CN105263885A - 陶瓷材料 - Google Patents

陶瓷材料 Download PDF

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CN105263885A
CN105263885A CN201380067388.0A CN201380067388A CN105263885A CN 105263885 A CN105263885 A CN 105263885A CN 201380067388 A CN201380067388 A CN 201380067388A CN 105263885 A CN105263885 A CN 105263885A
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stupalith
metal oxide
impurity
preparation
crystalline ceramics
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L·施内特
F·维蒂希
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Ceramtec ETEC GmbH
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Abstract

本发明涉及透明陶瓷的制备。特别地，本发明涉及含杂质的原材料用于制备透明陶瓷的用途。

Description

陶瓷材料
本发明涉及陶瓷材料，特别地，本发明涉及用于制备透明陶瓷的陶瓷材料。
从现有技术已知透明陶瓷和其制备。DE102004004259B3公开了例如具有高的机械负荷能力的多晶陶瓷，对于0.8mm厚度的抛光盘和在600至650nm之间的波长情况下，其具有大于理论最大值的75％的真实直线透过率(RIT)，其中平均粒度D在60nm至10μm之间的范围内。
多晶陶瓷盘的透明度受各种不同的因素影响。因此必须当然地使用仅具有极其小的光吸收的材料。此外，多晶陶瓷盘的透明度主要取决于光散射，其一方面由晶体结构和另一方面由陶瓷体的组织结构引起。优选地使用具有立方晶系的材料，因为不发生双折射。此外，如下地优化用于制备透明陶瓷的工艺，从而发生尽可能低的多孔性或孔径大小在光波长以下，以便降低相界处的光散射。
制备透明陶瓷时的另一个基本因素是高纯原材料的使用，因为大于100ppm的已经最低的杂质导致陶瓷中白色或黑色的斑点。因此，原则上仅使用具有＞99.99％，优选地甚至于＞99.9999％的纯度的原材料。然而，这些原材料是非常昂贵的。
本发明的任务因此在于，提供备选的陶瓷材料，其适合于制备透明陶瓷并且其比从现有技术已知的高纯原材料成本低。
该任务通过根据权利要求1的陶瓷材料得到解决。该陶瓷材料以此而出众，即它由通过水滑石的煅烧而获得的金属氧化物组成。可以优选地为此使用该材料以制备透明陶瓷。
根据本发明的水滑石为按照水滑石工艺制备的金属氢氧化物。本发明范围内的透明陶瓷，理解为这样的陶瓷，其在300nm、600nm和/或1500nm光波长下拥有至少40％的RIT。就纯理论而言，透明度是不取决于厚度的，如果存在完美的材料并且由此制备完美的陶瓷。然而，一旦陶瓷包含如上所提到的孔，就会在孔的相界处发生散射效应，其随增加的陶瓷厚度而更强。该效应导致下降的透明度。因此，在本文件中所说的透明陶瓷是指具有50μm和100mm之间的壁厚的陶瓷。
特别优选地，由其通过煅烧获得根据本发明的陶瓷材料的水滑石通过水滑石工艺制备。
水滑石工艺是现有技术已知的。此类工艺例如在EP0807086B1中作了描述。本发明中的水滑石工艺理解为这样的工艺，其包含至少下列步骤：
·提供金属，例如铝，和醇类，例如乙醇
·使金属和醇转化为金属醇盐，例如铝醇盐，并释放氢气
·使金属醇盐在添加水的情况下转化为金属氢氧化物，例如勃姆石，并释放醇。
根据本发明的一个特别优选的实施方案，通过煅烧从金属氢氧化物获得的金属氧化物，可以包含100至500ppm之间，优选地100至200ppm之间的杂质，特别是Fe、Mn、Cr、V、Zn、Sn、Ti、Si、Zr、Ca、Na、K、Li、Y、Ni、Co、Cu。这是特别有利的，因为对原材料的纯度提出了比在根据现有技术的材料的情况下更低的要求。通常，在此仅使用具有＞99.99％的纯度的原材料或具有＜100ppm杂质的原材料。所需要的较低纯度，其不有损于透明度，因此使使用明显价格上有利的原材料成为可能。
推测较高的杂质程度是可能的，因为杂质非常分散地和非常均匀地，可能在原子水平上，存在于材料中。它们无论如何不形成分离的相，例如晶界相(Korngrenzphase)，其在烧结的陶瓷中会导致透明度的下降。推测杂质嵌入金属氧化物的晶格中。这意味着金属阳离子在尖晶石晶格中的嵌入，例如阳离子晶格、填隙空间等。
在这种情况下令人意外的是，不仅观察不到透明度的降低，而且此外也不发生陶瓷的明显着色。特别地，用根据本发明的原材料可制备这样的透明陶瓷，其在300nm至700nm之间，特别是在300nm和700nm下具有＜10％的RIT-值偏差和因此达到高的白度值。
优选地，通过水滑石工艺制备金属氢氧化物，其金属氧化物具有立方晶系。除了氧化物例如Al2O3或MgO，特别优选地制备尖晶石，特别是Mg-Al-尖晶石。但是，透明陶瓷也可从ZrO2，Y和Al的混合氧化物以及Al、N、O的混合材料或者甚至非立方氧化铝用该工艺优选地制备。
与现有技术，例如DE102004004259B3相反，可以在使用根据本发明的材料的情况下完全放弃烧结辅料的使用。烧结辅料使在较少的晶粒生长情况下使用更低的烧结温度成为可能。然而，烧结辅料必须借助于挥发性化合物例如LiF至少部分地再被除去，因为它们否则就会以分离的相存在于陶瓷中，这反过来会对透明度具有不利的影响。该添加料在使用根据本发明的陶瓷材料以制备透明陶瓷的情况下不是必需的。
下面，借助实施例更详细地说明本发明。
实施例1
使用按照水滑石工艺制备的具有总共406ppm杂质的MgOAl2O3-原材料，具有下列组成(ICP-分析)：
MgO：28.9％，
Na：18ppm，
Si：196ppm，
Fe：98ppm，
Cr：7ppm，
Ti：10ppm，
Mn：40ppm，
Zn：37ppm，
其余：Al2O3。
比表面积(BET)：18m2/g，
起始粒度分布d90：5.5μm，d502.4μm，d10：0.8μm
将1500g原材料拌入1500g具有7％柠檬酸氢二氨的去离子水中。将经如此预均匀化的浆料用搅拌球磨机(500μm-Al2O3-研磨珠)研磨这样久，直至取得1.60kWh/kg的能量输入。随后存在下列粒度分布：d90：375nm，d50：224nm，d10：138nm(用Microtrac的Nanoflex测量仪测量的)。比表面积(BET)为25.5m2/g。
