CN112500162A - 一种yag透明陶瓷及其致密化烧结方法 - Google Patents
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Abstract
一种YAG透明陶瓷及其致密化烧结方法，传统的YAG透明陶瓷配方采用Y3Al5O12，Y2O3与Al2O3的摩尔比为3:5，辅以SiO2、MgO、CaO、LiF等烧结助剂促进致密化。本发明不添加其它任何烧结助剂，避免因烧结助剂的添加引入杂质或缺陷。通过引入微量Y离子缺位（化学式为Y3‑ xAl5O12‑1.5x），降低烧结温度，结合真空烧结与热等静压烧结技术，制备高透明YAG透明陶瓷材料。
Description
技术领域
本发明属于透明陶瓷材料领域，特别涉及一种YAG透明陶瓷及其致密化烧结方法。
背景技术
YAG透明陶瓷由于其优异的机械性能、高热导率以及低热膨胀系数等优点，是理想的透明陶瓷装甲材料和激光增益介质宿主材料。与传统的透明单晶材料相比，透明陶瓷材料具有较短的制备周期、成本低、掺杂均匀性好、复合多功能等优点。与传统的激光玻璃材料相比，YAG透明陶瓷具有更高的热导率和机械强度。
1995年，日本科学家Ikesue采用SiO2作为烧结助剂，首次制备出激光级Nd:YAG透明陶瓷并实现激光输出。此后，YAG透明陶瓷的研究获得了国际广泛的关注。为了制备高光学质量YAG透明陶瓷，人们做了大量的研究工作。2000年，Li Ji-guang等人采用碳酸氢铵作为沉淀剂，制备出高分散性、高烧结活性YAG纳米粉体。2009年，宾夕法尼亚州立大学使用SiO2作为烧结助剂，采用真空烧结结合热等静压烧结方式制备了Nd:YAG透明陶瓷。2018年，Zhou等人采用MgO作为烧结助剂制备YAG透明陶瓷，样品在1064 nm透过率可达84%。但是，烧结助剂的添加将不可避免导致样品热导率的降低，而且过量的烧结助剂将会在晶界处富集，产生第二相，影响样品光学均匀性。因此，如果不采用烧结助剂便能实现高光学质量YAG透明陶瓷的制备，将使材料具有更优异的热性能与激光性能。
发明内容
解决的技术问题：本申请公开了一种YAG透明陶瓷及其致密化烧结方法，解决的技术问题是无需采用烧结助剂，减少样品热导率的损耗，不存在杂质于晶界处富集的现象，没有第二相生成，样品的光学均匀性优异。
技术方案：
一种YAG透明陶瓷，所述YAG透明陶瓷化学式为Y3-xAl5O12-1.5x。
优选的，所述x取值范围为0-0.05。
优选的，所述YAG透明陶瓷的原料为Y2O3与Al2O3，所述Y2O3与Al2O3的摩尔比为(3-x):5，x=0-0.05。
优选的，所述Y2O3与Al2O3为高纯Y2O3和高纯Al2O3，所述Y2O3纯度>99.99%，Al2O3纯度>99.99%。
本申请还公开了一种YAG透明陶瓷的致密化烧结方法，包括以下步骤：
第一步：按照摩尔比称取Y2O3与Al2O3；
第二步：用固相球磨法制备Y2O3与Al2O3浆料，固相球磨法采用乙醇为球磨介质，经高速行星式球磨后把浆料倒入干燥皿中，经鼓风式烘箱60℃干燥，过140目筛，得到YAG粉体，球磨时间为15h，球磨转速为150 转/分钟，鼓风式烘箱干燥时间为24小时；
第三步：通过煅烧、成型及烧结工艺制备成YAG透明陶瓷，真空烧结温度为1500-1750℃，热等静压温度为1500-1780℃。
优选的，所述制得的YAG透明陶瓷1000 nm直线透过率不低于83%。
优选的，所述制得的YAG透明陶瓷的平均晶粒尺寸为0.5-20μm。
优选的，所述球磨后的YAG粉体煅烧温度为800-1000 ℃，保温时间大于3小时。
优选的，煅烧后的YAG填充至不锈钢模具中，先在5MPa下干压成型，再在200 MPa冷等静压下成型，得到素坯。
优选的，所述素坯在马弗炉中采用800-1100℃下煅烧5-10h，之后将样品置于真空炉中1500-1750℃真空气氛中烧结2-15h，真空度低于1.0×10-3Pa，再在1500-1780℃下热等静压烧结2-5h，所述热等静压烧结使用196 MPa氩气介质，最后，在马弗炉中采用1100-1500℃空气或氧气气氛下热处理1-20 h，得到所述YAG透明陶瓷。
有益效果：
1、制得的YAG透明陶瓷1000 nm直线透过率不低于83%。
2、制得的YAG透明陶瓷的平均晶粒尺寸为0.5-20 μm。
3、在YAG粉体制备及压制成型过程中，无需额外添加任何烧结助剂。
