A kind of silver-colored, golden binary elemental metals nano particle dispersed alumina nonlinear optical film and preparation method

A kind of silver-colored, golden binary elemental metals nano particle dispersed alumina nonlinear optical film and preparation method

  • CN 104,007,596 B
  • Filed: 06/12/2014
  • Issued: 12/26/2017
  • Est. Priority Date: 06/12/2014
  • Status: Active Grant
First Claim
Patent Images

1. a kind of preparation method of silver-colored, golden binary elemental metals nano particle dispersed alumina nonlinear optical film, its featureIt is:

  • Using aluminium secondary butylate, isopropanol, ethyl acetoacetate, distilled water, silver nitrate, four hydration gold chlorides as raw material, use is moltenGlue-gel method synthesis stoichiometric proportion is accurate, the uniform precursor colloidal sol of composition, is then entered on a glass substrate using sol evenning machineRow film, Ag is obtained after annealingxAuy/(Al2O3)(1-x-y)Laminated film, concretely comprise the following steps:

    1) precursor colloidal sol is prepared:

    Aluminium secondary butylate is dissolved in isopropanol first, the molar ratio of aluminium secondary butylate and isopropanol is1;

    6.25~66.6, it is stirred at room temperature 15~30 minutes, adds ethyl acetoacetate, aluminium secondary butylate and ethyl acetoacetateMolar ratio is 1;

    1.5~22, it is stirred at room temperature 0.5~1 hour, adds deionized water, aluminium secondary butylate and deionized waterMolar ratio is 1;

    1.25~33.3,1-6 hour is stirred at room temperature, obtains the alumina precursor colloidal sol of water white transparency;

    SoAfterwards according to AgxAuy/(Al2O3)(1-x-y)Stoichiometric proportion is separately added into silver nitrate and four hydration chlorine into parent colloidal solGoldAcid, nitreSour silver and four hydration chlorineGoldThe molar ratio of acid is 0.001~0.0067;

    0.001~0.003, it is small that 1~3 is stirred at room temperatureWhen, obtain the transparent Ag of brownxAuy/(Al2O3)(1-x-y)Precursor colloidal sol;

    2) film is prepared:

    Film is carried out using sol evenning machine on a glass substrate, before spin coating, ultrasound is clear in acetone by substrate leachingWash, then clean with distilled water flushing, the Ag for preparing step

         1) after dryingxAuy/(Al2O3)(1-x-y)Precursor colloidal sol coatsOn substrate, during spin coating, sol evenning machine is first operated 10 seconds with 300rpm speed, then is operated 30 seconds with 3000rpm speed, per evenGlue once carries out a thermal decomposition process, and to remove the water and organic matter in film, heat decomposition temperature is 120~180 DEG C, the timeFor 1~5 minute, film next time is carried out after sample cooling, after film terminates, sample is placed in heat-treatment furnace and annealed,Annealing temperature is 200~900 DEG C, annealing time 30 minutes, finally gives silver, gold nano grain dispersed alumina laminated film.

View all claims
    ×
    ×

    Thank you for your feedback

    ×
    ×