We prepared a layered antiferromagnet KNiB4O6F31 by hydrothermal synthesis, and characterized its structure and physical properties by X-ray diffraction, magnetization and specific heat measurements as well as thermal stability, FTIR and UV–vis–NIR measurements. 1 consists of layers of composition [NiB4O6F3]- separated by layers of K+ cations. And Ni2+ ions are arranged in slightly distorted triangular pattern in each [NiB4O6F3]- layer. The magnetic susceptibility measurements indicate no divergence between the zero-field-cooled and field-cooled curves down to 7.9 K, below which a long-range order takes place as verified by specific heat measurements. The M(H) curve linearly increases when the field is weak (below ∼2 T), confirming that the ground state of 1 is antiferromagnetic. At 7 T, the magnetization of 1 is 1.67 μB which is lower than the saturation magnetization.
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