给如此预备的浆料掺入6％的短链聚乙二醇并借助于喷雾冷冻法颗粒化。在冷冻干燥之后，存在从具有2.17g/cm3的生坯密度(Nettogründichte)的样本形成的可压制颗粒。将这在1455℃下预烧结2小时至3.519g/cm3，随后在1650℃下在200MPa下恒温再压缩(HIP＝热等静压)6小时。
将样品为了透射测量，打磨和抛光至2mm厚度。
测出下列的取决于波长的RIT-值：
300nm：74％，600nm：78％，700nm：80％，1500nm：81％。
实施例2
使用按照水滑石工艺制备的具有232ppm杂质的MgOAl2O3-原材料，具有下列组成(ICP-分析)：
MgO：33.9％
Na：18ppm
Si：83ppm
Fe：71ppm
Ca：5ppm
Cr：4ppm
Ni：2ppm
Ti：18ppm
Mn：27ppm
Cu：1ppm
Zr：3ppm
其余：Al2O3
比表面积(BET)：58m2/g
起始粒度分布d90：7.85μm，d503.2μm，d10：0.9μm
类似于实施例1地完成准备，直至取得1.05kWh/kg的能量输入。随后存在下列粒度分布：d90：345nm，d50：195nm，d10：124nm(用Microtrac的Nanoflex测量仪测量的)，BET23.5m2/g。
给如此预备的浆料掺入6％的短链聚乙二醇并借助于喷雾冷冻法颗粒化。在冷冻干燥之后，存在从具有2.07g/cm3的生坯密度的样本形成的可压制颗粒。将这在1400℃下预烧结2小时至3.512g/cm3，随后在1650℃下在200MPa下恒温再压缩6小时。
将样品为了透射测量，打磨和抛光至2mm厚度。
测出下列的取决于波长的RIT-值：
300nm：60％，600nm：71％，700nm：75％，1500nm：77％。
实施例3
使用按照水滑石工艺制备的具有156ppm杂质的MgOAl2O3-原材料，具有下列组成(ICP-分析)：
MgO：28.9％，
Na：22ppm
Si：83ppm
Fe：31ppm
Cr：1ppm，
Ca：3ppm，
Ti：1ppm，
Mn：8ppm，
Zn：7ppm，
Al2O3：其余
比表面积(BET)：7.3m2/g
起始粒度分布d90：4.7μm，d502.1μm，d10：0.3μm
将600g原材料拌入600g具有4.7％柠檬酸氢二氨的去离子水中。将经如此预均匀化的浆料用搅拌球磨机(500μm-Al2O3-研磨珠)研磨这样久，直至取得1.5kWh/kg的能量输入。那时比表面积(BET)为51.3m2/g。
给如此预备的浆料掺入5％的水性聚合物分散体和4％脂肪酸配制品并借助于喷雾冷冻法颗粒化。在冷冻干燥之后，存在从具有2.18g/cm3的生坯密度的样本形成的可压制颗粒。将这在1550℃下预烧结2小时至3.413g/cm3，随后在1650℃下在200MPa下恒温再压缩6小时。
将样品为了透射测量，打磨和抛光至2mm厚度。
测出下列的取决于波长的RIT-值：
300nm：70％，600nm：75％，700nm：77％，1500nm：79％。
实施例4(比较实施例)
使用不按照水滑石工艺制备的具有461ppm杂质的MgOAl2O3-原材料。下列组成根据ICP-分析测定：
Mg：17.1％，
Al：37.9％，
Na：69ppm，
K：32ppm，
Ca：130ppm
Ti：19ppm，
V：41ppm，
Cr：14ppm，
Mn：7ppm，
Fe：95ppm，
Ni：5ppm，
Zn：14ppm，
Ga：35ppm，
其余：O。
比表面积22.2m2/g。
将540g原材料拌入800g具有1.5％柠檬酸氢二氨的去离子水中。将该浆料用搅拌球磨机(500μm-Al2O3-研磨珠)研磨这样久，直至取得1.50kWh/kg的能量输入。随后存在下列粒度分布：d90：234nm，d50：156nm，d10：84nm(用Microtrac的Nanoflex测量仪测量的)。BET68.1m2/g。
将浆料如在实施例1和2下描述的那样颗粒化。将具有1.89g/cm3的生坯密度的可比较地制备的压制品在1430℃下预烧结2小时至3.524g/cm3，随后在1650℃下在200MPa下恒温再压缩6小时。
将样品为了透射测量，打磨和抛光至2mm厚度：未能测量到RIT-值。样品是不透明的。
实施例5(比较实施例)
使用不按照水滑石工艺制备的具有60ppm杂质的MgOAl2O3-原材料。尖晶石中的转化率(用X射线衍射仪的晶体相测定)99.5％，游离的α-Al2O30.4％，游离的MgO0.1％。下列杂质用ICP-分析测定：
Na：15ppm，
K：32ppm，
Fe：2ppm，
Si：11ppm
其余O。
平均粒度d50(Sedigraph)：0.18μm。
比表面积(BET)：28.2m2/g。
将4000g原材料拌入3605g具有2.3％柠檬酸氢二氨的去离子水中。将该浆料用搅拌球磨机(500μm-研磨珠)研磨这样久，直至取得0.85kWh/kg的能量输入。随后存在下列粒度分布：d90：252nm，d50：152nm，d10：101nm(用Malvern的Zetasizer测量仪测量的)。BET31.7m2/g。
将如此预备的浆料掺入6％的短链聚乙二醇并借助于喷雾冷冻法颗粒化。在冷冻干燥之后，存在从具有1.91g/cm3的生坯密度的样本形成的可压制颗粒。将这在1530℃下预烧结2小时至3.507g/cm3，随后在1650℃下在200MPa下恒温再压缩4小时。
将样品为了透射测量，打磨和抛光至2mm厚度。
测出下列的取决于波长的RIT-值：
300nm：86％，600nm：85％，700nm：84％，1500nm：87％。
实施例6(比较实施例)
使用不按照水滑石工艺制备的具有398ppm杂质的MgOAl2O3-原材料。下列组成根据ICP-分析测定：
Mg：17.1％，
Al：37.9％，
Na：46ppm，
K：25ppm，
Ca：145ppm
Ti：15ppm，
V：27ppm，
Cr：5ppm，
Mn：5ppm，
Fe：80ppm，
Ni：5ppm，
Zn：11ppm，
Ga：34ppm，
O：其余
比表面积20.1m2/g。
将540g原材料拌入800g具有1.5％柠檬酸氢二氨的去离子水中。将该浆料用搅拌球磨机(500μm-Al2O3-研磨珠)研磨这样久，直至取得1.0kWh/kg的能量输入。随后存在下列粒度分布：d90：274nm，d50：156nm，d10：101nm(用Microtrac的Nanoflex测量仪测量的)。BET58.0m2/g。
将浆料如在实施例5下描述的那样颗粒化。将具有1.87g/cm3的生坯密度的可比较地制备的压制品在1410℃下预烧结2小时至3.452g/cm3，随后在1650℃下在200MPa下恒温再压缩6小时。
将样品为了透射测量，打磨和抛光至2mm厚度：未能测量到RIT-值。样品是不透明的。

