Preparation method of flaky iron sulfide single crystal nano-material
A technology of ferric tetrasulfide and nano-single crystal, which is applied in the direction of chemical instruments and methods, single crystal growth, single crystal growth, etc., can solve the problem that the morphology of ferric tetrasulfide is difficult to control, and there is no monodisperse ferric tetrasulfide nano single crystal. Crystal and phase purity problems, etc., to achieve the effect of controllable particle size and shape, regular shape, and uniform size
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Embodiment 1
[0037] Example 1 A preparation method of sheet-shaped iron tetrasulfide nanometer single crystal, comprising the following steps:
[0038] ⑴Mix the iron source—ferrous chloride with a concentration of 0.05mol / L and trioctylphosphine oxide (TOPO) at a molar ratio of 1:1.5, and dissolve in oleylamine, stir and pass the purity to 98.5% After removing oxygen from the above nitrogen or argon gas, an iron source precursor is obtained.
[0039] Among them: the mass volume ratio (g / ml) of iron source and oleylamine is 1:50.
[0040] (2) Heating the iron source precursor to 120° C. in an oil bath and stirring for 1.5 hours to obtain an iron source solution.
[0041] (3) Dissolve the sulfur source—sulfur powder in oleylamine, and after stirring and passing argon or nitrogen with a purity of more than 98.5% to remove oxygen, obtain a sulfur source solution.
[0042] Among them: the mass volume ratio (g / ml) of sulfur source and oleylamine is 1:50.
[0043] (4) Heating the sulfur ...
Embodiment 2
[0047] Example 2 A preparation method of sheet-shaped iron tetrasulfide nanometer single crystal, comprising the following steps:
[0048] ⑴Mix the iron source—ferrous chloride with a concentration of 0.5 mol / L and trioctylphosphine oxide (TOPO) at a molar ratio of 1:3, and dissolve in oleylamine, stir and pass the purity to 98.5% After removing oxygen from the above nitrogen or argon gas, an iron source precursor is obtained.
[0049] Among them: the mass volume ratio (g / ml) of iron source and oleylamine is 1:150.
[0050] (2) Heating the iron source precursor to 170° C. in an oil bath and stirring for 0.5 hours to obtain an iron source solution.
[0051] (3) Dissolve the sulfur source—thiourea in oleylamine, and after stirring and passing argon or nitrogen with a purity of more than 98.5% to remove oxygen, obtain a sulfur source solution.
[0052] Among them: the mass volume ratio (g / ml) of sulfur source to oleylamine is 1:100.
[0053] (4) Heating the sulfur source...
Embodiment 3
[0057] Example 3 A preparation method of sheet-shaped iron tetrasulfide nanometer single crystal, comprising the following steps:
[0058] ⑴Mix the iron source—ferrous chloride with a concentration of 0.25 mol / L and trioctylphosphine oxide (TOPO) at a molar ratio of 1:2.5, and dissolve in oleylamine, stir and pass the purity to 98.5% After removing oxygen from the above nitrogen or argon gas, an iron source precursor is obtained.
[0059] Among them: the mass volume ratio (g / ml) of iron source and oleylamine is 1:100.
[0060] (2) Heating the iron source precursor to 150° C. in an oil bath and stirring for 1 hour to obtain an iron source solution.
[0061] (3) Dissolve the sulfur source—sulfur powder in oleylamine, and after stirring and passing argon or nitrogen with a purity of more than 98.5% to remove oxygen, obtain a sulfur source solution.
[0062] Among them: the mass volume ratio (g / ml) of sulfur source to oleylamine is 1:75.
[0063] (4) Heating the sulfur so...
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