CN112540108B - Method for detecting oxygen permeation of gold foil - Google Patents
Method for detecting oxygen permeation of gold foil Download PDFInfo
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- CN112540108B CN112540108B CN201910898293.2A CN201910898293A CN112540108B CN 112540108 B CN112540108 B CN 112540108B CN 201910898293 A CN201910898293 A CN 201910898293A CN 112540108 B CN112540108 B CN 112540108B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Abstract
The invention discloses a method for detecting oxygen permeability of gold foil, which utilizes electrochemistry to measure an anodic polarization curve of the gold foil in NaOH solution so as to obtain an oxygen evolution potential; and measuring a potentiodynamic cathode polarization curve of the gold foil in the sodium chloride solution, finally adopting a D-S double electrolytic cell, taking the gold foil as a common working electrode, generating oxygen in an anode pool, detecting the cathode polarization of the cathode pool under the corresponding potential of the selected oxygen diffusion section, and reflecting whether the oxygen can permeate the gold foil or not by detecting the change fluctuation of current. The technical scheme of the invention is simple in whole, accurate and timely in test and convenient for popularization and use.
Description
Technical Field
The invention belongs to the technical field of electrochemical application, and particularly relates to a method for detecting oxygen permeation of gold foil.
Background
The gold foil made of gold has good oxidation resistance, moisture resistance, corrosion resistance and radiation resistance due to the stable chemical property of gold. In the aerospace field, for the protection of some precise instruments and other reasons, some components are plated with a layer of gold foil, the thickness is very thin, however, the compactness of the gold foil with the extremely thin thickness has great significance on the utility value, and whether oxygen atoms can penetrate through the gold foil is decisive for the effective work of the gold foil. Therefore, in the evaluation and inspection process of the performance of the gold foil, the detection of the permeability of the gold foil to oxygen is an important link, and at present, no complete mature detection means and method aiming at the oxygen permeation of the gold foil exist.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for detecting the oxygen permeation of the gold foil.
The technical purpose of the invention is realized by the following technical scheme.
The method for detecting the oxygen permeation of the gold foil comprises the following steps:
step 1, determining an oxygen evolution potential and an oxygen permeation detection potential of a gold foil respectively;
(1) After the cathode polarization current density of the gold foil is stable, when the gold foil is oxygenated, the cathode polarization current density is increased, which shows that oxygen atoms penetrate through the gold foil to enter the cathode side, so that the dissolved oxygen concentration of the cathode side is increased, and the limit diffusion current density of the cathode is also increased;
(2) After the polarization current density of the gold foil cathode is stable, the gold foil sample is oxygenated, and the current density does not change obviously for a long time, which indicates that no oxygen permeates the gold foil to enter the cathode side at the moment.
And determining the oxygen evolution potential of the gold foil, selecting 0.2mol/L NaOH aqueous solution as a reaction medium, performing potentiodynamic anodic polarization curve test on the gold foil at a scanning rate of 0.5mV/s by utilizing a PARSTAT 2273 electrochemical workstation produced by Princeton company in America, and determining the oxygen evolution potential according to the obtained potentiodynamic anodic polarization curve.
Further, the gold foil was subjected to determination of oxygen permeation detection potential: a3.5 wt% NaCl aqueous solution is selected as a reaction medium, a PARSTAT 2273 electrochemical workstation produced by Princeton company in America is utilized to carry out potentiodynamic cathodic polarization curve test on the gold foil at a scanning rate of 0.5mV/s, and the ultimate diffusion current and the oxygen permeation detection potential range corresponding to the ultimate diffusion current are determined according to the obtained potentiodynamic cathodic polarization curve.
Further, in the double electrolytic cell, one side was a cathode cell and was provided with a 3.5wt% aqueous NaCl solution, and the other was an anode cell and was provided with a 0.2mol/L aqueous NaOH solution.
Compared with the prior art, the gold foil oxygen permeation detection method disclosed by the invention utilizes electrochemical measurement of an anode polarization curve of a gold foil in a NaOH solution to obtain an oxygen evolution potential; and measuring a potentiodynamic cathode polarization curve of the gold foil in the sodium chloride solution, finally adopting a D-S double electrolytic cell, taking the gold foil as a common working electrode, generating oxygen in an anode pool, detecting the cathode polarization of the cathode pool under the corresponding potential of the selected oxygen diffusion section, and reflecting whether the oxygen can permeate the gold foil or not by detecting the change fluctuation of current. The technical scheme of the invention is simple in whole, accurate and timely in test and convenient to popularize and use.
Drawings
FIG. 1 is a graph showing the anodic polarization of gold foil in an aqueous solution of sodium hydroxide according to the present invention.
FIG. 2 is a graph showing the cathodic polarization of gold foil in an aqueous solution of sodium chloride according to the present invention.
