Preparation method for SnO2/ZnO compound micro-nano fibers and product thereof

[0031] Example 1

[0032] (1) Add 0.7419 g of zinc nitrate hexahydrate (Zn(NO 3 ) 2 ∙6H 2 O) and 0.8188 g of 2-methylimidazole were respectively dissolved in 50mL methanol solvent, stirred to obtain a transparent solution, mixed well and stirred for 1 h, after standing for 24 h, centrifuged and washed with methanol solvent for 3 times, placed in an evaporating dish Dry naturally to obtain Zif-8 product;

[0033] (2) Dissolve 0.0041 g of diammonium hydrogen citrate, 0.0082 g of octadecylamine, 0.0186 g of ethyl cellulose and 0.0068 g of Zif-8 in 2.0 mL of ethanol solvent, and stir to obtain a transparent solution;

[0034] (3) Add 0.3541 g of tin tetrachloride pentahydrate (SnCl 4 ∙5H 2 O) and 0.7000 g of PVP were added to a mixed solvent of 1.0 mL of ethanol and 4.0 mL of DMF, stirred to obtain a transparent solution, and then slowly added dropwise to the solution obtained in (2) at 0.2 mL/min, and stirred at room temperature for 10 h The precursor spinning solution is obtained, and the precursor fiber is obtained by electrospinning. The spinning parameters are: positive voltage is 18 KV, negative voltage is 0.5 KV, receiving distance is 20 cm, and syringe advancing speed is 0.002 mm/s;

[0035] (4) Put the precursor fiber in a muffle furnace, raise the temperature from room temperature to 600 ℃ at a temperature rise rate of 1 ℃/min, and keep it for 2 hours. After the sample is cooled in the furnace, SnO is obtained. 2 /ZnO composite micro-nano fiber.

[0036] The XRD results of the product are as follows figure 1 As shown in the figure, it can be seen that all the diffraction peaks are consistent with the standard XRD card (41-1445), which proves that the obtained product is tetragonal SnO2. Due to the low addition of Zif-8, the XRD detection limit There is no obvious ZnO crystal phase in the XRD results; the SEM of the product is as figure 2 with 3 As shown in the figure, it can be seen that the product obtained by the present invention has SnO on the surface of the fiber 2 Granular SnO 2 /ZnO composite micro-nano fiber structure, the main fiber is made of SnO 2 It is compounded with ZnO nanoparticles, the fiber diameter is 0.12-0.14 μm, the spherical structure on the fiber surface is composed of SnO2 nanoparticles, and the diameter of the spherical structure is 0.12-0.17 μm; the TEM of the product is as Figure 4 As shown, it can be seen from the figure that the morphology of the sample is basically consistent with the SEM result; the HRTEM of the product is as Figure 5 As shown in the figure, it can be seen that the main fiber part is made of SnO 2 Compounded with ZnO nanoparticles, the spherical structure on the fiber surface is made of SnO 2 Composition of nanoparticles.

[0037] Example 2

[0038] (1) Add 0.7419 g of Zn(NO 3 ) 2 ∙6H 2 O and 0.7269 g of 2-methylimidazole were respectively dissolved in 46 mL of methanol solvent and stirred to obtain a transparent solution. After mixing, stir for 2 h. After standing for 24 h, after centrifugal washing with methanol solvent for 3 times, place it in an evaporating dish. Dry naturally to obtain Zif-8 product;

[0039] (2) Dissolve 0.0010 g of diammonium hydrogen citrate, 0.0014 g of octadecylamine, 0.0037 g of ethyl cellulose and 0.0014 g of Zif-8 in 2.0 mL of ethanol solvent, and stir to obtain a transparent solution;

[0040] (3) Add 0.3541 g of SnCl 4 ∙5H 2 O and 0.6200 g of PVP were added to a mixed solvent of 1.1 mL of ethanol and 4.4 mL of DMF, stirred to obtain a transparent solution, and then slowly added dropwise to the solution obtained in (2) at 0.3 mL/min, and stirred at room temperature for 10 h to obtain The precursor spinning solution, the precursor fiber is obtained by the electrospinning method, the spinning parameters are: the positive voltage is 16KV, the negative voltage is 0.5KV, the receiving distance is 18 cm, and the injector advancing speed is 0.001 mm/s;

[0041] (4) Put the precursor fiber in a muffle furnace, raise it from room temperature to 550 ℃ at a temperature rise rate of 1 ℃/min, and keep it for 1 hour. After the sample is cooled in the furnace, the surface of the fiber has SnO 2 Granular SnO 2 /ZnO composite micro-nano fiber structure, the main fiber is made of SnO 2 Compounded with ZnO nanoparticles, the fiber diameter is 0.08-0.10 μm, and the spherical structure on the fiber surface is made of SnO 2 The diameter of the spherical structure is 0.08-0.12 μm.

[0042] Example 3

[0043] (1) Add 0.7419 g of Zn(NO 3 ) 2 ∙6H 2 O and 0.9009 g of 2-methylimidazole were respectively dissolved in 48 mL of methanol solvent and stirred to obtain a transparent solution. After mixing evenly, stir for 1 h. After standing for 24 h, after centrifugal washing with methanol solvent for 3 times, place in an evaporating dish. Dry naturally to obtain Zif-8 product;

[0044] (2) Dissolve 0.0325 g of diammonium hydrogen citrate, 0.0594 g of octadecylamine, 0.1327 g of ethyl cellulose and 0.0431 g of Zif-8 in 2.0 mL of ethanol solvent, and stir to obtain a transparent solution;

[0045] (3) Add 0.3541 g of SnCl 4 ∙5H 2 O and 0.7700 g of PVP were added to the mixed solvent of 1.2 mL of ethanol and 4.8 mL of DMF, stirred to obtain a transparent solution, and then slowly added dropwise to the solution obtained in (2) at 0.2 mL/min, and stirred at room temperature for 8 h to obtain The precursor spinning solution, the precursor fiber is obtained by the electrospinning method, the spinning parameters are: positive voltage is 17 KV, negative voltage is 0.5 KV, receiving distance is 22 cm, and syringe advancing speed is 0.003 mm/s;

[0046] (4) Put the precursor fiber in a muffle furnace, raise it from room temperature to 650 ℃ at a heating rate of 2 ℃/min, and keep it for 4 hours. After the sample is cooled in the furnace, the surface of the fiber has SnO 2 Granular SnO 2 /ZnO composite micro-nano fiber structure, the main fiber is made of SnO 2 Compounded with ZnO nanoparticles, the fiber diameter is 0.95-1.2 μm, and the spherical structure on the fiber surface is made of SnO 2 Composed of nanoparticles, the diameter of the spherical structure is 1.7-2.2 μm.