CN1005335B - 气密烧结半透明铝的氧化物 - Google Patents

气密烧结半透明铝的氧化物 Download PDF

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CN1005335B
CN1005335B CN86105927.1A CN86105927A CN1005335B CN 1005335 B CN1005335 B CN 1005335B CN 86105927 A CN86105927 A CN 86105927A CN 1005335 B CN1005335 B CN 1005335B
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erbium
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oxide
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彼得·罗伯特·普鲁多姆·范赖恩
杰拉达斯·亨里克斯·玛丽亚·西伯斯
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Koninklijke Philips NV
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Abstract

本发明涉及具有含量至少为９９．５％的气密烧结半透明的铝的氧化物，其中包含按重量计至多为１０００ｐｐｍ的氧化镁。按本发明所述铝的氧化物中也包含按重量计至少为２０ｐｐｍ至按重量计至多为２００ｐｐｍ以三氧化二铒表示的铒。所获得的材料具有较大的机械强度，较高的抗钠的侵袭及令人满意的半透明度。因此，该材料极适合于用作高压放电灯管的放电容器的器壁材料。

Description

气密烧结半透明铝的氧化物
本发明关于气密烧结半透明的铝的氧化物，其含量至少为99.5%并含按重量计至多为1000ppm的氧化镁。本发明还涉及由这种材料制造制品的方法，这种材料在美国专利第3，905，845中可知的。该已知材料是气密的、高度半透明的、尤其广泛地应有于高压放电灯管的放电容器中。除氧化镁外，为获得具有令人满意的含量和有规则晶体大小分布的烧结材料，还须在材料中加入三氧化二钇（Y2O3）及三氧化二镧（La2O3）。然而由于添加三氧化二钇及三氧化二镧会导致产生β铝酸盐晶体结构，此种结构会严重地影响材料的耐用性。特别是该材料制成放电容器的器壁情况里，在该容器又装有钠时，发现β铝酸盐结构极易为钠所侵袭。
作为本发明的目的是提供一种方法来获取具有有规则晶体大小分布但不具有β铝酸盐结构的气密烧结半透明铝的氧化物。
为此目的，按本发明的本文开头的段落中所述的那种材料，其特征在于所述的铝的氧化物中也包含以三氧化二铒（Er2O3）表示的、其含量按重量计至少为20ppm但至多为200ppm的铒。
按本发明所述的材料具有有规则的晶体大小分布且在烧结形式下是高度半透明的。此外，发现该材料在抗钠的侵袭方面极为耐用。所述材料的优点特别在于材料中钙杂质是分凝在铒钙铝酸盐的晶界周围。进而证实铒钙结构不属β型，该非β型对于抗钠侵袭的耐用性具有良好的效果。据此，按本发明所述的材料特别适宜用作高压放电灯管的放电容器的器壁材料。
铒的含量按重量计低于20ppm时，其结果会使所述材料具有无规则的晶体大小分布;特别是在材料的表面呈粗晶状并呈多孔。其原因是烧结时氧化镁由材料的表面蒸发掉，导致发生了不受限制的晶体生长。
当铒的含量高于为获取有规则的晶体大小分布所需的含量时，则发现会导致发生无规则的晶体生长。曾经发现，铒的含量高于200ppm，即使在极为有利的条件下，仍发生无规则的晶粒生长，其结果甚至导致发生二次结晶化现象。由此导致材料的含量及半透明程度皆受到非常不利的影响。
从文献（室业协会志Yogyo-Kyokai-Shi87卷第12期1979，633-641页，88卷第11期，1980，660-673页;88卷，第9期，531-538）中已知铝的氧化物烧结过程中三氧化二铒是作为掺杂剂而加入的。但是，该文献中所述在任何情况下，其相关的量均为按重计500ppm或以上。可是，在那样高铒浓度的情况下，气密半透明铝的氧化物实事上是不可能形成的。
