びＺｒＯ＿２換算で２：８〜
７：３であり、且つその合計量がＡｌ＿２Ｏ＿３に対し
０．１〜０．６５重量％である量を秤量し、これらを混
合し、焼成することを特徴とするアルミナ磁器の製造方
法。(1) MgO powder, magnesium compound that can be converted to MgO by firing, ZrO_2 powder, ZrO_2 powder by firing
Zirconium compound that can be changed into 2, MgO・ZrO_
2 sintered body powder, Al_2O_3 powder, Al_
An aluminum compound, a magnesium compound, and a zirconium compound are selected from aluminum compounds that can be converted into 2O_3, and the weight ratio of the magnesium compound and zirconium compound is 2:8 to 2:8 in terms of MgO and ZrO_2.
7:3, and the total amount thereof is 0.1 to 0.65% by weight based on Al_2O_3. A method for producing alumina porcelain, comprising weighing, mixing, and firing.
とする特許請求の範囲第１項記載のアルミナ磁器の製造
方法。(2) The method for manufacturing alumina porcelain according to claim 1, wherein the firing is performed in a hydrogen atmosphere.
特許請求の範囲第１項記載のアルミナ磁器の製造方法。(3) The method for producing alumina porcelain according to claim 1, wherein the firing is performed in the atmosphere.
なくとも１種がゾルゲル法を用いて造られたものである
ことを特徴とする特許請求の範囲第（１）項、第（２）
項又は第（３）項記載のアルミナ磁器の製造方法。(4) Claims (1) and (2) characterized in that at least one of the above Al_2O_3, MgO and ZrO_2 is produced using a sol-gel method.
The method for producing alumina porcelain according to item (3) or item (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1131495A JPH0214874A (en) | 1989-05-26 | 1989-05-26 | Production of alumina ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1131495A JPH0214874A (en) | 1989-05-26 | 1989-05-26 | Production of alumina ceramic |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP56162823A Division JPS5864262A (en) | 1981-10-14 | 1981-10-14 | Alumina ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0214874A true JPH0214874A (en) | 1990-01-18 |
| JPH0448749B2 JPH0448749B2 (en) | 1992-08-07 |
Family
ID=15059339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1131495A Granted JPH0214874A (en) | 1989-05-26 | 1989-05-26 | Production of alumina ceramic |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0214874A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5172169A (en) * | 1990-04-09 | 1992-12-15 | Ricoh Company, Ltd. | Developer carrier of a developing device and a method of producing the same |
| US5315061A (en) * | 1989-10-13 | 1994-05-24 | Ricoh Company, Ltd. | Developing apparatus using a developer carrier capable of forming microfields |
| WO2018223544A1 (en) * | 2017-06-09 | 2018-12-13 | 深圳市光峰光电技术有限公司 | Luminous ceramic and preparation process thereof |
| WO2020045432A1 (en) * | 2018-08-29 | 2020-03-05 | 京セラ株式会社 | Electrostatic chuck and method for manufacturing electrostatic chuck |
-
1989
- 1989-05-26 JP JP1131495A patent/JPH0214874A/en active Granted
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5315061A (en) * | 1989-10-13 | 1994-05-24 | Ricoh Company, Ltd. | Developing apparatus using a developer carrier capable of forming microfields |
| US5451713A (en) * | 1989-10-13 | 1995-09-19 | Ricoh Company, Ltd. | Developing apparatus using a developer carrier capable of forming microfields |
| US5172169A (en) * | 1990-04-09 | 1992-12-15 | Ricoh Company, Ltd. | Developer carrier of a developing device and a method of producing the same |
| WO2018223544A1 (en) * | 2017-06-09 | 2018-12-13 | 深圳市光峰光电技术有限公司 | Luminous ceramic and preparation process thereof |
| WO2020045432A1 (en) * | 2018-08-29 | 2020-03-05 | 京セラ株式会社 | Electrostatic chuck and method for manufacturing electrostatic chuck |
| KR20210011408A (en) * | 2018-08-29 | 2021-02-01 | 교세라 가부시키가이샤 | Electrostatic chuck and manufacturing method of electrostatic chuck |
| CN112534565A (en) * | 2018-08-29 | 2021-03-19 | 京瓷株式会社 | Electrostatic chuck and method for manufacturing electrostatic chuck |
| JPWO2020045432A1 (en) * | 2018-08-29 | 2021-08-26 | 京セラ株式会社 | Manufacturing method of electrostatic chuck and electrostatic chuck |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0448749B2 (en) | 1992-08-07 |
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