FIG. 3 is a graph showing the measurement of the change in the cathodic polarization current of the gold foil in the presence of oxygen permeation in an oxygen permeation test according to the present invention.
FIG. 4 is a graph showing the change of cathode polarization current in the absence of oxygen permeation in the oxygen permeation test of the gold foil of the present invention.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
The gold foil is used as a sample to be tested by utilizing the electrochemical principle to judge whether oxygen can permeate the gold foil: on one hand, the oxygen production method is designed by utilizing the electrochemical principle: testing an anodic polarization curve of the gold foil in 0.2mol/L NaOH solution to obtain an oxygen evolution potential under the system, and selecting the oxygen evolution potential to carry out constant potential polarization to generate oxygen; on the other hand, the oxygen permeation detection is realized through the traditional permeation experiment method: the gold foil samples were subjected to potentiodynamic cathodic polarization curve in 3.5-vol% NaCl solution, and potentiostatic polarization test at a certain potential was selected for the oxygen diffusion zone. A traditional D-S double electrolytic cell is adopted, gold foil is used as a common working electrode, oxygen is generated in an anode pool, cathode polarization of a cathode pool is detected under the corresponding potential of a selected oxygen diffusion section, and whether oxygen can permeate the gold foil or not can be reflected through detecting the fluctuation of current.
Determination of oxygen evolution potential: a0.2 mol/L NaOH aqueous solution is selected as a reaction medium, and a PARSTAT 2273 electrochemical workstation produced by Princeton company in America is utilized to carry out potentiodynamic anodic polarization curve test on the gold foil at a scanning rate of 0.5mV/s, as shown in attached figure 1, and an anodic polarization curve graph of the gold foil in the NaOH aqueous solution is shown. In the test, when the potential is shifted to the potential corresponding to the A point, H is generated 2 O electrolysis evolves oxygen, and an inflection point A appears on the polarization curve, and the inflection point corresponds to the potential, namely the oxygen evolution potential.
Determination of oxygen permeation detection potential: a potentiodynamic cathodic polarization curve test was carried out on the gold foil using a PARSTAT 2273 electrochemical workstation, manufactured by Princeton, USA, with a scanning rate of 0.5mV/s, using a 3.5wt% NaCl aqueous solution as a reaction medium, as shown in FIG. 2, the cathodic polarization curve of the gold foil in an aqueous sodium chloride solution. A certain section of potential corresponding to an oxygen diffusion control section in a cathode polarization curve is selected as a detection potential, cathode reaction is controlled by oxygen diffusion under the section of potential (namely, a potential range marked by a dotted line in figure 2), current density is basically stable along with the change of the potential, and corresponding current is called limiting diffusion current. Under the condition of other unchanged conditions of temperature, solution flow rate and the like, the limit diffusion current density is only related to the dissolved oxygen concentration in the solution, so that the potential is selected in the section for oxygen permeation detection, and the corresponding change of the cathode polarization current density can reflect whether oxygen can permeate through the gold foil or not, thereby changing the dissolved oxygen concentration of the cathode pool.
And (3) oxygen permeation detection: oxygen permeation testing was performed using a D-S dual cell, gold foil samples were placed between the two cells, one cell was selected as the cathode cell, set to 3.5wt% nacl aqueous solution, constant potential cathodic polarization test was performed using ZF100 at the previously determined oxygen permeation testing potential; the other electrolytic cell is selected as an anode cell, and a gold foil sample clamped between the two cells is oxygenated by constant potential anodic polarization in 0.2mol/L NaOH aqueous solution by adopting a constant potential rectifier under an oxygen evolution potential. In the experiment, the cathode cell is firstly connected, the anode cell is connected for oxygenation after the cathode polarization current is stable, and whether oxygen permeates the gold foil or not is judged by observing the change of the cathode polarization current.
As shown in fig. 3 and 4, the test graphs of the change of the cathode polarization current of the gold foil in the presence/absence of oxygen permeation in the oxygen permeation test of the invention are as follows: after the cathode polarization current density of the gold foil is stable, when the gold foil sample is oxygenated, the cathode polarization current density is increased (the absolute value of the current density is increased), which shows that oxygen atoms penetrate through the gold foil and enter the cathode side, so that the dissolved oxygen concentration of the cathode side is increased, and the limit diffusion current density of the cathode is also increased; after the polarization current density of the gold foil cathode is stable, the gold foil sample is oxygenated, the current density of the gold foil sample does not change obviously in a long time (the absolute value of the current density is not increased obviously, and only certain fluctuation is generated above and below the stable value), which indicates that oxygen does not permeate the gold foil to enter the cathode side at the moment.
The invention being thus described by way of example, it should be understood that any simple alterations, modifications or other equivalent alterations as would be within the skill of the art without the exercise of inventive faculty, are within the scope of the invention.
