US20150056379A1 - Method of manufacturing gold thin film by using electroless-plating method - Google Patents

Method of manufacturing gold thin film by using electroless-plating method Download PDF

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US20150056379A1
US20150056379A1 US14/467,035 US201414467035A US2015056379A1 US 20150056379 A1 US20150056379 A1 US 20150056379A1 US 201414467035 A US201414467035 A US 201414467035A US 2015056379 A1 US2015056379 A1 US 2015056379A1
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thin film
alcohol
minutes
reaction mixture
sers
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Kuan Soo SHIN
Young Kwan CHO
Myung Chan Park
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Foundation of Soongsil University Industry Cooperation
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1635—Composition of the substrate
    • C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1635—Composition of the substrate
    • C23C18/1639—Substrates other than metallic, e.g. inorganic or organic or non-conductive
    • C23C18/1641—Organic substrates, e.g. resin, plastic
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/166—Process features with two steps starting with addition of reducing agent followed by metal deposition
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/1664—Process features with additional means during the plating process
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1675—Process conditions
    • C23C18/1676—Heating of the solution
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
    • C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
    • C23C18/1886—Multistep pretreatment
    • C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
    • C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
    • C23C18/2073—Multistep pretreatment
    • C23C18/2086—Multistep pretreatment with use of organic or inorganic compounds other than metals, first

