Preparation method of composite material based on metal organic framework and carbon nanotubes, and preparation method of device
A metal-organic framework and carbon nanotube technology, which can be applied in the manufacture/processing of thermoelectric devices, and lead-out materials of thermoelectric device nodes, etc. effect of value
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[0056] The preparation process of the present invention is specifically as follows:
[0057] (1)Ni 3 (HITP) 2 Material preparation process:
[0058] 1.1 Disperse 141.9mg HATP·6HCl (0.267mmol) in 20-50mL deionized water, and record it as liquid A;
[0059] 1.2 Add 95.7mg NiCl 2 ·6H 2 O (0.4mmol) was dispersed in 20-50mL deionized water, and 2-6mL ammonia water was added (the mass concentration of ammonia water was 25%), which was recorded as liquid B;
[0060] 1.3 Place liquid A in an oil bath at 40-80°C, add liquid B to make it evenly mixed;
[0061] 1.4 Air bubbling for 25-60 minutes;
[0062] After 1.5, react at reflux under nitrogen protection for 1-4 hours;
[0063] 1.6 The solid obtained by the reaction is centrifuged and washed three times with ethanol, acetone and deionized water;
[0064] 1.7 Disperse the obtained powder in deionized water and reflux at 105°C for 20-40 hours (change the water once every 10-15 hours);
Embodiment 1
[0090] (1)Ni 3 (HITP) 2 Material preparation process:
[0091] 1.1) Disperse 141.9 mg of HATP·6HCl (0.267 mmol) in 30 ml of deionized water, and record it as liquid A;
[0092] 1.2) 95.7mg NiCl 2 ·6H 2 O (0.4 mmol) was dispersed in 30 milliliters of deionized water, and 3 milliliters of ammonia water was added (the mass concentration of ammonia water was 25%), which was recorded as liquid B;
[0093] 1.3) Place liquid A in a 65°C oil bath, add liquid B to mix evenly;
[0094] 1.4) Air bubbling for 45 minutes;
[0095] 1.5) then react for 2 hours under nitrogen protection reflux;
[0096] 1.6) The solid obtained by the reaction is centrifuged and washed three times with ethanol, acetone and deionized water;
[0097] 1.7) Disperse the obtained powder in deionized water, and reflux at 105°C for 36 hours (change the water every 12 hours);
[0098] 1.8) Then reflux with acetone at 65°C for 3 hours;
[0099] 1.9) The powder sample obtained by the reaction is repeatedly wash...
Embodiment 2
[0128] Ni 3 (HITP) 2 Preparation of materials:
[0129] 1.1) Disperse 0.267mmol HATP·6HCl in deionized water to obtain liquid A; wherein, the ratio of HATP·6HCl to deionized water is 0.267mmol: 20mL;
[0130] 0.4mmol NiCl 2 ·6H 2 O is dispersed in deionized water, and ammonia water is added to obtain liquid B; among them, NiCl 2 ·6H 2 O, the ratio of deionized water to ammonia water is 0.4mmol: 30mL: 2mL, and the mass concentration of ammonia water is 25%.
[0131] 1.2) Heat liquid A to 40°C, then add liquid B, and mix evenly; air bubbles for 25 minutes, and then reflux reaction under nitrogen protection for 4 hours to obtain a solid, which is post-treated to obtain Ni 3 (HITP) 2 Material.
[0132] N-type Ni 3 (HITP) 2 Preparation of / CNT composites:
[0133] (1) Carbon nanotubes (10mg) are mixed with sodium dodecylbenzenesulfonate, then added to the solvent, ultrasonically treated to obtain a carbon nanotube dispersion, and an N-type dopant is added to the carbon n...
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