CN107848889A - 透明陶瓷作为不易破裂的光学元件的组件 - Google Patents

透明陶瓷作为不易破裂的光学元件的组件 Download PDF

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Publication number
CN107848889A
CN107848889A CN201680047631.6A CN201680047631A CN107848889A CN 107848889 A CN107848889 A CN 107848889A CN 201680047631 A CN201680047631 A CN 201680047631A CN 107848889 A CN107848889 A CN 107848889A
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corundum
transparent
corundum ceramic
ceramics
component
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L.施内特
T.施赖纳
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Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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陶瓷技术－Etec有限责任公司
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Abstract

本发明涉及透明刚玉陶瓷部件，所述部件的制造和用途。

Description

透明陶瓷作为不易破裂的光学元件的组件
本发明涉及透明刚玉陶瓷部件，所述部件的制造和用途。
透明陶瓷可用于多种应用。由高应用温度和高硬度导致相比于玻璃材料的优先考虑。例如，透明陶瓷目前用于光学元件（例如，作为激光设备的防护外壳(Schutzeinhausung)，作为光学元件中的抗磨板）以及作为由透明材料系统组成的军用车辆的防护板。单晶（蓝宝石）和多晶（刚玉）氧化铝是具有极高硬度的陶瓷。优异的对硬质材料（如矿石）的抵抗和高抗压强度和出色的抗弯强度以及适度的断裂韧度的组合使得其是不易破裂(bruchfeste)的光学元件的理想材料解决方案。
陶瓷的透明度(Transparenz)主要(vordergruendig)取决于材料的折射率和部件的无错误。材料的折射率n通过表面反射来确定理论透射率(Transparenzgrad)T0，其在真实部件中由于光吸收和光散射而变小。陶瓷的理论透射率为85-87％。对于刚玉，得出理论透射率T0 = 85.7％（其中nλ= 600nm = 1.76）。为了达到理论透射率，需要理想制造的，即无孔的内部结构(Gefuege)（孔隙率<100ppm）和纯相组成（纯度> 99.9％，更好地99.99％）。
晶体尺寸<500nm的多晶亚微米刚玉（α-Al2O3）的机械性能优于所有透明立方陶瓷如镁铝尖晶石、氮氧化铝和钇铝石榴石的机械性能。可以实现至最多2200HV10的硬度、700-1000MPa的抗弯强度、> 400GPa的弹性模量和至最多4MPa√m的断裂韧度。目前作为透明材料的用途受到光学各向异性晶体系统和导致的光波的双折射的限制，因为不能实现>65％的足够的透射率。
只有当晶体尺寸保持在光波波长（380-480nm）以下时，才能实现刚玉部件的>65％高透明度。这样的材料可以通过具有<150nm，更好地<80nm，且理想地<50nm的初级粒径的最细起始粉末在技术上实现。具有至最多1500ppm外来物质（优选高达500ppm的氧化镁）的掺杂被称作晶粒生长抑制剂。此外，晶粒的定向排列(Ausrichtung)可导致提高的透明度。
陶瓷的透明度通常通过真实在线透射率（RIT）来指定。在此，光（通常是单色光）照射通过样品，检测器仅捕捉具有最大0.5°的低孔径角的散射光。该测量尺寸目前是用以可靠说明光学组件的透明度的标准值。
透明组件的不透明性由人眼来记录，并且仅在有限程度上经RIT描绘。不透明区域降低高价值显示-组件（例如智能手机、平板电脑、表盖玻璃、抗刻划传感器板）的品质。白色不透明性的度量(Masszahl)是以非常敏感的方式考虑散射光的雾度(Haze)。低雾度在显示-组件和光学应用中是必不可少的。在透明陶瓷的情况下，迄今尚未考虑“雾度”参数。
由于折射率的偏离，光波在相变时在不同的方向上衍射，这由于光波的偏转而导致透明度损失。为了高透明度，必须避免外来相，或者将外来相含量设定得尽可能小。在非立方和光学各向异性的刚玉晶体中，由于折射率是方向依赖性的（Δn= 0.008），因此光波在晶界处额外衍射。如果晶体尺寸小于各自的光波长，则可以减少透明度损失；例如，对于可见光光谱（380-780nm）中的高透明度，需要直径小于380nm的晶粒。特别是，不含外来元素的纯晶界是所需的。
尽管有已知的掺杂策略，但由于晶粒生长在高固结温度下发生，迄今尚未实现具有高透射率（RIT> 65％）且无掺杂物的透明刚玉陶瓷的制造。在US 7396792 B2中描述了一种透明多晶刚玉，其可以以RIT≥30％的透明度值制造，其中通过掺杂有MgO（≤0.3重量％）和ZrO2（0.1-0.5重量％）来限制晶粒生长。刚玉组件的厚度为0.8mm。其他掺杂剂是金属氟化合物，其至最多2000ppm被添加到超纯刚玉粉末（杂质<100ppm）中（DE 102009035501A1）。由此可以生产高密度和微细结晶的刚玉陶瓷（平均内部结构晶粒尺寸d50 <500nm）。本文件中没有描述透明部件。
因此，本发明的目的是制造和加工(Fertigung)刚玉陶瓷部件，以及用于制造部件的方法。