Definitions

  • the present invention relates to a method of manufacturing a gold (Au) thin film on a dielectric surface, and more particularly, to a method of manufacturing an Au thin film on a glass surface, which has increased activity of surface enhanced Raman scattering (SERS) by using an electroless-plating method.
  • Au gold
  • SERS surface enhanced Raman scattering
  • a gold (Au) thin film is manufactured by using one of three methods, i.e., an electroplating or electro-deposition method, a vapor deposition method, and an electroless-plating method.
  • the vapor deposition method has a few intrinsic weaknesses. In various application fields, elaborate and high vacuum equipment is required, and a large amount of Au metal is consumed during an evaporation process. In addition, it is difficult to attach evaporated Au only to a selected area in a plated surface. In other words, it is not easy to design a pattern having Au by using the vapor deposition method.
  • SERS surface enhanced Raman scattering
  • a technology using such SERS is applied to various molecular electronics, for example, to a chemical analyte, an etching agent, a lubricant, a catalyst, and a sensor.
  • KR1277357 provides a layer having a barrier function and catalytic power and excelling in formation uniformity and coverage of an ultrathin film, provides a pretreatment technique wherein an ultrafine wiring can be formed and a thin seed layer of uniform film thickness can be formed, and discloses a substrate including a thin seed layer formed with a uniform film thickness via electroless plating by using the pretreatment technique.
  • the present invention provides a method of manufacturing a gold (Au) thin film conveniently and stably having an effect of surface enhancement Raman scattering (SERS) activity by using an electroless-plating method, without having to not only use expensive equipment but also perform an additional process.
  • Au gold
  • SERS surface enhancement Raman scattering
  • a method of manufacturing a gold (Au) thin film by using an electroless-plating method including: manufacturing a reaction mixture by adding an Au chloride compound and an alkaline compound to an alcohol-water mixed solution; and forming an Au thin film by putting a substrate in the reaction mixture and stirring the reaction mixture.
  • the alcohol-water mixed solution may be a mixed solution containing 70 to 90 wt % of alcohol and 30 to 10 wt % of water.
  • the alcohol may be C1 to C4 alcohol, and in detail, may be methanol or ethanol.
  • the Au chloride compound may be selected from the group consisting of potassium Au chloride (KAuCl 4 ), gold potassium cyanide (KAu(CN) 2 ), and chloroauric acid (HAuCl 4 ).
  • the alkaline compound may be selected from the group consisting of potassium carbonate, sodium hydroxide, potassium hydroxide, butylamine, and sodium hydrogen carbonate.
  • the substrate may be formed of a dielectric material selected from the group consisting of glass, plastic, and silicon.
  • FIG. 1 is field emission scanning electron microscopic (FE-SEM) images of gold (Au) thin films deposited on glass substrates according to reaction times of 20 minutes, 40 minutes, 60 minutes, and 80 minutes, respectively;
  • FE-SEM field emission scanning electron microscopic
  • FIG. 2 illustrates ultraviolet-visible (UV-vis) absorption spectra of the Au thin films deposited on the glass substrates according to the reaction times of 20 minutes, 40 minutes, 60 minutes, and 80 minutes;
  • UV-vis ultraviolet-visible
  • FIG. 3 ( a ) illustrates X-ray diffraction (XRD) patterns of the Au thin films deposited on the glass substrates according to the reaction times of 40 minutes and 80 minutes
  • FIG. 3 ( b ) illustrates an X-ray photoelectron spectroscopy (XPS) spectrum of the Au thin film deposited on the glass substrate according to the reaction time of 80 minutes;
  • XRD X-ray diffraction
  • XPS X-ray photoelectron spectroscopy
  • FIG. 4 ( a ) illustrates surface enhancement Raman scattering (SERS) spectra of benzenthiol (BT) adsorbed on the Au thin film deposited on the glass substrates
  • FIG. 4 ( b ) illustrates relative Raman peak intensities of BT at 1574 cm ⁇ 1 adsorbed on the Au thin films deposited on the glass substrates;
  • FIG. 5 illustrates SERS spectra of BT at 1574 cm ⁇ 1 adsorbed on five different batches A through E of an Au film.
  • a reaction mixture is manufactured by adding an Au chloride compound and an alkaline compound to an alcohol-water mixed solution.
  • alcohol is a reducing agent that supplies electrons.
  • the reaction mixture After putting the substrate into the reaction mixture, the reaction mixture is stirred to form an Au thin film.
  • the alcohol-water mixed solution may contain 70 to 90 wt % of alcohol and 30 to 10 wt % of water.
  • the alcohol may be C1 to C4 alcohol, and in detail, may be methanol or ethanol.
  • the Au chloride compound may be selected from the group consisting of potassium Au chloride (KAuCl 4 ), gold potassium cyanide (KAu(CN) 2 ), and chloroauric acid (HAuCl 4 ), and the alkaline compound may be selected from the group consisting of potassium carbonate, sodium hydroxide, potassium hydroxide, butylamine, and sodium hydrogen carbonate.
  • the substrate may be formed of a dielectric material selected from the group consisting of glass, plastic, and silicon.
  • the Au chloride compound and the alkaline compound are put into the water-alcohol mixed solution that is methanol or ethanol and a temperature is maintained to 50° C. to 70° C.
  • Au nanoparticles adhere to any one of various dielectric surfaces, such as glass, silicon, and plastic surfaces, and sizes of the Au nanoparticles or a thickness of the Au thin film may be adjusted by varying the concentrations of reactants or by adjusting a reaction time.
  • a state of the Au thin film adhered on the dielectric surface as such was analyzed by using an ultraviolet-visible (UV-vis) spectrum analyzer, a field emission scanning electron microscope, an X-ray diffraction (XRD) analyzer, and an X-ray photoelectron spectroscopy (XPS) analyzer, and as results, it was determined that the Au thin film adhered on the dielectric surface was formed as Au particles having nanometer sizes gather together, and sizes of the Au particles and a thickness of the Au thin film depend on a reaction time.
  • UV-vis ultraviolet-visible
  • XRD X-ray diffraction
  • XPS X-ray photoelectron spectroscopy
  • the Au thin film manufactured by using the electroless-plating method showed uniform surface enhancement Raman scattering (SERS) activity on a surface up to hundreds of thousands of square micrometers, and an enhancement factor (EF) calculated by using benzenthiol (BT) as a prototype adsorbent reached up to 7.6 ⁇ 10 4 .
  • SERS surface enhancement Raman scattering
  • EF enhancement factor
  • the cover glass was washed with ethanol and then was finally dried in an oven at a temperature of 60° C. for 30 minutes.
