▎ 摘　　要

NOVELTY - Preparation of graphene-nano-nickel thermoelectric composite thin film involves preparing sulfonated graphite from a surface-treated oxidized graphite, freeze-drying, preparing a dispersion (d1) by dispersing sulfonated graphite and polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer in ethylene glycol, mixing with dispersion (d2) of nickel chloride ethylene glycol solution, obtaining wave-absorbing material by reacting with e.g. ammonium persulfate, adding to deionized water, and electrodepositing the obtained solution on copper substrate. USE - Preparation of graphene-nano nickel thermoelectric thin film (claimed). ADVANTAGE - The method enables convenient preparation of graphene-nano nickel thermoelectric thin film having excellent electroconductivity. DETAILED DESCRIPTION - Preparation of graphene-nano-nickel thermoelectric composite thin film involves preparing a surface-treated oxidized graphite, adding 1 g surface-treated graphite oxide to a reactor containing 500 g deionized water at room temperature, placing reactor in an ultrasonic disperser, stirring for 10-15 minutes, adjusting pH of system to 11 with aqueous ammonia solution, heating to 70 degrees C, adding 5-10 g sodium borohydride aqueous solution to the reactor, ultrasonically oscillating for 30-60 minutes, cooling the resultant product to 15 degrees C, adding 25 g p-aminobenzenesulfonic acid, ultrasonically oscillating for 2-4 hours, leaving still for 3 hours, suction-filtering the resultant product to remove the solvent, washing 2 times or more with deionized water, redispersing filtrate in 400-1600 g deionized water, adding 1-4 g hydrazine hydrate, reacting at 80 degrees C for 12-24 hours, suction-filtering the product, washing 2 times or more with deionized water, drying the filtrate for 24-48 hours to obtain sulfonated graphite, freeze-drying 1-2 g sulfonated graphite at -10 degrees C to 30 degrees C, preparing a homogeneous dispersion (d1) by dispersing sulfonated graphite and 1-10 g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer in 500 ml ethylene glycol, preparing a dispersion (d2) by dissolving 20-40 ml 0.1 mol/ml nickel chloride ethylene glycol solution, 6-25 g polyvinylpyrrolidone and 10-50 g ammonium acetate in 500-1000 ml ethylene glycol, mixing dispersions (d1) and (d2), stirring, adjusting pH of the resultant product using aqueous ammonia to 9-11 to obtain a clear solution, placing 100 ml clear solution in a reactor, sealing, heating to 130 degrees C, heat-preserving for 2 hours, heating to 150 degrees C at a rate of 2-4 degrees C/minute, heat-preserving for 4 hours, heating the resultant product to 200 degrees C at a rate of 3-6 degrees C/minute, heat-preserving for 3 hours, cooling the resultant product to 180 degrees C at a rate of 5-7 degrees C/minute for 2 hours, heating the resultant product to 200 degrees C at rate of 3-6 degrees C/minute, heat-preserving for 7 hours, reacting, taking out the product, cooling to room temperature at a rate of 3-6 degrees C/minute, centrifuging the resultant powder for 10 minutes at a speed of 8000-10000 rpm, washing the resultant product with anhydrous ethanol and deionized water three times, vacuum drying at 50-70 degrees C for 24 hours, obtaining a product (p1), adding 5 g product (p1) and 5-10 g aniline monomer to a solution of dodecylbenzenesulfonic acid, ultrasonically dispersing for 65 minutes to form product (p2), dissolving 3 g ammonium persulfate in 80-120 ml distilled water, slowly dripping product (p2) in the resultant product, stirring-reacting for 15 hours, filtering the resultant product, washing with distilled water and ethanol until the filtrate is colorless, vacuum drying at 50-70 degrees C for 24-36 hours to obtain wave-absorbing material, adding the wave-absorbing material to deionized water, obtaining 5-25 g/L aqueous solution, mechanically stirring the resultant product for 10-15 minutes, ultrasonically dispersing at ultrasonic frequency of 30 Hz for 30-50 minutes, obtaining a homogeneous solution, placing the solution in a container, providing copper substrate as base material, successively treating base material with acetone, deionized water, methanol and deionized water, cleaning for 5-10 minutes, vacuum drying at 90-120 degrees C for 10-30 minutes, placing the substrate in the container as a negative electrode, providing iron film as positive electrode, and forming thermoelectric thin film by electrodepositing in electrophoretic device. Surface-treated oxidized graphite is prepared by forming graphite powder having size of 50-200 mesh, adding the resultant product to 35 %mass hydrochloric acid solution, stirring for 30 minutes, washing with deionized water to neutral, drying, adding dried graphite powder, potassium persulfate and phosphorus pentoxide into concentrated sulfuric acid, obtaining mixture (m1) having pH of 1.5, heating, diluting with distilled water to pH of 3.6, filtering, drying at room temperature, adding dried mixture (m2) to concentrated nitric acid for 45-60 minutes, stirring, adding potassium permanganate at -8 degrees C, stirring for 30 minutes, cooling to -12 degrees C, adding potassium permanganate, stirring the resultant product for 30 minutes, adding potassium permanganate at -15 degrees C, stirring for 20 minutes, filtering, drying, heat treating in a muffle furnace at 1100 degrees C for 10-20 seconds, further heat treating at 1150 degrees C for 15-20 seconds and at 1180 degrees C for 20-30 seconds, obtaining expanded pre-oxidized graphite mixture, heating the resultant product to 40 degrees C, reacting for 3 hours, adding distilled water, and hydrogen peroxide in volume ratio of 4-20:1 for 10-60 minutes, reacting, centrifuging at speed of 8000-10000 rpm for 10 minutes, washing the resultant product with hydrochloric acid solution, dialyzing for 7-8 days to obtain oxidized graphite, dissolving oxidized graphite in dimethyl sulfoxide, adding N-hydroxysuccinimide and self-made surface treatment agent at 35 degrees C for 2 hours, suction-filtering the resultant product, washing and drying. The mass ratio of graphite powder, potassium persulfate and phosphorus pentoxide is 1-3:1-2:1-2:5-10. The mass ratio of mixture (m2) and concentrated nitric acid is 1-4:50-100. The mass ratio of potassium permanganate in three additions is 1:2:3. The mass ratio of dried mixture and total potassium permanganate is 1-2:10-15. The mass ratio of the product (p1) and dodecylbenzenesulfonic acid is 1-1.5:8-15.