CN112225568B - 用于红外光学窗口的MgLiAlON透明陶瓷及制备方法 - Google Patents

用于红外光学窗口的MgLiAlON透明陶瓷及制备方法 Download PDF

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CN112225568B
CN112225568B CN202011000878.7A CN202011000878A CN112225568B CN 112225568 B CN112225568 B CN 112225568B CN 202011000878 A CN202011000878 A CN 202011000878A CN 112225568 B CN112225568 B CN 112225568B
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mglialon
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王跃忠
田猛
孙鹏
刘孟寅
张高峰
刘华松
张荣实
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Tianjin Jinhang Institute of Technical Physics
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Abstract

本发明提供了一种MgLiAlON透明陶瓷及制备方法，用以解决现有技术中红外光学窗口材料不能兼具高强度和高红外透过率的问题。所述制备方法包括如下步骤：按预定比例称取MgO、LiAl5O8、α‑Al2O3、AlN粉料，球磨混合后，将混合粉体模压成型，再经冷等静压处理，得到坯料；坯料置于气氛烧结炉中，升温至1600～1800℃并保温，得到初步样品；再将初步样品置于热等静压炉中，升温到1800～1950℃、压强为150～200MPa下进行热等静压处理；再对样品表面抛光，得到MgLiAlON透明陶瓷。本发明通过Mg2+、Li+双元素掺杂及组分调配，获得MgLiAlON透明陶瓷，具有红外高透过率和高强度的特点，满足红外光学窗口材料的要求。

