采用全反模式的红外(ATR-IR)光谱实时研究了不同氘含量KH2-xDxPO4(DKDP)晶体的结晶过程,其中DKDP溶液氘含量范围为0到99％.通过υ1(PO4)和υ3(PO4)振动表征了DKDP结晶溶液中(H2PO4-)1-x(D2PO4-)x离子基团浓度的变化.υ1(PO4)振动强度的变化和υ3(PO4)振动宽度的变化说明生长溶液中的(H2PO4-)1-x(D2PO4-)x离子浓度随着测试时间延长而不断增大.同时,δ(P—O…H/D—O—P)振动峰的形成说明DKDP晶体的生长基元为(H2PO4-)n-x(D2PO4-)x离子团簇.波数在1448 cm-1到1653 cm-1范围内H—O—H和D—O—D振动强度的变化解释了DKDP晶体在结晶过程中氘含量分布不均的现象.“,”The crystallization of KH2-x Dx PO4 ( DKDP) crystals with different deuterium contents ranged from 0 to 99％ were investigated in solution by Attenuated Total Reflectance Infrared ( ATR-IR) spectroscopy. The ( H2 PO4 -) 1-x ( D2 PO4 -) x ionic groups were characterized by theυ1 ( PO4 ) andυ3 ( PO4 ) vibrations. The intensity changes of theυ1 ( PO4 ) vibration peaks and the broadened width changes of theυ3 ( PO4 ) vibration peaks indicate that the ( H2 PO4 -) 1-x ( D2 PO4 -) x concentration increases with the measurement time increases. Besides, the appearance ofδ( P—O…H/D—O—P) vibration illustrates the formation of ( H2 PO4 -) n-x ( D2 PO4 -) x clusters, which can be confirmed as growth unite. The intensity changes of the H—O—H and D—O—D vibration at the wavenumbers from 1448 cm-1 to 1653 cm-1 can illustrate the un-uniform distribution of deuterium con-tents in DKDP crystallization process.