Claims (7)

1.包含通过水滑石的煅烧而获得的金属氧化物的陶瓷材料，其特征在于，所述材料用于制备在300nm、600nm或1500nm光波长下具有＞40％的RIT值的透明陶瓷。
2.根据权利要求1的陶瓷材料，其特征在于，所述材料用于制备在300nm至700nm光波长之间具有在＜10％的RIT值内的偏差的透明陶瓷。
3.根据权利要求1或2的陶瓷材料，其特征在于，所述金属氧化物包含100至500ppm之间，优选地100至200ppm之间的杂质，特别是Fe、Mn、Cr、V、Zn、Sn、Ti、Si、Zr、Ca、Na、K、Li、Y、Ni、Co和/或Cu。
4.根据权利要求3的材料，其特征在于，所述杂质在原子水平上非常分散地存在于金属氧化物中。
5.根据前述权利要求任一项的陶瓷材料，其特征在于，所述金属氧化物具有立方晶系。
6.根据前述权利要求任一项的陶瓷材料，其特征在于，具有立方晶系的金属氧化物在立方和非立方晶体结构中包含尖晶石，特别是Mg-Al-尖晶石，ZrO2，Y以及Al的混合氧化物，Al、N、O的混合材料以及氧化铝。
7.根据上述权利要求任一项的陶瓷材料用于制备透明陶瓷的用途。
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