Description

用于红外光学窗口的MgLiAlON透明陶瓷及制备方法
技术领域
本发明属于红外光学材料领域，具体涉及一种用于红外光学窗口的MgLiAlON透明陶瓷及制备方法。
背景技术
红外制导具有精度高、抗干扰能力强等优势，因此受到世界各国高度重视。中波红外(3.0～5.0μm)是当前国内外红外制导系统中应用最多、最为成熟的方案，涉及的红外材料有MgF2、蓝宝石、MgAl2O4、AlON等。MgF2由于力学性能相对较差，难以满足未来高速高热环境的应用需求；蓝宝石制备技术相对较为成熟，但由于单晶生长周期长、成本高不利于规模化生产；MgAl2O4和AlON是一种立方尖晶石结构的材料，通过低成本的陶瓷烧结的方法，可以制备出透明的块体材料，是优异的中波红外窗口材料候选方案。
现有技术中，红外光学窗口材料要应用于高速高热的环境下，因此不仅需要窗口材料具有良好的红外透过等光学性能，还要具备相应的强度、硬度等力学性能。目前，采用反应烧结/热等静压方法制备出的高透明的AlON基的LiAlON陶瓷，强度与AlON材料十分接近，且高于MgAlON和MgAl2O4，但是其红外波段尤其是4.5μm附近透过率相对较低，无法满足红外窗口材料的要求；采用无压烧结法制备出的高透明的AlON基的MgAlON陶瓷，在3.0～4.5μm波段具有优异的光学透过性能，但是其强度要低于LiAlON，也无法应用于红外光学窗口。
发明内容
鉴于现有技术中的上述缺陷或不足，本发明旨在提供一种用于红外光学窗口的MgLiAlON透明陶瓷及制备方法，通过Mg2+、Li+双元素掺杂及组分调配，并选择合适的烧结方法，获得新型AlON基陶瓷材料，即MgLiAlON透明陶瓷，具有红外高透过率和高强度的特点，在3.0～4.5μm具有较高透过率(不低于70％)、且强度不低于270MPa，满足红外光学窗口材料的要求。
为了实现上述目的，本发明实施例采用如下技术方案：
第一方面，本发明实施例提供了一种用于红外光学窗口的MgLiAlON透明陶瓷的制备方法，其特征在于，所述制备方法包括如下步骤：
步骤S1，按预定比例称取MgO、LiAl5O8、α-Al2O3、AlN粉料，进行球磨混合，得到混合粉体；
步骤S2，将所述混合粉体进行模压成型，再经冷等静压处理，得到坯料；
步骤S3，将坯料置于N2气氛保护的烧结炉中，以5～10℃/min的速率升温至1600～1800℃保温5～20h，以5～10℃/min的速率却至室温，得到初步样品；
步骤S4，将初步样品置于热等静压炉中，以5～10℃/min的速率升温到1800～1950℃进行热等静压，保温时间为1～5h，且保温期间热等静压压强为150～200MPa；以5～10℃/min的速率冷却至300℃，再自然冷却至室温后，得到准样品；
步骤S5，对准样品进行表面抛光，得到MgLiAlON透明陶瓷。
上述方案中，所述MgO、LiAl5O8、α-Al2O3、AlN粉料的预定比例，以混合粉体的质量为基准，MgO+LiAl5O8、AlN、α-Al2O3的质量分数分别为6.0～23.0wt％、7.0～24.0wt％、70～87wt％。
上述方案中，所述MgO+LiAl5O8中，MgO、LiAl5O8的质量比为2:1～1:4。
上述方案中，所述MgO、LiAl5O8、α-Al2O3、AlN粉料的中位粒度D50均不高于1μm。
上述方案中，所述步骤S1的球磨混合，将称取的各原料，放入球磨罐中，以耐磨氧化铝为球磨介质，无水乙醇为分散介质，球料比为4:1～12:1，球磨时间为10～24h，得浆料，再经50～80℃干燥处理去除分散介质，最后经过筛处理得到混合粉体。
上述方案中，所述步骤S2中，模压成型压力为10～30MPa，保压时间1～10min；冷等静压压力为150～300MPa，保压时间5～15min。
上述方案中，所述步骤S3还包括：将坯料置于装有包埋粉的BN或石墨坩埚中，再放入烧结炉中；包埋粉的成分为BN、LiAlON的混合物，其中LiAlON的质量分数为50～80wt％。
上述方案中，所述步骤S4还包括：将初步样品置于钨坩埚或BN坩埚中，放入热等静压炉中进行热等静压。
上述方案中，所述步骤S5中采用平均颗粒度低于5μm的金刚石悬浮液作为抛光介质。
第二方面，本发明实施例还提供了一种由上述制备方法所制备的用于红外光学窗口的MgLiAlON透明陶瓷，Mg2+、Li+双元素掺杂，所述MgLiAlON透明陶瓷，3.0～4.5μm波段红外透过率不低于70％，弯曲强度不低于270MPa。
本发明具有如下有益效果：
本发明所提供的用于红外光学窗口的MgLiAlON透明陶瓷及制备方法，显著提高了传统LiAlON材料的中红外波段(3.0～4.5μm)的透过率，也提高了MgAlON材料的强度，获得了一种兼具高强度、高红外透过率的MgLiAlON透明陶瓷，满足高速高热环境的中波红外光学窗口或头罩的材料要求。
附图说明
通过阅读参照以下附图所作的对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：
图1是本发明实施例1～2及对比例1～2所得样品D1～D4的红外透过率曲线图。
具体实施方式
下面结合附图和实施例对本发明作进一步的详细说明。可以理解的是，此处所描述的具体实施例仅仅用于解释相关发明，而非对该发明的限定。另外还需要说明的是，为了便于描述，附图中仅示出了与发明相关的部分。
需要说明的是，在不冲突的情况下，本发明中的实施例及实施例中的特征可以相互组合。下面将参考附图并结合实施例来详细说明本发明。
本发明针对红外光学窗口材料的应用要求，提供了一种用于红外光学窗口的MgLiAlON透明陶瓷及其制备方法，通过Mg2+、Li+双元素掺杂及组分调配，获得新型AlON基陶瓷材料，即MgLiAlON透明陶瓷，兼具MgAlON的红外高透过率和LiAlON的高强度，具体表现为在3.0～4.5μm具有较高透过率、且强度不低于270MPa。所述制备方法，采用气氛保护烧结炉和热等静压炉获得样品，并对样品进行抛光处理后，获得MgLiAlON透明陶瓷，可应用于制备红外光学窗口，满足红外透过率及强度要求。
下面通过具体的实施例，对本发明作进一步详细的说明，各个实施例仅作为本发明的一个举例，并不构成对本发明的限制，同时，各个实施例间也不构成相互限制。
实施例1
