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Preparation method of poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene

A technology of polysilsesquioxane and silsesquioxane, which is applied in the field of preparation of metal-coated graphene and polyaminopropylsilsesquioxane-doped nickel-coated graphene, can solve problems The development direction of palladium nickel plating, high resistivity of graphene, pollution of precious metal palladium, etc., to achieve excellent electrical conductivity and electromagnetic shielding performance, promote dispersion, and high electrical conductivity

Active Publication Date: 2017-06-23
SOUTH CHINA UNIV OF TECH
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  • Claims
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Problems solved by technology

[0003] The above-mentioned prior art utilizes the electroless plating method to obtain nickel-coated graphene, but palladium chloride is used, not only the process is complex, the processing cost is high, and the environment is caused serious pollution of precious metal palladium, which is contrary to palladium-free plating. The development direction of nickel; in addition, sodium hypophosphite is used in the reducing agent, and the resulting coating contains a relatively high content of phosphorus, so that the resulting graphene resistivity is still high

Method used

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  • Preparation method of poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene
  • Preparation method of poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene

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Embodiment 1

[0028] (1) Preparation of polyaminopropylsilsesquioxane solution: add 10g of γ-aminopropyltriethoxysilane (brand: CG-550, Nanjing Chengong Organic Silicon Material Co., Ltd.), 100g of absolute ethanol (analytical grade ) and 5g deionized water in a 250ml three-neck flask, stirred and reacted at room temperature for 5 hours to obtain a polyaminopropyl silsesquioxane solution;

[0029] (2) Preparation of inorganic nickel salt-hydrazine hydrate complex solution: at room temperature, sequentially add 1g of nickel sulfate (analytical pure), 4g of 50% hydrazine hydrate (analytical pure) and 8g of deionized water into a 50ml beaker, and mix well to get final product;

[0030] (3) Preparation of graphite oxide: under ice bath conditions, add 1g of graphite, 6g of potassium permanganate, 25g of concentrated sulfuric acid with a mass concentration of 98% and 6g of phosphoric acid with a mass concentration of 85%, and heat up to 55°C after stirring for 1 hour , reacted for 8 hours, then ...

Embodiment 2

[0037] (1) Preparation of polyaminopropyl silsesquioxane solution: add 10g N-(β- Aminoethyl) -γ- Aminopropyltrimethoxysilane (trademark: CG-792, Nanjing Chengong Organic Silicon Material Co., Ltd.), 80g of absolute ethanol (analytical grade) and 10g of deionized water were placed in a 250ml three-necked flask, stirred and reacted at room temperature for 3 hours, Obtain polyaminopropyl silsesquioxane solution;

[0038] (2) Preparation of inorganic nickel salt-hydrazine hydrate complex solution: at room temperature, sequentially add 1g of nickel chloride (analytical pure), 6g of 50% hydrazine hydrate (analytical pure) and 5g of deionized water into a 50ml beaker, and mix well to obtain ;

[0039] (3) Preparation of graphite oxide: under ice bath conditions, add 1g of graphite, 5g of potassium permanganate, 15g of concentrated sulfuric acid with a mass concentration of 98% and 5g of phosphoric acid with a mass concentration of 85%, and heat up to 65°C after stirring for 2 hour...

Embodiment 3

[0042] (1) Preparation of polyaminopropyl silsesquioxane solution: add 10g N- Aminoethyl -γ- Aminopropyltrimethoxysilane, 90g of absolute ethanol (analytical grade) and 8g of deionized water were placed in a 250ml three-necked flask, stirred and reacted at room temperature for 4 hours to obtain a polyaminopropylsilsesquioxane solution;

[0043] (2) Preparation of inorganic nickel salt-hydrazine hydrate complex solution: at room temperature, sequentially add 1g of nickel acetate (analytical pure), 5g of 50% hydrazine hydrate (analytical pure) and 6g of deionized water into a 50ml beaker, and mix well to get final product;

[0044] (3) Preparation of graphite oxide: under ice bath conditions, add 1g of graphite, 4g of potassium permanganate, 20g of concentrated sulfuric acid with a mass concentration of 98% and 4g of phosphoric acid with a mass concentration of 85%, and heat up to 60°C after stirring for 4 hours , reacted for 12 hours, then poured into 200g of ice water, added...

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Abstract

The invention discloses a preparation method of poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene. The method comprises the following steps: mixing graphite oxide and absolute ethyl alcohol; adding a poly(aminopropylphenyl) silsesquioxane solution and stirring at 50 DEG C to 70 DEG C for 3h to 5h; transferring into an ultrasonic cleaner and carrying out ultrasonic treatment; carrying out the ultrasonic treatment, and standing and filtering to obtain poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene turbid liquid; adding an inorganic nickel salt-hydrazine hydrate complexing solution into the obtained poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene turbid liquid; stirring and reacting at 60 DEG C to 80 DEG C; centrifuging and separating; washing and drying in vacuum to obtain the poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene. According to the palladium-free preparation method provided by the invention, the electrical resistivity of the poly(aminopropylphenyl) silsesquioxane doped nickel-coated graphene is lower than 0.1ohm.cm, the saturation magnetization intensity is more than 3.5A.m<2> / kg and the magnetic conductivity is more than 0.3mH / m.

Description

technical field [0001] The present invention relates to a method for metal-coated graphene, in particular to a palladium-free method for coating nickel on the surface of graphene, in particular to a polyaminopropyl silsesquioxane-doped nickel-coated graphene The preparation method belongs to the technical field of inorganic material modification. Background technique [0002] Graphene is made of carbon atoms and is only one atomic thickness two-dimensional crystal , has the advantages of low density, electrical and thermal conductivity, and good stability, but its magnetic loss is weak and its magnetic permeability is low. Metal nickel has high electrical conductivity, high magnetic permeability, and good electromagnetic shielding effect. Using electroless plating to coat metal nickel on the surface of graphene can endow graphene with a certain degree of magnetic permeability. The invention patent of Central South University of Forestry and Technology (CN201310296080.5) di...

Claims

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Application Information

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IPC IPC(8): C08K9/10C08K9/04C08K9/02C08K3/04
CPCC08K3/04C08K9/02C08K9/08C08K9/10C08K2201/001
Inventor 刘述梅徐弘灏赵建青陈振江林朝炀林永强
Owner SOUTH CHINA UNIV OF TECH
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