  • the washed cover glass was dipped in a reaction mixture and then the reaction mixture was vigorously stirred at a temperature of 50° C.
  • the reaction time was varied from 20 minutes to 80 minutes.
  • the reaction mixture was obtained by mixing an aqueous solution containing 0.5 mL of 0.1 M HAuCl 4 and 1 mL of 1 M K 2 CO 3 with 8.5 mL of methanol solution, and at this time, the pH of the reaction mixture was adjusted to 11 to 12.
  • An Au-coated glass obtained as such was washed with ethanol and then dried in air.
  • the Au-coated glass was immersed in a 10 mM methanol solution of BT for 30 minutes, washed with deionized water several times, and then dried in air.
  • UV-vis spectra were obtained by using a spectrum analyzer (Avantes 3648), and field emission scanning electron microscopic (FE-SEM) images were obtained by using a field emission scanning electron microscope (JSM-6700F) that operated at 5.0 kV.
  • XRD was analyzed by using an X-ray diffractometer (Rigaku Model MiniFlex powder diffractometer) using Cu K ⁇ radiation. Also, XPS measurements were performed by using an AXISH model using Mg K ⁇ X-ray as a light source.
  • SERS was analyzed by using a spectroscope (Renishaw Raman System Model 2000) equipped with an integral microscope (Olympus BH2-UMA). The 632.8 nm line from a 17 mW He/Ne laser (Spectra Physics Model 127) was used as an excitation source. A Raman band of a silicon wafer at 520 cm ⁇ 1 was used to calibrate the spectroscope. Accuracy of a measured spectrum value was at least 1 cm ⁇ 1 .
  • Atomic force microscopic (AFM) images were obtained by using an atomic force microscope (Instruments Nanoscope IIIa system), and at this time a nominal spring constant was from 20 N/m to 100 N/m, and an 125 ⁇ m long etched cantilever was used. Topographic images were recorded in a tapping mode under an operating frequency within 300 kHz at a scanning speed of 2 Hz.
  • FIG. 1 is FE-SEM images of Au thin films deposited on glass substrates according to reaction times, for example, 20 minutes, 40 minutes, 60 minutes, and 80 minutes, respectively.
  • An average particle size of the Au thin film according to the reaction time of 20 minutes is 22.8 ⁇ 3.8 nm
  • an average particle size of the Au thin film according to the reaction time of 40 minutes is 176 ⁇ 18 nm
  • Au nanoparticles coalesce into large grains to form a network structure and cover an entire surface of the glass substrate. Meanwhile, it is difficult to determine grain sizes of the Au thin films according to the reaction times of 60 minutes and 80 minutes.
  • FIG. 2 illustrates UV-vis absorption spectra of the Au thin films deposited on the glass substrates according to the reaction times, for example, 20 minutes, 40 minutes, 60 minutes, and 80 minutes.
  • the Au thin film according to the reaction time of 20 minutes shows maximum absorption at 534 nm
  • the Au thin films according to the reaction times of 40 minutes, 60 minutes and 80 minutes show maximum absorption at 563 nm, 584 nm, and 639 nm, respectively.
  • FIG. 3 ( a ) illustrates XRD patterns of the Au thin films deposited on the glass substrates, wherein XRD peaks positioned at 38.2°, 44.4°, 64.6°, and 77.6° respectively correspond to (111), (200), (220), and (311) lattice planes of face centered cubic gold particles.
  • FIG. 3 ( b ) illustrates an XPS spectrum of the Au thin film deposited on the glass substrate according to the reaction time of 80 minutes, wherein XRD peaks at 83.7 eV and 87.4 eV respectively correspond to 4 f 7/2 and 4 f 5/2 peaks of zero-valent Au.
  • FIG. 4 ( a ) illustrates SERS spectra of BT adsorbed on the Au thin films deposited on the glass substrates, wherein bands at 998 cm ⁇ 1 , 1021 cm ⁇ 1 , 1072 cm ⁇ 1 , and 1573 cm ⁇ 1 respectively correspond to an in-plane ring-breathing mode, an in-plane C-H bending mode, an in-plane ring-breathing mode coupled with a C-S stretching mode, and a C-C stretching mode,
  • FIG. 4 ( b ) illustrates relative Raman peak intensities of BT at 1574 cm ⁇ 1 adsorbed on the Au thin films deposited on the glass substrates, wherein the Au thin film according to the reaction time of 60 minutes shows the most intense SERS peak of BT, whereas the Au thin films according to the reaction times of 20 minutes and 80 minutes show very weak SERS peaks.
  • Such results highlight the importance of gaps and crevices in a metal nanostructure in SERS measurements.
  • an SERS EF may be calculated according to Equation 1 below.
  • I SERS and I NR respectively denote SERS intensity of BT on an Au thin film and normal Raman (NR) scattering intensity of BT in a bulk.
  • N NR and N SERS denote numbers obtained by illuminating BT molecules by using a laser beam to respectively obtain SERS and NR spectra.
  • N SERS and I NR were measured at 1574 cm ⁇ 1 , and N NR and N SERS were calculated based on estimated concentration of surface BT species, density of bulk BT, and sampling areas. It was assumed that equilibrated surface concentration of BT is the same as that of Au and silver (Ag), i.e., up to 7.1 ⁇ 10 ⁇ 10 .
  • N SERS was calculated to be 1.0 ⁇ 10 ⁇ 17 mol considering a sampling area having a diameter of 1 ⁇ m and a surface roughness factor (up to 1.47) obtained from AFM measurement of the thin film according to the reaction time of 60 minutes. When an NR spectrum of pure BT was measured, a sampling volume was a product of a laser spot and a penetration depth was about 15 ⁇ m. N NR was 1.1 ⁇ 10 13 mol when density of BT was 1.07 g/cm 3 .
  • FIG. 5 illustrates SERS spectra of BT at 1574 cm ⁇ 1 adsorbed on five different batches A through E of the Au film according to the reaction time of 60 minutes. Peak intensities at 1574 cm ⁇ 1 were normalized with respect to silicon wafers, and batch-to-batch relative deviation was 15% whereas spot-to-spot relative deviation was 12%.
  • an Au thin film manufactured by using an electroless-plating method shows uniform SERS activity on an area up to hundreds of thousands of square micrometers, and an EF calculated by using BT as a prototype adsorbent reached up to 7.6 ⁇ 10 4 .
  • an Au thin film having an effect of SERS activity may be conveniently and stably formed on a dielectric surface.
  • an Au thin film having an SERS effect may be conveniently and stably formed on a dielectric surface without having to use expensive additional equipment, such as a vacuum device.
  • the Au thin film since a thickness of an Au thin film formed on a dielectric substrate, such as glass, may be adjusted, the Au thin film may be applied to various fields, such as semiconductor fields, energy fields, catalyst fields, medical fields, and diagnosis fields.

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CN105821398A (zh) * 2016-03-21 2016-08-03 上海交通大学 双连续内联通结构的周期性金属材料的制备方法及其应用
US12110594B2 (en) * 2020-10-13 2024-10-08 Foundation Of Soongsil University-Industry Cooperation Composition for electroless platinum plating and electroless platinum plating method using the same

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