A kind of preparation method of spiro-ometad monoclinic crystal
A monoclinic crystal, crystallization technology, applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problem of no growth and so on
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Embodiment 1
[0022] The present embodiment provides a kind of preparation method of Spiro-OMeTAD monoclinic crystal, comprises the following steps:
[0023] (1) Weigh 15mg of Spiro-OMeTAD powder drug, dissolve in 3mL of 1,2-dichloroethane solvent, and mix well;
[0024] (2) Filter the solution obtained in step (1) using a filter head with a pore size of 0.22 μm, and then stand in the sun for 1 hour until the solution changes from colorless to red;
[0025] (3) Put the red solution into a container containing 5mL of methanol solution, seal it and let it stand for 7 days to crystallize.
Embodiment 2
[0027] The present embodiment provides a kind of preparation method of Spiro-OMeTAD monoclinic crystal, comprises the following steps:
[0028] (1) Weigh 15mg of Spiro-OMeTAD powder drug, dissolve in 1mL 1,2-dichloroethane solvent, and mix well;
[0029] (2) Filter the solution obtained in step (1) using a filter head with a pore size of 0.22 μm, and then stand in the sun for 1 hour until the solution changes from colorless to red;
[0030] (3) Put the red solution into a container containing 3mL of methanol solution, seal it and let it stand for 7d to crystallize.
Embodiment 3
[0032] The present embodiment provides a kind of preparation method of Spiro-OMeTAD monoclinic crystal, comprises the following steps:
[0033] (1) Weigh 15mg of Spiro-OMeTAD powder drug, dissolve in 15mL 1,2-dichloroethane solvent, and mix well;
[0034] (2) Filter the solution obtained in step (1) using a filter head with a pore size of 0.22 μm, and then stand in the sun for 1 hour until the solution changes from colorless to red;
[0035] (3) Put the red solution into a container containing 50mL of methanol solution, seal it and let it stand for 7d to crystallize.
[0036] Use X-ray diffractometer to test the crystal structure that embodiment 1 prepares, as figure 1 As shown, the Spiro-OMeTAD single crystal prepared and grown by the present invention is a monoclinic crystal, and the unit cell parameters are: α=90°, β=112°, γ=90°; if figure 2 As shown, through the I-V test of the conductive atomic force microscope, the current response of the monoclinic crystal prepar...
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