按本发明所述的材料的一个较好的实施方案中氧化镁的含量按重量计要低于500ppm。其中的铒的含量以三氧二铒表示，其含铒量按重量计至多为130ppm。此材料之优点在于它是坚硬的、均匀的、气密的、也是半透明的，同时还具有高的抗钠侵袭的耐用性。少量的氧化镁已证实对材料的耐用性是有利的。可能用于解释这一事实是没有发生含镁的第二相分离现象。三氧化二铒所促进的均匀的晶体大小分布，不管氧化镁的含量的那么小，仍然也可以在材料中实现的。
按本发明所述的气密烧结半透明铝的氧化物的制品最好是这样按一种方法制造，该方法的特征在于：将氧化镁化合物加到三氧化二铝的混合物粉中;将所获得的三氧化二铝粉末最好是在经过瓦解作用后，制成所需形状的模坯件，然后，在1150℃与1400℃温度之间的氧化气氛下加热;接着，将所需要的三氧化二铒的量加到模坯件中，其方法是将模坯件浸渍在含铒的溶液中;再其后，将模坯件在氢气或在至多为0.13帕的压强的真空中，温度至多为1800℃的条件下烧结。
所述含铒溶液以乙酰丙酮铒的醇溶液为最好。所述溶液的优点在于：此溶液极易制备;浸渍于此溶液中模坯件可达到合理的可重复制造性结果。其优点还在于：在此方法中，加在模坯件的三氧化铒的含量可用简单的方式加以改变，即一方面可通过改变浸渍的时间而另一方面也可通过改变溶液中铒的浓度来实现。
实例
用经过瓦解作用的、纯度为99.99%的、比表面积为6平方米1克的三氧化二铝为原料制造一定数量的柱形管。在制备捏合材料时将掺杂剂氧化镁加入其中。通过挤压机制出柱形管后，于空气中在1280℃里将柱形管烘烤。然后将所获得柱形管浸渍在乙酰丙酮铒的醇溶液中。通过改变乙酰丙酮铒浓度以及浸渍的时间而获得不同铒掺杂剂含量的柱形管。其后，将各管进行烧结成半透明的气密管。烧管的管壁厚度为6毫米。对所获各管的各种性质进行测定。下表列出不同制品的不同组分和性质。
在标题为G最大及G宝石的纵栏内，分别表示最大晶体大小和平均晶体大小，均用微米作单位，晶体大小的数值是用电子显微镜测定的。
机械强度是在以δf为标题的纵栏内表示，其单位为百万牛顿/平方米，这用环形测定法确定其数值。半透明的程度是通过直线光线传播测定法来确定其数值，其结果列于标题为RLD的纵栏内，它是用相对测量所获得结果来表示的。各管在氢气气氛及温度为1750℃条件下烧结5小时。
对一些管的钠渗透深度是通过如下确定：将所述的管排列放置于钼质容器中，在该容器中也放置汞齐，所述汞齐按重量计包含30%的钠，并将之在1100℃加热100小时，其结果，管子显示出抛光的和受侵蚀的截面，然后应用微谱分析法测出钠渗透入晶体中的渗透深度。
编号为2号至6号管含有本发明的铝的氧化物，作为对比的不含铒的管编为1号，而含过高铒含量的管编为7号。2号管至6号管具有有规则晶体大小分布。2号管至6号管的平均晶体大小则小于1号管及7号管的晶体大小，从而说明了2号管至6号管的半透明度的值低于1号管及7号管的原因所在。相反，2号管至6号管之机械强度则远较1号管及7号管为大。
1号和、3号管及4号管的钠渗透深度用上述方法确定。其结果显示1号管的钠渗透深度大于250微米，而且可观察到整个管壁厚度上晶体边界有受侵袭的现象。至于3号管及4号管钠渗透深度分别为60及50微米，并且两者都没有观察到在晶体边界有特别受侵袭的现象。
表
序 氧按 三按 G G δf PLD 钠
化重 氧重 最大 宝石 渗
号 镁量 化量 微 最 透
计 二计 米 大 深
% 铒% 度
1 300 0 ＞300 20 135 157 ＞250微米晶体大
小整个器壁厚度
2 300 20 35 12 296 138
3 300 50 35 12 296 122 60微米具优良的
晶体边界
4 300 125 100 18 238 142 50微米具优良
的晶体边界
5 1000 20 35 12 322 131
6 1000 50 60 14 251 125
7 1000 390 150 30 187 167

Claims (4)