本实施例提供了一种Mg、Li双掺的AlON基透明陶瓷(即MgLiAlON透明陶瓷)及制备方法。
所述制备方法包括如下步骤：
步骤S101，按MgO+LiAl5O8、AlN、α-Al2O3的质量分数分别为23.0wt％、7.0wt％、70wt％称取MgO、LiAl5O8、α-Al2O3、AlN原料粉共50g，其中MgO、LiAl5O8的质量比为2:1；放入球磨罐中，以耐磨氧化铝为球磨介质，无水乙醇为分散介质，球料比为4:1，球磨时间为24h，得浆料，再经80℃干燥处理去除分散介质，最后经过筛处理得到混合粉体A1。
本步骤中，MgO、LiAl5O8、α-Al2O3、AlN粉料的中位粒度D50分别为0.1μm、0.2μm、0.15μm、1.0μm。
步骤S102，取40g混合粉体A1，在10MPa、保压时间10min下模压成型得到尺寸Φ50mm的圆片；再将成型后的坯料在150MPa、保压时间15min下冷等静压处理，得坯料B1。
步骤S103，将坯料B1置于装有包埋粉的BN坩埚中，再放入烧结炉中；包埋粉的成分为BN、LiAlON的混合物，其中LiAlON的质量分数为80wt％；再将BN坩埚置于N2气体保护的烧结炉中，升温至1700℃保温20h，自然冷却后，得初步样品。
本步骤中，烧结升、降温速率控制在5℃/min；所述N2气纯度为99.99vol％。
步骤S104，将初步样品装入BN坩埚中，再将BN坩埚置于Ar气作为传压介质的热等静压炉中，以5℃/min的速率升温至1800℃并保温5小时，保温期间热等静压压强为200MPa；然后以5℃/min的速率降温至300℃，再自然冷却至室温后取出，得到准样品C1；
步骤S105，采用平均颗粒度为4μm的金刚石悬浮液作为抛光介质，将准样品C1打磨抛光至1mm厚，得透明陶瓷样品D1。
对透明陶瓷样品D1进行成分分析、红外透过率测试及弯曲强度测试，其成分为含Mg、Li的AlON基尖晶石结构，平均晶粒尺寸为95μm，是MgLiAlON透明陶瓷。红外透过率测试结果见图1，弯曲强度及晶粒尺寸列于表1中。
对比例1：
此处是制备一种含Mg、无Li的AlON基透明陶瓷(即MgAlON)作为对比。按MgO、AlN、α-Al2O3的质量分数分别为23wt％、7.0wt％、70wt％的比例称取MgO、α-Al2O3、AlN原料粉共50g，采用与实施例1相同的步骤及参数，制备得到MgAlON透明陶瓷样品D3。
对样品D3进行透过率测试，结果见图1；并进行弯曲强度试验，结果列于表1中。
实施例2：
本实施例提供了一种Mg、Li双掺的AlON基透明陶瓷(即MgLiAlON透明陶瓷)及制备方法。
所述制备方法包括如下步骤：
步骤S101，按MgO+LiAl5O8、AlN、α-Al2O3的质量分数分别为6.0wt％、7.0wt％、87wt％称取MgO、LiAl5O8、α-Al2O3、AlN原料粉共50g，其中MgO、LiAl5O8的质量比为2:1；放入球磨罐中，以耐磨氧化铝为球磨介质，无水乙醇为分散介质，球料比为12:1，球磨时间为24h，得浆料，再经80℃干燥处理去除分散介质，最后经过筛处理得到混合粉体A2。
本步骤中，MgO、LiAl5O8、α-Al2O3、AlN粉料的中位粒度D50分别为0.18μm、0.55μm、0.25μm、0.88μm。
步骤S102，取40g混合粉体A2，在30MPa、保压时间1min下模压成型得到尺寸Φ50mm的圆片；再将成型后的坯料在300MPa、保压时间5min下冷等静压处理，得坯料B2。
步骤S103，将坯料B2置于装有包埋粉的石墨坩埚中，再放入烧结炉中；包埋粉的成分为BN、LiAlON的混合物，其中LiAlON的质量分数为50wt％；再将石墨坩埚置于N2气体保护的烧结炉中，升温至1800℃保温5h，降温至室温后，得初步样品。
本步骤中，烧结升、降温速率控制在10℃/min；所述N2气纯度为99.99vol％。
步骤S104，将初步样品装入钨坩埚中，再将钨坩埚置于Ar气作为传压介质的热等静压炉中，以10℃/min的速率升温至1950℃并保温1小时，保温期间热等静压压强为200MPa；然后以10℃/min的速率降温至300℃，再自然冷却至室温后取出，得到准样品C2。
步骤S105，采用平均颗粒度为4.5μm的金刚石悬浮液作为抛光介质，将准样品C2打磨抛光至1mm厚，得透明陶瓷样品D2。
对透明陶瓷样品D2进行成分分析、红外透过率测试及弯曲强度测试，其成分为含Mg、Li的AlON基尖晶石结构，平均晶粒尺寸为110μm，是MgLiAlON透明陶瓷。红外透过率测试结果见图1，弯曲强度及晶粒尺寸列于表1中。
对比例2：
此处是制备一种含Li、无Mg的AlON基透明陶瓷(即LiAlON)作为对比。按LiAl5O8、AlN、α-Al2O3的质量分数分别为6wt％、7.0wt％、87wt％的比例称取MgO、α-Al2O3、AlN原料粉共50g，采用与实施例2相同的步骤及参数，制得LiAlON透明陶瓷样品D4。
对样品D4进行透过率测试，结果见图1；并进行弯曲强度试验，结果列于表1中。
表1
性能 样品D1 样品D2 样品D3 样品D4
弯曲强度/MPa 279 316 243 323
平均晶粒尺寸/μm 110 95 100 100
由表1可以看出，本发明实施例1～2所制备的MgLiAlON透明陶瓷样品(D1和D2)，弯曲强度明显高于对比案例1中的MgAlON(即D3样品)，仅次于对比例2中的LiAlON(样品D4)；如图1所示，本发明实施例1～2所制备的MgLiAlON透明陶瓷样品(D1和D2)，红外透过率明显提升，高于对比案例2中的LiAlON(即D4样品)，仅次于对比例1中的MgAlON(样品D3)。这表明通过Mg2+、Li+双元素掺杂及组分调配，可以实现力学、光学性能的调控，实现二者的均衡取舍。获得MgLiAlON透明陶瓷，兼具红外高透过率和高强度的特点。
以上描述仅为本发明的较佳实施例以及对所运用技术原理的说明。本领域技术人员应当理解，本发明中所涉及的发明范围，并不限于上述技术特征的特定组合而成的技术方案，同时也应涵盖在不脱离所述发明构思的情况下，由上述技术特征或其等同特征进行任意组合而形成的其它技术方案。例如上述特征与本发明中公开的(但不限于)具有类似功能的技术特征进行互相替换而形成的技术方案。

