Preparation method of three-dimensional graphene/silver nanoflower stretchable biosensor material

Preparation method of three-dimensional graphene/silver nanoflower stretchable biosensor material

  • CN 106,546,720 B
  • Filed: 10/31/2016
  • Issued: 05/05/2020
  • Est. Priority Date: 10/31/2016
  • Status: Active Grant
First Claim
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1. A preparation method of a three-dimensional graphene/silver nanoflower stretchable biosensor material is characterized by comprising the following steps:

  • the method comprises the following steps;

    1) putting foamed nickel with the size of 8cm multiplied by 8cm into a tubular furnace;

    2) opening a vacuum pump to pump the air pressure of the tube furnace to a limit vacuum state of 3 multiplied by 10-6Torr;

    3) Maintaining vacuum state 3X 10-6After 15 minutes of Torr, the gas pressure of the quartz tube was raised to 3X 10-3Torr;

    4) Setting the hydrogen flow meter to be 100sccm, and injecting hydrogen into the vacuum cavity;

    5) after the temperature of the tube furnace is raised to 300 ℃

    , keeping the temperature for 20 minutes for annealing;

    6) after the temperature of the tubular furnace is raised to 1000 ℃

    , injecting methane into the vacuum cavity, setting the gas flow meter to be 200sccm, and staying for 30 minutes for growth;

    7) closing the methane gas flowmeter and rapidly cooling the temperature of the tubular furnace to room temperature at a speed of 50 ℃

    /min;

    8) closing the hydrogen flowmeter and the vacuum pump;

    9) opening the valve, and filling the quartz tube with air to an atmospheric pressure state;

    10) opening a vacuum interface of the quartz tube, and taking out the foam nickel deposited with the graphene;

    11) FeCl is added3Adding the etching solution into deionized water according to a certain mass for dissolving to prepare etching solution FeCl with the concentration of 5mol/L3

    12) The prepared graphene/foamed nickel is soaked in 5mol/L FeCl at the temperature of 20 DEG C3In solution for 140 minutes;

    13) observing the morphology of the graphene/foamed nickel until the nickel metal is completely dissolved to obtain three-dimensional graphene;

    14) cleaning three-dimensional graphene in deionized water for 3 times, wherein each time lasts for 10 minutes;

    15) stretching the PDFS elastic substrate to 1.5 to 4 times of the original length along one direction, or stretching to 2 to 10 times of the original area along two orthogonal directions, and sticking the stretched elastic substrate on a circular hollow bracket;

    16) pressing the elastic substrate on the surface of the flexible graphene structure tightly, and lightly pressing for 3 seconds;

    17) slowly and lightly lifting from one side surface of the substrate, and fishing out the three-dimensional graphene composite structure by utilizing small contact force between the graphene and the substrate;

    18) airing in a vacuum drying oven for 3 hours;

    19) taking down the elastic substrate covered with the three-dimensional graphene from the hollow round or square bracket, and adhering one side of the elastic substrate to the bracket;

    20) naturally recovering for 5 hours in a vacuum drying oven to recover the original size;

    21) soaking in 0.02mol/L stannous chloride solution for 2 minutes, then washing with deionized water for 2 minutes, taking out, and naturally drying;

    22) soaking in 0.02mol/L silver nitrate solution for 2 minutes, then washing with deionized water for 2 minutes, taking out, and naturally drying;

    repeating the steps

         21),

         22) three times;

    23) soaking in 0.1mol/L ascorbic acid and 0.01mol/L silver nitrate mixed solution for 8 minutes, cleaning with deionized water for 2 minutes, taking out, and naturally drying to obtain the final product.

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