借助根据权利要求1的透明刚玉陶瓷部件可以实现该目的。在从属权利要求中规定了优选实施方案。本发明还涉及一种包括本发明部件的层压件和用于制造该部件的方法。
如果起始刚玉粉末超纯（> 99.9％）且仅轻度掺杂（<2000ppm，更好地<1000ppm）地存在，刚玉陶瓷具有高透射率。
然而，掺杂策略对于小的晶体尺寸是决定性的调节尺寸，这对于高透明度和低雾度是重要的。在此，多重掺杂，即掺杂物氧化镁、氧化钇和氧化镧或其他氧化物的组合，优选两种、三种、四种或五种掺杂物（氧化物）的组合或者用所述氧化物之一进行单一掺杂是可行的。与未掺杂的陶瓷相比，通过多重掺杂，晶粒尺寸可以减小超过40％，优选甚至减小超过65％。
如果透明刚玉陶瓷部件具有<10％，优选<6％且特别优选<3％的雾度，那么对于所述部件是有利的。考虑到无孔陶瓷，晶粒尺寸应在750nm以下，优选在500nm以下，特别优选在250nm以下，以产生相应的雾度。
在制造透明刚玉陶瓷部件时可以使用不同方法，其是针对完全密实部件（孔隙率<100ppm或0.01％）中的低晶粒尺寸的。
刚玉粉末或粉末混合物可以例如与合适的有机材料(Organik)混合并造粒。其后优选通过单级或双级干压进行成型，其由单轴压制或由单轴压制和后置的冷等静压的组合方法组成。如果通过大量压制操作（至最多250次循环）的循环压制辅助该方法，则可以生产具有高生坯密度和高均匀度的陶瓷。
在另一种方法中，可以通过快速烧结方法（例如，场辅助烧结）使刚玉微细粉末密实。高加热速率和短处理时间在此抑制有损透明度的晶粒生长。
在另一种方法中，通过工艺技术使光学各向异性刚玉晶粒定向排列。与具有统计分布的晶粒的陶瓷相比，这导致具有增加的透明度的织构化陶瓷。这种织构化可以通过例如利用> 5特斯拉，更好地> 8特斯拉的强磁场来实现。对于这一目的，需要稳定的，即少沉积和少附聚的初级颗粒<150nm，更好地<50nm的刚玉粉末的陶瓷悬浮液。通过与凝胶浇铸方法的组合产生特别积极的效果。因此该变型尤其适合于生产具有> 65％的RIT和<10％的雾度的透明陶瓷（US20110039685 A1）。
如果所使用的刚玉粉末具有单一-或多重掺杂，则可以改善根据上述方法制造的部件的性能，由此例如可以实现<6％的雾度。这特别适用于厚度<800μm，优选<500μm，特别优选<250μm的薄部件。在此，掺杂剂含量≤2000ppm（掺杂物的总量）被证明是特别有利的。
可以另外通过在限定的气氛（例如空气、氧气、惰性气体）和温度下的额外的预烧结步骤，实现具有至少99.99％的所需密实度的固结。特别地，可以通过包括预烧结和多重掺杂的组合的方法来制造特别有利的部件。
另外，如果要达到高透明度和低雾度，则可以为此将密实部件中的碳含量设定得低。密实部件中的碳含量可以在工业用空气中通过HIP方法通过工艺技术设定。可容忍的C-含量可在此设定为<0.2％，优选<0.05％。
由于材料硬度高和材料脆性大，迄今尚未实现厚度小于1mm的薄刚玉组件的制造。这种部件在本发明的范围内被称为晶片，其可被实施为圆形、方形和矩形。加工晶片的优选方法是采用特制的装有金刚石的线材和优化的工艺流体的线锯。晶片加工的另一个实施方案是借助激光的能量的点状引入，其导致在厚度方向（z-方向）上的材料损坏和材料破裂。晶片机械分离，其中该方法可以在具有或不具有额外的温度作用的情况下实施。
晶片加工后，研磨-和抛光工艺是所需的，以达到最终的表面质量和光学性能。在此，应使用合适的方法，其特别以选择最佳的冷却润滑剂和具有限定粒度的研磨-和抛光操作的次序著称。
意料之外的是，可以制造RIT> 65％的组件。由此才使得能够在诸如显示板（例如潜水电脑、手机、平板电脑、笔记本、表）、表盖玻璃、抗刻划传感器、地面灯、机器窗和照相机镜头等的许多市场领域中应用。这可以通过加工至<800μm，优选<500μm，特别优选<250μm的部件厚度来实现。刚玉陶瓷的平均晶粒尺寸D50 <750nm，优选<500nm，特别优选<350nm。在此，这些通常是内部结构晶粒尺寸。它们是通过截线法确定的。
陶瓷以显著更高的抗压强度和硬度优于塑料和玻璃，和因此相对沙粒、天然岩石（花岗岩等）和玻璃碎片等硬质颗粒显著更耐磨。由于材料的脆性，整体式构型(monolithische Ausfuehrung)的陶瓷并不总是值得期望的。
基底材料（例如塑料，玻璃）和硬质陶瓷层的复合构造方式理想地将这两种材料联结。接合部件被称为层压件，通过利用压力和温度进行联结，通过有机或无机粘合剂进行粘合，和在形成高粘附力下不用中间层进行接合。
根据本发明，层压件包括根据本发明的透明刚玉陶瓷部件层和至少一个另外的基底材料层。然而，除了透明刚玉陶瓷部件之外，还可以存在多个基底材料层，其中不同层的基底材料可以彼此相同或不同。
令人惊奇地，在此已显示，用厚度<500μm，优选<300μm，特别优选<200μm的透明刚玉陶瓷部件与基底材料优选化学硬化玻璃的组合作为层压件，在硬质表面(Untergrund)上的跌落测试中得出极好的结果。
商用常见的玻璃具有较低的断裂韧性（<100MPa）和抗弯强度（<1MPa√m），并且不特别良好地适用于显示板应用。可以在靠近表面的区域（>50μm）中通过锂铝硅酸盐玻璃的离子交换，使新型玻璃受压。诱导的压应力至少为600MPa（DE 102010009584 A1）。由此拉应力的阻力增加。这些玻璃的缺点是由于材料硬度低导致的耐刻划性降低和耐压性降低。例如，硬化玻璃和薄刚玉陶瓷的层压件是在显示板的可忍受的显示板下落高度和耐刻划性方面具有优势的组合。与不具有透明陶瓷的常规层压件相比，直到断裂发生的最大可能的下落高度可以增加至少80％。
透明刚玉陶瓷部件可以加工成至最多400mm的高横向尺寸。透明刚玉陶瓷部件还可以具有特定的纵横比。在本发明的范围内，纵横比被理解为是指组件的长度与宽度的最大比例。可以实现纵横比小于5的矩形部件。由此得出透明刚玉陶瓷部件的优选纵横比在1（方形）至5（矩形）的范围内。然而，透明刚玉陶瓷部件也可以作为具有直径至最多400mm的圆形板存在。