Claims (6)

1.一种用于红外光学窗口的MgLiAlON透明陶瓷，其特征在于，所述MgLiAlON透明陶瓷，通过Mg2+、Li+双元素掺杂及组分调配， 3.0~4.5μm波段红外透过率不低于70%，弯曲强度不低于270MPa；
所述MgLiAlON透明陶瓷的制备方法包括如下步骤：
步骤S1，按预定比例称取MgO、LiAl5O8、α-Al2O3、AlN粉料，进行球磨混合，得到混合粉体；其中，以混合粉体的质量为基准，MgO+LiAl5O8、AlN、α-Al2O3的质量分数分别为6.0～23.0wt%、7.0～24.0 wt%、70～87 wt%，MgO、LiAl5O8的质量比为2:1；
步骤S2，将所述混合粉体进行模压成型，再经冷等静压处理，得到坯料；
步骤S3，将坯料置于装有包埋粉的BN或石墨坩埚中，再放入N2气氛保护的烧结炉中，以5～10℃/min的速率升温至1600～1800℃保温5～20h，以5～10℃/min的速率冷却至室温，得到初步样品；所述包埋粉的成分为BN、LiAlON的混合物，其中LiAlON的质量分数为50~80wt%；
步骤S4，将初步样品置于热等静压炉中，以5～10℃/min的速率升温到1800～1950℃进行热等静压，保温时间为1～5h，且保温期间热等静压压强为150～200MPa；以5～10℃/min的速率冷却至300℃，再自然冷却至室温后，得到准样品；
步骤S5，对准样品进行表面抛光，得到MgLiAlON透明陶瓷。
2.根据权利要求1所述的MgLiAlON透明陶瓷，其特征在于，所述MgO、LiAl5O8、α-Al2O3、AlN粉料的中位粒度D50均不高于1μm。
3.根据权利要求1所述的MgLiAlON透明陶瓷，其特征在于，所述步骤S1的球磨混合，将称取的各原料，放入球磨罐中，以耐磨氧化铝为球磨介质，无水乙醇为分散介质，球料比为4:1~12:1，球磨时间为10~24 h，得浆料，再经50~80℃干燥处理去除分散介质，最后经过筛处理得到混合粉体。
4.根据权利要求1所述的MgLiAlON透明陶瓷，其特征在于，所述步骤S2中，模压成型压力为10~30 MPa，保压时间1~10 min；冷等静压压力为150~300 MPa，保压时间5~15 min。
5.根据权利要求1所述的MgLiAlON透明陶瓷，其特征在于，所述步骤S4还包括：将初步样品置于钨坩埚或BN坩埚中，放入热等静压炉中进行热等静压。
6.根据权利要求1所述的MgLiAlON透明陶瓷，其特征在于，所述步骤S5中采用平均颗粒度低于5μm的金刚石悬浮液作为抛光介质。
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