1、气密烧结半透明铝的氧化物，其含量至少为99.5%，并含按重量计至多为1000ppm的氧化镁，其特征在于所述铝的氧化物也包含其含量以三氧化二铒表示的按重量计至少为20ppm至按重量计至多为200ppm的铒。
2、按权利要求1所述的铝的氧化物，其特征在于所述氧化镁的含量按重量计为小于500ppm，而以三氧化二铒表示的铒的含量按重量计至多为130ppm。
3、一种由权利要求1或2所述的铝的氧化物制造制品的方法，其特征在于将氧化镁的化合物加到三氧化二铝的混合物粉末中，将所获得的三氧化二铝粉末最好是在经过瓦解作用后，制成所需形状的模坯件。然后，在1150℃与1400℃温度之间的氧化气氛下加热;其后，将所需要的三氧化二铒的量加到所述的模坯件中，其方法是将模坯件浸渍在含铒的溶液中;再其后，将模坯件在氢气或在至多为0.13帕的压强的真空中，且温度至多为1800℃的条件下烧结。
4、按权利要求3所述的方法，其特征在于所述含铒溶液包括乙酰丙酮铒的醇溶液。
CN86105927.1A 1985-09-09 1986-09-06 气密烧结半透明铝的氧化物 Expired CN1005335B (zh)

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NL8700844A (nl) * 1987-04-10 1988-11-01 Philips Nv Ceramisch lichtdoorlatend materiaal, werkwijze voor het vervaardigen van een dergelijk materiaal en hogedrukontladingslamp voorzien van een dergelijk materiaal.
AU612346B2 (en) * 1988-03-02 1991-07-11 Unitek Corporation Ceramic orthodontic appliance
JP2729113B2 (ja) * 1991-02-27 1998-03-18 株式会社ミツトヨ アブソリュートエンコーダ
US5780377A (en) * 1993-09-02 1998-07-14 Toto Ltd. Light-transmissive ceramics and method of manufacturing same
US5411583A (en) * 1993-11-15 1995-05-02 E. I. Du Pont De Nemours And Company HF-resistant ceramics and use thereof
US5587346A (en) * 1995-06-16 1996-12-24 Osram Sylvania, Inc. Translucent polycrystalline alumina
US6346495B1 (en) 1999-12-30 2002-02-12 General Electric Company Die pressing arctube bodies
AU2002347557A1 (en) * 2002-01-04 2003-07-30 Koninklijke Philips Electronics N.V. Sintered body and electric lamp
JP2005532977A (ja) * 2002-07-10 2005-11-04 コーニンクレッカ　フィリップス　エレクトロニクス　エヌ　ヴィ 透明多結晶酸化アルミニウム
US7678725B2 (en) * 2007-05-14 2010-03-16 General Electric Company Translucent polycrystalline alumina ceramic
US20080283522A1 (en) * 2007-05-14 2008-11-20 Shuyl Qin Translucent polycrystalline alumina ceramic
EP3310740B1 (de) * 2015-06-16 2020-08-05 CeramTec-Etec GmbH Transparente keramik als komponente für bruchfeste optiken
CN108585802A (zh) * 2018-06-28 2018-09-28 南京大学 一种高介电性能陶瓷的烧结制备方法
EP3992169A1 (de) * 2020-11-03 2022-05-04 Polycrystal design GmbH Gefärbte technische korund-keramik und verfahren zu deren herstellung

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US3905845A (en) * 1969-08-27 1975-09-16 Ngk Insulators Ltd Translucent alumina containing magnesia yttria and lanthium oxide
NL7204638A (zh) * 1972-04-07 1973-10-09
US3834915A (en) * 1972-07-24 1974-09-10 Gte Sylvania Inc Fine grain translucent alumina
JPS5477481A (en) * 1977-12-02 1979-06-20 Ngk Insulators Ltd Polycrystal transparent alumina light emitting tube and high voltage vapor discharge lamp using same
JPS6022670B2 (ja) * 1978-05-12 1985-06-03 日本碍子株式会社 多結晶透明アルミナ及びその製造法ならびに高圧蒸気放射灯用発光管
JPS6048466B2 (ja) * 1980-05-15 1985-10-28 日本碍子株式会社 多結晶透明アルミナ焼結体の製造法

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DE3662254D1 (en) 1989-04-13
JPH0572346B2 (zh) 1993-10-12
NL8502457A (nl) 1987-04-01
EP0218279A1 (en) 1987-04-15
US4699774A (en) 1987-10-13
CN86105927A (zh) 1987-03-11
JPS6259569A (ja) 1987-03-16
EP0218279B1 (en) 1989-03-08
CA1256128A (en) 1989-06-20

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