• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a device for real-time measurement of the growth of an Au thin film by a TFBG, comprising a light source (1) for generating an increased spontaneous emission, a polarizer (2), a polarizer controller (3), a TFBG (4), a Temperature control (5), and a spectrometer (8). After the Au thin layer has been deposited on a surface of the TFBG, the spectral properties of the TFBG are influenced. After two light beams s and p polarized at right angles to one another have passed through the TFBG, the transmission spectra of the light beams show a relatively large difference, caused by a surface plasmon resonance effect of the Au thin layer and an interface to a medium. A change in a polarization-dependent loss of the TFBG in a coating process of an Au thin film is monitored in real time in order to carry out a controllable deposition of the Au thin film, so that the thickness of the nano thin film provided can be controlled in order to use a high-quality metallic nano thin film to get a hydrogen sensor.
    公开号:CH715639A2
    申请号:CH00985/19
    申请日:2019-08-05
    公开日:2020-06-15
    发明作者:Shen Changyu；Zhang Chong；Gong Jiaqi
    申请人:Univ Jiliang China；
    IPC主号:
    专利说明:

    Technical area
    The present invention belongs to the technological field of metallic nano-thin film production and relates in particular to a device for real-time monitoring of the growth of an Au thin film by TFBG.
    background
    As a very important clean energy of today's society, hydrogen gas is also an important industrial raw material and is widely used in different areas. However, hydrogen gas is colorless and odorless and it diffuses and leaks relatively easily from a medium and it is highly flammable if it comes into contact with an open flame. It is therefore quite necessary to study a hydrogen sensor for detection and monitoring. Although known hydrogen gas sensors have fairly high sensitivity, it is relatively difficult to design a fiber optic hydrogen gas sensor. Therefore, a metal-coated fiber optic hydrogen gas sensor has been investigated, and it has many advantages such as small size and high sensitivity. As a hydrogen sensitive material, precious metals play a key role in this type of sensor. A chemical reduction process is used to manufacture metallic nanoparticles, and these metallic nanoparticles are manufactured to be placed on a substrate to form a nanoscale that can optimize the performance of a hydrogen gas sensor.
    During the growth process of the metallic nano-thin film, growth parameters such as substrate temperature, growth time and the external environment have a major effect on the product quality of a finally manufactured one-piece thin film. In a previous experiment, all technological processes were carried out by hand. Not only is it difficult to set up the experiment, manual operation also inevitably involves operating errors. In this regard, a practical method for real-time monitoring of the growth of an Au thin film is being investigated. A change in a polarization-dependent loss of a TFBG in a coating process of an Au thin film is monitored in real time in order to carry out a controllable deposition of the Au thin film, so that the thickness of the provided nano thin film can be controlled, which effectively improves the coating quality.
    Summary
    In view of the disadvantages in the prior art, the present invention provides an apparatus for real-time monitoring of the growth of an Au thin film by TFBG. The device can monitor a polarization-dependent loss of a TFBG in a process for coating an Au nano thin film in real time in order to carry out a controllable deposition of the Au thin film and to obtain a high quality metallic nano thin film for use in a hydrogen sensor. Because the present invention has advantages such as a simple structure and low cost, the thickness and other physical properties of the metallic nano thin film according to the present invention can be conveniently set and controlled. There are therefore tremendous perspectives in development and importance in research.
    The present invention is realized by the following technical solution: A device for real-time monitoring of a growth of an Au thin film by a TFBG is provided, comprising a light source for generating an amplified spontaneous emission (1), a polarizer (2), a Polarizer control (3), a TFBG (4), a temperature control (5), a working basin (6), a working solution (7) and a spectrometer (8), whereby light emitted by the light source to generate a spontaneous emission (1) output after passing through the polarizer (2) hits the polarizer control (3); a right end of the polarizer control is connected to the TFBG (4) and the TFBG is placed in the working basin (6) and heated by the temperature control (5); a right end of the TFBG (4) is connected to the spectrometer (8); Measured spectral data are correlated with a result from a calibration of the thickness of a thin film carried out with an atomic force microscope AFM in order to carry out the monitoring of the thickness of the thin film produced.
    Before the coating is carried out, the TFBG (4) is first pretreated: The TFBG is ultrasonically cleaned for 5 minutes using the organic solutions ethanol, acetone and methanol and for 15 minutes at 80 ° C in a solution of concentrated H2SO4und H2O2mit treated at a volume ratio of 7: 3; the hydroxylated TFBG is immersed in a 1% APTMS methanol solution for 0.5 hours in order to absorb Au nanoparticles.
    The temperature control (5) regulates the temperature to a constant 22.5 ° C.
    The working solution (7) is a mixed solution of chloroformic acid with a concentration of 0.01% and 0.4 mmol of hydroxylamine hydrochloride.
