The method of multiphase synthesis of NH4Hf2F9 for accelerator mass spectrometry (AMS) measurement was researched. The structure and composition of NH4Hf2F9 powder were characterized by XRD, SEM, XPS and TG-DTA. When the NH4Hf2F9 powder was heated at 573 K for 1 h, the powder phase was still NH4Hf2F9. After being heated at 773, 973, 1173 and 1373 K for 1 h, respectively, they all transformed to HfO2. When the temperature was above 573 K, NH4Hf2F9 powder began to decompose. When the temperature reached 1073 K, the weight loss of NH4Hf2F9 powder was about 78%. The powder shape was irregular, and powder size was between 5 and 20 μm in the SEM images. The XPS results show that there were Hf, N and Hf in NH4Hf2F9 powder, and Hf mainly existed in quadrivalent state (+ 4).%研究了加速器质谱测量用NH4Hf2F9的制备方法,用XRD,SEM,XPS和TG-DTA表征其结构和组成.结果表明:NH4Hf2F9样品在573K热处理1h后物相并未变化,而在773,973,1173,1373K热处理1h后物相则都转变为HfO2-TG—DTA的分析表明从573K开始NH4Hf2F9样品逐渐开始分解,至1073K时失重约78%.样品微观形貌为不规则的固体颗粒,颗粒的粒径分布较大,范围在5~20m之间.粉末样品主要含有Hf,N和F元素,其中Hf主要以(+4)价存在.
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