Claims (10)

1.透明刚玉陶瓷部件，其特征在于，陶瓷是单一或多重掺杂的。
2.根据权利要求1所述的部件，其特征在于，所述掺杂剂的总量≤2000ppm。
3.根据权利要求1或2所述的部件，其特征在于，所述部件具有<10％，优选<6％，且特别优选<3％的雾度。
4.根据前述权利要求中任一项所述的部件，其特征在于，所述部件具有<800μm，优选<500μm，特别优选<250μm的厚度。
5.根据前述权利要求中任一项所述的部件，其特征在于，刚玉陶瓷的平均晶粒尺寸D50<750nm，优选<500nm，特别优选<350nm。
6.制造透明刚玉陶瓷部件的方法，其特征在于，该方法中使用的刚玉粉末具有单一或多重掺杂。
7.根据权利要求6所述的方法，其特征在于，所述掺杂剂的总量≤2000ppm。
8.根据权利要求6或7所述的方法，其特征在于，所述方法包括额外步骤，预烧结。
9.层压件，其包括根据权利要求1至5中任一项所述的本发明透明刚玉陶瓷部件层和至少一个另外的基底材料层。
10.根据权利要求9所述的层压件用于潜水电脑、手机、平板电脑、笔记本或表的显示板、表盖玻璃、抗刻划传感器、地面灯、机器窗或照相机镜头的用途。
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US20180155247A1 (en) 2018-06-07
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US11639312B2 (en) 2023-05-02
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