The invention discloses a chiral mononuclear nine-coordinated beta-diketone complex which has a molecular formula of Nd(tta)3L, wherein L is [(-)-2,6-bis(4,5-pinene-2-pyridyl)pyridine]; tta is a 1-thiophene trifluoromethyl1,3-butanedione anion. The preparation method of the chiral mononuclear nine-coordinated beta-diketone complex comprises the following steps: dissolving the 1-thiophene trifluoromethyl1,3-butanedione in absolute ethyl alcohol, adding ammonium hydroxide and a NdCl3.6H2O aqueous solution to generate precipitates, filtering, washing and drying to obtain Nd(tta)3.2H2O, adding an acetonitrile solution of the Nd(tta)3.2H2O into an acetone solution in which a trident nitrogenous chiral chelation organism L, stirring and filtering to obtain pink crystals after 3 days, and filtering, washing and drying to obtain the target product. As the preparation process is simple and the reaction is carried out at a normal temperature, the complex has favorable near-infrared luminescence property and is expected to serve as a near-infrared luminescence material which has wide application prospect in the aspects of lasers and the like.