▎ 摘　　要

NOVELTY - Preparation of graphene-loaded 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-loaded nano-nickel thermoelectric composite thin film (claimed). ADVANTAGE - The method enables convenient preparation of graphene-loaded nano-nickel thermoelectric composite thin film having excellent conductivity. DETAILED DESCRIPTION - Preparation of graphene-loaded 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 dodecylbenzene sulfonic 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, ultrasonically cleaning for 5-10 minutes, vacuum drying the cleaned base material 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 at voltage of 30-120 V in constant pressure mode for 30-90 minutes. The surface-treated oxidized graphite is prepared by forming graphite powder having size of 50-200 mesh using graphite, adding the resultant product to 35 %mass hydrochloric acid solution, stirring for 30 minutes, repeatedly washing with deionized water to neutral, drying, adding dried graphite powder, potassium persulfate and phosphorus pentoxide into concentrated sulfuric acid, obtaining a mixture (m1) having pH of 1.5, heating, diluting with distilled water to a pH of 3.6, filtering, drying at room temperature, adding dried mixture (m2) to concentrated nitric acid for 45-60 minutes, homogeneously 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, obtaining an expanded pre-oxidized graphite mixture, heating the resultant product in an incubator to 40 degrees C, reacting for 3 hours, adding distilled water, heat-preserving at 40 degrees C for 2.5 hours, adding distilled water in an amount of 1-1.5 times the previously added 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 in an amount of 10-50 times the volume of the centrifuged product, 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.