    The operation of the present invention is as follows: After the Au thin film has been deposited on a surface of the TFBG, the spectral properties of the TFBG are affected. After two light beams s and p polarized at right angles to each other have passed through the TFBG, the transmission spectra of the light beams show a relatively large difference, caused by an SPR effect of the Au thin film and an interface to a medium. A polarization dependent loss (PDL) can be used to describe this characteristic. The PDL is defined as follows: Tx and Tys are transmission spectra in an s polarization state and in a P polarization state, respectively. Based on the above basic principle, a designed structure can be used for real-time monitoring of a spectrum in a thin film growth process. Measured spectral data are correlated with a result from a calibration of the thickness of the thin film carried out with an AFM in order to carry out the monitoring of the thickness of the thin film produced. In addition, the SPR characteristic of a TFBG modified with an Au thin film is normally used for measurement, this requiring an optimal SPR adaptation of the thin film and a very obvious erasure phenomenon. Therefore, even if a reaction condition changes, the coating can be stopped immediately if a very obvious erasure phenomenon is observed in a spectrum measured in real time.
    Brief description of the drawings
    1 is a schematic view of a device for real-time monitoring of the growth of an Au thin film by TFBG.
    Detailed description
    Before the coating is carried out, a TFBG (4) is pretreated: The TFBG is ultrasonically cleaned for 5 minutes using the organic solutions ethanol, acetone and methanol, rinsed with ultrapure water and blow-dried and for 15 minutes at 80 ° C in one Treated solution of concentrated H2SO4 and H2O2 with a volume ratio of 7: 3; the hydroxylated TFBG is immersed in a 1% APTMS methanol solution for 0.5 hours in order to absorb Au nanoparticles. During a coating process, the TFBG (4) is placed in a mixed solution of chloroformic acid with a concentration of 0.01% and 0.4 mmol of hydroxylamine hydrochloride in order to form an Au nano-thin layer by deposition and the temperature controller (5) regulates the temperature to a constant level 22.5 ° C.
    As shown in FIG. 1 shows a device for real-time monitoring of a growth of an Au thin film provided by a TFBG and has a light source for generating an amplified spontaneous emission (1), a polarizer (2), a polarizer controller (3), a TFBG (4), a Temperature control (5), a working basin (6), a working solution (7) and a spectrometer (8), whereby light that is emitted by the light source to generate a spontaneous emission (1) is output after passing through the polarizer (2) the polarizer control (3) hits; a right end of the polarizer control (3) is connected to the TFBG (4) and the TFBG (4) is placed in the working basin (6) and heated by means of the temperature control (5); a right end of the TFBG (4) is connected to the spectrometer (8); a time lapse is started and real-time monitoring of a spectrum is carried out. During the coating process, the temperature of the solution is kept at a constant 22.5 ° C.
    By measuring in an experiment it can be determined that in the first five minutes during the coating a decrease at 1530nm - 1540nm is relatively small; when the coating time reaches 30 minutes, an apparent decrease at 1540nm begins to occur and an amplitude of polarization dependent loss at 1540nm falls with an increase in the deposition time and shifts towards a long wavelength and when the coating time is 50 minutes, a largest decrease in the polarization-dependent loss up to close to 1542nm.
    In a final step, the coated TFBG is cleaned with water and blow-dried with nitrogen gas. The AU nanotin-coated TFBG is dipped successively in water and pure ethyl alcohol and exposed to air. From a test result it can be learned that no obvious SPR phenomenon occurs on the TFBG in air. When the TFBG is immersed in ultrapure water, a very obvious extinguishing phenomenon occurs at 1543nm. In an anhydrous ethanol solution, an SPR resonance wavelength is close to 1565nm, but the quenching is not very obvious, it indicates that the SPR wavelength is not an optimal match value in this case.
    权利要求:
    Claims (1)
    [1]
    1. Device for real-time measurement of growth of an Au thin film by a TFBG, comprising a light source for generating an increased spontaneous emission (1), a polarizer (2), a polarizer control (3), a TFBG (4), a temperature control (5 ), a work basin (6), a working solution (7) and a spectrometer (8), whereby light, which is emitted by the light source to generate a spontaneous emission (1) after passing through the polarizer (2) onto the polarizer control ( 3) hits; a right end of the polarizer control is connected to the TFBG (4) and the TFBG is placed in the work basin (6) and heated by means of the temperature control (5); a right end of the TFBG (4) is connected to the spectrometer (8); the TFBG (4) being pretreated before the coating is carried out: the TFBG is ultrasonically cleaned for 5 minutes using the organic solutions ethanol, acetone and methanol and for 15 minutes at 80 ° C. in a solution of concentrated H2SO4 and H2O2 with a volume ratio of 7 : 3 treated; the hydroxylated TFBG is immersed in a 1% APTMS-methanol solution for 0.5 hours in order to absorb Au-nano-particles; During the coating process, the TFBG (4) is placed in a mixed solution of chloroformic acid with a concentration of 0.01% and 0.4 mmol hydroxylamine hydrochloride in order to form an Au nano-thin layer by deposition and the temperature control (5) regulates the temperature to a constant 22.5 ° C.
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    同族专利:
    公开号 | 公开日
    CN109373916A|2019-02-22|
    引用文献:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CN201811451508.8A|CN109373916A|2018-11-30|2018-11-30|It is a kind of to realize the real time monitoring apparatus grown to Au film with TFBG|
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