降低m-CVDZnS多晶残余应力的带压退火研究  

Pressure Annealing Study for Reducing Residual Stress of m-CVDZnS Products

作　　者：周杰明 黎建明[2] 李冬旭 赵永田[2] 杨海[1,2] 魏乃光[1,2] ZHOU Jieming;LI Jianming;LI Dongxu;ZHAO Yongtian;YANG Hai;WEI Naiguang(Beijing General Research Institute of Nonferrous Metals,Beijing 100088,China;Beijing General Research Institute of Nonferrous Metals Guojing Advanced Materials Co.,Ltd.,Sanhe 065201,Hebei,China)

机构地区：[1]北京有色金属研究总院,北京100088 [2]北京有色金属研究总院有研国晶辉新材料有限公司,河北三河065201

出　　处：《材料导报》2022年第8期72-75,共4页Materials Reports

摘　　要：硫化锌(ZnS)具有较高的红外透过率及良好的力学、热学和光学等综合性能,经热等静压透明化处理后得到的多光谱硫化锌(m-CVDZnS)透射范围更宽(0.3~13μm),满足复合制导的需求,是红外双波段飞行器观察窗口和头罩的关键材料。而m-CVDZnS多晶中的残余应力直接影响窗口和头罩的光学均匀性和光学成像质量。本工作在热等静压设备中对CVDZnS多晶样品进行原位退火,采用的保护气体Ar气达到热等静压高温恒温所需压力后,退火过程不再进行充压或泄压(带压退火)。退火样品为多个尺寸约120 mm×165 mm×10.2 mm的m-CVDZnS多晶抛光样品,典型带压退火的优化工艺如下:高温退火条件采用990℃/150 MPa,结合600℃恒温和慢降温至室温退火。样品应力双折射测量结果表明,带压退火处理使残余应力明显减小,应力双折射平均值从12~13 nm/cm减少到3~5 nm/cm,降幅约100%;退火处理后应力分布均匀性明显提高。Zinc sulfide(ZnS)has high infrared transmittance and good mechanical,thermal and optical properties.The multi-spectral zinc sulfide(m-CVDZnS)has a wider transmission range(0.35—13μm)after hot isostatic pressing,meeting the needs of composite guidance,and is the key material for the infrared dual-band aircraft observation windows and domes.The residual stress in the m-CVDZnS polycrystal directly affects the optical uniformity of the windows and domes and the optical imaging quality.In this work,the in-situ annealing of CVDZnS poly-crystalline samples in the hot isostatic pressing equipment is carried out.After the protective Ar gas reaches the pressure required by the hot isostatic pressing at a constant high temperature,the annealing process is no longer carried out for pressure charging or pressure relief,ie.stress annealing.The annealing samples are a number of m-CVDZnS polycrystalline polished samples with a size of about 120 mm×165 mm×10.2 mm.The optimized process of typical pressure annealing is as follows:high temperature annealing conditions using 990℃/150 MPa,combined with 600℃constant temperature annealing and slow cooling annealing,Ar gas used as shielding gas during the whole annealing treatment.The results of sample annealing stress birefringence measurement show that the residual stress after the annealing treatment decreases significantly with the average value of stress birefringence reduced from 12—13 nm/cm to 3—5 nm/cm,which is approximately 100%reduction.The uniformity of stress distribution after annealing treatment is improved markedly.

关 键 词：硫化锌多晶 残余应力 应力双折射 带压退火 

分 类 号：TN213[电子电信—物理电子学]