4、制得的YAG透明陶瓷室温25 °C热导率达到11 W/m˙K。
5、在致密化烧结过程中，真空烧结温度及热等静压温度可低至1500 °C，样品即可实现高透明度。该烧结温度远低于目前YAG的主流烧结温度1600-1800 °C。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
一种YAG透明陶瓷的致密化烧结方法，包括以下步骤：
第一步：采用高纯Y2O3（>99.99%）和Al2O3（>99.99%）商业粉为原料，按照化学式Y2.98Al5O11.97，分别称取30 g Y2O3粉体及22.7280 g Al2O3粉体；
第二步：用固相球磨法制备Y2O3与Al2O3浆料，将称好的粉体倒入球磨罐中，加入50mL无水乙醇为球磨介质，经高速行星式球磨15小时后把浆料倒入干燥皿中，经鼓风式烘箱60℃，过140目筛，得到Y2.98Al5O11.97粉体，球磨转速为150 转/分钟，鼓风式烘箱干燥时间为24小时；
第三步：将Y2.98Al5O11.97粉体填充至不锈钢模具中，先在5 MPa下干压成型，之后再在200 MPa冷等静压下成型，得到高密度YAG陶瓷素坯；将素坯在马弗炉中采用800 ℃煅烧10小时，之后将样品取出并在真空炉中1550℃烧结10小时，真空度低于1.0×10-3Pa，再在1600 ℃热等静压烧结3小时（使用196 MPa氩气介质）。最后在马弗炉中经1400 ℃空气退火10小时得到所述YAG透明陶瓷。
如图1所示，为本发明实例提供的Y2.98Al5O11.97透明陶瓷与传统Y3Al5O12透明陶瓷样品烧结后的对比照片。在先后经过真空烧结1550 °C/10 h 以及热等静压烧结1600 °C/3 h后，x=0.02（化学配方为Y2.98Al5O11.97）的陶瓷样品可以完全实现透明化，其透明度远高于传统Y3Al5O12配方的陶瓷样品。
Claims (10)
1.一种YAG透明陶瓷，其特征在于：所述YAG透明陶瓷化学式为Y3-xAl5O12-1.5x。
2.根据权利要求1所述YAG透明陶瓷，其特征在于：所述x取值范围为0-0.05。
3.根据权利要求1所述YAG透明陶瓷，其特征在于：所述YAG透明陶瓷的原料为Y2O3与Al2O3，所述Y2O3与Al2O3的摩尔比为(3-x):5，x=0-0.05。
4.根据权利要求3所述YAG透明陶瓷，其特征在于：所述Y2O3与Al2O3为高纯Y2O3和高纯Al2O3，所述Y2O3纯度>99.99%，Al2O3纯度>99.99%。
5.一种权利要求4所述YAG透明陶瓷的致密化烧结方法，其特征在于：包括以下步骤：
第一步：按照摩尔比称取Y2O3与Al2O3；
第二步：用固相球磨法制备Y2O3与Al2O3浆料，固相球磨法采用乙醇为球磨介质，经高速行星式球磨后把浆料倒入干燥皿中，经鼓风式烘箱60℃干燥，过140目筛，得到YAG粉体，球磨时间为15h，球磨转速为150 转/分钟，鼓风式烘箱干燥时间为24小时；
第三步：通过煅烧、成型及烧结工艺制备成YAG透明陶瓷，真空烧结温度为1500-1750℃，热等静压温度为1500-1780℃。
6.根据权利要求5所述YAG透明陶瓷的致密化烧结方法，其特征在于：所述YAG透明陶瓷1000 nm直线透过率不低于83%。
7.根据权利要求5所述YAG透明陶瓷的致密化烧结方法，其特征在于：所述YAG透明陶瓷的平均晶粒尺寸为0.5-20μm。
8.根据权利要求5所述YAG透明陶瓷的致密化烧结方法，其特征在于：所述YAG陶瓷粉体在球磨后，经800-1000 ℃空气煅烧。
9.根据权利要求5所述YAG透明陶瓷的致密化烧结方法，其特征在于：煅烧后的YAG粉体填充至不锈钢模具中，先在5MPa下双面压制成型，再在200 MPa冷等静压下成型，得到素坯。
10.根据权利要求5所述YAG透明陶瓷的致密化烧结方法，其特征在于：成型后的素坯在马弗炉中采用800-1100℃下煅烧5-10h，之后将样品置于真空炉中1500-1750℃真空气氛中烧结2-15h，真空度低于1.0×10-3Pa，再在1500-1780℃下热等静压烧结2-5h，所述热等静压烧结使用196MPa氩气介质，最后，在马弗炉中采用1100-1500℃空气或氧气气氛下热处理1-20 h，得到所述YAG透明陶瓷。
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