Nickel doped copper sulfide nano material as well as preparation method and application thereof
A nanomaterial, copper sulfide technology, applied in the field of medical nanomaterials to achieve the effect of increasing the ability of magnetic resonance imaging
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Embodiment 1
[0152] combine figure 1 The preparation process flowchart of nickel-doped copper sulfide nano-material shown, the invention provides a kind of preparation method of nickel-doped copper sulfide nano-material, comprises the following steps:
[0153] (1) Preparation of S precursor: Add S powder (calculated as S element, 2 mmol) into a 10 mL glass bottle in the glove box, then add oleylamine (8 mL, density 0.813 g / mL); Cap the vial and remove from the glove box, sonicate until S is completely dissolved;
[0154] (2) CuCl 2 (according to Cu element, the addition amount is 1.6mmol), NiCl 2 (Based on Ni element, the addition amount is 0.4mmol) and oleylamine (4mL, density 0.813g / mL) were added to a 25mL three-neck round bottom flask, vacuumed for 30min, and then passed through N 2 and heated to 180°C, then inject the S precursor solution obtained in step (1) into the solution in the reactor (injection speed is 4ml / s), cool down to 150°C and keep warm for 0.5 hours, then cool to ro...
Embodiment 2
[0167] (1) Preparation of S precursor: In the glove box, thiourea (according to S element, the addition amount is 2mmol) is added in the 10mL glass bottle, then adds oleic acid (20mL); Take it out from the glove box, and sonicate until S is completely dissolved;
[0168] (2) Copper nitrate (according to Cu element, the addition amount is 1.998mmol mmol), nickel nitrate (according to Ni element, the addition amount is 0.002mmol) and oleic acid (10mL) were added in a 25mL three-neck round-bottomed flask, pumped Vacuum for 45min, then pass N 2 and heated to 160°C, then inject the S precursor solution obtained in step (1) into the solution in the reactor (injection speed is 2.5ml / s), cool down to 120°C and keep it warm for 20 minutes, then cool to room temperature;
[0169] (3) After the reaction product is cooled to room temperature, centrifuge at 3000g / min to remove large particles, then add absolute ethanol to precipitate for 5 minutes according to 3 times the volume of the re...
Embodiment 3
[0171] (1) Preparation of S precursor: Add sodium thiosulfate (according to S element, the addition amount is 5mmol) into a 25mL glass bottle in the glove box, and then add oleylamine and oleic acid (volume ratio is 8:2) The mixed solution (12.5mL); Then cap the glass vial and take it out from the glove box, sonicate until S dissolves completely;
[0172] (2) Copper sulfate (according to Cu element, the addition amount is 1mmol), nickel sulfate (according to Ni element, the addition amount is 4mmol) and a mixed solvent of oleylamine and oleic acid (volume ratio is 8:2) (5mL ) was added to a 25mL three-neck round bottom flask, vacuumed for 15min, and then passed through N 2 and heated to 220°C, then inject the S precursor solution obtained in step (1) into the solution in the reactor (injection speed is 10ml / s), cool down to 130°C and keep warm for 12 minutes, then cool to room temperature;
[0173] (3) After the reaction product is cooled to room temperature, centrifuge at 20...
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