Claims (2)
1. The method for detecting the oxygen permeation of the gold foil is characterized by comprising the following steps of:
step 1, respectively determining an oxygen evolution potential and an oxygen permeation detection potential of a gold foil, wherein:
determination of oxygen evolution potential: selecting NaOH aqueous solution as a reaction medium, and carrying out potentiodynamic anodic polarization curve test on the gold foil at a scanning rate of 0.5mV/s by using an electrochemical workstation to obtain an anodic polarization curve graph of the gold foil in the sodium hydroxide aqueous solution, wherein an inflection point appears on the polarization curve and corresponds to a potential, namely an oxygen evolution potential;
determination of oxygen permeation detection potential: selecting an aqueous solution as a reaction medium, and carrying out potentiodynamic cathodic polarization curve test on the gold foil at a scanning speed of 0.5mV/s by utilizing an electrochemical workstation to obtain a cathodic polarization curve graph of the gold foil in a sodium chloride aqueous solution; selecting a certain section of potential corresponding to an oxygen diffusion control section in a cathode polarization curve as a detection potential, wherein under the section of potential, cathode reaction is controlled by oxygen diffusion, current density is kept stable along with potential change, and corresponding current is called as limiting diffusion current; determining the limit diffusion current and the oxygen permeation detection potential range corresponding to the limit diffusion current according to the obtained potentiodynamic cathode polarization curve;
step 2, arranging the gold foil in a double electrolytic cell, wherein one side is a cathode cell, the other side is an anode cell, firstly switching on the cathode cell, selecting the potential as an oxygen permeation detection potential, carrying out a constant potential cathodic polarization test, switching on the anode cell after the cathodic polarization current is stable, carrying out constant potential anodic polarization under the oxygen evolution potential by adopting a constant potential instrument, oxygenating the gold foil, and judging whether the gold foil is subjected to oxygen permeation by observing the change of the cathodic polarization current:
(1) After the density of the gold foil cathode polarization current is stable, when the gold foil is oxygenated, the density of the cathode polarization current is increased, which shows that oxygen atoms penetrate through the gold foil to enter the cathode side, so that the concentration of dissolved oxygen at the cathode side is increased, and the density of the cathode limit diffusion current is also increased;
(2) After the polarization current density of the gold foil cathode is stable, the gold foil sample is oxygenated, and the current density does not change obviously for a long time, which indicates that no oxygen permeates the gold foil to enter the cathode side at the moment.
2. The method for detecting oxygen permeation through gold foil according to claim 1, wherein in the double electrolytic cell, one side is a cathode cell, 3.5wt% aqueous NaCl solution is provided, and the other side is an anode cell, and 0.2mol/L aqueous NaOH solution is provided.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09259942A (en) * | 1996-03-18 | 1997-10-03 | Nippon Telegr & Teleph Corp <Ntt> | Photochemically hydrogenated secondary air battery |
| CN1455755A (en) * | 2000-04-10 | 2003-11-12 | 普莱克斯技术有限公司 | Oxygen transport membrane for silicon oxide plant |
| JP2015031554A (en) * | 2013-08-01 | 2015-02-16 | 日本電信電話株式会社 | Hydrogen penetration potential prediction method |
| CN104897744A (en) * | 2015-04-23 | 2015-09-09 | 中国石油大学(华东) | Metal hydrogen permeation behavior research device and method |
| CN104962957A (en) * | 2015-07-07 | 2015-10-07 | 安徽铜冠铜箔有限公司 | Method for detecting potential variation of anode strip for electrolytic copper foil |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8647876B2 (en) * | 2010-03-31 | 2014-02-11 | Fujifilm Corporation | Oxygen permeability measuring apparatus and method, and defect inspection apparatus and method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09259942A (en) * | 1996-03-18 | 1997-10-03 | Nippon Telegr & Teleph Corp <Ntt> | Photochemically hydrogenated secondary air battery |
| CN1455755A (en) * | 2000-04-10 | 2003-11-12 | 普莱克斯技术有限公司 | Oxygen transport membrane for silicon oxide plant |
| JP2015031554A (en) * | 2013-08-01 | 2015-02-16 | 日本電信電話株式会社 | Hydrogen penetration potential prediction method |
| CN104897744A (en) * | 2015-04-23 | 2015-09-09 | 中国石油大学(华东) | Metal hydrogen permeation behavior research device and method |
| CN104962957A (en) * | 2015-07-07 | 2015-10-07 | 安徽铜冠铜箔有限公司 | Method for detecting potential variation of anode strip for electrolytic copper foil |
Non-Patent Citations (1)
| Title |
|---|
| Surface oxide reduction by hydrogen permeation through iron foil detected using a scanning Kelvin probe;Williams G. 等;《Electrochemistry Communications》;20121124;第27卷;第144-147页 * |
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